638-94241A

(M393-E189)

PC-Controlled Total Organic Carbon

Analyzer

TOC-VCPH/CPN &
TOC-Control V Software
User Manual

Read this manual carefully and keep it with the

instrument for future reference.

SHIMADZU CORPORATION
ANALYTICAL & MEASURING
INSTRUMENTS DIVISION
KYOTO, JAPAN
 TOC-VCPH/CPN

Copyright  Shimadzu Corporation 2003. All rights reserved, including those to reproduce this publication or
parts thereof in any form without permission in writing from Shimadzu Corporation.
Read and understand this manual before operation. Save this manual.
Information in this publication is subject to change without notice and does not represent a guarantee on the part
of the vendor.
Any errors or omissions which may have occurred in this publication despite the utmost care taken in its produc-
tion will be corrected as soon as possible, but not necessarily immediately upon detection. We appreciate notifica-
tion of any errors or omissions.
Shimadzu does not have any responsibility for errors or injuries resulting from following the instructions in this
manual.

Windows is a registered trademark of Microsoft Corporation.

TOC-VCPH/CPN
0

Introduction

Thank you for purchasing the TOC-VCPH/TOC-VCPN Total Organic Carbon Analyzer and
the TOC-Control V software.

This instruction manual is a TOC-V user manual. It provides operation and maintenance
procedures for the TOC-V. The procedures related to TOC-Control V software system
administration are described in detail in the TOC-V Administrator's Manual.

Be sure to read this documentation carefully before using the instrument for the first time.
Read the Operational Precautions before operating the instrument. Follow the procedures in
the manual to avoid compromising user or instrument safety.

CAUTION
• Do not operate this instrument before understanding the contents of this manual.
• If this manual or the warning labels on the instrument become lost or damaged,
promptly obtain replacements from your Shimadzu representative.
• To ensure safe operation, read and follow the procedures in Section 1.2 "Opera-
tional Precautions" before operating the instrument.
 Product Warranty and Post Sale Service

Product Warranty and Post Sale Service

Product Warranty

The warranty does not cover malfunctions that result from:

• misuse
• repairs or modifications made by any company other than the manufacturer or a
manufacturer-approved company
• external factors
• operation in environments with severe conditions, such as high temperature, high
humidity, corrosive gas, or vibration
• fire, earthquake or other forces of nature
• moving or transporting the unit after its initial installation
• the consumption of items or parts that can be regarded as consumable. For
example, the service life of an LCD display panel depends on actual operating
conditions.

Post Sale Service

If any problems occur with this instrument, inspect it and take appropriate corrective action
as described in Section 5.7 "Troubleshooting". If the problem persists or symptoms not
covered in the Troubleshooting section occur, contact your Shimadzu representative.

iv TOC-VCPH/CPN
 Contents of This Manual

Contents of This Manual

Chapter 1 Overview
This chapter provides an overview of the instrument and operational precautions for its use.

Chapter 2 System Description

This chapter describes the TOC-V system components and optional accessories.

Chapter 3 Software Overview, Administration, and Setup

This chapter provides an overview of the TOC-Control V software and describes the
software’s Administration and Instrument Setup Wizard tools, which are used to manage
user accounts and configure new systems.

Chapter 4 Operation
This chapter describes pre-analysis preparations and instrument and software functions,
such as setting measurement parameters, starting up the instrument, generating calibration
curves, and conducting sample analysis. This chapter also includes a tutorial that covers
setup and measurement procedures.

Chapter 5 Maintenance
This chapter describes maintenance procedures and periodic checks required to ensure that
the instrument provides consistently high accuracy analyses. Troubleshooting procedures
and error messages are also included in this chapter.

Chapter 6 Reference Information

This chapter describes principles of analysis and lists specifications, standard and optional
accessories, and specialized terms associated with this instrument. This chapter also
includes the installation procedure, for use in the event that instrument is moved to another
site.

Appendix A Method Validation

This appendix describes the software’s Method Validation tool, which is used to test the
variance and linearity of a data set.

Appendix B Control Charts

This appendix describes the software’s Control Charts tool, which is used to monitor the
precision and accuracy of a data set.

TOC-VCPH/CPN v
 Notation Conventions

Notation Conventions

Precautionary Conventions Used in this Manual

The following precautionary conventions are used in this manual.

Convention Description

CAUTION Indicates the possibility of slight to moderate injury or equipment dam-

age.

Note: Provides additional information to ensure the correct use of the instru-
ment.

Other Conventions Used in this Manual

Instrument Model Names

Descriptions in this documentation pertain to two models of the TOC-V Total Organic
Carbon Analyzer, namely the TOC-VCPH and TOC-VCPN. These models will be referred to
in relevant descriptions as the H Type and N Type, respectively.

Supplementary Conventions
In addition to the precautionary conventions, the “Tips” and “Reference” conventions are
used to supply additional information.

Convention Description

TIP » Indicates a particular technique, alternative means of operation, or useful advice.

Reference: Indicates a reference location in the manual where more detailed information can
be found.

vi TOC-VCPH/CPN
 Warning Labels Used on this Instrument

Warning Labels Used on this Instrument

High Temperature Warning

When the electric furnace is heating up, or is at its operational temperature (680°C or
720°C), the central portion of the electric furnace is extremely hot. To prevent burns,
NEVER touch the electric furnace area with bare hands. Allow the furnace to cool before
performing any maintenance on the combustion tube or catalyst.

The internal temperature of the ozone treatment unit reaches 50°C while the instrument is
running. To prevent burns, switch off the TN unit and wait at least 2 hours for the unit to
cool sufficiently before performing any maintenance.

TOC-VCPH/CPN vii
 Warning Labels Used on this Instrument

Electric Shock Warning

Do not remove this panel, as there is danger of electric shock.

Due to the danger of electric shock, do not remove this cover. In the event that the cover
must be removed, first disconnect the TNM-1 power cord.

viii TOC-VCPH/CPN
 Warning Labels Used on this Instrument

Injury Warning
The sample injection components of this instrument move during operation. To prevent
injury, keep hands away from this mechanism.

During operation, the pressure in the CO2 absorber of the gas purifier is about 200kPa. To
prevent injuries, turn off the carrier gas and switch off power to the TOC main unit. Wait
until the pressure inside the container and the instrument flow lines return to normal
atmospheric pressure before performing any maintenance.

TOC-VCPH/CPN ix
 Warning Labels Used on this Instrument

Corrosion Warning
Acid and other corrosive substances are present in the liquid waste drained from this
instrument. Be careful not to touch or spill the liquid waste.

The soda lime in the CO2 absorber of the carrier gas purifier is a corrosive chemical
substance. Be careful not to touch or spill this substance.

x TOC-VCPH/CPN
 Warning Labels Used on this Instrument

The liquid discharged from the drain tube connected to the TC injector contains acid and
other corrosive substances. Verify that the tip of the drain tube is securely inserted into the
Y-shaped fitting when connecting the combustion tube and sample injector.

The IC reaction solution is acidic. Be careful not to touch or spill the IC reaction solution.

TOC-VCPH/CPN xi
 Warning Labels Used on this Instrument

Hydrochloric acid is a corrosive chemical substance. Be careful not to touch or spill the
hydrochloric acid.

xii TOC-VCPH/CPN
 Table Of Contents
Introduction............................................................................................ iii
Product Warranty and Post Sale Service .................................................... iv
Product Warranty ........................................................................................... iv
Post Sale Service ............................................................................................ iv
Contents of This Manual ............................................................................. v
Notation Conventions ................................................................................. vi
Precautionary Conventions Used in this Manual ........................................... vi
Other Conventions Used in this Manual ........................................................ vi
Warning Labels Used on this Instrument .................................................. vii

1 Overview ................................................................................................... 1
1.1 Overview ..................................................................................................... 2
1.2 Operational Precautions............................................................................... 3

2 System Description................................................................................... 7
2.1 TOC-VCPH/CPN Construction...................................................................... 8
2.1.1 Front View ...................................................................................................... 8
2.1.2 Right Side View .............................................................................................. 8
2.1.3 Left Side View ................................................................................................ 9
2.1.4 Rear View........................................................................................................ 9
2.1.5 Inside Front View.......................................................................................... 10
2.1.6 Inside Top View............................................................................................ 11
2.1.7 Flow Diagrams .............................................................................................. 11
2.2 Autosampler ASI-V (Option) .................................................................... 14
2.2.1 Front View .................................................................................................... 14
2.2.2 Rear View...................................................................................................... 14
2.3 8-Port Sampler OCT-1 (Option)................................................................ 15
2.3.1 Front View .................................................................................................... 15
2.3.2 Rear View...................................................................................................... 15
2.4 TN Unit TNM-1 (Option).......................................................................... 16
2.4.1 Front and Right Side Views .......................................................................... 16
2.4.2 Inside Front View.......................................................................................... 17
2.4.3 Rear View...................................................................................................... 18

3 Software Overview, Administration, and Setup ................................. 19

3.1 Introduction to System Administration Functions.................................... 20
3.1.1 Screen Lock Function ................................................................................... 20
3.1.2 Change Password .......................................................................................... 21
3.1.3 Add Event Log .............................................................................................. 22

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 Table Of Contents
3.2 Instrument Setup and System Properties ................................................... 23
3.2.1 System Information Window ....................................................................... 23
3.2.2 Options Window........................................................................................... 24
3.2.3 TOC Window ............................................................................................... 26
3.2.4 ASI Window................................................................................................. 28
3.2.5 SSM Window ............................................................................................... 29
3.2.6 Communication Window.............................................................................. 30
3.2.7 History Function Window ............................................................................ 31
3.2.8 Instrument Properties Dialog Box ................................................................ 32
3.2.9 Removing a Configured System................................................................... 33

4 Operation ............................................................................................... 35
4.1 Analysis Preparation .................................................................................. 36
4.1.1 Catalyst Filling ............................................................................................. 36
4.1.1.1 Catalyst for TOC Analysis ................................................................ 37
4.1.1.2 TOC/TN Catalyst (Option) ............................................................... 39
4.1.2 Connecting the Combustion Tube ................................................................ 40
4.1.3 Installing the Syringe.................................................................................... 45
4.1.3.1 Syringe Pump Zero Point Detection ................................................. 47
4.1.4 Water Supply to the Cooler Drain Container ............................................... 48
4.1.5 Filling the Humidifier with Water................................................................ 49
4.1.6 Preparation of Dilution Water ...................................................................... 50
4.1.7 Acid Preparation........................................................................................... 51
4.1.8 Installation of the CO2 Absorber.................................................................. 52
4.1.9 Adjusting Sparge Gas Flow Rate ................................................................. 53
4.1.10 Installing the Suspended Solids Kit.............................................................. 54
4.1.11 IC Analysis Preparations .............................................................................. 56
4.1.12 Preparation for POC analysis ....................................................................... 58
4.1.13 TN Analysis Preparations............................................................................. 59
4.1.14 Preparation and Storage of Standard Solutions ............................................ 60
4.1.14.1 Preparation of Standard Solutions..................................................... 60
4.1.14.2 Storage of Standard Solutions........................................................... 62
4.1.15 Sample Preparation....................................................................................... 63
4.1.15.1 High Sensitivity Analysis.................................................................. 63
4.1.15.2 TC Blank Check Analysis................................................................. 66
4.1.15.3 Pretreatment for IC Removal (Sparging) .......................................... 68
4.1.15.4 Analysis of Samples Containing Suspended Solids.......................... 69
4.1.15.5 Handling Samples Containing Acids, Bases or Salts........................ 71
4.1.16 Sample Preparation....................................................................................... 72
4.1.16.1 Vial Types ......................................................................................... 72
4.1.16.2 Filling Vials with Sample.................................................................. 72
4.1.16.3 Placing Vials in the Vial Rack .......................................................... 74
4.1.16.4 High Sensitivity Autosampler Analysis ............................................ 75
4.1.16.5 Acid Addition in NPOC Analysis ..................................................... 76
4.1.16.6 Sparging in NPOC Analysis.............................................................. 77
4.1.16.7 Stirrer Preparation ............................................................................. 78

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 Table Of Contents
4.1.17 8-Port Sampler Measurement........................................................................ 80
4.1.17.1 Type of Sampler Container................................................................ 80
4.1.17.2 High Sensitivity Using the 8-Port Sampler........................................ 82
4.2 Setting General Measurement Parameters................................................. 83
4.2.1 TOC Parameter Settings................................................................................ 83
4.2.2 ASI Parameter Settings ................................................................................. 84
4.2.3 Setting Default Measurement Parameters..................................................... 87
4.2.4 Maintenance History Settings ....................................................................... 88
4.3 Measurement Procedures and Tutorial ...................................................... 89
4.3.1 Starting Up the Instrument ............................................................................ 89
4.3.1.1 Turning on the Power ........................................................................ 89
4.3.1.2 Carrier Gas Pressure .......................................................................... 89
4.3.1.3 Carrier Gas Flow Rate ....................................................................... 90
4.3.1.4 Electric Furnace ................................................................................. 90
4.3.1.5 TN Unit .............................................................................................. 91
4.3.1.6 Ozone Source Airflow Rate for the TN Unit..................................... 91
4.3.2 Tutorial.......................................................................................................... 92
4.3.3 Ending Measurement .................................................................................. 120
4.4 Sample Table Editor ................................................................................ 122
4.4.1 Sample Table Window Overview ............................................................... 122
4.4.1.1 Toolbar Functions ............................................................................ 122
4.4.1.2 Status Bar and Notification Bar ....................................................... 124
4.4.2 File Menu .................................................................................................... 125
4.4.2.1 New.................................................................................................. 125
4.4.2.2 Calibration Curve............................................................................. 126
4.4.2.3 Method Wizard ................................................................................ 135
4.4.2.4 Open................................................................................................. 143
4.4.2.5 Close ................................................................................................ 144
4.4.2.6 Save.................................................................................................. 144
4.4.2.7 Save As ............................................................................................ 145
4.4.2.8 ASCII Export Options ..................................................................... 146
4.4.2.9 Database Export............................................................................... 148
4.4.2.10 Print>Table ...................................................................................... 149
4.4.2.11 Print>Sample Report ....................................................................... 150
4.4.2.12 Print Preview>Table ........................................................................ 150
4.4.2.13 Print Preview>Sample Report ......................................................... 151
4.4.2.14 Print Setup........................................................................................ 151
4.4.2.15 Page Setup........................................................................................ 152
4.4.2.16 Exit................................................................................................... 155

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 Table Of Contents
4.4.3 Edit Menu ................................................................................................... 156
4.4.3.1 Undo................................................................................................ 156
4.4.3.2 Cut/Copy/Paste................................................................................ 156
4.4.3.3 Replace............................................................................................ 157
4.4.3.4 Find ................................................................................................. 157
4.4.3.5 Exclude............................................................................................ 158
4.4.3.6 Recalculate>All............................................................................... 158
4.4.3.7 Recalculate>Highlighted................................................................. 158
4.4.3.8 Delete Data>All .............................................................................. 158
4.4.3.9 Delete Data>Highlighted ................................................................ 159
4.4.3.10 Import.............................................................................................. 159
4.4.4 View Menu ................................................................................................. 160
4.4.4.1 Calibration Curve ............................................................................ 160
4.4.4.2 Method ............................................................................................ 161
4.4.4.3 Sample Window .............................................................................. 167
4.4.4.4 Outlier Test...................................................................................... 169
4.4.4.5 Properties......................................................................................... 170
4.4.4.6 Customize........................................................................................ 177
4.4.4.7 Toolbar ............................................................................................ 178
4.4.4.8 Status Bar ........................................................................................ 178
4.4.4.9 ASI / 8-Port Sampler Vials ............................................................. 179
4.4.4.10 Data Profile ..................................................................................... 180
4.4.5 Insert Menu................................................................................................. 181
4.4.5.1 Auto Generate ................................................................................. 181
4.4.5.2 Sample............................................................................................. 185
4.4.5.3 Control............................................................................................. 193
4.4.6 Instrument Menu ........................................................................................ 203
4.4.6.1 Background Monitor ....................................................................... 203
4.4.6.2 Connect ........................................................................................... 205
4.4.6.3 Standby............................................................................................ 206
4.4.6.4 Measurement Start .......................................................................... 207
4.4.6.5 Stop>Peak Stop ............................................................................... 207
4.4.6.6 Stop>Finish Current Sample ........................................................... 207
4.4.6.7 Stop>Halt ........................................................................................ 207
4.4.7 Maintenance Menu ..................................................................................... 208
4.4.8 Tools Menu................................................................................................. 208
4.4.8.1 Control Charts ................................................................................. 208
4.4.8.2 Method Validation .......................................................................... 208
4.4.8.3 Administration................................................................................. 208
4.4.8.4 Screen Lock..................................................................................... 209
4.4.9 Options Menu ............................................................................................. 210
4.4.9.1 General Information ........................................................................ 210
4.4.9.2 Default Measurement Parameters ................................................... 212
4.4.9.3 Display Settings>Display Font ....................................................... 213
4.4.9.4 Display Settings>Table Settings ..................................................... 214
4.4.9.5 Display Settings>Notification Bar Settings .................................... 215
4.4.9.6 Display Settings>Floating Point Number Formats ......................... 216
4.4.9.7 Directories ....................................................................................... 217

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 Table Of Contents
4.4.10 Window Menu............................................................................................. 218
4.4.10.1 Cascade ............................................................................................ 218
4.4.10.2 Tile ................................................................................................... 218
4.4.10.3 Arrange Icons................................................................................... 218
4.4.11 Help Menu................................................................................................... 218
4.5 Application Operations............................................................................ 219
4.5.1 Manual Injection Analysis .......................................................................... 219
4.5.1.1 Analysis Preparation ........................................................................ 219
4.5.1.2 Measurement.................................................................................... 221
4.5.1.3 Measurement Precautions for Low Concentration Samples............ 225
4.5.1.4 Maintenance..................................................................................... 226
4.5.2 Gas Sample Analysis................................................................................... 227
4.5.2.1 Analysis Preparation ........................................................................ 228
4.5.2.2 Measurement.................................................................................... 229

5 Maintenance ......................................................................................... 235

5.1 Daily Inspection....................................................................................... 236
5.1.1 Checking Dilution Water ............................................................................ 236
5.1.2 Checking Acid............................................................................................. 236
5.1.3 Checking Drain Vessel Water Level .......................................................... 236
5.1.4 Checking Humidifier Water Level ............................................................. 237
5.2 Periodic Inspections................................................................................. 238
5.2.1 Catalyst Regeneration ................................................................................. 238
5.2.2 Washing or Replacing Catalyst................................................................... 239
5.2.2.1 Washing Catalyst ............................................................................. 239
5.2.2.2 Replacing Catalyst ........................................................................... 240
5.2.2.3 Replacing the Carrier Gas Purification Tube and Catalyst.............. 240
5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes.. 242
5.2.4 Replacing the High-Purity Air Cylinder ..................................................... 242
5.2.5 Replacing the CO2 Absorber....................................................................... 242
5.2.6 Replacing the Halogen Scrubber................................................................. 243
5.2.7 Replacing the Syringe Plunger Tip ............................................................. 244
5.2.8 Replacing Ferrules at the Combustion Tube Outlet Connection ................ 245
5.2.9 Replacing the Sliding Sample Injector O-rings .......................................... 245
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor ....................................... 246
5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier ........... 248
5.2.12 Replenishing IC Reaction Solution............................................................. 249
5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump.................... 250
5.2.14 Replacing the Filler of the Optional POC Analysis CO2 Absorber ............ 251
5.3 Autosampler (ASI-V) Maintenance......................................................... 252
5.3.1 Rinse Bottle Inspection ............................................................................... 252
5.3.2 Sample Catcher Inspection.......................................................................... 252
5.3.3 Replacing the Pump Head of the Rinse Pump ........................................... 253
5.4 8-Port Sampler (OCT-1) Maintenance .................................................... 254

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5.5 TN Unit (TNM-1) Maintenance............................................................... 256
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit................................. 256
5.5.2 Chemiluminescence Detector ..................................................................... 259
5.5.3 Ozone Generator Replacement................................................................... 260
5.5.4 Replacing the NOx Absorber...................................................................... 260
5.6 Software-Controlled Maintenance Functions .......................................... 261
5.6.1 Zero Point Detection................................................................................... 261
5.6.2 Regeneration of the TC Catalyst ................................................................ 262
5.6.3 Regeneration of the IC Solution ................................................................. 262
5.6.4 Residue Removal........................................................................................ 263
5.6.5 Replace Flowline Content ......................................................................... 263
5.6.6 Flowline Washing....................................................................................... 264
5.6.7 Mechanical Check ...................................................................................... 265
5.6.8 ASI / 8-Port Sampler Initialization............................................................. 267
5.6.9 ASI Rack Change ....................................................................................... 267
5.6.10 ASI Needle Change .................................................................................... 268
5.6.11 Change Syringe .......................................................................................... 268
5.6.12 Blank Check ............................................................................................... 269
5.6.13 Maintenance Log ........................................................................................ 269
5.6.14 History ........................................................................................................ 269
5.6.15 Sparge Gas Valve ....................................................................................... 269
5.6.16 Adjust Sparging Flow Rate (Wet Chem.)................................................... 269
5.7 Troubleshooting ....................................................................................... 270
5.7.1 Error Messages ........................................................................................... 270
5.7.2 Troubleshooting.......................................................................................... 274
5.7.2.1 TOC-V............................................................................................. 274
5.7.2.2 ASI-V .............................................................................................. 278
5.7.2.4 Corrective Actions for Poor Reproducibility .................................. 280

6 Reference Information ........................................................................ 283

6.1 Principles of Analysis .............................................................................. 284
6.1.1 Principles of TC (Total Carbon) Analysis.................................................. 284
6.1.2 Principles of IC (Inorganic Carbon) Analysis ............................................ 285
6.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis............... 286
6.1.4 Principles of POC (Purgeable Organic Carbon) Analysis.......................... 287
6.1.5 Principles of Measuring TOC..................................................................... 288
6.1.6 Principles of Measuring TN (Total Nitrogen) ............................................ 288
6.2 Analysis-Related Technical Information ................................................. 289
6.2.1 Peak Area Analysis..................................................................................... 289
6.2.2 Peak Shape.................................................................................................. 289
6.2.3 Calibration Curves...................................................................................... 290
6.2.3.1 Types of Calibration Curves ........................................................... 290
6.2.3.2 Shifting of Calibration Curves ........................................................ 290
6.2.4 Sparging During Standard Solution Analysis............................................. 292
6.2.5 Automatic Selection of Optimum Calibration Curve................................. 292

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6.3 Specifications........................................................................................... 294
6.3.1 TOC-VCPH/CPN ........................................................................................... 294
6.3.2 ASI-V .......................................................................................................... 295
6.3.3 OCT-1 8-Port Sampler ................................................................................ 295
6.3.4 TNM-1......................................................................................................... 295
6.3.5 POC Kit....................................................................................................... 296
6.3.6 Carrier Gas Purifier Kit............................................................................... 296
6.3.7 Manual Injection Kit (Gas Sample Injection Kit) ....................................... 296
6.3.8 PC Hardware Requirements........................................................................ 297
6.4 Standard Accessories............................................................................... 298
6.5 Special Accessories ................................................................................. 303
6.6 Consumable Parts List ............................................................................. 304
6.7 Maintenance Parts List ............................................................................ 308
6.8 Installation ............................................................................................... 310
6.8.1 Before Installation....................................................................................... 310
6.8.2 Installation Site............................................................................................ 310
6.8.2.1 Installation Site Selection ................................................................ 310
6.8.2.2 Installation Site Conditions.............................................................. 311
6.8.3 Installation Procedure.................................................................................. 312
6.8.3.1 Connecting Power Supply and Ground ........................................... 312
6.8.3.2 Changing the Power Supply Voltage............................................... 313
6.8.3.3 Connecting Gas................................................................................ 313
6.8.3.4 Connecting the Drain Tubing .......................................................... 316
6.8.3.5 PC Cable Connections ..................................................................... 317
6.8.4 Installing the Autosampler .......................................................................... 317
6.8.5 OCT-1 8-Port Sampler Installation ............................................................. 325
6.8.5.1 Installation Procedure ...................................................................... 325
6.8.6 Installing the TN Unit ................................................................................. 328
6.8.6.1 Connecting the Power and Installation ............................................ 328
6.8.6.2 Connecting Ozone Source Air ......................................................... 329
6.8.6.3 Connecting Gas Exhaust Tubing ..................................................... 332
6.9 Material Safety Data Sheets .................................................................... 333
6.9.1 Hydrochloric Acid (HCl) ............................................................................ 333
6.9.2 Phosphoric Acid .......................................................................................... 334
6.9.3 CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime .................................. 335
6.9.4 Lithium Hydroxide (monohydrate) ............................................................. 336
6.9.5 Halogen Scrubber........................................................................................ 337
6.9.6 Quartz Wool ................................................................................................ 338
6.9.7 High Sensitivity Catalyst............................................................................. 339
6.9.8 Normal Sensitivity Catalyst ........................................................................ 340
6.9.9 Potassium Nitrate ........................................................................................ 341
6.9.10 Sodium Bicarbonate .................................................................................... 342
6.9.11 Sodium Carbonate....................................................................................... 343
6.9.12 Potassium Hydrogen Phthalate ................................................................... 344
6.9.13 Water ........................................................................................................... 345

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 Table Of Contents
Appendix A Method Validation ................................................................. 347
A.1 Main Window .......................................................................................... 348
A.2 File Menu ................................................................................................. 349
A.2.1 New............................................................................................................. 349
A.2.2 Open ........................................................................................................... 350
A.2.3 Save ............................................................................................................ 351
A.2.4 Save As....................................................................................................... 351
A.2.5 Print ............................................................................................................ 351
A.2.6 Print Preview .............................................................................................. 352
A.2.7 Print Setup .................................................................................................. 353
A.2.8 Page Setup .................................................................................................. 353
A.2.9 Exit ............................................................................................................. 355
A.3 Edit Menu................................................................................................. 356
A.3.1 Undo ........................................................................................................... 356
A.3.2 Cut/Copy/Paste ........................................................................................... 356
A.3.3 Insert Row .................................................................................................. 356
A.3.4 Delete Row ................................................................................................. 357
A.3.5 Insert Column ............................................................................................. 357
A.3.6 Delete Column............................................................................................ 357
A.3.7 Recalculate ................................................................................................. 357
A.4 View Menu............................................................................................... 358
A.5 Options Menu........................................................................................... 359
A.5.1 General Parameter ...................................................................................... 359
A.5.2 Method Validation Parameter..................................................................... 360
A.5.3 Font............................................................................................................. 361
A.5.4 Floating Point Numbering Format.............................................................. 362
A.5.5 ASCII Export Options ................................................................................ 363
A.5.6 Validation Strictly Following DIN38402................................................... 364
A.6 Help Menu ............................................................................................... 365

Appendix B Control Charts........................................................................ 367

B.1 File Menu ................................................................................................. 368
B.1.1 New............................................................................................................. 368
B.1.2 Following Control Chart............................................................................. 372
B.1.3 Open ........................................................................................................... 373
B.1.4 Save ............................................................................................................ 373
B.1.5 Save As....................................................................................................... 373
B.1.6 Print>Data................................................................................................... 373
B.1.7 Print>Graph ................................................................................................ 373
B.1.8 Print Preview>Data/Print Preview>Graph ................................................. 373
B.1.9 Print Setup .................................................................................................. 374
B.1.10 Page Setup .................................................................................................. 374
B.1.11 Exit ............................................................................................................. 376
B.2 Edit Menu................................................................................................. 377

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B.3 View Menu .............................................................................................. 378
B.3.1 Statistics ...................................................................................................... 378
B.3.2 Comparison ................................................................................................. 379
B.3.3 Out of Control Events ................................................................................. 380
B.3.4 Toolbar/Status Bar ...................................................................................... 380
B.4 Options Menu .......................................................................................... 381
B.4.1 Control Chart Options ................................................................................. 381
B.4.2 Font ............................................................................................................. 381
B.4.3 Floating Point Numbering Format .............................................................. 382
B.4.4 ASCII Export Options................................................................................. 383
B.4.5 Enable Exclusion......................................................................................... 383
B.5 Help Menu ............................................................................................... 384

TOC-VCPH/CPN xxi
 Table Of Contents

xxii TOC-VCPH/CPN
 1

1Overview
This chapter provides an overview of the instrument and operational precautions for its
use.

1.1 Overview

Provides an overview of the TOC-VCPH/TOC-VCPN instrument.

1.2 Operational Precautions

Lists precautions necessary to ensure that the instrument is used correctly.

 1.1 Overview

1.1 Overview

The TOC-VCPH/TOC-VCPN (hereinafter referred to as TOC-V) instrument measures the

amount of total carbon (TC), inorganic carbon (IC) and total organic carbon (TOC) in
water. Purgeable organic carbon (POC) can also be measured when the POC accessory is
installed. “Oxidative combustion-infrared analysis” is a widely-used TOC measurement
method that has been adopted by the JIS1 and other international standards. The TOC-V
instrument can also measure total water-borne nitrogen (TN) if the optional TN unit is
installed. TN is measured using the principles of “oxidative combustion-
chemiluminescence.”

Moreover, when the ASI-V Autosampler or OCT-1 8-Port Sampler is used in combination
with the main unit, a fully automatic system is created, allowing automatic analysis of
multiple samples.

This instruction manual covers both the TOC-VCPH and TOC-VCPN models. These models
will be referred to in relevant descriptions as the H Type and N Type, respectively.

Read this user manual carefully before using the TOC-V instrument to ensure its proper
use. The manual should be stored in a convenient location for future reference.

CAUTION
Safety may be compromised if the instrument is used in a fashion other than that
indicated in this user manual. Pay particular attention to the CAUTION sections
to ensure safety when using the instrument.

1. JIS K-0102 "Industrial Waste Water Testing", JIS K-0551: "Total organic carbon (TOC) testing methods for
ultra-pure water", U.S. Pharmacopoeia, EPA 415.1, EPA 9060A, ASTM D2575, Standard Methods for
Examination of Water and Waste Water 5310B

2 TOC-VCPH/CPN
 1.2 Operational Precautions

1.2 Operational Precautions

Take the following precautions when using this instrument.

CAUTION
• Do not touch the electric furnace while it is heating. The center of the electric furnace
(near the combustion tube insertion opening) reaches very high temperatures, and burns
may result. <Burn prevention>
• To prevent high sensitivity catalyst from being forced upward in the combustion tube,
verify that carrier gas is flowing when heating the electric furnace. <Prevents the
floating of high sensitivity catalyst>
• Allow the electric furnace to cool to room temperature before removing or exchanging
the combustion tube. Burns may result if this procedure is attempted when the furnace
is at a high temperature. <Burn prevention>
• Do not heat the electric furnace without the combustion tube installed. Parts employed
by the TC injection port (slider block assembly) will be exposed to radiant heat from the
center of the electric furnace and may be deformed. If the furnace must be heated with-
out a combustion tube installed, first remove the TC injection port parts to prevent
deformation, or close off the furnace core opening with a heat-insulating material such
as quartz wool. <Part damage prevention>
• To reduce back pressure, verify that the external drain tubing connected to the waste
port on the right side of the instrument does not touch the surface of the liquid in the
waste container. The height of the external tube must always be lower than the height of
the drain port. Excessive back pressure will result in insufficient drainage and waste will
overflow inside the instrument. <Part corrosion prevention>

TOC-V Drain tubing (Tubing

placement should be as
indicated by the solid line.)

Drain container
(Supplied by user.)

Figure 1.1 External Drain Tubing

• Hand tighten the various connectors to the 8-port valve. Use of a tool may cause
deformation and leakage in the valve. <Part damage prevention>

TOC-VCPH/CPN 3
 1.2 Operational Precautions

• Stop operation of the instrument when performing maintenance on any of the drive
components, such as connecting lines to the 8-port valve, or connecting/disconnecting
lines on the sample injector. If these parts are manipulated or if the lines are
disconnected during operation, the drive component could move and cause injury or
discharge of liquid. <Injury prevention, corrosion prevention>
• To shut down the instrument, first select “Shut down instrument” in the TOC-Control V
Standby window. Refer to Section 4.3.3 "Ending Measurement" for more information.
The electric furnace turns off and, after 30 minutes, the power supply shuts off. This
shutdown process extends the life of the TC injection port parts by preventing
unnecessary wear. This procedure does not apply to emergency shutdown.
<Maintaining durability of TC injection port parts>
• The lever of the 3-way valve at the bottom of the IC reaction vessel should normally be
turned to the left position. Refer to Figure 1.2 "Lever Position of 3-Way Valve on the IC
Reaction Vessel". The lever should never be turned to the lower position. The lower
position allows carrier gas to flow at a pressure of 200kPa upstream from the 3-way
valve, causing possible disconnection of joints and damage to parts such as the
combustion tube.

Carrier gas is discharged Never turn the lever

to the front of the IC to this position.
reaction vessel. (Turn
the lever to this position
only when detaching an
IC reaction vessel that
contains liquid.)

Figure 1.2 Lever Position of 3-Way Valve on the IC Reaction Vessel

• To use the ozone generator of the TN unit, verify that air is supplied at a rate of 0.5 L/
min to the ozone air source flow meter inside the instrument. Refer to Figure 2.5 "Inside
Front View". Turn ON the ozone generator. This prevents ozone leaks and line
corrosion. <Ozone leak prevention, line corrosion prevention>
• If ozone odor is detected during operation of the TN unit, stop the gas supply by turning
the ozone generator OFF, and contact your Shimadzu representative to request
maintenance. Ozone can cause respiratory organ injury and equipment damage.
<Prevention of injury to respiratory organs and equipment damage>
• To shut down the TN unit, turn the ozone generator OFF at least 3 minutes prior to
switching OFF the TN unit power to stop ozone generation. This prevents ozone leaks
and line corrosion. <Ozone leak prevention, line corrosion prevention>

4 TOC-VCPH/CPN
 1.2 Operational Precautions

• The optional POC measurement circuit incorporates a carbon dioxide (CO2) absorber
packed with lithium hydroxide for removal of carbon dioxide gas. Misuse of lithium
hydroxide can cause bodily harm. During packing or replacing the CO2 absorber
container, exercise adequate precaution. After use, treat the material as industrial waste.
The properties and handling guidelines for lithium hydroxide are described in the mate-
rial safety data sheets (MSDS) in Section 6.9 "Material Safety Data Sheets".
• To clean the instrument, wipe the surface with a soft cloth moistened with water. Do not
use chemicals.
• Repairs to the inside of the instrument can be dangerous. Contact your Shimadzu
representative to have a trained service engineer perform repairs.
• Do not disassemble or modify the instrument beyond the scope of the maintenance
procedures described in this manual, as safety may be compromised.
• The construction of the instrument is not explosion-proof. It must not be used in
dangerous areas.
• Use the instrument with a power supply of AC 100-127V ±10% (100V systems) or AC
220-240V ±10% (200V systems).
• The instrument backup battery will last for approximately one year. Connection to a PC
may not be possible if the instrument has been idle for more than one year. If this is the
case, turn the instrument power ON for at least 30 seconds, then turn the instrument
power OFF for 10 seconds and back ON again.
If the instrument usually remains idle for extended periods, turn the instrument power
ON for 24 hours once every six months.
• Do not use the following characters when naming files or systems to be saved:
/ , . \ (back slash) : ; (these are all normal-width characters), space (normal width, em
width)
• Turn OFF the Power Management function of the PC to prevent shutdown of the PC
power while it is controlling the TOC analyzer. A shutdown of this nature would
adversely affect performance.
• Hand-tighten the connectors to the 8-port valve of the 8-port sampler. Over-tightening
with a tool may exert excessive force to the internal valve body, causing deformation
and internal leakage. <Part damage prevention<
• Shut down the instrument before connecting or disconnecting tubing to the 8-port valve
or performing maintenance to the drive parts. Liquid may be discharged from tubes
during operation. <Part corrosion prevention>)
• When utilizing the software's printing function, set the paper size to letter or A4 and
printer graphic resolution to 600 dpi.

TOC-VCPH/CPN 5
 1.2 Operational Precautions

6 TOC-VCPH/CPN
 2

2System Description
This chapter describes the components of the TOC-VCPH/CPN, autosampler (ASI-V), 8-
port sampler (OCT-1), and the TN unit (TNM-1).

2.1 TOC-VCPH/CPN Construction

Describes the construction of the TOC-V unit using front, right, left, rear and
internal views of the instrument, as well as flow diagrams.

2.2 Autosampler ASI-V (Option)

Describes the construction of the ASI-V unit using front and rear views of the
autosampler.

2.3 8-Port Sampler OCT-1 (Option)

Describes the construction of the 8-port sampler using front and rear views of the
unit.

2.4 TN Unit TNM-1 (Option)

Describes the construction of the TNM-1 unit using front, right and internal
views of the unit.
 2.1 TOC-VCPH/CPN Construction
2.1.1 Front View

2.1 TOC-VCPH/CPN Construction

2.1.1 Front View

Start Button

Front Door

Power Switch
Stop Button

Figure 2.1 Front View

2.1.2 Right Side View

Tubing and Wiring

Opening for the
TN Unit

Drain Tubing

Figure 2.2 Right Side View

8 TOC-VCPH/CPN
 2.1 TOC-VCPH/CPN Construction
2.1.3 Left Side View

2.1.3 Left Side View

Sample Tubing

Hydrochloric Acid

Dilution Water
Bottle

IC Reagent

Figure 2.3 Left Side View

2.1.4 Rear View

Carrier Gas Inlet CO2 Absorber

AC Cord Socket

1
2 4 5
3 6

Figure 2.4 Rear View

1) Flash ROM rewrite switch

2) Printer cable terminal
3) RS-232C terminal (1)
4) RS-232C terminal (2)
5) ASI-V/OCT-1 signal cable connector
6) ASI-V/OCT-1 power cable connector

TOC-VCPH/CPN 9
 2.1 TOC-VCPH/CPN Construction
2.1.5 Inside Front View

2.1.5 Inside Front View

1 2 4 5
3

16

8
15

14

10

13
Front Door

12 11

Figure 2.5 Inside Front View

1) Sliding sample injector (H Type only)
2) IC reagent vessel (H Type only)
3) Solenoid valve (for IC drainage) (H Type only)
4) Carrier gas pressure gauge
5) Carrier gas flow adjustment knob
6) Carrier gas flowmeter
7) Carrier gas pressure adjustment knob
8) Sparge gas flowmeter (option)
9) Sparge gas flow adjustment knob (option)
10) Halogen scrubber
11) Humidifier
12) Pump (for IC reagent supply) (H Type only)
13) Syringe pump cover
14) 5mL syringe
15) 8-port valve
16) 3-way valve

10 TOC-VCPH/CPN
 2.1 TOC-VCPH/CPN Construction
2.1.6 Inside Top View

2.1.6 Inside Top View

Slide Motor
Cooling Fan for
Sample Injection
Block

Slider
Sample Injection
Tubing

Sample Injection Block

Figure 2.6 Inside Top View

2.1.7 Flow Diagrams

Figure 2.7 Flow Diagram (TOC-VCPH)

TOC-VCPH/CPN 11
 2.1 TOC-VCPH/CPN Construction
2.1.7 Flow Diagrams

Figure 2.8 Flow Diagram (TOC-VCPH+TNM-1)

Figure 2.9 Flow Diagram (TOC-VCPH+POC Option)

12 TOC-VCPH/CPN
 2.1 TOC-VCPH/CPN Construction
2.1.7 Flow Diagrams

Figure 2.10 Flow Diagram (TOC-VCPN)

Figure 2.11 Flow Diagram (TOC-VCPN+TNM-1)

TOC-VCPH/CPN 13
 2.2 Autosampler ASI-V (Option)
2.2.1 Front View

2.2 Autosampler ASI-V (Option)

2.2.1 Front View

Needle Replacement Window

Sample Tubing

Stirrer Speed
Sample Cover Control (option)

Figure 2.12 Front View

2.2.2 Rear View

Rinse Solution Tubing

Signal Cable
Terminal

Power Cable
(attached to ASI) Drain Tubing

Figure 2.13 Rear View

14 TOC-VCPH/CPN
 2.3 8-Port Sampler OCT-1 (Option)
2.3.1 Front View

2.3 8-Port Sampler OCT-1 (Option)

2.3.1 Front View

8-Port Valve

Figure 2.14 Front View

2.3.2 Rear View

8-Port Sampler 1 8-Port Sampler 2

Signal Power Signal Cable

Cable Cable (with Power Supply)

Figure 2.15 Rear View

TOC-VCPH/CPN 15
 2.4 TN Unit TNM-1 (Option)
2.4.1 Front and Right Side Views

2.4 TN Unit TNM-1 (Option)

2.4.1 Front and Right Side Views

Ozone Air Source Flowmeter

POWER: Power Lamp

REACT: Reactor Temperature

Control Heater Lamp

O3GEN: Ozone Generator

Status Lamp

PRESS: Ozone Source Air

Supply Warning Lamp

Ozone Generator Switch

Figure 2.16 Front and Right Side Views

16 TOC-VCPH/CPN
 2.4 TN Unit TNM-1 (Option)
2.4.2 Inside Front View

2.4.2 Inside Front View

Reactor

Viton Joint

Flowmeter

Ozone Treatment Unit

Ozone Source Airflow

Adjustment Knob

Figure 2.17 Inside Front View

TOC-VCPH/CPN 17
 2.4 TN Unit TNM-1 (Option)
2.4.3 Rear View

2.4.3 Rear View

Ozone Source Air Inlet

AC Cable Socket

Gas Exhaust Port

Figure 2.18 Rear View

18 TOC-VCPH/CPN
 3

3 Software Overview, Administration,

and Setup
This chapter provides an overview of the TOC-Control V software and describes the
software’s Administration and Instrument Setup Wizard tools.

3.1 Introduction to System Administration Functions

Describes the system administration functions performed by the user.

3.2 Instrument Setup and System Properties

Describes the software’s Instrument Setup Wizard, which is used to configure
new systems by collecting information such as installed instrumentation,
instrument settings and communication parameters. Also describes procedures
for viewing the properties of and removing previously-configured systems.
 3.1 Introduction to System Administration Functions
3.1.1 Screen Lock Function

3.1 Introduction to System Administration Functions

This section describes the various system administration functions in the TOC-Control V
software that are available to the user. For a description of system administration functions
that can be performed by the system administrator, refer to the TOC-V Administrator's
Manual.

3.1.1 Screen Lock Function

If user must temporarily leave the PC during measurement, the screen can be locked to
protect the data from another individual making improper or malicious operations in TOC-
Control V.
This function can be used only if the User ID / Password item is checked in the Security
dialog box. Consult with the system administrator to implement changes in the security
settings.
To lock the screen, select Screen Lock in the Tools menu. The screen is locked and the Re-
enter Password dialog box displayed. Once the screen is locked it can only be unlocked by
entering the User ID and Password of the user who was logged on at the time the screen
was locked.

Figure 3.1 Screen Lock Command

Figure 3.2 Re-enter Password Dialog Box

20 TOC-VCPH/CPN
 3.1 Introduction to System Administration Functions
3.1.2 Change Password

3.1.2 Change Password

This function is used to change the password of a registered user.
Select Change Password in the TOC-Control V Administrator window to open the Change
Password dialog box. This function can be used only if the User ID/Password item is
checked in the Security dialog box. Refer to Section 3.2.4 “Security” in the Administrator’s
Manual for more information.

Figure 3.3 TOC-Control V Administrator Window

Figure 3.4 Change Password Dialog Box

TOC-VCPH/CPN 21
 3.1 Introduction to System Administration Functions
3.1.3 Add Event Log

3.1.3 Add Event Log

This function is used when a comment is to be included with the operation history. This
function is useful for documenting items in the operation history, such as the replacement
of catalyst, that cannot be recorded automatically through the software. Only users with
access rights to Add Event Log can use this function.
This function can be used only if Audit Trail is checked in the Security dialog box. Refer to
Section 3.2.4 “Security” in the Administrator’s Manual for more information.
When Add Event Log is selected in the TOC-Control V Administrator window, the Add
Event Log dialog box is displayed.

Figure 3.5 Add Event Dialog Box

Select one of the items in the Select Item array, and then enter a comment in the
Comment text field. If the Comment text field is left blank, an error message is
displayed, and the comment is not added to the Event Log.

22 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.1 System Information Window

3.2 Instrument Setup and System Properties

This section describes the Instrument Setup Wizard, which is used to configure new
systems. This section also describes procedures for viewing the properties of and removing
previously-configured systems.
The TOC-Control V Instrument Setup Wizard is used to enter properties for a new system.
Access the Wizard by double-clicking the “New System” icon in the TOC-Control V main
window.
Multiple instruments can be configured for the TOC-Control V software system by
entering information into the series of Wizard screens.

TIP » Use the Back and Next buttons to move among the various Instrument Setup Wizard
windows.

3.2.1 System Information Window

The System Information window of the Instrument Setup Wizard is used to enter basic
system information.

Figure 3.6 Instrument Setup Wizard: System Information Window

System
Enter a unique name for the system, using up to 32 characters. A name must be entered
before continuing to the next Wizard page. If a system with the entered name already exists,
an error message is displayed requesting entry of a unique name.

Serial Number
Enter the serial number of the TOC-V. The serial number of the unit is an 8-character
number (No. ********) that is printed on the plate attached to the lower right side of the
instrument.

TOC-VCPH/CPN 23
 3.2 Instrument Setup and System Properties
3.2.2 Options Window

User
The name of the current user is automatically entered into the User field and cannot be
edited.

Date of Creation
The current date is automatically entered into the Date of Creation field and cannot be
edited.

Comment
Enter additional system information in the Comment text box. The Comment field is
optional and can contain up to 512 characters.

3.2.2 Options Window

The Options window of the Instrument Setup Wizard is used to specify the instrument
hardware configuration and attached accessories.

Figure 3.7 Instrument Setup Wizard: Options Window

Oxidation
Select “Combustion” from the drop-down list to specify the oxidation method.

Options
Select the installed instrument components by clicking the appropriate check boxes. The
options include TOC, ASI, SSM (solid-sampler unit), POC, IC Unit, TN, Sparge Kit,
Manual Injection Kit, 8Port Sampler-1, 8Port Sampler-2 and ESU (external scrubbing
unit). The selected options determine which Instrument Setup Wizard screens are
displayed.
Select the IC Unit for the H-type. If Manual Injection Kit is selected, the ASI, SSM, and
POC options are disabled.

24 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.2 Options Window

Option Description
TOC Displays the TOC screen of the Instrument Setup Wizard to allow TOC
instrument parameters to be set.
ASI Displays the ASI screen of the Instrument Setup Wizard to allow
autosampler parameters to be set. This option is disabled if the Manual
Injection Kit option is selected.
SSM Displays the SSM screen of the Instrument Setup Wizard to allow solid
sampler unit parameters to be set. This option is disabled if the Manual
Injection Kit option is selected.
POC Specifies that the purgeable organic carbon accessory is installed.
IC Unit Specifies that the instrument will be used to measure inorganic carbon.
Select this option for only instrument model TOC-VCPH. Do not select
this option for instrument model TOC-VCPN. If the IC Unit is selected as
an option, the “Auto regeneration of IC solution” check box will be
enabled on the Instrument Setup Wizard TOC screen.
TN Specifies that the TN accessory is installed. If the TN Unit is selected as
an option, the “TN Power” check box will be enabled on the Instrument
Setup Wizard TOC screen.
Sparge Kit Specifies that the Sparge Kit accessory is installed and that external
sparging is desired. If the Sparge Kit is selected as an option, the “Nee-
dle” parameter will be enabled on the Instrument Setup Wizard ASI
screen.
Manual Inj. Kit Specifies that the Manual Injection Kit accessory is installed. The ASI,
SSM, and POC accessories cannot be used simultaneously with the Man-
ual Injection Kit. If the Manual Injection Kit is selected as an option, the
options for ASI, SSM, and POC are deselected and disabled.
8-Port Sampler 1 Select this option when one 8-port sampler accessory is installed. 8-Port
Sampler 1 cannot be selected if the ASI or SSM are selected.
8-Port Sampler 2 Select this option when two 8-port sampler accessories are installed. 8-
Port Sampler 2 can only be selected if 8-Port Sampler 1 is selected.

TOC-VCPH/CPN 25
 3.2 Instrument Setup and System Properties
3.2.3 TOC Window

3.2.3 TOC Window

The TOC window of the Instrument Setup Wizard is used to set TOC instrument
parameters.

Figure 3.8 Instrument Setup Wizard: TOC Window

Catalyst Type
Select the type of catalyst to be used in TC or TC/TN measurement from the drop-down
list. Available options are:
• Regular: for TC measurements (concentrations of 500ppb or greater)
• High Sense: for TC measurements (concentrations below 500ppb)
• TC/TN: for combined TC and TN measurements
Note: The instrument does not automatically recognize the type of cata-
lyst that is installed. Be sure to select the catalyst type that is actu-
ally installed in the instrument.
The high sensitivity catalyst should be used when the expected sample concentrations are
below 500ppb or when detection of minute changes in concentration is necessary.

Tubing Diameter
Select the diameter size of the sample injection tubing from the drop-down list. Available
options are:
• Regular: 0.5mm diameter
• Suspended Particle: 0.8mm diameter
The typical tubing diameter is 0.5mm. Select a tubing diameter of 0.8mm if the Suspended
Solids kit is used.

Cell Length
Select the length of the NDIR detection cell from the drop-down list. Available options are:
• Long: for typical measurements
• Short: for measurements using the Suspended Solids kit

26 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.3 TOC Window

Buzzer
Enables the internal buzzer function. Select this option to allow the buzzer to sound during
measurement.

Auto regeneration of IC solution

Select this option to automatically regenerate the IC solution. This option is enabled only if
IC Unit was selected in the Options window of the Instrument Setup Wizard.
The acidity of the IC solution gradually decreases over time, as the acid is used to convert
the IC components in samples into carbon dioxide. Unless the IC solution is periodically
regenerated, it eventually loses its ability to fully convert IC into carbon dioxide, which can
affect the accuracy of analysis.
When the Auto Regeneration option is selected, the pH and volume of the IC solution are
automatically maintained at the appropriate levels. The instrument automatically pumps IC
solution from the IC reagent reservoir in the following cases:
• When the instrument is turned on
• Prior to the initial IC measurement, following a preset number of injections and preset
volume of injected samples
• If peak tailing is observed during an IC measurement. (The system notifies the user of
peak tailing by inserting a “T” into the Notes column of the Injection Table and the
Remark column of the Sample Table.)

Enable ready status check

Select this option to enable the Ready Status Check function. When the function is enabled,
the software always verifies that the instrument is in the Ready state prior to starting
measurement. Enabling the Ready Status Check function is recommended. When the
function is deselected, measurement can be performed when the instrument is not in the
Ready state, an option that is mainly for use by service personnel.

TN Power
This item is displayed if “TN” was selected as an option in the previous screen. Select this
item to perform TN analyses.

TC Furnace
Select the desired TC furnace temperature by clicking the appropriate radio button. Select
680 (°C) for regular or high sensitivity catalyst. Select 720 (°C) for TC/TN catalyst.

TOC-VCPH/CPN 27
 3.2 Instrument Setup and System Properties
3.2.4 ASI Window

3.2.4 ASI Window

The ASI window of the Instrument Setup Wizard is displayed if ASI was selected in the
Options window of the Wizard. Use the ASI screen to set the autosampler parameters.

Figure 3.9 Instrument Setup Wizard: ASI Window

Tray Type
Select the ASI tray type from the drop-down list. Options are 24mL Vial and 40mL Vial.

Needle
Select the needle type from the drop-down list. Options are:
• Sample: for analysis using only a sample needle
• Sample+Sparge: for analysis using both a sample needle and a sparge needle
• Coaxial: for analysis using an integrated sample and sparge needle
• Coaxial+Sparge: for analysis using both the coaxial needle and a sparge needle,
which allows a sample to be measured while the next sample is sparged.
The Needle field is enabled only if Sparge Kit was selected in the Options window of the
Wizard.
Note: The instrument does not automatically recognize the type of needle installed. Be
sure to select the type of needle that is actually installed in the instrument.

No. of Needle Washes

Enter the number of times (0-10) the outside of the needle will be washed with water from
the dilution water bottle, at the end of a sample run.

No. of Flow Line Washes

Enter the number of times (0-10) the flow lines will be washed after all samples listed in the
Sample Table have been measured. Water from the dilution water bottle is used to wash the
flow lines.

28 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.5 SSM Window

Rinse
Select this option to rinse the sampling needle between each sample with water from the
dilution water bottle.

Rinse After Acid Addition

Select this option to rinse the sampling needle after each acid addition with water from the
dilution water bottle.

Stirrer On
Select this item to use the optional magnetic stirrer during measurement.

3.2.5 SSM Window

The SSM window of the Instrument Setup Wizard is displayed if SSM was selected in the
Options window of the Wizard. Use the SSM screen to set the SSM parameters. Refer to
the SSM-5000A User Manual for details.

Figure 3.10 Instrument Setup Wizard: SSM Window

SSM TC Furnace On
Select this option for TC measurement.

SSM IC Furnace On
Select this option for IC measurement.

TOC-VCPH/CPN 29
 3.2 Instrument Setup and System Properties
3.2.6 Communication Window

3.2.6 Communication Window

The Communication window of the Instrument Setup Wizard is used to set parameters for
communication between the instrument and the PC.

Figure 3.11 Instrument Setup Wizard: Communication Window

Com Port
Select the communication port from the drop-down list. Options include Com1, Com2,
Com3, and Com4.

Stop Bits
The Stop Bits value is determined by the hardware and is set automatically based on the
Com Port selection. This field is disabled and cannot be edited by the user.

Parity
The Parity value is determined by the hardware and is set automatically based on the Com
Port selection. This field is disabled and cannot be edited by the user.

30 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.7 History Function Window

3.2.7 History Function Window

The History Function window of the Instrument Setup Wizard is used to enable the History
Log. The History Log records all modifications to the system properties. The History Log
can be set to require users to enter comments for each modification.
Note: Once the History Log is enabled, it cannot be disabled. All modifications to the
system properties will be tracked. If the mandatory comment option is selected,
the user will be required to enter a comment each time any system parameter is
modified.

Figure 3.12 Instrument Setup Wizard: History Function Window

Enable History Log

Select this option to enable the software to monitor all modifications to the system
properties. Once the History Log is enabled, the check box is disabled and the log cannot be
turned off. The History Log is maintained on the History tab of the Instrument Properties
dialog box. Refer to Section 3.2.8 "Instrument Properties Dialog Box". If the History Log is
not required, it need not be enabled, as the software operates properly without it.

A Comment is Required for All Modifications

Select this option to require the user to comment on or obtain approval for all
modifications. Once this option is selected, the check box is disabled and the option cannot
be turned off. If the History Log is not required, it need not be enabled, as the software
operates properly without it.

Finish Button
The History Function window is the final screen in the Instrument Setup Wizard. Make the
appropriate selections, then click the Finish button. The new instrument is created and
saved, and its icon appears in the TOC-Control V main window.

TOC-VCPH/CPN 31
 3.2 Instrument Setup and System Properties
3.2.8 Instrument Properties Dialog Box

3.2.8 Instrument Properties Dialog Box

Instrument parameters can be viewed and modified using the Instrument Properties dialog
box, shown below. Open the dialog box by double-clicking the instrument icon in the TOC-
Control V main window.

Figure 3.13 Instrument Properties Dialog Box

System Tab
The System tab displays the System Information window for the selected system and
allows editing of the Comment field.

Options Tab
The Options tab displays the oxidation method and instrument components that were
selected in the Options window of the Instrument Setup Wizard. Information on this tab can
be viewed but not changed.

TOC Tab
The TOC tab is identical to the TOC window in the Instrument Setup Wizard. Some fields
on the TOC tab can be edited. If the History Log was enabled during setup, edits to the
TOC tab will be tracked and listed in the History tab.

ASI Tab
The ASI tab is identical to the ASI window in the Instrument Setup Wizard. Some fields on
the ASI tab can be edited. If the History Log was enabled during setup, edits to the ASI tab
will be tracked and listed in the History tab.

Communication Tab
The Communication tab is identical to the Communication window in the Instrument Setup
Wizard. Some fields on the Communication tab can be edited. If the History Log was
enabled during setup, edits to the Communication tab will be tracked and listed in the
History tab.

32 TOC-VCPH/CPN
 3.2 Instrument Setup and System Properties
3.2.9 Removing a Configured System

SSM Tab
The SSM tab is identical to the SSM window in the Instrument Setup Wizard. Some fields
on the SSM tab can be edited. If the History Log was enabled during setup, edits to the
SSM tab will be tracked and listed in the History tab.

History Tab
If the History Log was not enabled during setup, the History tab is identical to the History
Function window in the Instrument Setup Wizard. Use this screen to enable the History log.
If the History Log was enabled during setup, the History tab lists all changes made to the
system parameters. The log lists modifications chronologically, with the most recent
modification at the top. If the mandatory comment option was selected during setup, all
modifications listed in the History tab window contain a comment describing the reason for
the change. View or edit previously entered comments by selecting the modification from
the list and clicking the Edit Comment button. If the History Log is not required, it need not
be enabled, as the software operates properly without it.

Figure 3.14 Comment Dialog Box

Note that if the mandatory comment option was selected in the History Function window
during instrument setup, the Comment dialog box (shown above) is displayed after any
change is made in the Instrument Properties dialog box.

3.2.9 Removing a Configured System

Systems are removed from the TOC-Control V software using the main window. To
remove a system, right-click the appropriate system icon and select Delete. Once a system
is deleted, it cannot be restored.

TOC-VCPH/CPN 33
 3.2 Instrument Setup and System Properties
3.2.9 Removing a Configured System

34 TOC-VCPH/CPN
 4

4Operation
This chapter describes procedures for pre-analysis preparations, setting measurement
parameters, starting up the instrument, generating calibration curves, and conducting
sample analysis. This chapter also includes a tutorial that covers setup and measure-
ment procedures.

4.1 Analysis Preparation

This section describes instrument preparation procedures such as catalyst filling,
combustion tube connection, and syringe replacement as well as other
preparation procedures for actual sample analysis.

4.2 Setting General Measurement Parameters

This section describes procedures for setting TOC, ASI and default measurement
parameters using the TOC-Control V software.

4.3 Measurement Procedures and Tutorial

This section describes and provides a tutorial for measurement procedures, such
as instrument startup, calibration curve generation, method development, sample
analysis, halting of analysis and instrument shutdown.

4.4 Sample Table Editor

This section provides a detailed description of the TOC-Control V Sample Table
Editor menus and commands. The Sample Table Editor is used for instrument
startup, calibration curve generation, method development, sample analysis,
halting of analysis and instrument shutdown.

4.5 Application Operations

The procedures for performing manual injection analysis and gaseous sample
analysis are described in this section.
 4.1 Analysis Preparation
4.1.1 Catalyst Filling

4.1 Analysis Preparation

4.1.1 Catalyst Filling

Three types of catalyst are available: TOC standard catalyst, TOC high sensitivity catalyst
(H Type only), and TOC/TN catalyst (option). The procedures for filling the combustion
tube with catalyst are described in this section. For TOC standard and high sensitivity
catalyst filling, follow the procedure in Section 4.1.1.1 "Catalyst for TOC Analysis". For
TOC/TN catalyst filling, follow the procedure in Section 4.1.1.2 "TOC/TN Catalyst
(Option)".

CAUTION
Exercise caution when handling the combustion tube to prevent breakage, as it is
made of quartz glass.

Note: When filling the combustion tube, verify that the catalyst does not become con-
taminated. Contamination will cause high blank values and abnormal analysis
values.

Using New Catalyst

Broad blank peaks are obtained when using new catalyst for the first time. The blank peaks
will become progressively smaller and more stable with repeated injections, and their size
will stabilize. If calibration or analysis is performed while the blank peaks are large, the
measurements are affected by the changing magnitude of the blank peaks, resulting in
errors in the analysis values. Such errors are especially significant for high sensitivity TC
analysis.

TC Analysis Using New Catalyst

Catalyst regeneration should be conducted 1-2 times for TC analysis using new catalyst.
This reduces the size of the blank peaks. Use continuous injections of pure water until the
blank peak area becomes small and stable. The blank peak magnitude depends on the
quality of the water (TC impurity concentration) and the TC analysis range used for
analysis. For example, a blank peak of 1mg/L has little influence on results greater than
100mg/L but has a significant influence on results equal to or less than 10mg/L. Analyses
for expected concentrations around 10mg/L must have stable blank peaks of 0.5mg/L or
less.
For TOC high sensitivity catalyst, conduct the TC blank check analysis described in
Section 4.1.15.2 "TC Blank Check Analysis".

TN Analysis Using New Catalyst

Blank peak magnitude poses no practical problems for TN analysis using new catalyst. The
blank peaks are fairly small and stable. Perform analysis with distilled or deionized water to
confirm the size of the blank peaks.

36 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.1 Catalyst Filling

4.1.1.1 Catalyst for TOC Analysis

Either standard or high sensitivity catalyst can be used for TOC analysis. The furnace
temperature is set to 680°C for TOC analysis.

¬TOC Standard Catalyst

The TOC standard catalyst is appropriate for both the TC-IC method and NPOC method of
analysis.
Note: Analyze TOC high precision samples (with expected concentrations of about
1mg/L) using the TOC high sensitivity catalyst because smaller blank peaks are
generated.

Filling Combustion Tube with TOC Standard Catalyst

1. Insert two sheets of platinum mesh into the combustion tube.
2. Layer about 5mm. of quartz wool onto the platinum mesh using the catalyst filling
rod.
3. Fill the TOC standard catalyst to a height of about 100mm.

Combustion Tube

TOC Standard Catalyst

100mm

Quartz Wool

Platinum Mesh

Figure 4.1 Combustion Tube with TOC Standard Catalyst

¬TOC High Sensitivity Catalyst (H Type only)

Use the TOC high sensitivity catalyst for low level TC analysis. The blank values are
controlled to negligible levels, and analysis is performed primarily for trace TOC in pure
water (1mg/L or less).

TOC-VCPH/CPN 37
 4.1 Analysis Preparation
4.1.1 Catalyst Filling

Samples containing IC in excess of 5mg/L

The detection rate for IC decreases with increasing concentration. As a result, use the
NPOC method instead of the TC-IC method when analyzing samples that contain IC
concentrations in excess of 5mg/L.

Filling Combustion Tube with TOC High Sensitivity Catalyst

Two cylindrical containers of catalyst are required for a single load.
1. Place two sheets of platinum mesh in the combustion tube.
2. Fit together the combustion tube opening and the opened end of the cylindrical
catalyst container.
3. Use the catalyst filling rod to push catalyst into the combustion tube from the other
opened end of the cylindrical catalyst container.
4. Transfer the contents of the two cylindrical catalyst containers to achieve a catalyst
layer height of 130mm in the combustion tube.

Combustion Tube

TOC High-Sensitivity
Catalyst

130mm

Platinum Mesh

Figure 4.2 Filling of TOC Combustion Tube with High Sensitivity Catalyst

38 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.1 Catalyst Filling

4.1.1.2 TOC/TN Catalyst (Option)

TOC/TN catalyst is used for TN analysis and TOC/TN simultaneous analysis. The
detection rate is low for the IC component when it exceeds 10mg/L; as a result, TOC in
samples containing more than 10mg/L IC cannot be measured using the TC-IC method and
should be measured using the NPOC method. The furnace temperature is set to 720°C for
TOC/TN and TN analysis.

Filling Combustion Tube with Catalyst for TN Analysis

1. Insert two sheets of platinum mesh into the combustion tube.
2. Layer about 5mm of quartz wool onto the platinum mesh using the catalyst filling rod.
3. Introduce the TOC standard catalyst into the combustion tube to a height of 140mm
from the top end of combustion tube.
4. Introduce a small amount of ceramic fiber to cover the catalyst.
5. Lightly press with a catalyst filling rod so that the thickness of the ceramic fiber is
10mm.
Note: • The thickness of the ceramic fiber must be uniform, covering the entire
surface of the catalyst, or a poor TN detection rate may result.
• The filling heights of the catalyst and ceramic fiber influence the TN
detection rate, so it is important that the dimensions are close to those
indicated below.
Catalyst: 140mm from the top end of combustion tube
Ceramic fiber: 10mm

Combustion Tube

140mm
Ceramic Fiber 10mm

TOC Standard Catalyst

Quartz Wool
Platinum Mesh

Figure 4.3 Filling Combustion Tube with Catalyst for TOC/TN Analysis

TOC-VCPH/CPN 39
 4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube

4.1.2 Connecting the Combustion Tube

The procedure for installing the combustion tube differs depending on whether the
instrument is the H Type or the N Type. The procedure for each type is described below.

CAUTION
• Due to the potential for burns, maintenance of the combustion tube and catalyst
should be performed after the electric furnace temperature has cooled to room
temperature.
• When connecting the combustion tube, handle it carefully to avoid breakage. The
combustion tube is constructed of quartz glass, and injury is possible.
• Do not use a wrench or other tool. Injury could result if the combustion tube
breaks.

Installation for the H Type

1. Push the capillary end of the catalyst-filled combustion tube downward, into the
center of electric furnace (about 22mm diameter).
2. Apply an extremely thin layer of the provided high-vacuum silicone grease to the
outside of the combustion tube tip (part in contact with O-ring).
Note: Use the smallest possible amount of silicone grease. Absolutely no
grease should be applied to the interior of the combustion tube.
3. Insert the tip of the combustion tube, with the silicone grease, securely into the
opening at the bottom of the sample injector.
Note: At this point, be sure to connect the drain tubing exiting the slide
injector to the Y-fitting of the system drain line.
4. Connect the tubing at the bottom end of combustion tube, as shown in Figure 4.4
"Connecting Combustion Tube to the Compression Fitting". Push the narrow end of
the combustion tube into the compression fitting. Adjust the distance between the
bottom of the compression fitting and the base of the instrument to 1mm or less, and
then tighten the top compression fitting nut firmly by hand.

40 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube

TC Combustion Tube

Nut

Rear Ferrule Sleeve Set 6F-T

Front Ferrule (P/N 035-62994-03)

TC Combustion Tube

Stainless Tubing
(toward detector)

Compression Fitting

Figure 4.4 Connecting Combustion Tube to the Compression Fitting

CAUTION
• The instrument is sealed sufficiently if the combustion tube does not move when
pulled upwards.
• The quartz glass combustion tube will break if the compression fitting is over-
tightened.
• Use only the provided Teflon ferrules for the front and rear ferrules. Do not use
any other material, such as metal.
• Do not allow organic contaminants such as grease or oil to touch the inner or
outer surfaces on the tip of the combustion tube and gas connection parts of the
ferrules. This is especially important for high sensitivity analysis.

TOC-VCPH/CPN 41
 4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube

Combustion
Tube

Figure 4.5 Connecting the Combustion Tube

5. Secure the sample injector with the knurled thumbscrew.

Knurled
Thumbscrew

Figure 4.6 Securing the Sample Injector

6. To prevent heat escape from the furnace, pack the space around the capillary part of
the combustion tube with the provided ceramic fiber.

CAUTION
Use caution to avoid inhaling ceramic fibers when inserting the fibers into the
combustion tube.

42 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube

7. Verify that the gap between the adjustable base at the bottom of the instrument and the
bottom-most part of the compression fitting is 1mm or less (preferably no gap).
8. If the gap is too large, loosen the nut at the top of the compression fitting and pull the
combustion tube upwards. Since the TC combustion tube is inserted into the
compression fitting, pulling up on the combustion tube shortens the insertion length
and ultimately lowers the compression fitting assembly. When almost no gap remains,
firmly tighten the nut at the top of the compression fitting.
Note: The sample rapidly vaporizes in the combustion tube when injected
in large quantities with a gap present between the bottom-most part
of the compression fitting and the base of the instrument. The
pressure increases, resulting in a separation at the connection
between combustion tube and sample injector.

Installation for the N Type

1. Push the capillary part of the catalyst-filled combustion tube downward into the
center of electric furnace (about 22mm diameter).
2. Apply an extremely thin layer of the provided high-vacuum silicone grease to the
outside of the combustion tube tip (part in contact with O-ring).
Note: Use as small amount of silicone grease as possible. Absolutely no
grease should be applied to the interior of the combustion tube.
3. Insert the silicone grease coated tip of the combustion tube into the opening at the
bottom of the sample injector.
Note: Connect the drain tubing exiting the slide injector to the Y-fitting of
the system drain line.
4. Connect the tubing at the bottom of the combustion tube, as shown in Figure 4.7
"Connecting the Combustion Tube".

CAUTION
• The instrument is sealed sufficiently if the combustion tube does not move when
it is pulled upwards.
• The quartz glass combustion tube will break if the compression fitting is over-
tightened.
• Do not allow organic contaminants such as grease or oil to touch the inner or
outer surfaces on the tip of the combustion tube and gas connection parts of the
ferrules. This is especially important for high sensitivity analysis.

TOC-VCPH/CPN 43
 4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube

Combustion
Tube

Figure 4.7 Connecting the Combustion Tube

5. Secure the sample injector with the knurled thumbscrew, as shown in Figure 4.8
"Securing the Sample Injector".

Knurled
Thumbscrew

Figure 4.8 Securing the Sample Injector

6. To prevent heat escape from the furnace, pack the space around the capillary part of
the combustion tube with the provided ceramic fiber.

CAUTION
Use caution to avoid inhaling ceramic fibers when inserting the fibers into the
combustion tube.

44 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.3 Installing the Syringe

4.1.3 Installing the Syringe

This section describes the procedure for attaching the syringe to the syringe pump
assembly.
Depending on the instrument status, flow lines are connected to each of the 8 ports of the
syringe pump valve. If the syringe is installed or removed without following the sequence
described below, acid can be released from the syringe connection port. The sequence
described below must be followed.

CAUTION
• Due to the potential for injury, keep hands away from the sample injector during
operation of the syringe pump unit.
• The syringe barrel is made of glass and must be handled carefully to avoid break-
age.

Syringe Installation
1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>Change Syringe.
The Syringe Change dialog box is displayed.

Figure 4.9 Syringe Change Dialog Box

3. Click the Preparation Start button to begin the procedure. A progress bar is active
while the syringe moves to the position where it can be replaced.
4. When the progress bar begins blinking, remove the screw at the bottom of the syringe
pump cover, and remove the cover.
5. Remove the sparge gas line from the syringe.
6. Remove the syringe from the syringe connection port of the 8-port valve.
7. Attach the new syringe to the syringe connection port of the 8-port valve.

TOC-VCPH/CPN 45
 4.1 Analysis Preparation
4.1.3 Installing the Syringe

8. Connect the sparge gas line to the syringe using the bushing and spacer.
Note: Do not use tools when replacing the syringe; hand-tighten only.
Over-tightening can deform the components of the 8-port valve and
result in leaks.

Syringe

Plunger
Retaining
Screw

Figure 4.10 Installing the Syringe

9. Verify that the syringe moves smoothly between the upper and lower positions by
clicking the directional arrows on the Syringe Change dialog box.
10. With the syringe in this position, hand-tighten the plunger retaining screw on the
plunger holder.
11. Click the Finish Replacement button to move the syringe to its initial position.
12. Click the Close button.
Note: Once the syringe is installed, perform the syringe pump zero point
detection operation.See Section 4.1.3.1 "Syringe Pump Zero Point
Detection" for details.

46 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.3 Installing the Syringe

4.1.3.1 Syringe Pump Zero Point Detection

This section describes the procedure for performing automatic detection of the syringe
pump zero point.
Note: Perform the zero point detection procedure whenever a new syringe is installed
or the syringe is replaced.

Procedure
1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>Zero Point Detection.
The Zero Point Detection dialog box is displayed.

Figure 4.11 Zero Point Detection Dialog Box

3. Click the Start button.

A progress bar is active while the syringe moves to the position where the zero point
can be detected. When the progress bar stops blinking, the procedure is complete.
4. Click the Close button.

TOC-VCPH/CPN 47
 4.1 Analysis Preparation
4.1.4 Water Supply to the Cooler Drain Container

4.1.4 Water Supply to the Cooler Drain Container

The drain container must be filled with water to prevent carrier gas from being released
from the drain tubing.

Procedure
1. Remove the rubber cap from the drain container.
2. Remove the drain container from the mounting clip.
3. Introduce pure water (deionized water is acceptable) into the cooler drain container up
to the level of the drain discharge tube on the side of the container.
4. Cap the drain container with the rubber cap.
5. Return the drain container to its position in the mounting clip.
6. Verify that the cooler drain tube reaches to the bottom of drain container.

CAUTION
Do not bend drain tubing, as this may prevent drain discharge.

Rubber Cap Drain Discharge Tube

Drain Tubing

Mounting Clip

Drain Container

Pure Water

Figure 4.12 Filling the Cooler Drain Container with Water

48 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.5 Filling the Humidifier with Water

4.1.5 Filling the Humidifier with Water

The carrier gas must be humidified for high sensitivity analysis to ensure high analysis
precision. Water is supplied to the humidifier using the following procedure.

Procedure
1. Remove the cap from the water supply port at the top of the humidifier.
2. Introduce water through the water supply port to the “Hi” marking on the side of the
humidifier.
Note: Use pure water containing as little TC as possible for high
sensitivity analysis.

Water Supply
Port

Pure Water
Humidifier

“Hi” Marking

Figure 4.13 Filling the Humidifier with Water

TOC-VCPH/CPN 49
 4.1 Analysis Preparation
4.1.6 Preparation of Dilution Water

4.1.6 Preparation of Dilution Water

This section describes the preparation of water used to automatically dilute samples.

Procedure
1. Wash the provided dilution water bottle with laboratory glassware detergent, rinse
well with tap water, then wash a number of times with pure water.
2. Fill the container with pure water to the 2 liter level.
3. Place the container to the left of the instrument, toward the rear.
4. Pass the dilution water intake tubing, labeled DILUTION, through the hole in the cap.
5. Secure the tubing, using a wire clamp about 200mm from the end of the tubing, to
prevent the tubing and cap from separating.
6. Place the cap on the container.
Note: Verify that the tip of the intake tubing nearly reaches the bottom of
the container.

Dilution Water
Intake Tubing

Dilution Water
Bottle

Figure 4.14 Preparing Dilution Water

Note: About pure water:

• Use the purest water that can be obtained.
• Refer to Section 4.1.14.1 "Preparation of Standard Solutions" for details on
the degree of purity of “pure water”.

50 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.7 Acid Preparation

4.1.7 Acid Preparation

This section describes the preparation of acid used for IC removal in NPOC analysis or for
IC analysis with the N Type instrument.

Procedure
1. Prepare 2 M HCl by diluting 1 part commercially available concentrated HCL (12 M)
with 5 parts pure water. A final concentration accuracy of ±2% is acceptable.
Note: The pure water used as the diluent must have a TOC concentration
no greater than 0.5 mg/L. Since the TOC value of the diluent pure
water can have a large effect on the analysis result with high
sensitivity analysis (low TOC concentrations), it is necessary to use
pure water having a very low TOC concentration.

CAUTION
Hydrochloric acid is a hazardous chemical. Use precautions to avoid contact when handling
this substance. For details, refer to Section 6.9 "Material Safety Data Sheets".

2. Transfer the prepared acid to the 250 mL bottle provided as a standard accessory, and
place it to the left of the instrument, toward the front.
3. Pass the acid intake tubing through the hole in the cap.
4. Secure the tubing, using a wire clamp about 100mm from the end of the tubing, to
prevent the tubing and cap from separating.
5. Place the cap on the container.
Note: Verify that the tip of the acid intake tubing nearly reaches the
bottom of the container.

Acid Intake Tubing

Cap

Hydrochloric Acid
Container

Figure 4.15 Acid Preparation

TOC-VCPH/CPN 51
 4.1 Analysis Preparation
4.1.8 Installation of the CO2 Absorber

4.1.8 Installation of the CO2 Absorber

A CO2 absorber is used to remove CO2 from the carrier gas that purges the optical system
of the detector. The CO2 absorber is installed using the following procedure.

Procedure
1. Cut the tips of the 2 rigid tubes in the lid of the CO2 absorber with a knife.
2. Connect the flexible tubing that exits the rear panel of the instrument (near the top) as
follows:
Tubing labeled “L”: Connect to tube labeled “L” on CO2 absorber.
Tubing labeled “S”: Connect to tube labeled “S” on CO2 absorber.
Note: The flexible tubing should not be bent.
3. Place CO2 absorber in the holder behind the instrument.

Flexible Tubing

Rigid Tubes

CO2 Absorber

Figure 4.16 Installation of the CO2 Absorber

52 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.9 Adjusting Sparge Gas Flow Rate

4.1.9 Adjusting Sparge Gas Flow Rate

The sparge gas flow rate should be adjusted before sparging is performed using the optional
external sparge kit. The procedure for adjusting the sparge gas flow rate is described below.

Procedure
1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>Sparge Gas Valve.
The sparge gas solenoid valve opens and sparge gas begins to flow.
3. Open the front door of the instrument.
4. Adjust the flow rate to about 100mL/min using the sparge gas flow rate adjustment
knob.
Note: The flow rate should be adjusted according to the size and shape of
the sample container.
5. Close the front door of the instrument.

Sparge Gas Flow

Rate Adjustment Knob

Halogen
Scrubber

Figure 4.17 Sparge Gas Flow Rate Adjustment

TOC-VCPH/CPN 53
 4.1 Analysis Preparation
4.1.10 Installing the Suspended Solids Kit

4.1.10 Installing the Suspended Solids Kit

To analyze samples containing suspended solids, the sample flow line diameter can be
increased from 0.5mm to 0.8mm by installing the optional Suspended Solids Kit.
This section describes the installation of the Suspended Solids Kit.
There are two kits available:
(1) For TOC-V (TOC-V main unit only)
(2) For TOC-V+ASI-V (used with TOC-V and autosampler)

CAUTION
Switch OFF the TOC-V before attempting to install the Suspended Solids Kit.

¬Replacing the Flow Line Parts and Slider

This procedure is used for both kits.

Procedure
1. Remove the bushing from port 7 of the 8-port syringe pump valve, and disconnect the
TC injection tubing. For the H-type, remove the bushing from port 5, and disconnect
the IC injection tubing.
2. Remove the slider mounting screws from the TC and IC injection blocks, and detach
the sliders.
3. Remove the slider bushings and replace the sample injection tubing with the 0.8mm
diameter sample injection tubing provided in the kit.
4. Reinstall the sliders on the sample injection blocks.
5. Connect the TC injection tubing and the IC injection tubing to port 7 and port 5,
respectively.
Note: During analysis, verify that the sample flow is normal. Refer to
Section 5.7.2.4 "Corrective Actions for Poor Reproducibility"
If the sample stream is not normal, the tip of the Teflon tube may be
deformed or scratched. Use a knife to cut off a portion of the tube.

54 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.10 Installing the Suspended Solids Kit

¬Replacing Sample Tubing

For TOC-V (TOC-V main unit only)

1. Remove the bushing from port 1 of the 8-port syringe pump valve and replace the
sample tubing with the 0.8mm diameter tubing provided in the kit.
2. Connect the new sample tubing to the 8-port valve in the original position.

For TOC-V+ASI-V (TOC-V and autosampler)

Refer to Section 6.8.4 "Installing the Autosampler" to remove the autosampler sample
needle and sample tubing. Replace these with the sample needle and tubing provided in the
Suspended Solids Kit.

Precautions for Measuring Suspended Solids

When performing measurement of solid samples using the Suspended Solids
Measurement kit, follow the precautions below to ensure the best possible
conditions for measurement. Refer to Section 4.1.15.4 "Analysis of Samples
Containing Suspended Solids".
• Before measurement, use a homogenizer, etc. to make the sample as uniform as
possible. After homogenizing the sample, depending on the type of suspended
substance, precipitation and coagulation may occur after a period of time. Prior
to measurement, mix the sample again using a magnetic stirrer to ensure that pre-
cipitated/coagulated material is well dispersed throughout the sample.
• If the suspended material is present in large quantities, clumping of the material
and obstruction may occur inside the sample flow line even if the particles are of
smaller diameter that the sample flow line diameter. Take measures such as sam-
ple dilution to prevent flow line obstruction,
• The suspended solids measurement kit employs a 0.8mm Teflon tube for sample
injection. Diminished reproducibility may occur with small sample injection vol-
umes. Make injection volumes as large as possible.
• When conducting IC measurement of suspended solid samples using the H type
instrument, obstruction of the IC measurement flow line drain tube may occur.
Sufficiently pulverize the suspended particles to allow free flow through the
drain tube.

TOC-VCPH/CPN 55
 4.1 Analysis Preparation
4.1.11 IC Analysis Preparations

4.1.11 IC Analysis Preparations

Certain preparations are necessary for the H Type instrument. These include installing and
replenishing the IC reagent in the IC reaction vessel. This section describes the procedures
for installing and replenishing the IC reagent.

CAUTION
The IC reagent contains phosphoric acid. Use care while handling to prevent contact or
spills. For details, refer to Section 6.9 "Material Safety Data Sheets".

¬Preparing and Placing the IC Reagent

Procedure
1. Prepare the IC reagent by diluting 50 mL of commercial 85% phosphoric acid (ACS
Reagent grade) to a final volume of 250 mL with pure water.
Note: Since the specific gravity of 85% phosphoric acid is about 1.7, the
concentration of the phosphoric acid is about 25% (weight%) in the
prepared IC reagent. A final concentration accuracy of ±2% is
acceptable.
2. Transfer the prepared acid to the 250 mL bottle provided as a standard accessory, and
place it on the left side of instrument, toward the front.
3. Pass the tip of the IC reagent tubing through the hole in the cap.
4. Secure the tubing, using a wire clamp at a point about 100mm from the end of the
tubing tip, to prevent the tubing and cap from separating.
5. Replace the cap on the container.

56 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.11 IC Analysis Preparations

¬Replenishing IC Reaction Vessel with IC Reagent

Use the following procedure to replenish the IC reagent.

Procedure
1. Verify that the lever of the 3-way valve at the bottom of the IC reaction vessel is
positioned to the left as shown in Figure 4.18 "Lever Position of IC Reaction Vessel 3-
Way Valve".

Figure 4.18 Lever Position of IC Reaction Vessel 3-Way Valve

2. Open the TOC-Control V Sample Table Editor and connect the instrument.
3. From the Instrument menu, select Maintenance>Regeneration of the IC solution.
The Regeneration of IC solution dialog box is displayed.

Figure 4.19 Regeneration of IC Solution Dialog Box

4. Click the Start button. The IC reagent will be delivered to the IC reagent vessel by the
liquid delivery pump. During the process, the Start button is disabled.
5. A progress bar is active until the IC reagent is completely regenerated. Click the Close
button.

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 4.1 Analysis Preparation
4.1.12 Preparation for POC analysis

4.1.12 Preparation for POC analysis

POC analysis can be performed if the optional POC analysis kit is installed on the
instrument. This section describes preparations required for POC analysis.

Installation of the CO2 Absorber for POC Analysis

1. Remove the CO2 absorber.
2. Insert about 5mm of quartz wool into the bottom of the container.
3. Add commercially available anhydrous lithium hydroxide to the container on top of
the quartz wool until it reaches just below the screw threads of the container.
Note: About 6g of anhydrous lithium hydroxide is required for a single
load.
4. Place about 5mm of quartz wool on top of the lithium hydroxide.
5. Attach the O-ring and nipple to the top of the container, and firmly tighten the cap.
6. Install the CO2 absorber for POC analysis in the original position.

CAUTION
• Lithium hydroxide is a corrosive (strongly basic) powder. Use care when han-
dling to prevent contact or inhalation. Refer to Section 6.9 "Material Safety Data
Sheets" for details.
• Lithium hydroxide is available in anhydrous and hydrated forms. Since the abil-
ity of the hydrated form to absorb carbon dioxide is slightly inferior to that of the
anhydrous form, use anhydrous lithium to fill the CO2 absorber container.
• When introducing the quartz wool and lithium hydroxide into the container, do
not pack too tightly.
• The CO2 absorber container is constructed of glass. Handle it carefully to prevent
breakage.

Cap

Nipple

O-Ring

Lithium Hydroxide
Quartz Wool

Figure 4.20 Preparing the CO2 Absorber for POC Analysis

58 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.13 TN Analysis Preparations

4.1.13 TN Analysis Preparations

TN analysis can be performed if the optional TN unit is installed on the instrument. The
NOx absorber also must be connected to perform TN analysis. The CO2 absorber (soda
lime) is used as the NOx absorber. Connect it to the instrument using the following
procedure.

Procedure
1. Cut the tips of the rigid tubes (2) in the lid of the CO2 absorber with a knife.
2. Connect the Viton tubing to the 2 rigid tubes as follows:
Tubing labeled “L”: Connect to tube labeled “L” on the CO2 absorber.
Tubing labeled “S”: Connect to tube labeled “S” on the CO2 absorber.
3. Place the NOx absorber behind the instrument.

Viton Tubing

TN Unit

Rigid Tubing

Figure 4.21 Connecting the NOx Absorber

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 4.1 Analysis Preparation
4.1.14 Preparation and Storage of Standard Solutions

4.1.14 Preparation and Storage of Standard Solutions

4.1.14.1 Preparation of Standard Solutions

Zero water refers to a standard solution with zero concentration of TC, IC or TN; zero
water also refers to the water used to prepare these standard solutions. Water that is, in
theory, absolutely free of carbon (TC) or nitrogen (TN) is used as zero water. In practice, it
is difficult to obtain this type of water. Even ultra-pure water obtained using a high-
performance membrane technique and water that has been repeatedly distilled will have a
TC content of about 10µg/L. This value is measured directly after manufacture, and
increases when the water is stored in a container. Carbon dioxide is contained in the
atmosphere at concentrations ranging from 300 to 500mg/L. The CO2 content of ambient
air is higher in a room with many people or where combustion equipment is used. Carbon
dioxide in ambient air dissolves in stored water, taking the form of IC. The dissolved
amount is generally about 0.2mg/L, but depends on the water temperature and carbon
dioxide content of the air in contact with the water. Refer to Table 6.2 • "CO2 Content
(ppm) in Distilled Water Equilibrated with Atmosphere Temperature (°C)". Instruments
that prevent contact with air are not incorporated in water uptake, retention or storage
processes during common distillation and purification of water. For this reason, IC is
present in most types of distilled and purified water. In some cases, the TC content of
commercially-available distilled water stored in plastic or glass containers is 1ppm.
Note: The degree of purity required varies depending on the analysis range. Use of
commercially-available purified water is acceptable when measuring samples
with expected TC concentrations around 100ppm. The quality of the zero water
should be considered along with the analysis range.

Preparation of TC Standard Solutions

1. Accurately weigh 2.125g of reagent grade potassium hydrogen phthalate that was
previously dried at 105-120°C for about 1 hour and cooled in a desiccator.
2. Transfer to a 1 L volumetric flask and dissolve in zero water.
3. Add zero water to the 1 L mark, and stir the solution.
The carbon concentration of the solution is 1000mgC/L (1000mgC/L = 1000ppmC).
This solution is the standard stock solution.
Note: The standard stock solution may be prepared at other
concentrations. For example, a 2000mgC/L solution can be used as
the standard stock solution.
4. The standard stock solution is diluted with zero water to prepare standard solutions at
the required concentrations.
Note: The TC standard solution reagent need not be potassium hydrogen
phthalate. Depending on the application, other substances are also
acceptable (e.g., sucrose, etc.).

60 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.14 Preparation and Storage of Standard Solutions

Preparation of IC Standard Solution (HV)

1. Accurately weigh 3.50g of reagent grade sodium hydrogen carbonate that was
previously dried for 2 hours in a silica gel desiccator, and 4.41g of sodium carbonate
previously dried for 1 hour at 280-290°C and cooled in a desiccator.
2. Transfer the weighed materials to a 1L volumetric flask.
3. Add zero water to the 1L mark.
4. Stir well to mix.
In this instance, the carbon concentration of 1000mg/L is indicated as 1000mgC/L.
The concentration of this solution is 1000mgC/L (1000ppmC) and is referred to
below as the “TC Standard Solution”.

Preparation of TN Standard Solution

1. Accurately weigh 7.219g of special reagent grade potassium nitrate dried for 3 hours
at 105-110°C and cooled in a desiccator.
2. Transfer the weighed material to a 1L volumetric flask.
3. Add zero water to the 1L mark.
4. Stir well to mix.
In this instance, the nitrogen concentration of 1000mg/L is indicated as 1000mgN/L.
The concentration of this solution is 1000mgN/L (1000ppmN) and is referred to
below as the “TN Standard Solution”.

Preparation of POC Standard Solution (using the optional POC analysis kit)
IC standard solution is used as the POC standard solution with this instrument for the
following reasons.
• In POC analysis, the measured substance is an organic material that is volatile and
poorly soluble in water (for example, benzene or chloroform). Preparing a stan-
dard solution at an appropriate concentration using these types of organic sub-
stances is difficult.
• Volatile and poorly soluble organic substances tend to undergo changes in concen-
tration during storage or handling after preparation.
• Standard solutions that are produced using volatile and poorly soluble organic sub-
stances are difficult to use.
Consequently, the IC standard solution is used for this instrument. The preparation
method is listed above.

TC/TN Mixed Standard Solution Preparation Procedure

When TC (or NPOC) and TN analyses are performed simultaneously, a mixed TC and
TN standard solution is prepared.
The mixed standard solution is prepared by mixing the TC standard solution and TN
standard solution. The mixed standard solution must contain 0.05M hydrochloric
acid.

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 4.1 Analysis Preparation
4.1.14 Preparation and Storage of Standard Solutions

Preparation of 100mgC/L TC - 100mgN/L TN Mixed Standard Solution

1. Prepare 1L of 1000mgC/L TC standard solution using the preparation method
described above.
2. Prepare 1L of 1000mgN/L TN standard solution using the preparation method
described above.
3. Introduce 100mL of each of the prepared standard solutions into a 1L volumetric
flask.
4. Add 25mL of 2M hydrochloric acid to the flask
5. Add zero water to the 1L level.
6. Stir well to mix.
The hydrochloric acid concentration will be about 0.05M after dilution.

4.1.14.2 Storage of Standard Solutions

The standard solutions undergo concentration changes, particularly when low-

concentration solutions are stored even for short periods. As a result, high-concentration
standard stock solutions (for example, 1000mgC/L) should be stored in airtight containers
in a cool, dark place. Glass bottles are suitable storage containers. Dilute the stock solution
prior to each use.

Storage Time
The limitation on storage of standard solutions is about 2 months for 1000mgC/L standard
stock solutions and about 1 week for diluted standard solutions (for example, 100mgC/L).
The limitations are for cold storage in sealed containers.
Note: IC standard solution absorbs atmospheric carbon dioxide and undergoes concen-
tration changes. As a result, it is particularly important to store IC standard solu-
tion in a sealed container.

Prepare fresh standard solutions:

• If reproducibility of analysis values is poor or concentration fluctuates.
• If contaminants, including even small amounts of dust, are present in the standard
solution.

62 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.15 Sample Preparation

4.1.15 Sample Preparation

4.1.15.1 High Sensitivity Analysis

High sensitivity analysis refers to use of the high sensitivity analysis kit to measure trace
amounts (commonly 0.5mg/L or less) of TOC in samples such as ultra-pure water. The
precautions described in the sections below should be followed when conducting trace
analysis on the order of 10 - 100µg/L.

Precautions for High Sensitivity Analysis

• Use TOC high sensitivity catalyst.
Carefully fill the combustion tube with high sensitivity catalyst to prevent contamina-
tion of the combustion tube. Measuring high-concentration samples using TOC high
sensitivity catalyst that is intended for the analysis of ultra-pure water will influence the
results of subsequent analyses on ultra-pure water samples. This is primarily caused by
remaining sample residue. The residue may be removed by running repeated analyses of
zero water.
Since removal is difficult with residual salt, alkali or highly acidic samples, a separate
combustion tube containing TOC high sensitivity catalyst should be prepared for use
only with ultra-pure water samples.
Verify that both ends of the combustion tube are sealed when storing catalyst that is to
be used only for ultra-pure water samples.
• Measure samples immediately.
Samples containing trace carbon (such as ultra-pure water) should be measured immedi-
ately after collection. If analysis cannot be performed immediately, store the sample in a
dark location at 0-10°C (without freezing) and perform analysis as soon as possible.
To collect the water, introduce water into a well-washed container, leaving no head-
space, and seal the container.
• Use glass sample containers.
Glass containers are optimal for samples containing trace carbon. Commercially-avail-
able 500mL to 1 L glass screw-lid jars with Teflon seals (generally referred to as heat-
resistant screw-top jars or hermetic jars) are appropriate for use as water collection and
transport containers.
Note: Exercise caution with plastic containers, as elution of TOC-
containing components can occur.

TOC-VCPH/CPN 63
 4.1 Analysis Preparation
4.1.15 Sample Preparation

• Use NPOC analysis for ultra-pure water samples.

Use the NPOC method for analysis of ultra-pure water samples. Measuring TOC in
ultra-pure water samples by using the difference between TC and IC is prone to large
analysis errors for the following reasons:
• The TOC value is significantly affected since a large portion of TC often comprises
IC. Errors in TC analysis and IC analysis are additive.
• Carbon dioxide is absorbed from the atmosphere during sample collection and anal-
ysis. During the elapsed time between TC analysis and IC analysis, the sample
absorbs more carbon from the atmosphere, causing the IC result to be higher than the
IC content in the TC result. As a result, subtracting the elevated IC result from the
TC result yields a biased TOC value.
• The TOC value can also be greatly influenced if standard solutions are not prepared
and measured carefully. Errors are compounded since two calibration curves must be
generated for TC and IC.
• The calibration curves are used in sample analysis by extending a two-point calibra-
tion curve through the origin.
• In NPOC analysis, POC may be volatilized from the sample during sparging for IC
removal. This is not a problem since the ultra-pure water contains practically no
POC.

Cautions in Calibration Curve Generation and Sample Measurement Using High

Sensitivity Analysis
The case below describes the generation of a 2-point calibration curve shifted through the
origin. The calibration standard concentrations are 0µg/L and 400µg/L.

Preparation of Standard Solutions

A 2-point calibration curve using 0µg/L and 400µg/L is generated. The calibration curve is
shifted through the origin to correct for the TC contained in purified water used for
preparation of the standard solutions.
The 0µg/L and 400µg/L TC standard solutions should be prepared at the same time using
the same purified water. Wash well, two 250mL volumetric flasks with purified water
(preferably water containing low TC concentration). Carefully introduce 1mL of 100mg/L
TC standard stock solution (for a 400µg/L solution) into one of the volumetric flasks.
Distilled water is introduced up to the graduation line in both volumetric flasks.
Standard preparation procedures should be performed as quickly as possible, using caution
to avoid inclusion of external contaminants. If a water purification apparatus is the source
of purified water, allow the water to flow for a few minutes prior to use, as the initial water
will have a higher TC concentration. Alternate the flasks a number of times while filling
them with water to equalize, as much as possible, the TC concentration of the purified
water.
Use fresh purified water when filling the volumetric flask to the graduation line. Do not use
rinse bottle water that has been standing for a long period of time because the TC
concentration continually increases with time.

64 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.15 Sample Preparation

Instrument Preparation
The blank peaks present at the start of high sensitivity analysis will become progressively
smaller and gradually stabilize. As a result, calibration curves generated too soon after the
start of analysis may be inaccurate because they contain data collected during unstable
conditions. To prevent this problem, perform 5 or more measurements of purified water
containing 2-3 drops of 1M HCl per 100mL of water prior to analyzing the calibration
standards. Use the same measurement parameters (injection volume, sparge time) that will
be used for the calibration standards and samples.

Calibration Curve Analyses

Calibration curves are generated using the following two methods.
(1) Using standard solution in a 250mL volumetric flask
Insert the sample tubing directly into the volumetric flask until it reaches the bottom
of the flask. Perform analyses quickly. Four to five repeated analyses can be made
with almost no effects from the absorption of atmospheric carbon dioxide. Cover the
opening of the volumetric flask with sealing film or paraffin to prevent contamination.
Use this method when the IC value of the purified water used for standard solution
preparation (specifically, 0µg/L standard solution) is about 50µg/L or less.
(2) Sparging the standard solution
To sparge in the sample injection syringe, set the acid addition ratio to 0.5%, and the
sparge time to 2 minutes. To sparge using the optional external sparge kit, transfer
about 60mL of the standard solution to a clean sample container, add 1-2 drops of 2M
hydrochloric acid, sparge for 10 minutes and analyze.
Cover the sample container with paraffin or sealing film to prevent contamination. A
glass container with an external diameter of 24-25mm and a height of 200-250mm is
appropriate. Test tubes, stopper-equipped test tubes and chromatography tubes of
suitable size are available commercially. If the outer diameter of the container is too
large, the air-to-water contact efficiency is decreased, requiring a longer sparge time.
Ensuring that the tip of the sparge tube is near the bottom of the container will
improve the sparging efficiency.

Reference: Refer to Section 4.3.2 "Tutorial" and Section 4.4.2.2 "Calibration Curve" for detailed
descriptions of generating calibration curves using the TOC-Control V software.

Sample Analysis
Use the calibration curve generated in the previous section to measure NPOC in the sample.
Measure the sample using the same method used for the calibration standards. If the values
gradually decrease with each repeated analysis using the optional external sparge kit,
extend the sparge time to ensure sufficient sparging. The shape of the sample container, the
sample amount, the amount of sparge gas and the IC content of the sample all have a
bearing on the required sparge time. Determine the appropriate sparge time in accordance
with these parameters.

Reference: Refer to Section 4.3.2 "Tutorial" and Section 4.4.5.2 "Sample" for detailed descriptions of
conducting sample analysis using the TOC-Control V software.

TOC-VCPH/CPN 65
 4.1 Analysis Preparation
4.1.15 Sample Preparation

4.1.15.2 TC Blank Check Analysis

A TOC system invariably contains substances in the instrument flow lines that produce
peaks. These peaks are referred to as blank values or system blank values, and are present
even in water samples containing absolutely no carbon. The magnitude of peaks in the
blanks differs based on various factors such as system construction and the catalyst used.
For the TOC-V, every effort has been made to minimize these peaks, which can affect the
accuracy of TC analyses. Accuracy is particularly affected when trace TOC is measured
(such as in high sensitivity analysis of ultra-pure water samples); for this type of analysis,
the blank peaks must be small and stable. To check and correct for the magnitude of the
system blank peaks, use the TOC-Control V Blank Check procedure described below.
Note: • The Blank Check procedure is available only when the high sensitivity
catalyst is used.
• The Blank Check procedure takes approximately 8 hours to complete and
does not require continuous monitoring by the user. As a result, performing
the procedure overnight is recommended.
• Blank values measured during the Blank Check procedure should rapidly
decrease in magnitude and stabilize. If the instrument flow lines, syringe
pump interior, or catalyst have been contaminated, the blank values will not
rapidly decrease. In such instances, the Blank Check procedure should be
repeated.
• Blank peaks are negligible in the IC analysis flow line. The IC value will be
zero if the water is acidified and sparged. This can easily be confirmed by
conducting analysis using the IC flow line; however, this is not normally
necessary. Consequently, there are no special IC flow line check procedures,
as with the TC blank check.

66 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.15 Sample Preparation

Blank Check Procedure

1. Open the TOC-Control V Sample Table Editor and create a blank Sample Table for
the high sensitivity system.
Note: Do not insert a sample into the Sample Table. The Blank Check
procedure only works in an empty Sample Table.
2. Connect the instrument by selecting Connect from the Instrument menu.
3. From the Instrument menu, select Maintenance>Blank Check.
The Blank Check Parameters dialog box is displayed.

Figure 4.22 Blank Check Parameters Dialog Box

4. Enter the desired injection volume, and click the Start button.
The Standby dialog box is displayed.

Figure 4.23 Standby Dialog Box

5. Select an option to determine the condition of the instrument after the blank check is
complete. Options are:
• Keep running
• Shut down instrument
• Auto Restart (TC furnace, carrier gas, restart time)
6. Fill the dilution water bottle to full capacity with purified water, and place it in the
specified position. About 200mL of dilution water is used for the blank check
measurement.
7. Click the Standby button.
The Save As dialog box is displayed.
8. Enter a file name and click the Save button. Data from the Blank Check procedure
will be stored in the created file.
Blank check analysis begins. The procedure that the instrument executes is described
below.

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 4.1 Analysis Preparation
4.1.15 Sample Preparation

Description of TC Blank Check Analysis Procedure

1. Washing the inside of the trap
First, the trap is washed with water from the dilution water bottle. A 6mL aliquot from
the dilution water bottle is drawn into the ultra-pure water trap and the trap is emptied.
This step is repeated using another 6mL aliquot from the dilution water bottle.
Next, the trap and the system is washed with ultra-pure water. The ultra-pure water
used to wash the trap is created when a 2mL aliquot of water from the dilution water
bottle is injected through the TC injector and onto the catalyst. The ultra-pure water
resulting from the analysis fills the trap and is then drawn into the syringe and
discharged a total of 4 times.
2. Preparation of purified water for blank check
The ultra-pure water that will be used for the Blank Check procedure is created as
follows: Six 2mL aliquots of water from the dilution water bottle are injected through
the TC injector and onto the catalyst. The ultra-pure water resulting from the analysis
is caught in the ultra-pure water trap. Water in the trap is further purified by injecting
it onto the catalyst five more times in 2mL aliquots.
3. Blank check analysis
Using the ultra-pure water created in Step 2 and caught in the purified water trap, TC
analysis is conducted 5 times. The results of each analysis are stored in the data file.
Steps 2 and 3 are then repeated 9 more times.
Note: The magnitude and stability of the system blank value can be
evaluated from the blank check results. If the blank value is not
stable, repeat the Blank Check procedure until the magnitude of the
blank peak stabilizes.

4.1.15.3 Pretreatment for IC Removal (Sparging)

Errors for TC and IC analyses are additive. For samples that have a comparatively large IC
concentrations relative to TOC concentrations, the TOC analysis error is large if it is
determined by the difference between TC and IC results. Samples of this type include
samples from water treatment facilities or from the natural environment, such as rivers,
lakes, swamps, oceans and groundwater.
Using the difference between TC and IC to determine TOC is not appropriate for purified
water or ultra-pure water samples. The CO2 in air dissolves in the sample and is measured
as IC, causing the concentration to vary.
In such cases, the sample is pretreated with aeration or sparging before analysis to remove
the IC. The sample is then subjected to TC analysis, immediately followed by TOC
analysis using the NPOC method.

Sparge Sequence
There are two methods for sparging with this instrument.
(1) Sparging in the sample injector syringe
This is performed only when the instrument is set for automatic sparging before
analysis.

68 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.15 Sample Preparation

(2) Independent sparging of sample using the optional external sparge kit
Sample is introduced into a clean sample container, acidified, and then sparged.
A glass container with an external diameter of 24-25mm and a height of 200-250mm
is appropriate for use as the sample container. Test tubes, stopper-equipped test tubes
and chromatography tubes of suitable size are available commercially. If the outer
diameter of the container is too large, the air to water contact efficiency is decreased,
requiring a longer sparge time.

Sparge Procedure
1. Refer to Section 4.1.9 "Adjusting Sparge Gas Flow Rate" for the sparge gas delivery
procedure.
2. Add 2M hydrochloric acid to the sample to adjust the pH to 2-3.
3. Insert the sparge tubing into the sample.
To improve the sparging efficiency, the tip of the sparge tubing should be as close to
the bottom of the sample container as possible.
Note: In this method, sparge gas can be used independently. While the first sample is
being measured, another sample can be sparged, thereby improving analysis effi-
ciency.

4.1.15.4 Analysis of Samples Containing Suspended Solids

Effect on Analysis
Large variations sometimes occur in TOC analyses of samples containing suspended solids
because TOC is often contained in the suspended material. This effect is evident when the
same sample is analyzed on two different TOC analyzers. Good results are not obtained if
the suspended solids are handled differently in the gathering of biochemical oxygen
demand (BOD) and TOC correlative data.
The suspended solids described here are primarily considered impurities in the sample that
will pass through a 50 mesh strainer (openings of approximately 0.28mm). When larger
solid particles are present, analysis should be performed without drawing water into the
instrument.
The procedure described below is for TOC analysis, but is also valid for TN analysis.

Analysis Restrictions
Since Teflon tubing with an inner diameter of about 0.5mm is used in the instrument for
injecting the sample, suspended solids that do not pass through cannot be measured.
Analysis reproducibility is poor for samples that do not uniformly contain such solids even
if they should pass through the tubing.
Solids that are heavy and readily form sediment, such as silt, can accumulate at the bottom
of the syringe. This can scratch the rotor of the sample injector 8-port valve, causing leaks.
Sedimentation and separation should be performed to as great an extent as possible prior to
analysis.

TOC-VCPH/CPN 69
 4.1 Analysis Preparation
4.1.15 Sample Preparation

Countermeasures
The following types of processing operations are normally used for measuring samples
containing suspended solids.
(1) TOC Analysis of Supernatant
In situations when the suspended solids are of no great concern, sedimentation occurs
in the sample container, and the supernatant sample is used. Results depend on the
sedimentation and separation properties of the suspended solids, but usually the
dissolved TOC (DOC: dissolved organic carbon) is measured.
(2) TOC Analysis of Filtrate
The suspended solids are removed using glass fiber filter paper or a membrane filter,
and only the dissolved TOC is measured. Because the filter paper or filter itself is
likely to contain TOC, thorough washing with water or sample is performed prior to
use until no TOC is present in the eluate. Perform heat treatment on the filter for glass
fiber filter paper.
(3) TOC Analysis of Stirred Samples
To perform intentional analysis of suspended solids, the sample is stirred using a
magnetic stirrer or other instrument. Simple stirring can lead to extreme variability in
the results because the suspended solids contained in the sample may not be
distributed uniformly throughout the suspension.
(4) TOC Analysis after Homogenization of the Sample
If the application requires that the suspended solids be included in the analysis, it is
critical that the solids are as fine as possible and distributed uniformly throughout the
suspension. Accurate and reproducible TOC results can be obtained when the sample
is highly homogenized to form uniform micro-size particles.
Homogenizing systems may include a mixer to perform high-speed stirring or an
ultrasonic system. (These are homogenizers with outputs of 150-300W. Typical
washing sonicators do not have sufficient output for this use.) Ultrasonic systems are
generally more powerful, though performance varies with the type of suspended
solids.
Uniform suspension cannot always be achieved with all types of suspended solids.
Sludge-like materials are comparatively easy to process while fibrous materials are
more difficult.

70 TOC-VCPH/CPN
 4.1 Analysis Preparation
4.1.15 Sample Preparation

4.1.15.5 Handling Samples Containing Acids, Bases or Salts

Various problems can be encountered when measuring samples that contain acids, bases or
salts. Such problems include corrosion of the NDIR analysis cell as well as detrimental
effects on analysis values and the life of the combustion tube and catalyst. If corrosion of
the inner surface of the NDIR cell occurs, baseline stability will decline and noise will
increase. Samples containing acids, bases or salts should be handled as described below.
The concentration at which adverse effects are produced varies depending on the type of
acid or salt and the TOC or TN concentration. Prior to analysis, dilute the sample so that
acid, base and salt concentrations are reduced to 1000mg/L or less. Neutralization is also
required for bases. The TOC-V is equipped with an automatic dilution function to perform
these dilutions.

Acids
Acids should be diluted to a concentration of 1000mg/L or less. Concentrations up to
5000mg/L can be used if this level of dilution cannot be reached. The acidity of
hydrochloric acid or sulfuric acid can be reduced to a pH of 2-3 with sodium hydroxide or
potassium hydroxide. This process produces thermally stable sodium chloride or sodium
sulfate, which prevent the generation of acidic gas when combusting the sample.
Neutralization of the acid is stopped at a pH of about 2-3, and TOC direct analysis (NPOC
analysis) with sparging to remove the IC is performed. It is necessary to consider the TOC
associated with impurities contained in the alkali reagents used for neutralization. All salts
of nitric acid generate acidic gas under thermal decomposition; as a result, neutralization is
ineffective. When the sample contains hydrochloric or hypochlorous acid, hydrochloric
acid gas is generated from salts that are readily subject to thermal decomposition, such as
ammonium chloride, calcium chloride and magnesium chloride. The instrument is
equipped with a halogen scrubber; however, the scrubber’s main function is absorb
hydrochloric acid gas generated by corrosion of the gold plating on the internal surface of
the NDIR cell.

Alkaline samples
When performing TC analysis on alkaline samples, the following problems can arise:
• Rapid decrease in sensitivity and loss of reproducibility
• Rapid degradation of catalyst or wear of the combustion tube
• Likelihood that IC will be high due to absorption of carbon dioxide
For these reasons, the NPOC analysis is suitable for alkaline samples.
In NPOC analysis, dilute hydrochloric acid is added to adjust the solution to a pH of 2-3,
thereby forming a salt. For example, calcium chloride will be formed as a salt if the sample
contains calcium hydroxide as the base. Since it is preferable for this salt concentration to
be low, alkaline samples should be diluted as much as possible.

Salt accumulation
Samples should be diluted as much as possible to reduce the salt concentration and extend
the life of the combustion tube and catalyst. Conducting a large number of analyses on
samples containing salts will allow the salts to accumulate in the combustion tube,
gradually increasing resistance to the flow of carrier gas and resulting in decreased analysis
reproducibility. When decreased reproducibility is observed, perform the combustion tube
maintenance procedure described in Section 5.2.3 "Washing/Replacing the Combustion
and Carrier Gas Purification Tubes".

TOC-VCPH/CPN 71
 4.1 Analysis Preparation
4.1.16 Sample Preparation

Identifying Salt Accumulation

The following situations arise when salts accumulate and clog the catalyst:
• The sound of gas release is heard when the slider moves during analysis.
• A dramatic fluctuation in carrier gas flow is noticed after the sample is injected.

4.1.16 Sample Preparation

4.1.16.1 Vial Types

Two types of autosampler vials are available. The sample volume associated with each vial
type is shown below. Introduce the specified volume of sample into the vials; introducing
too little sample may result in insufficient sample for analysis.

Table 4.1 • Vial Types

Vial Typical Sample Volume1 Sample Volume for NPOC Analysis2
24mL 24mL 20mL
40mL 40mL 35mL
Note 1: Sample volume when sample is introduced to the bottom of vial cap.
Note 2: Sample volume when sample is introduced to about 1cm from bottom of vial cap.
In NPOC analysis, the sample volume is decreased to reduce its contact with the sample
cap during sparging.
Note: Vials to be used for the first time should be washed with laboratory detergent and
then rinsed well with water.

4.1.16.2 Filling Vials with Sample

In most cases, vials can be placed in the ASI-V turntable and analyzed without being
sealed. Vials must be sealed in the following situations:
(1) sparging with the autosampler for NPOC analysis
(2) measuring acidic samples
(3) IC analysis
(4) POC analysis
(5) low-concentration samples (as a guideline, less than 10mg/L)
(6) alkaline samples (pH 7 or higher)
(7) samples that contain volatile organic hydrocarbon components
(8) a large number of samples to be measured
(9) standard solutions

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

In situations (1) and (2) above, corrosion of the instrument may occur due to spattering of
sample, which contains acid. If the samples are left in the autosampler following
measurement, there is danger that the autosampler may be subjected to corrosion due to the
volatilization of acid.

In situations (3) through (9), results may be affected by either volatilization of the TOC
components in the sample or contamination from substances that absorb CO2 from the
atmosphere. If aluminum foil is used to cap the sample vial for NPOC or acidic sample
measurement, there is a danger of acid volatilization through the hole caused by insertion of
the needle. Do not use aluminum foil to cap the vials.

Methods of Sealing Vials

Two methods of sealing the vials are acceptable.
(1) Using the caps provided with the vials.
(2) Using a sealing material marketed under such names as Parafilm or Sealon Film.
Note: Use caps only after washing them with water, or washing them with laboratory
cleaning solution and then rinsing with water.

¬Using Caps

For 24mL vials

Holed caps and seals are provided with the vials.
1. Place a seal over the vial opening.
2. Cap the vial over the seal.
Note: Because the seals are perforated during injection, discard the seals
after use.

For 40mL vials

Seal-equipped caps are provided with the vials.
1. Using a seal-equipped cap provides an adequate seal for the vial.
Note: Because the seals are perforated during injection, discard the seal-
equipped cap after use.

¬Using Parafilm or Other Sealing Materials

Procedure
1. Cut the Parafilm or other sealing material into approximately 25 x 25mm squares.
2. Place a square over the opening of the vial, and stretch it to seal to the edges of the
vials.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

3. Press the edges down so that they wrap around the outside of the vial.

Be careful that
film edges do not
descend below
vial threads.

Figure 4.24 Sealing the Vial

4.1.16.3 Placing Vials in the Vial Rack

Remove the vial rack from the ASI-V before inserting the sample vials. There are three
different types of vial racks, each accommodating a different vial size.
The ASI-V permits random access of vials in the vial rack. Vials are measured according to
the sequence set in the Sample Table Editor, thus enabling analysis to start from any
position number in the vial rack, and for analysis to occur in non-sequential vial positions.

TIP » When samples are to be sparged using the optional external sparge kit, analysis is
performed more efficiently if the vials are placed in sequential rack positions without gaps.
This allows a vial to be sparged while an adjacent vial is being measured.

Installing the Vial Rack

Install the rack using the following procedure.
1. Insert the vials into the vial rack and place the rack on the ASI-V turntable.
2. Place the cover over the turntable.
Note: During analysis, the turntable must be covered. The ASI-V will not
operate if the turntable cover is not detected.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

4.1.16.4 High Sensitivity Autosampler Analysis

If samples with TOC concentrations of 100µg/L or less (such as purified water or ultra-pure
water) are measured using an autosampler, the following precautions associated with high
sensitivity analysis must be considered. Refer to Section 4.1.15.1 "High Sensitivity
Analysis" for additional information.
(1) NPOC analysis is recommended. TOC (TC-IC) analysis tends to have a greater
variation in measured values than the NPOC analysis because IC often accounts for a
significant portion of the TC, and the errors in the two values are additive, which
significantly affects TOC analysis.
(2) To generate a calibration curve, fill well-washed vials with standard solutions to about
5-10mm from the top of the vial, and immediately seal each vial.
Use a cap that has been washed with purified water prior to use.
When placing the vial in the rack, handle the vial carefully to avoid contact between
the standard solution and the cap.
Low-concentration standard solutions must be prepared each time they are used.
(3) To stabilize the peaks, perform 4 to 5 injections using the same analysis parameters
prior to analyzing the calibration standard solutions. For example, to generate a
400µg/L calibration curve, place a 0µg/L standard solution in vial position 1 and
measure it 4 to 5 times using the same analysis parameters that were selected for the
calibration curve. Refer to Section 4.4.4.1 "Calibration Curve". The objective at this
point is not to generate a calibration curve, but to inject water using the same injection
volume used for the calibration curve that is to be generated. This not only stabilizes
peaks but also thoroughly washes the sample needle and sparge needle with purified
water.
After the stabilizing injections are complete, place the 0µg/L and 400µg/L calibration
standard solutions in vial positions 2 and 3, insert the calibration standards into the
Sample Table Editor, and start measurement. Refer to Section 4.4.4.1 "Calibration
Curve".
(4) Acid addition for NPOC analysis can be performed automatically using the ASI-V. It
is best to perform manual addition of hydrochloric acid for NPOC analysis on the
order of 10µg/L. This is because, automatic acid addition pierces the vial seal and
allows CO2 contamination from the air.
(5) To prevent rinsing of the needle, deselect the “Rinse” option and set the “No. of
Needle Washes” field to zero in the Instrument Properties Dialog Box>ASI Window.
Refer to Section 3.2.4 "ASI Window".
Even if ultra-pure water is used as rinse water, the TOC concentration of the rinse
water will increase during the time it is exposed. For best results, do not rinse the
needle for analyses on the order of 100µg/L.
(6) Do not use the analysis value acquired from the first sample vial. In sample analysis,
particularly analysis on the order of 10µg/L, the first sample measured may yield high
results.
(7) When using the optional external sparge kit, perform sparging using a sparge gas flow
rate of 100mL/min.
As a guideline, use sparge times of 5 to 10 minutes for 24 and 40mL vials. Increase
the gas flow rate or sparge time if sparging is insufficient.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

4.1.16.5 Acid Addition in NPOC Analysis

Automatic addition of acid is possible using the autosampler when the optional external
sparge kit is installed. Using the ASI-V, acidification and sparging can be performed on
samples during NPOC analysis. To perform acid addition using the autosampler, enter the
desired amount in the “Acid Addition” field on the Injection Parameters window of the
Sample Wizard (refer to Section 4.4.5.2 "Sample") or Method Wizard (refer to 4.4.2.3
"Method Wizard").
When analysis is started, acid is drawn from the acid bottle into the syringe, and the set
amount of acid is added from the sample needle into each of the vials that have been
designated for acid addition. Use 2M hydrochloric acid. The acid addition ratio (ratio of
acid with respect to sample) should be set to about 2-5%. However, a setting of about 0.5%
is used for purified water analysis.
The hydrochloric acid concentration or amount added should be adjusted in accordance
with the sample pH or buffering strength to bring the sample pH to 2-3. Prior to analysis,
verify that the pH is 2-3 using pH paper. The pH need not be checked each time if the same
type of sample is routinely measured.

CAUTION
Hydrochloric acid is a hazardous chemical. Exercise caution when handling to
prevent contact and spills. For details, refer to Section 6.9 "Material Safety Data
Sheets".

If the sample pH does not reach a value between 2 and 3, increase the acid addition ratio or
the acid concentration. Excessively increasing the acid addition ratio will result in dilution
of the sample. On the other hand, if the acid amount is too small, the size of the acid droplet
on the tip of the needle will not be large enough to drop from the needle.
Visually observe the process through the glass vial to determine if the acid droplet is
actually added to the sample.
The needle will be rinsed following each acid addition by selecting the “Rinse after acid
addition” option in the Instrument Properties Dialog Box>ASI Window. To save time
during the analysis sequence, rinsing of the needle is unnecessary if the variation in NPOC
concentration among the samples is not large.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

4.1.16.6 Sparging in NPOC Analysis

Samples placed in the autosampler can be sparged by setting a sparge time if the optional
external sparge kit is installed.
If the coaxial needle is used (24mL or 40mL vials), sparging can be performed for the
specified time, followed immediately by drawing sample into the syringe and then by
analysis.
If the coaxial+sparge needle is used (24mL and 40mL vials), the next sample to be
measured can be sparged while the sample vial in the sampling position is being measured.
In this case, sparging is not performed again on the sample when it reaches the sampling
position, which does not pose a problem for ppm-level NPOC.
When measuring NPOC at the µg/L level, use the coaxial needle. This will prevent
atmospheric CO2 and other contaminants from entering the vial.
If the sparge gas flow rate is set too high, sample will be spattered onto the cap seal. Adjust
the sparge gas flow rate to avoid this undesirable spattering.
To verify that enough IC is removed during sparging using the autosampler to enable
unhindered NPOC analysis, perform IC analysis on the remaining sample following NPOC
analysis.

CAUTION
When the vials are capped and sparging is performed without automatic acid
addition via autosampler, pierce the caps before analysis by using the tip of a
provided needle or other instrument. This allows the sparge gas to vent. If sparge
gas is not vented from the vials, pressure will build inside the vials and prevent
effective sparging.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

4.1.16.7 Stirrer Preparation

This section describes the procedure for enabling the optional stirrer.

Procedure
1. Open the TOC-Control V Sample Table Editor.
2. From the Instrument menu, select Properties.
The Instrument Properties dialog box is displayed.
3. Click the ASI tab, then click in the “Stirrer On” check box to enable the stirrer.
4. Click the OK button.

Adjusting the Rotation Speed

Turn the knob at the bottom of the right side of the autosampler to adjust the stirring speed.
Note: Capabilities of the Optional ASI-V Magnetic Stirrer
• The stirrer bar rotates inside the vial to agitate and mix suspended solids in
the sample. The magnetic stirrer cannot be expected to pulverize and
homogenize suspended solids, except when they are extremely easy to crush.
Pretreatment of samples that contain suspended solids should include sample
homogenization to a point where the particles are distributed uniformly in as
small a particle size as possible. Well-homogenized samples can be measured
with good reproducibility. Stirring a non-homogeneous suspension will not
provide a uniform suspension, resulting in poor measurement reproducibility.
First apply a powerful enough homogenization process (ultrasonic waves,
etc.) to crush every particle in the sample as much as possible, and then
perform the TOC measurement.
• The ASI-V stirrer bar may not be able to sufficiently agitate and mix the
sample because of the wide variety of characteristics of suspended particles,
such as shape, specific gravity, size, strength, degree of cohesion, etc. For
example, solid particles with a high specific gravity sink to the bottom and
prevent formation of a good mixture.

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 4.1 Analysis Preparation
4.1.16 Sample Preparation

Note: Operation of the Optional ASI-V Magnetic Stirrer

• Two types of magnetic stirrers available, one for the 24mL and one for the 40mL
size vials.
• All of the vial positions may be used with 40mL vials. All positions except the
innermost row can be used with 24mL vials.
• The magnetic stirrer will only properly agitate vials in the sampling position and
the position just in front of the sampling position (advance processing position).
For example, if vial number 20 is selected, stirring is performed for vial 20 (sam-
pling position) and vial 21 (advance processing position). The stirrer bar may not
work normally for other vial positions. The stirrer bar rotation axis may shift,
depending on the shape of the vial bottom; this has almost no effect on the effec-
tiveness of the stirring.
• Adjust the stirrer rotation speed according to the sample properties. Use the stirrer
rotation speed adjustment control on the right side of the ASI-V.
Increasing the speed excessively may cause the stirrer bar to jump around instead
of rotate.
• Turning the stirrer on and off repeatedly, while the stirrer is set at the slowest
speed could cause the rotation speed to become uneven.
In this situation, adjust the rotation speed using the following procedure. ON /OFF
control of the stirrer is performed on the screen.

Setting the Stirrer Rotation Speed

Perform the following steps to achieve nearly equivalent rotation speeds in all of the
instruments used.
1. Turn the stirrer OFF.
2. Set the stirrer speed to the highest speed using the “Stirrer Rotation Speed Adjustment
Knob”.
3. Turn the stirrer ON and OFF several times.
4. With the stirrer ON, lower the stirrer speed.

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 4.1 Analysis Preparation
4.1.17 8-Port Sampler Measurement

4.1.17 8-Port Sampler Measurement

4.1.17.1 Type of Sampler Container

There are no restrictions on the type of sample containers that can be used with the 8-Port
Sampler. It is only necessary that the containers be placed so the sample tubing from the
various ports can be inserted directly into the containers.
Note: Wash all sample containers with an appropriate laboratory detergent, and rinse
them thoroughly with water before using them for the first time.
Loading the Sample
Although it is possible to perform measurement of a sample using the 8-Port Sampler,
while the container open, in the following situations, it is necessary to seal the sample
container.
(1) When performing IC measurement
(2) When performing POC measurement
(3) When performing measurement of low concentration samples (e.g., 10 mg/L)
(4) When performing measurement of alkali samples of pH 7 or higher
(5) When performing measurement of samples containing volatile organic carbon
compounds
(6) When the number of samples is so great as to require a long measurement time
(7) When performing measurement of standard solutions
Note: If the sample container openings are not sealed in the situations listed above,
measurement values may be influenced by such factors as absorption of atmo-
spheric CO2, contamination with carbon containing substances, and evaporation
of TOC constituents from the samples.
Sealing the Sample Containers
Sample containers may be sealed using commercial sealing films such as Parafilm. It is also
possible to pierce the lid of the container and insert the sample tubing into the container
through this opening.
Note: In either case, wash the container with a laboratory detergent, and rinse it thor-
oughly with water before use.

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 4.1 Analysis Preparation
4.1.17 8-Port Sampler Measurement

Sealing the Container with Parafilm

1. Cut a piece of Parafilm to size according to the size of the sample vessel opening.
2. Insert the tip of the sampling tube into the vessel, cover the opening with the prepared
Parafilm, and seal the opening of the vessel, stretching the Parafilm over the edges. Be
sure that a very small gap in the seal is formed to prevent creation of negative pressure
inside the vessel.
3. Press the overlapping portions of the Parafilm around the neck of the opening.

Parafilm

Figure 4.25 Sealing the Container

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 4.1 Analysis Preparation
4.1.17 8-Port Sampler Measurement

4.1.17.2 High Sensitivity Using the 8-Port Sampler

If samples such as purified water or ultra-pure water, having a TOC concentration of

100ppb or less, are to be measured using the 8-Port Sampler, it is necessary to consider the
following precautions associated with high sensitivity analysis. Refer to Section 3.3.1.4
“High Sensitivity Autosampler Analysis” in the TOC-VCSH/CSN User Manual for more
information.
1) NPOC analysis is recommended because TOC (TC-IC) analysis tends to have a
greater variation in measured values than NPOC. This is because IC often accounts
for a significant portion of the TC, and the errors in the two values are additive using
TOC (TC-IC) analysis. This affect significantly influences TOC analysis.
2) For calibration measurement of standard solutions, fill well-washed containers
with standard solutions to about 5-10 mm from the top of the container, and
immediately seal each container. When placing the container below the 8-Port
Sampler, handle it carefully to avoid the standard solution contacting the sealing
surface. Low-concentration standard solutions must be prepared each time they
are used.
3) To ensure that the peaks are stable for generating the calibration curve, perform
4-5 injections using the same analysis parameters prior to performing the
calibration curve analysis. For example, to generate a 400ppb calibration curve,
set 400ppb as the 1st standard solution concentration, and enter 1 as the
container number. Actually place a 0ppb solution in the container for port No. 1.
The objective at this point is not to generate a calibration curve, but to inject
water using the same injection volume that will be used to generate the
calibration curve. This not only stabilizes the instrument but also thoroughly
washes the sampling needle with purified water.
In the 2nd row of the settings screen and using the same calibration curve number
as above, set the analysis parameters for 0ppb and 400ppb. When sample mea-
surement starts, the calibration curve to be used will be created with the correct
standard solutions.

82 TOC-VCPH/CPN
 4.2 Setting General Measurement Parameters
4.2.1 TOC Parameter Settings

4.2 Setting General Measurement Parameters

4.2.1 TOC Parameter Settings

The following parameters must be set for analysis using the PC-controlled TOC-V
analyzer: The items available for editing change depending on the options that are installed.
• Tubing Diameter
• Buzzer
• Auto regeneration of IC solution
• Ready status check
• TN Power Source

Setting Procedure
1. In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.

Figure 4.26 Instrument Properties Dialog Box: TOC Tab

2. Click the TOC tab.

The Main Unit Version field displays the instrument version number; this field cannot
be changed by the user.
3. Enter the parameters as described below:
Tubing Diameter
Specifies the diameter size of the sample injection tubing. Select the tubing diameter
from the drop-down list. Available options are:
• Regular: 0.5mm diameter
• Suspended Particle: 0.8mm diameter
The typical tubing diameter is 0.5mm. Select a tubing diameter of 0.8mm if the Sus-
pended Solids kit is used.

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 4.2 Setting General Measurement Parameters
4.2.2 ASI Parameter Settings

Buzzer
Enables the internal buzzer function. Select this option to allow the buzzer to sound
during measurement.
Auto regeneration of IC solution
Enables the automatic regeneration of IC solution. This option is enabled only when
IC measurement is being performed, and is typically selected. Refer to Section 3.2.3
"TOC Window" for a detailed description of this option.
Enable ready status check
Enables the Ready Status Check function. When the function is enabled, the software
always verifies that the instrument is in the Ready state prior to starting measurement.
Enabling the Ready Status Check function is recommended. When the function is
deselected, measurement can be performed when the instrument is not in the Ready
state, an option that is mainly for use by service personnel.
TN Power Source
Select this item if the optional TNM-1 unit is installed to perform TN analyses.
TC Furnace
Select the desired TC furnace temperature by clicking the appropriate radio button. If
“Combustion” is the selected oxidation method, select 680 or 720. If “Wet Chemical”
is the selected oxidation method, the TC Furnace field is set to Off and disabled.

4.2.2 ASI Parameter Settings

The following parameters must be set when using the ASI-V:
• Tray type
• Needle
• Number of needle washes
• Number of flow line washes
• Rinse
• Rinse after acid addition
• Stirrer ON

Setting Procedure
1. In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.

84 TOC-VCPH/CPN
 4.2 Setting General Measurement Parameters
4.2.2 ASI Parameter Settings

2. Click the ASI tab.

Figure 4.27 Instrument Properties Dialog Box: ASI Tab

3. Enter the parameters as described below:

Tray Type
Specifies the size of the vials used in the ASI rack. Select the vial size from the drop-
down list. Available options are 24mL Vial and 40mL Vial.
Needle
Specifies the type of needle used for analysis. Select the needle type from the drop-
down list. Options are:
• Sample: for analysis using only a sample needle
• Sample+Sparge: for analysis using both a sample needle and a sparge needle
• Coaxial: for analysis using an integrated sample and sparge needle
• Coaxial+Sparge: for analysis using both the coaxial needle and a sparge needle,
which allows a sample to be measured while the next sample is sparged.
• The instrument does not automatically recognize the type of needle
installed. Be sure to select the type of needle that is actually installed in
the instrument.
No. of Needle Washes
Specifies the number of times the needle will be rinsed after sample injection. This
operation rinses the outside of the needle using water drawn from the dilution water
bottle. Rinsing the needle can prevent poor injection quality that results from salt
buildup at the tip of the injection tube during sample analysis. Such salt buildup is
especially problematic when analyzing samples with high salt concentrations
(1000ppm or greater).
Enter a number ranging from 0 to 10 in the No. of Needle Washes field.
Note: Needle rinsing is not required when samples contain low salt con-
centrations. Three rinses are recommended for samples containing
salt concentrations of 1% or more.

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 4.2 Setting General Measurement Parameters
4.2.2 ASI Parameter Settings

No. of Flow Line Washes

Specifies the number of times the flow lines will be rinsed after all samples listed in
the Sample Table have been measured. This operation rinses the flow line from the
sample needle to the injection tube using water drawn from the dilution water bottle.
If the automatic acid addition option has been selected, the flow lines will be rinsed
the specified number of times following acid addition to each sample; rinsing after
acid addition removes acid that remains in the sample needle or flow lines.
Enter a number ranging from 0 to 10 in the No. of Flow Line Washes field.
Note: Typically, 2 flow line rinses are sufficient. Three to four rinses are
recommended for samples containing acid, base, or salt.
Rinse
Enables automatic rinsing of the sample needle and sparge needle between each sam-
ple using water from the dilution water bottle.
Note: • Rinsing between each sample prevents carryover from one sample to the
next. Rinsing is not necessary if all samples contain similar analyte con-
centrations.
• Rinsing is not recommended when analyzing ultra-pure water samples
with expected concentrations of less than a few hundred µg/L. The con-
centration of carbon in the rinse water may affect the sample results.
Rinsing with ultra-pure water will not reduce this effect, as the concen-
tration of carbon in the rinse water will increase with exposure to the
atmosphere.
Rinse after acid addition
Enables automatic rinsing of the sample needle and flow lines after each acid addi-
tion.
Note: Rinsing the needle after each acid addition is not necessary if all
samples contain similar NPOC concentrations. Eliminating the
rinsing operation will save time during the analysis sequence.
Stirrer On
Enables the magnetic stirrer. Select this option to stir the samples while measurement
is being performed.
Note: Stirring a sample during measurement prevents settling or clump-
ing of suspended solids, thereby including suspended solids when
the sample is drawn into the syringe.

86 TOC-VCPH/CPN
 4.2 Setting General Measurement Parameters
4.2.3 Setting Default Measurement Parameters

4.2.3 Setting Default Measurement Parameters

The Default Measurement Parameters window is used to enter the default values for sample
measurement parameters. The selections made in the Default Measurement Parameters
window will be displayed as the default values when setting calibration curve and sample
measurement parameters.

Procedure
1. From the Options menu in the Sample Table Editor, select Default Measurement
Parameters.
The Default Measurement Parameters window is displayed.

Figure 4.28 Default Measurement Parameters: TC/IC/NPOC/POC/TN Tabs

2. Enter the following parameters on each of the applicable tabs:
• Units: Select the default concentration units for the measurement results
• No. of Injections: Enter the default minimum/maximum number of injections
• No. of Washes: Enter the default number of times the syringe is to be washed with
sample prior to the first injection. In POC analysis and IC analysis with the N-type
this refers to the number of syringe rinses using dilution water.
• Max SD: Enter the default maximum standard deviation that is acceptable for
repeat measurements. If this value is met, no additional injections are required.
However, if both this value and the Max CV value are exceeded, the samples are
automatically reinjected up to the maximum number of times specified in the No.
of Injections field. The Max SD field is disabled if the Number of Injections is 1 or
if the minimum is equal to the maximum. The default value for Max SD is 0.1.
• Max CV: Enter the default maximum coefficient of variation that is acceptable for
repeat measurements. If this value is met, no additional injections are required.
However, if both this value and the Max SD value are exceeded, the samples are
automatically reinjected up to the maximum number of times specified in the No.
of Injections field. The Max CV field is disabled if the Number of Injections is 1
or if the minimum is equal to the maximum. The default value for Max CV is 2%.
Note: The “maximum” No. of Injections field refers to the maximum
number of repeat injections to be performed when the automatic
additional measurement function is enabled. Additional measure-
ments are performed when both the Max SD and Max CV settings
are exceeded. When both of these values are exceeded for the set
number of sample injections, the additional measurement function
is automatically activated and the sample is reinjected.

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 4.2 Setting General Measurement Parameters
4.2.4 Maintenance History Settings

4.2.4 Maintenance History Settings

Enter limits for the following parameters to display a warning message when the limits are
exceeded:
• Combustion Tube Sample Injection Volume: Refers to the total volume of sample that
can be injected into the combustion tube before catalyst and combustion tube mainte-
nance is required.
• Dilution Water: Refers to dilution water volume
• Total Acid Volume: Refers to the total volume of acid used
• Syringe Stroke: Refers to the number of syringe operations
• UV Lamp: Refers to time of operation of UV lamp
• IC Unit Pump Tubing: Refers to time of IC unit pump tubing use. The recommended
warning value is 300 hours.
• ASI Rinse Pump: Refers to time of ASI rinse pump tubing use. The recommended
warning value is 300 hours.

Procedure
1. From the Instrument menu in the Sample Table Editor window, select
Maintenance>History.
The Maintenance History dialog box is displayed.

Figure 4.29 Maintenance History Dialog Box

2. Enter warning limits by placing the cursor in the appropriate fields and entering
numeric values.
3. Click the OK button.
TIP » Measurement will be interrupted if the dilution water or acid reservoirs run dry during
analysis. To prevent measurement interruption, set the dilution water and total acid volume
limits to values slightly less than the remaining volume of each respective liquid. A warning
message will be generated before each liquid is completely consumed.Click the Reset
button to the right of a parameter to clear its current value.

88 TOC-VCPH/CPN
 4.3 Measurement Procedures and Tutorial
4.3.1 Starting Up the Instrument

4.3 Measurement Procedures and Tutorial

4.3.1 Starting Up the Instrument

4.3.1.1 Turning on the Power

Turn on the power to the instrument by pressing the power key on the bottom right of the
front panel.
Note: Press the power key again to turn off power to the instrument.

4.3.1.2 Carrier Gas Pressure

Procedure for setting the carrier gas pressure

1. Set the supply pressure of the carrier gas to 300kPa using the pressure regulator at the
carrier gas supply source (cylinder).
Note: If compressed air or instrumentation air is used, verify that the
supply pressure is greater than 300kPa and does not exceed 600kPa.
2. Open the front door of the instrument and adjust the carrier gas pressure to 200kPa
using the carrier gas pressure regulation knob.

Carrier Gas
Pressure Regulator

Carrier Gas Pressure

Regulation Knob

Figure 4.30 Setting the Carrier Gas Pressure

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 4.3 Measurement Procedures and Tutorial
4.3.1 Starting Up the Instrument

4.3.1.3 Carrier Gas Flow Rate

Procedure for setting the carrier gas flow rate

1. Open the front door of the instrument.
2. Turn the carrier gas flow adjustment knob. For H Type, adjust the flow rate to
150mL/min, as indicated on the flow rate gauge.

Carrier Gas Flow

Rate Adjustment
Knob

Flow Rate Gauge

Figure 4.31 Setting Carrier Gas Flow Rate

Note: • Do not change the carrier gas flow rate during analysis. The peak area
changes in an inversely proportional relationship and may cause errors in
analysis precision.
• With the N Type, although the flow rate is adjusted to indicate 130mL/min on
the flow rate gauge, the actual flow rate used is 230mL/min.

4.3.1.4 Electric Furnace

The electric furnace power must be turned on for TC, TOC, NPOC, POC and TN analyses.
The electric furnace does not need to be turned on if only IC analysis is performed. When
TN analysis is conducted, the TN unit must also be turned on.

Turn On Power to the Electric Furnace

1. In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
2. Click the TOC tab.
3. Set the TC furnace temperature to either 680°C or 720°C (used for TN measurement).
4. Click the OK button.
The screen returns to the TOC-Control V main window.
Note: It takes 30-40 minutes after the electric furnace power is turned on for the tem-
perature to reach the set value. Refer to Section 4.3.3 "Ending Measurement" to
turn Off the instrument,.

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4.3.1.5 TN Unit

When TN analysis is to be performed using the optional TN unit, power to the TN unit and
ozone generator must be turned on.

Turning Power to the TN Unit ON

1. In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
2. Click the TOC tab.
3. Click in the TN Power check box to select the option.
4. Click the OK button.
The screen returns to the TOC-Control V main window.

Turning Power to the Ozone Generator ON

1. Press the power switch at the lower right of the TN unit.
ON
TIP » Power Button positions:
OFF

4.3.1.6 Ozone Source Airflow Rate for the TN Unit

Adjust the ozone source airflow knob on the TN unit to indicate 500mL/min on the flow
rate gauge.

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4.3.2 Tutorial
This tutorial gives step-by-step instructions on the use of the TOC-Control V software. The
tutorial assumes that the hardware and software have been installed in the manner
described in Chapters 2 and 3, and that users have a configured system that includes the
TOC-VCPH, ASI and TNM-1 unit.
Note: • If your system does not include the ASI and TNM-1 units, please adjust the
tutorial procedure as appropriate.
In the tutorial, a three-point TC/TN calibration curve and one unknown sample will be
measured. Pure water and the following calibration standards are needed for the tutorial:
• A calibration standard mixture of 0ppm potassium hydrogen phthalate and 0ppm
ammonium chloride
• A calibration standard mixture of 50ppm potassium hydrogen phthalate and 10ppm
ammonium chloride
• A calibration standard mixture of 100ppm potassium hydrogen phthalate and 20ppm
ammonium chloride

Reference: Prepare calibration standards as described in Section 4.1.14.1 "Preparation of Standard

Solutions".

¬The following topics are covered in the tutorial:

Step 1 Configuring the instrument
Step 2 Connecting the instrument
Step 3 Creating a sample table
Step 4 Setting up the calibration standard runs
Step 5 Setting up an unknown sample run
Step 6 Performing measurement
Step 7 Evaluating the results
Step 8 Printing a report

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¬Configuring the Instrument (Step 1)

Procedure
1. Start the TOC-Control V software by double clicking the icon or selecting it from the
Start>Programs list.
The TOC-Control V main window is displayed.

Figure 4.32 TOC-Control V Main Window

2. The instrument configuration must be specified in the software before the instrument
can be connected to the PC for the first time. Only users with administrative privileges
can configure the instrument. If the system has already been configured, proceed to
Step 2 of the tutorial.
3. From the TOC-Control V main window, double-click the New System icon.
The User dialog box is displayed.
4. Enter your user name and password as shown below.

Figure 4.33 Enter User Name and Password

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Click the OK button. The Instrument Setup Wizard opens.

Figure 4.34 Enter the Name of the System

5. In the System Information window of the Instrument Setup Wizard, enter the System
Name and Instrument Serial Number. Click the Next button.
The Options window of the Instrument Setup Wizard is displayed.

Reference: For details on the System Name and Instrument Serial Number, refer to Section 3.2.1
"System Information Window".

Figure 4.35 Configured Options

6. Specify the options that are configured on the system by clicking in the appropriate
check boxes, as shown in the above figure.
7. Click the Next button. The TOC window of the Instrument Setup Wizard is displayed.

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8. Select the TOC analysis parameters, as shown in the figure below.

Note: Be sure that the “Enable ready status check” option is selected.
Enabling the ready status check function means that the instrument
will not begin a new injection until the instrument status is Ready.

Figure 4.36 TOC Analysis Parameters

Reference: For details on TOC parameters, refer to Section 4.2.1 "TOC Parameter Settings"
9. Click the Next button. The ASI window of the Instrument Setup Wizard is displayed.
Verify that the ASI parameters match those shown on the figure below.

Figure 4.37 Autosampler Parameters

10. Click the Next button. The Communication window of the Instrument Setup Wizard
is displayed.
11. Verify the communication information (COM Port, Stop Bits, and Parity).
Note: If a Shimadzu representative installed your TOC-Control V soft-
ware, the correct settings for your system are already configured.
Please do not change the settings. Refer to Section 3.2.6 "Commu-
nication Window" for more information on Communication set-
tings.

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12. Click the Next button. The History Function window of the Instrument Setup Wizard
is displayed. If desired, enable the History Log to track all changes to the method.
Refer to Section 3.2.7 "History Function Window" for more information about the
History Log.
Note: If Audit Trail was checked for the GLP/GMP 21 CFR item in
System Administration Tools of the TOC-Control V main menu,
the History Log function is automatically activated.
13. Click the Finish button.
An icon for the system now appears in the TOC-Control V main window.

TIP » To edit the system configuration, double-click the system icon in the TOC-Control V main
window or, when in the Sample Table Editor window, select Properties from the Instrument
menu. The Instrument Properties dialog box opens, and system configuration options are
displayed on tabs in the dialog box.

¬Connecting the Instrument (Step 2)

Opening a New Sample Table

1. In the TOC-Control V main window, double-click the Sample Table Editor

icon. The User dialog box is displayed.
2. Enter your user name and password. Click the OK button.

3. Open a new Sample Table by either selecting New from the File menu or clicking the
New toolbar button. The New dialog box is displayed.

Change Graphic

Figure 4.38 Sample Run Icon

4. Click the Sample Run icon, then click the OK button.

The General Information dialog box opens.

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5. Click the System tab and select the desired system from the drop-down list.
6. Select Save File As in the File menu. Enter Tutorial and click the Save button.

Figure 4.39 Save As Dialog Box

7. Click the OK button.
A new, blank Sample Table is displayed.

Figure 4.40 New Sample Table

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Connecting to the Instrument

1. To establish communication between the software and the instrument, either select

Connect from the Instrument menu or click the Connect toolbar button.
The Parameter Configuration dialog box is displayed. Click the Use Settings on PC
button.
The Sequence dialog box is displayed.

Figure 4.41 Connection in Progress

2. The Sequence dialog box displays information about the attempt to establish
communication between the software and the instrument.
¬Creating a Sample Table (Step 3)

Procedure
Creating a Sample Table involves three steps. First, enter the default analysis parameters
for the Sample Table (.t32) file.
1. From the Options menu, select Default Measurement Parameters.
2. Three injections of each calibration standard and unknown sample will be made. On
the TC tab change the “No. of injections” value to 3.
The other default measurement parameters should not be changed.
3. On the TN tab change the “No. of injections” value to 3.
The other default measurement parameters should not be changed.

Figure 4.42 Default Measurement Parameters Dialog Box

Note: The selected measurement parameters will appear as default values
when setting up calibration and method files.

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Reference: For details, refer to Section 4.2.3 "Setting Default Measurement Parameters".
Modify the Sample Table window display settings so that all items contained in the
Sample Table are shown on the screen. The default display settings may not include
all of the Sample Table parameters.
4. From the Options menu, select Display Settings>Table Settings.
5. Ensure that all items on both tabs in the Table Options window are selected. If not,
click the Select All button.

Figure 4.43 Table Options Window

Note: Use this window in the future to create custom Sample Table win-
dows that display only the desired items.
6. Save the Sample Table (.t32) file.
7. From the File menu, select Save As.
The Save As dialog box is displayed. Enter “Tutorial” as the file name and click the
Save button.
Note: The name “Tutorial” appears at the top of the Sample Table win-
dow and for the directory name after the file is saved.
The basic instrument configuration and analysis parameters have been set up.

Reference: Refer to Section 4.4 "Sample Table Editor" for detailed descriptions of the Sample Table
Editor menus and commands.

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¬Setting up the Calibration Standard Runs (Step 4)

Setting up calibration standard runs involves two steps: creating a calibration file, which
stores information about calibration standard measurements, and inserting the calibration
standard runs in the Sample Table. Separate calibration files are created for the TC and TN
analyses. The calibration is a three-point curve generated using standard mixtures of
potassium hydrogen phthalate and ammonium chloride.

Creating the TC Calibration File

1. Open the Sample Table. From the File menu, select New.
The New dialog box is displayed. Click the Calibration Curve icon.

Figure 4.44 Creating a New Calibration File

2. Click the OK button to open the Calibration Curve Wizard. Specific information
about the calibration will be entered in the wizard.

Figure 4.45 System for Analyses of the Calibration Standard

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3. Select the system to be used for the analyses from the drop-down list on page 1 of the
Calibration Curve Wizard. Click the Next button.
Page 2 of the Calibration Curve Wizard, which lists options for calibration curve type,
is displayed. The four types of calibration curves available are:
• Calibration points are distributed uniformly over the concentration range
• Edit calibration points manually
• Calibration curve according to DIN38402/P-51
• Calibration curve according to USP/EP

Figure 4.46 Calibration Curve Type

4. Click the radio button for “Calibration points are distributed uniformly over the
concentration range.” In the future, other options may be more appropriate. Refer to
Section 4.4.2.2 "Calibration Curve" for a detailed description of the calibration curve
types.
Click the Next button.

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5. Page 3 of the Calibration Curve Wizard is displayed. The following options for
calibration analysis are displayed:
• Analysis
• Default Sample Name
• Default Sample ID
• Calculation Method: Linear Regression or Point to Point
• Check box for Zero Shift
• Check box for Multiple Injections
• Calibration File Name
Select the following options, as shown on the figure below:
• Analysis: TC
• Default Sample Name: Standard
• Default Sample ID: Tutorial
• Calculation Method: Linear Regression
• Check box for Zero Shift: Deselect this option
• Check box for Multiple Injections: Deselect this option
• Calibration File Name: TCTutorial.cal

Figure 4.47 TC Calibration Analysis Information

6. Click the Next button. Page 4 of the Calibration Curve Wizard is displayed.
Notice that the No. of Injections displayed matches the number entered when setting
the default measurement parameters for the Sample Table in Step 3 of the tutorial.

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7. Enter the TC calibration standard concentration range values of 0 to 100ppm.

Enter 3 as the number of calibration points.

Figure 4.48 TC Calibration Standard Information

8. Click the Next button.

Page 5 of the Calibration Curve Wizard displays the Calibration Points List.
9. Notice that the Calibration Points List was completed based on information entered
on the previous Wizard pages. To make any changes, select a row and click the Edit
button.

Figure 4.49 TC Calibration Points List

10. Click the Next button.

Page 6 of the Calibration Curve Wizard, which specifies peak integration parameters,
is displayed.
11. Settings can be made on this page to delay the peak detection start time or extend the
peak detection time. View but do not change the default setting on the page.

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12. Click the Next button.

Page 7 of the Calibration Curve Wizard is displayed. The History function can be
enabled on this page of the wizard. View but do not change the default setting.
13. Click the Finish button.
The Calibration Curve Wizard closes. The TC calibration curve file is now complete
and has been saved.

Creating the TN Calibration File

The TN calibration file is created by following the same steps used to create the TC
calibration file, with the exceptions described below.
1. On page 3 of the Calibration Curve Wizard, specify the Analysis as TN and enter
“TNtutorial.cal” as the calibration file name.

Figure 4.50 TN Calibration Analysis Information

2. On page 4 of the Calibration Curve Wizard, enter 0 to 20ppm for the Concentration
Range and 3 for the number of calibration points.

Figure 4.51 TN Calibration Measurement Parameters

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3. Page 5 of the Calibration Curve Wizard should match the following figure.

Figure 4.52 TN Calibration Points List

4. Complete the TN calibration file by viewing but not changing pages 6 and 7 of the
Wizard and clicking the Finish button.
The TN calibration curve file is now complete and has been saved.

Reference: Refer to Section 4.4.2.2 "Calibration Curve" for a detailed description of the Calibration
Curve Wizard.

Entering the Calibration Standard Runs in the Sample Table

Now that the calibration files have been created and saved, the calibration standard runs
must be inserted into the Sample Table. The TC and TN calibration standards are inserted
separately.
1. Insert the TC calibration standard runs by placing the cursor in the first line of the
Sample Table.
2. From the Insert menu, select Calibration Curve.
3. Specify the name of the TC Calibration Curve (TCtutorial.cal) and click the Open
button.
The Sparging/Acid Addition window is displayed. Notice that the TC calibration stan-
dards have been automatically added to the table.

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4. Enter the vial positions (1-3) for the calibration standards directly into the Vial
column of the table. As vial positions are entered in the table, they are highlighted on
the tray diagram in the Sparging/Acid Addition window.

Figure 4.53 Sparging/Acid Addition Window for the ASI-V Autosampler

OCT-1 8-Port Sampler Sparging/Acid Addition Window

Figure 4.54 Sparging/Acid Window for the OCT-1 8-Port Sampler

TIP » The vial position for a sample can also be entered by placing the cursor in the appropriate
row of the Sparging/Acid Addition window and then double-clicking the desired vial
position in the tray diagram.

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5. Verify the information, then click the OK button.

The Sample Table is displayed. Notice that the first row of the Sample Table now con-
tains complete TC calibration standard measurement information.

Figure 4.55 TC Calibration Standard Information in the Sample Table

6. Insert the TN calibration standard runs by placing the cursor in the second line of the
Sample Table.
From the Insert menu, select Calibration Curve. The Open dialog box is displayed.
Specify the name of the TN Calibration Curve (TNtutorial.cal) and click the Open
button.

Figure 4.56 Select the TN Calibration File

The Sparging/Acid Addition window is displayed. Notice that the TN calibration

standards have been automatically added to the table.
7. Enter the vial positions for the calibration standards directly into the Vial column of
the table. Because the calibration standards are TC/TN mixtures, enter the same vial
positions (1-3) for the TN standards that were entered for the TC standards.

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8. Click the OK button to display the Sample Table window. Notice that the second row
of the Sample Table now contains complete TN calibration standard measurement
information.
Take a moment to scroll through the completed Sample Table. Notice that the col-
umns in the left portion of the Sample Table contain the specified analysis parameters.
Actual measurement information will appear in the columns in the right portion of the
Sample Table once the measurements are completed.

9. Save the Sample Table by selecting Save from the File menu or by clicking the Save
button in the toolbar.

¬Setting up an Unknown Sample Run (Step 5)

In Step 4 of the tutorial, you learned that information about calibration standard
measurement is saved in a calibration file. You also learned that setting up a calibration
standard run involves two steps: creating a calibration file and then inserting the calibration
standards into the Sample Table.
By contrast, information about unknown sample measurement is saved in a method file.
Setting up an unknown sample run involves two steps: creating a method file and then
inserting the unknown sample into the Sample Table. In this tutorial, one “unknown”
sample will be analyzed. The “unknown” sample is actually the mid-level calibration
standard (50ppm TC/10ppm TN).

Creating a Method File

1. Open the Sample Table. From the File menu, select New.

2. The New dialog box is displayed. Click the Method icon and then click the OK
button. The Method Wizard opens.

3. Select the system to be used for the analysis from the drop-down list on page 1 of the
Method Wizard. Click the Next button.
Page 2 of the Method Wizard lists options for the analysis.
4. Select TC/TN from the Analysis drop-down menu. Enter “Sample” in the Default
Sample Name field and “Tutorial” in the Default Sample ID field. In the File Name
field, enter “Tutorial.met” as the name of the Method File.

Figure 4.57 Method Wizard (Page 2) Analysis Information

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5. Click the Next button.

Page 3 of the Method Wizard specifies the calibration curves to be used to calculate
unknown sample results.
Note: It is possible to enter the calibration curve file in this screen since it
contains the data that needs to be entered on this page.
6. Place the cursor in the Calibration Curve 1 field. Click the Browse button.
Select the file for the TC calibration curve created previously (TCtutorial.cal).

Figure 4.58 Method Wizard (Page 3) Calibration Curves

7. Click the Next button.

Page 4 of the Method Wizard is displayed.

Figure 4.59 Method Wizard (Page 4) Injection Parameters

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8. The following TC analysis parameters can be entered.

• Analysis (disabled)
• Units
• Injection Volume (disabled)
• Number of Injections
• SD Max
• CV Max
• Number of Washes
• Auto Dilution
• Acid Addition
• Expected Concentration Range
• Multiple Injections
• Use blank check area
• Auto reinjection If both the CV max and SD max values have been exceeded.
9. Click the Next button.
Page 5 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
10. Click the Next button.
The Method Wizard (Page 3) Calibration Curve screen is displayed. Enter the TN
measurement parameters.
11. Click the box beside [Calibration 1], and either select the TNtutorial.cal file or enter
the calibration curve file.
12. Click the Next button.
The Method Wizard (Page 4) Measurement Parameters screen is displayed. Set the
TN measurement parameters in the same way as for TC measurement.
13. Click the Next button.
The Method Wizard (Page 5) Peak Detection Time screen is displayed. Do not change
the default settings on this page.
14. Click the Next button.
Page 6 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
15. Click the Next button.
Page 7 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
16. Click the Finish button.
The Method Wizard closes. The method file is now complete and has been saved.
Insert the sample into the Sample Table.

Reference: Refer to Section 4.4.2.3 "Method Wizard" for a detailed description of the Method Wizard.

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17. Insert the unknown sample by placing the cursor in the third line of the Sample Table.
From the Insert menu, select Sample.
Page 1 of the Sample Wizard (Parameter Source) is displayed.

TIP » To set up multiple analyses using a previously created method, select the Auto Generate
Table command from the Insert menu. Refer to Section 4.4.5.1 "Auto Generate".

Figure 4.60 Sample Wizard (Page 1) Parameter Sources

18. Click the Method radio button. By selecting this option, the sample will be analyzed
using the measurement parameters specified in the method file we created previously.
Enter the name of the method file (Tutorial.met) or click the Browse button to search
for the file.
Click in the “Skip remaining Wizard pages and use measurement parameters from the
source” check box. By selecting this option, the analysis parameters for the unknown
sample are copied from the source (method) file. The parameters do not need to be
entered manually and the remaining pages of the Sample Wizard do not need to be
displayed.
19. Click the Finish button.
The Sparging/Acid Addition window is displayed.
20. Enter the vial position (2) for the unknown sample (the 50ppm TC/10ppm TN
calibration standard) directly into the Vial column of the table.
21. Verify the information, then click the OK button.
The third row of the Sample Table now contains the measurement parameters for the
unknown sample. (Note that a value will not be displayed in the Result column until
measurement is complete.)
22. Save the Sample Table by selecting Save from the File menu or by clicking the Save
button in the toolbar.

Measurement can now be performed.

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¬Performing Measurement (Step 6)

Procedure
1. Prepare the three calibration standards (0ppm potassium hydrogen phthalate/0ppm
ammonium chloride, 50ppm potassium hydrogen phthalate/10ppm ammonium
chloride, and 100ppm potassium hydrogen phthalate/20ppm ammonium chloride) and
place them in autosampler tray vial positions 1, 2, and 3.
Note: Calibration standards and unknown samples can be placed in any
vial position when controlling the instrument with the TOC-Control
V software.
2. Check the status of the instrument detectors before starting analysis. From the
Instrument menu, select Background Monitor, or click the Background Monitor
button on the toolbar.
The Background Monitor window is displayed; this window is used to monitor the
real time signal from the ASI and the detectors. On the TOC tab, the status of the
baseline should be OK for each parameter (position, fluctuation, and noise).
3. Click the TN tab to check the status of the nitrogen detector.

Figure 4.61 Background Monitor

4. Close the Background Monitor window. It cannot be open during analysis.

5. Place the cursor in the first row of the Sample Table; this allows the measurement
sequence to begin with the TC calibration. From the Instrument menu, select Start, or
click the Start button on the toolbar.
The Standby window is displayed.

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6. The Standby window displays 3 options:

• Keep running
• Shut down instrument
• Auto restart

Figure 4.62 Standby Window

Reference: Refer to Section 4.4.6.3 "Standby" for detailed descriptions of the Standby window options.
7. Click the Keep Running radio button. Then Click the Standby button.
The Sparging/Acid Addition window is displayed.
8. Verify the vial positions, then click the OK button.
9. The Start ASI measurement window is displayed. Click the Start button to begin the
analysis.

10. The status of the measurements can be monitored during analysis by viewing the
Sample Window. To open the Sample Window, either select Sample Window from the
View menu or select the Sample Window button on the toolbar.

Figure 4.63 Sample Window

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Note: • The Sample Window is divided into 3 sections, as shown in the above figure.
The Graph is in the upper left corner, the Parameter Table is in the upper right
corner, and the Injection Table is the bottom half of the window. The current
injection is displayed with asterisks in the Injection Table. As each
measurement occurs, information in the appropriate Injection Table row is
completed. Previous injections are shown above the current row. Use the
scroll bar to see all of the information, and use the tabs at the bottom of the
table to toggle between analysis types (between TC and TN, in this case).
• To view the peak profile of the measurement in progress, click the asterisk of
Sample No. To view a previous measurement, click that row.
• When the Sample Window is opened, the text on the graph may be overly
enlarged. In that situation, close the Sample Window and then open it again.
• During measurement, even if “All Peaks” is selected, because it takes time for
the screen to update, the peak display may not change. In this case, select “All
Peaks” following measurement.
• When the measurement Type is TC/TN, NPOC/TN, TOC/TN or
POC+NPOC/TN, the peak profile of the selected measurement type may not
be displayed even after clicking the measurement type (for example, TC and
TN toggle) tab in the Sample Window. In that situation, click the data in the
Sample Window corresponding to the peak you wish to display.
11. Statistical information about the current set of injections is calculated and displayed in
the Sample Window. As a result, preliminary decisions about the measurements can
be made while the analysis is still in progress.
Note: Information about the current injection is shown in the status box in
the upper right portion of the Sample Window.

TIP » The drop-down list above the graph is used to set the graph display. When Current Peak is
selected, the peak profile of the current injection is drawn in the graph as the measurement
is performed. Use this window to monitor the analysis as it occurs. The blue peak denotes
carbon, while the red peak denotes nitrogen. To see the peak profile of a previous injection,
click its row in the Injection Table. To see the peak profile of all the injections for a sample,
select All Peaks from the drop-down list at the top of the graph. Use the graph right-mouse
menu to customize the peak profile graph.

Reference: Refer to Section 4.4.4.3 "Sample Window" for a detailed description of the Sample Window
options.
12. When the measurements are complete, the autosampler moves to the rinse well for a
flow line rinse and the instrument status tab displays a Ready status. Close the Sample
Window.

¬Evaluating the Results (Step 7)

The Sample Table now contains measurement information in the columns in the right
portion of the table. Use the scroll bars to view the measurement information.
We will check the calibration curve results and then evaluate the results for the unknown
sample.

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Checking the TC Calibration Curve Results

1. Place the cursor in the first row of the Sample Table, which contains analysis
information for the TC calibration.

2. From the View menu, select Calibration Curve, or click the Calibration Curve button
on the toolbar.
The Calibration Curve Properties window for the TC calibration is displayed.
3. Select the Graph tab to view the TC calibration curve data in graph form.

Figure 4.64 Calibration Curve Properties: Graph Tab

The coefficient of determination (r2) value is a measure of the linearity of the

relationship between concentration and area. An r2 value was calculated for the TC
calibration and displayed in the window because we selected the linear regression
calculation when we created the calibration file. Use the r2 value to determine the
success of the calibration. A r2 value of 1 indicates a perfectly linear relationship
between concentration and area. Application methods used for future analyses may
specify an acceptable limit for the r2 value.
4. Select the Data tab to view calibration statistics such as Standard Deviation (SD) and
Coefficient of Variation (CV). These statistics can also be used to evaluate the success
of the calibration.

TIP » A successful calibration can be used for future analyses by specifying the calibration file
name (*.cal) in the method.
5. Close the TC Calibration Curve Properties window when the evaluation is complete.

Checking the TN Calibration Curve Results

Evaluate the TN calibration curve results by placing the cursor in the second row of the
Sample Table, which contains analysis information for the TN calibration. Then follow
Steps 2 through 5 in the procedure listed above for evaluating the TC calibration curve
results.

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Viewing Peak Profiles

1. View peak profiles by placing the cursor in the desired row of the Sample Table and
either selecting Sample Window from the View menu or clicking the Sample button
on the toolbar.
The Sample Window is displayed; this is the same window we used to observe the
real-time injections.
2. To view the peak profiles for all injections in a Sample Table row, select All Peaks
from the drop-down list at the top of the graph.
All peak profiles for the selected row are displayed in the graph.

TIP » When All Peaks is selected from the drop-down list at the top of the graph, clicking in
another row of the Sample Table will automatically update the Sample Window display with
the peak profiles for that row.
3. To view the peak profile for individual injections, click in the appropriate row of the
Injection Table and select Current Peak from the drop-down list at the top of the
graph.

Evaluating the Sample Results

1. Place the cursor in the third row of the Sample Table, which contains analysis
information for the sample.
2. Examine the concentration results by scrolling to the Result column in the Sample
Window.
Note: The results should be close to 50ppm for the TC analysis and
10ppm for the TN analysis.

Figure 4.65 View Sample Results

TIP » Use the TC and TN tabs at the bottom of the Sample Information table to view the results
for both analyses.

3. Close the Sample Window when the evaluation is complete.

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 4.3 Measurement Procedures and Tutorial
4.3.2 Tutorial

Outlier Test
The Outlier Test is used to provide additional information about the measurement result.
1. Place the cursor in the third row of the Sample Table, which contains analysis
information for the unknown sample.
2. From the View menu, select Outlier Test.
Note: The Outlier Test is conducted to identify suspect results. The test
statistically compares all unknown samples that have the same
sample name. Because this tutorial includes only one measurement
of the unknown sample, the outlier test calculation is not
meaningful.

¬Printing a Report (Step 8)

Print a report after measurement is complete and the results have been evaluated.

Selecting the Report Items

1. From the File menu, select Page Setup.
2. The Page Setup window is displayed. Each tab in the window represents a section of
the report and contains several items. Selections will be made on each tab to print a
typical report for the calibration standards and unknown sample.

Reference: Refer to Section 4.4.2.15 "Page Setup" for detailed descriptions of the Page Setup options.
3. On the Instrument tab, ensure that the Print system information check box is selected,
then select the options shown in the figure below.

Figure 4.66 Page Setup: Instrument Tab

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 4.3 Measurement Procedures and Tutorial
4.3.2 Tutorial

4. Click the Calibrations tab and select the options shown in the figure below.

Figure 4.67 Page Setup: Calibrations Tab

5. Click the Samples tab and select the options shown in the figure below.

Figure 4.68 Page Setup: Samples Tab

Note: Use the default selections on the Header and Grid tabs.
6. Click the Miscellaneous tab and enter “Tutorial” in the Organization name field.
Select the Footer check box to include page numbers on the report.
TIP » A company logo can be added to the report header by selecting the Logo check box and
specifying the logo graphic file.

Figure 4.69 Page Setup: Miscellaneous Tab

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 4.3 Measurement Procedures and Tutorial
4.3.2 Tutorial

Previewing the Report

1. Select the Preview button from any of the Page Setup tabs to preview the entire report
before printing.

TIP » The report can also be previewed from outside the Page Setup window by selecting Print
Preview>Sample Report from the File menu.

The Preview feature displays each page of the report exactly as it will be printed.
Notice that each item that was selected in the Page Setup window appears in the
report.

Figure 4.70 Report Appearance

TIP » Magnify the view by clicking the magnifying glass tool, or on the Zoom In button. Move
from page to page by clicking the Next Page and Previous Page buttons.
2. Print the report by clicking the Print button.

This ends the Tutorial.

Reference: The tutorial provided instructions for setting instrument configuration and analysis
parameters, adding calibration standard and unknown sample information to the Sample
Table, creating calibration curves and method files, conducting measurements, and
checking and printing results. More details on all of these procedures are discussed in
Section 3.2 "Instrument Setup and System Properties", Section 4.2 "Setting General
Measurement Parameters", and Section 4.4 "Sample Table Editor".

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 4.3 Measurement Procedures and Tutorial
4.3.3 Ending Measurement

4.3.3 Ending Measurement

Follow the procedure below to end measurement.

Procedure
1. From the Instrument menu, select Standby.

Figure 4.71 Standby Window

2. Two procedures are available for ending measurement:

• Shut down instrument
• Auto restart
These procedures are described below.

Shut Down Instrument

Use the “Shut down instrument” option to end measurement and switch off power to the
instrument.
1. Select “Shut down instrument” in the Standby window, then click the Standby button.
A 30-minute countdown to instrument shutdown begins. During the shutdown pro-
cess, the carrier gas flow and power to the furnace are automatically turned off and
after 30 minutes, the power to the instrument is switched off.
2. To end TN measurement, manually switch off the TN unit using the power switch
located in the lower right area of the ozone generator.
Note: When “Shut down instrument” is selected, the instrument power is
turned off and the power to the autosampler exhaust fan is turned
off. If acidic samples are being measured or if sparging is being
performed using the autosampler in NPOC measurement, there is a
danger that following measurement, volatilization of acid in the
sample could cause corrosion of the autosampler. Do not switch off
the power to the instrument. (Do not select Shutdown.)

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 4.3 Measurement Procedures and Tutorial
4.3.3 Ending Measurement

Auto Restart
The Auto Restart function is used to shut down the instrument and then restart it at a
specified time. Selections are made for the date and time that measurement will next be
performed, as well as for the instrument restart settings. After shutting down the
instrument, the carrier gas flow and power to the furnace are automatically turned off.
Approximately one hour before the restart time, the furnace and the carrier gas will
automatically be turned on to allow the instrument to achieve a Ready state by the restart
time.
1. Select Auto Restart in the Standby window.
2. Select the appropriate instrument restart settings (TC furnace, carrier gas, ozone
generator) and set the restart date and time. If a check is placed in the box beside a
unit, the furnace power remains on and the carrier gas continues to flow. In order to
have the power turned off automatically, do not place a check mark in any of these
boxes.
3. Click the Standby button.
Power to the instrument is automatically switched off and will be automatically
switched on approximately one hour before the restart date and time. Using Auto
Restart, measurement can be performed immediately at the specified startup time.

Reference: Refer to Section 4.4.6.3 "Standby" for detailed descriptions of the available instrument
shutdown options.

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 4.4 Sample Table Editor
4.4.1 Sample Table Window Overview

4.4 Sample Table Editor

The TOC-Control V Sample Table Editor menus and commands are described in this
section.

4.4.1 Sample Table Window Overview

4.4.1.1 Toolbar Functions

If the Toolbar is not visible, select Toolbar from the View menu, then specify the desired
Toolbar options.
Note: Many of the Toolbar functions are disabled until a Sample Table is opened or
communication is established with an instrument.

TIP » A description of each Toolbar button’s function appears when the mouse pointer is
positioned over the button.

TIP » All of the Toolbar commands are also accessible through the Sample Table Editor menus.

New File
Opens a new, blank Sample Table.
Open File
Opens a saved Sample Table. Clicking the button displays the Open dialog box,
in which a *.t32 file can be selected.
Save File
Saves the data in the open Sample Table. If the open Sample Table is new and has
not yet been saved, the Save As dialog box is displayed.
Cut
Removes data from highlighted cells in a table and saves them to the clipboard.
Copy
Copies data from highlighted cells in a table and saves them to the clipboard.
Paste
Copies the contents of the clipboard to a selected location in a table.
Print
Sends the data from the currently displayed window to the printer. Clicking the
button starts printing immediately using the current printer settings.
Help - About
Provides information about the TOC-Control V software.
Background Monitor
Displays the Background Monitor window, which displays the status of the ASI
and the instrument detector(s).

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 4.4 Sample Table Editor
4.4.1 Sample Table Window Overview

Connect
Opens or closes the electronic connection between the instrument and the PC.
Standby
Shuts down or reactivates the instrument.
Start/Continue
Starts measurement. Either the Manual Injection Parameter or Sparging/Acid
Addition window is displayed, depending on the instrument settings.
Stop
Stops the measurement sequence after all injections of the current sample are
complete.
Halt
Immediately stops the current measurement and discards data from the inter-
rupted measurement.
Peak Stop
Stops the measurement sequence and aborts analysis of the current sample. The
peak in progress is treated as if it were a completed analysis.
Properties
Displays the Sample/Method Properties dialog box.
Calibration Curve (View)
Displays the calibration curve data. Highlight the calibration standard row in a
Sample Table to select the calibration curve to examine.
Sample
Opens the Sample Window, which displays detailed information for each sample
injection and can be used to view measurement data in real time.
Method
Opens the Method Properties window, which contains the method parameters for
a selected sample.
Exclude
Excludes a selected sample or injection from the calculation. Toggles to include
an excluded sample.
Recalculate Highlighted
Recalculates the highlighted sample results after applying a new calibration
curve or excluding injections.
Recalculate All
Recalculates all sample results after applying a new calibration curve or exclud-
ing injections.
Delete Highlighted Data
Deletes the highlighted measurement data. This function does not change the
structure of the Sample Table.
Delete All Data
Deletes the measurement data for all samples. This function does not change the
structure of the Sample Table.

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 4.4 Sample Table Editor
4.4.1 Sample Table Window Overview

Format
Displays the Floating Point Format dialog box, where options for numeric for-
mats can be modified.
Font
Displays the Font dialog box, where options for fonts can be modified.
Insert Sample
Opens the Sample Wizard, and allows a sample to be inserted in the active posi-
tion of the Sample Table.
Autogenerate
Opens the Sample Group Wizard, and allows a specified group of samples to be
inserted in the active position of the Sample Table.
Insert Control
Displays the Open dialog box, and allows a selected control sample template to
be added to the Sample Table.
Insert Calibration Curve
Displays the Open dialog box, and allows a selected calibration curve to be added
to the Sample Table.

4.4.1.2 Status Bar and Notification Bar

The Status Bar displays the status of various software functions and is displayed at the
bottom of the open window for all applications. If the Status Bar is not visible, select Status
Bar from the View menu.
The Notification Bar displays information about the status of the TOC-Control V software,
the connection between the instrument and the PC, measurement events, and operation
errors. Use the Options>Display Settings>Notification Bar Settings window to enable,
disable, or select settings for the Notification Bar. Refer to Section 4.4.9.5 "Display
Settings>Notification Bar Settings".

Notification
Bar

Status Bar

Figure 4.72 Status Bar and Notification Bar

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 4.4 Sample Table Editor
4.4.2 File Menu

4.4.2 File Menu

Figure 4.73 File Menu

4.4.2.1 New

The New command opens the New dialog box, which displays the options for all new file
types. The options are Sample Run, Calibration Curve, Method, Control Sample Template,
and Parameter File, as shown in the figure below and described in the text following the
figure.

Figure 4.74 New Dialog Box

TIP » A new file can also be created by clicking the New File button on the Toolbar and typing in
the new file name.
Sample Run
Displays the General Information window, which can also be accessed by select-
ing General Information from the Options menu. Refer to Section 4.4.9.1 "Gen-
eral Information" for a detailed description of the General Information window.
Calibration Curve
Opens the Calibration Curve Wizard, which can also be accessed by selecting
Calibration Curve from the Insert menu. Refer to Section 4.4.2.2 "Calibration
Curve" for a detailed description of the Calibration Curve Wizard.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method
Opens the Method Wizard. Refer to Section 4.4.2.3 "Method Wizard" for a
detailed description of the Method Wizard.
Control Sample Template
Opens the Control Sample Wizard. Refer to Section 4.4.5.3 "Control" for a
detailed description of the Control Sample Wizard. Refer to Appendix B for a
description of the Control Charts function.
Parameter File
Displays the Save As dialog box, which can be used to save a parameter file.
OK Button
Opens a new file for the selected icon, and closes the New dialog box.
Cancel Button
Press the Cancel button to close the New dialog box without making a new file.

4.4.2.2 Calibration Curve

The Calibration Curve command is used to insert a calibration curve into the Sample Table.
Selecting the command displays the File>Open dialog box.

Figure 4.75 Selecting Insert>Calibration Curve displays the File>Open dialog box

A table of calibration information is displayed in the window at the bottom of the Open
dialog box after a calibration curve is selected. Click the OK button to insert the selected
calibration curve into the Sample Table. Click the Cancel button to abort the operation.
Note: • The Insert>Calibration Curve command is not available during sample
analysis.
• An error message is displayed if the selected file does not have the correct
format or is not a calibration curve.

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 4.4 Sample Table Editor
4.4.2 File Menu

To create a new calibration curve for insertion into the Sample Table, click the New button
to open the Calibration Curve Wizard. The Calibration Curve Wizard consists of several
windows, each of which defines specific parameters for the calibration curve, as described
below.

TIP » The Calibration Curve Wizard can also be accessed by selecting File>New and double-
clicking the Calibration Curve icon in the New dialog box.
Calibration Curve Wizard (Page 1) System Information

Figure 4.76 Calibration Curve Wizard (Page 1) System Information

Parameter Description
System Select the system to be used.
User Displays the user name. This field cannot be changed.
Date of Creation Displays the current system date and time. This field cannot
be changed.
Comment Enter a comment (512 characters maximum).

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 4.4 Sample Table Editor
4.4.2 File Menu

Calibration Curve Wizard (Page 2) Calibration Curve Type

The Calibration Curve Type window is used to specify the calibration curve type.

Figure 4.77 Calibration Curve Wizard (Page 2) Calibration Curve Type

Calibration Curve Wizard (Page 3) Analysis Information

Parameter Description
Calibration points are distrib- Select this option to calculate the calibration point concentra-
uted uniformly over the con- tions automatically. The software will calculate the concen-
centration range trations by distributing them in equal amounts over the
measuring range of the calibration curve.
Edit calibration points manu- Select this option to enter the calibration point concentrations
ally manually on a subsequent Wizard page, the Calibration
Points List.
Calibration curve according Select this option to create a calibration curve according to
to DIN 38402/P-51 DIN 38402. This type of curve consists of 10 calibration stan-
dards, with 10 injections of the lowest and highest standards
and a single injection of the intermediate standards.
Calibration curve according Select this option to create a calibration curve that consists of
to USP/EP 2 calibration standards with concentrations between 0 and
500µg/L and one control sample with a concentration of
500µg/L.

Calibrations using automatic dilution

Dilution Factor Manual Set- For manually setting dilution factor of standard solution.
ting Enter the dilution factor.
Dilution Factor Automatic Automatically calculates dilution factor for standard solution,
Setting and performs measurement using that dilution factor.
Use Source Dilution Function Prepares standard solution automatically inside the instru-
ment, and performs measurement using that diluted standard
solution.

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 4.4 Sample Table Editor
4.4.2 File Menu

Note: In the case of the TOC-VCPN, dilution measurement cannot be performed for IC
measurement. Therefore, since the dilution function will not work even if Use
Source Dilution Function or Dilution Factor Manual Setting are selected, select
Dilution Factor Automatic Setting. In IC measurement using the TOC-VCPH, the
dilution function can be used.
The Analysis Information window is used to specify the type of analysis and the standard
name for the calibration curve.

Figure 4.78 Calibration Curve Wizard (Page 3) Analysis Information

Parameter Description
Analysis Select the analysis type.
Default Sample Name Enter the sample name for the calibration standards (64 char-
acters maximum).
Default Sample ID Enter the default sample identification for the calibration
standards (64 characters maximum).
Calculation Method Select the calculation method to be used for the calibration
from the drop-down list. Available calculation methods are
point-to-point and linear regression. Refer to Section 4.4.4.5
for detailed descriptions of the calibration methods.
Zero Shift Select this option to shift the calibration curve through the
origin. Refer to Section 4.4.4.5 for a detailed description of
the Zero Shift option.
Multiple Injections Select to enable the syringe to draw up a single aliquot with a
volume equal to that required for all injections of the stan-
dard. When this option is not selected, the syringe will draw
up a separate aliquot for each injection; as a result, selecting
this option reduces analysis time.
File Name Enter the file name of the calibration curve.

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 4.4 Sample Table Editor
4.4.2 File Menu

Calibration Curve Wizard (Page 4) Calibration Measurement Parameters

The Calibration Measurement Parameters window is used to specify measurement
parameters for the calibration standards.

Figure 4.79 Calibration Curve Wizard (Page 4) Calibration Measurement Parameters

Parameter Description
Units Select the concentration units from the options on the drop-
down list.
Concentration Range Enter the maximum and minimum concentrations of the cali-
bration curve standard solutions.
No. of Cal. Points Enter the number of calibration standards that will be used to
create the calibration curve.
No. of Injections Enter the minimum/maximum number of injections for the
calibration standards.
No. of Washes Specifies the number of times the syringe is to be washed
with standard prior to the first injection. Note that if the Auto
Dilution option was selected, the standard will be diluted and
the syringe will then be washed with the diluted standard.
Enter an integer from 0 to 10.
SD Max and CV Max Specifies the maximum standard deviation and coefficient of
variation that is acceptable for the injections. Enter a value
ranging from 0 to 9999 for SD Max and from 0 to 100 for CV
Max. If either of these values are met, no additional injec-
tions are required. However, if both of these values are
exceeded, the calibration standards are automatically rein-
jected up to the maximum number of times specified in the
No. of Injections field. The SD Max and CV Max fields are
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
Sparge Time Enter the length of time sparging will occur. (0 - 20 minutes)
Acid Addition Enter the desired quantity of acid to be added. This option is
available only for NPOC or related analyses.

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4.4.2 File Menu

Calibration Curve Wizard (Page 5) Calibration Points List

The Calibration Points List window displays a list of parameters for each calibration point.
The parameters can be edited by using the buttons below the list. A user must have access
rights for updating data to edit calibration information.

Figure 4.80 Calibration Curve Wizard (Page 5) Calibration Points List

Parameter Description
No. Displays the calibration point number. Note that the standards
will be analyzed in the order shown. To add a calibration
point at a certain position, click the desired number in the
“No.” column, then click the Add button and enter the appro-
priate information. The new point will be added in the speci-
fied position, and the point that was previously in that
position will move down the list to the next position.
Inj. Volume Displays the injection volume for the calibration standards.
Calibration Points Displays a table of measurement parameters (such as those
entered in the previous page of the Calibration Curve Wizard)
for each calibration point. To edit the parameters for a cali-
bration point, highlight the point in the table and click the
Edit button. To add a calibration point, click the appropriate
number in the No. column to specify the insertion point, then
click the Add button. To delete a calibration point, highlight
the point in the table and click the Delete button. To delete all
calibration points, click the Delete All button.

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 4.4 Sample Table Editor
4.4.2 File Menu

Click the Edit and Add buttons to display the Edit Calibration Point Parameters window.
This window is used to enter calibration points manually and to edit the parameters of
existing calibration points.

Figure 4.81 Edit Calibration Point Parameters Window

Parameter Description
Calibration Point No. Displays the calibration point number. This field will reflect
the number selected by clicking in the “No.” field in the Cali-
bration Points List. The number cannot be changed directly in
the window.
Standard Solution Conc. Enter the concentration of the calibration standard solution.
When creating a calibration curve from a single standard
solution by using the Auto Dilution function, enter the con-
centration of the original standard solution in this field.
Auto Dilution Enter the factor by which the instrument should automati-
cally dilute the calibration standard solution to obtain the
desired concentration for the calibration point.
Cal. Point Conc. Displays the actual concentration of the calibration point. The
concentration is calculated automatically based on the values
entered into the Standard Solution Conc. and Auto Dilution
fields.
No. of Injections Enter the minimum and maximum number of injections.
SD Max and CV Max Enter the maximum standard deviation or coefficient of vari-
ation values.

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 4.4 Sample Table Editor
4.4.2 File Menu

Calibration Curve Wizard (Page 6) Peak Time Parameters

The Peak Time Parameters window is used to set peak detection parameters.

Figure 4.82 Calibration Curve Wizard (Page 6) Peak Time Parameters

Setting Item Description

Use default settings Select this option to use the default peak detection parame-
ters. When this option is selected, all other options in this
window are disabled.
Allowed peak start delay The allowed peak start delay is the amount of time (in min-
utes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.

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 4.4 Sample Table Editor
4.4.2 File Menu

Calibration Curve Wizard (Page 7) History

The History window is used to enable the History Log. The History Log records all
modifications to the calibration curve properties. The History Log can be set to require
users to enter comments for each modification.
If the History Log is not required, it need not be enabled, as the software operates properly
without it.
Note: Once the History Log is enabled, it cannot be changed. All modifications to the
calibration curve properties will be tracked. If the mandatory comment option is
selected, the user will be required to enter a comment each time any parameter in
the calibration curve is modified.

Figure 4.83 Calibration Curve Wizard (Page 7) History

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the system. Once the History Log is enabled, it
cannot be changed if GLP is selected during installation. The
GLP laboratory guidelines require that a history of changes
be maintained for the system.
User has to comment all Select this option to require the user to comment all modifi-
modifications cations.

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 4.4 Sample Table Editor
4.4.2 File Menu

4.4.2.3 Method Wizard

The Method Wizard is used to set method parameters and is accessed by selecting
File>New>Method. The Method Wizard consists of several windows, each of which is
described below. The Back and Next buttons are used to navigate between windows. Note
that each set of parameters selected for a specific method applies only to that method.
Note: Selected windows in the Method Wizard will be repeated for combined analysis
types such as TOC, POC + NPOC. Each duplicate window represents one analy-
sis type. Parameters that are not applicable to an analysis type will not appear in
the Method Wizard window.
Method Wizard (Page 1) System Information

Figure 4.84 Method Wizard (Page 1) System Information

Setting Item Description

System Select one of the configured instruments.
Operator Displays the current operator name.
Date of Creation Displays the current system time.
Comment Enter a comment (512 characters maximum), if desired.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method Wizard (Page 2) Analysis Information

The Analysis Information window is used to set analysis parameters for the method being
created.

Figure 4.85 Method Wizard (Page 2) Analysis Information

Setting Item Description

Analysis Select the analysis type from the drop-down list.
Default Sample Name Enter the default sample name (64 characters maximum).
Default Sample ID Enter the default sample ID (64 characters maximum).
Dilution Enter the preparation dilution factor, which will be used to
calculate concentration results. The default value is 1.
No. of Determinations Enter the number of times each sample is to be measured.
Note that determinations and injections are different; each
determination is made up of one or more injections.
File Name Enter the name of the new method. Click the Browse button
to save the file in a directory other than the default directory.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method Wizard (Page 3) Calibration Curves

The Calibration Curves window is used to specify the calibration curves that will be used to
calculate results for samples analyzed by the method. Up to 3 calibration curves can be
entered and, during analysis, the system automatically determines which curve is most
suitable for the sample. Refer to Section 6.2.5 "Automatic Selection of Optimum
Calibration Curve".

Figure 4.86 Method Wizard (Page 3) Calibration Curves

Setting Item Description

Analysis Displays the previously selected analysis type.
Calibration Curve 1/2/3 Enter the name of the calibration curve or click the Browse
button to select a file using the File>Open dialog box.
Skip the injection parameter Select this item to skip the Injection Parameters window of
pages of the wizard the Method Wizard. Use this option when the sample injec-
tion parameters will be the same as those used for calibration
curve measurements.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method Wizard (Page 4) Injection Parameters

The Injection Parameters window is used to specify the injection parameters for the
method.

Figure 4.87 Method Wizard (Page 4) Injection Parameters

Setting Item Description

Analysis Displays the previously selected analysis type.
Units Select the concentration units to be used for samples.
Injection Volume Enter the injection volume.
Expected Conc. Range Enter the expected sample concentration if it is known.
No. of Injections Enter the minimum/maximum number of injections for the
samples that will be analyzed using this method.
SD Max Enter the maximum standard deviation that is acceptable for
the injections. If this value is met, no additional injections are
required. However, if both this value and the CV Max value
are exceeded, the samples are automatically reinjected up to
the maximum number of times specified in the No. of Injec-
tions field. The SD Max field is disabled if the No. of Injec-
tions is 1 or if the minimum is equal to the maximum.
CV Max Enter the maximum coefficient of variation that is acceptable
for the injections. If this value is met, no additional injections
are required. However, if both this value and the SD Max
value are exceeded, the samples are automatically reinjected
up to the maximum number of times specified in the No. of
Injections field. The CV Max field is disabled if the No. of
Injections is 1 or if the maximum and minimum values are
the same.
No. of Washes Enter the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilu-
tion option was selected, the sample will be diluted and the
syringe will then be washed with the diluted sample.

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 4.4 Sample Table Editor
4.4.2 File Menu

Setting Item Description

Auto Dilution Enter a dilution factor for the samples. The instrument will
automatically dilute the samples by this factor, and the result
will be multiplied by the factor to obtain the final concentra-
tion. The default Auto Dilution value is 1.
Sparge Time Enter the desired sparge time. This option is available only
for POC, NPOC, and related analyses. The default Sparge
Time value is 1.
Acid Addition Enter the desired quantity of acid to be added. This option is
available only for NPOC or related analyses.
Multiple Injections Select to enable the syringe to draw up a single sample ali-
quot with a volume equal to that required for all injections of
the sample. When this option is not selected, the syringe will
draw up a separate sample aliquot for each injection. Select-
ing this option reduces analysis time.
Use blank check area Select to include blank check result in the concentration cal-
culation.
Auto correction of inj. vol. Select to enable the instrument to automatically adjust the
and dilution injection volume and dilution factor when the peak height for
the initial injection exceeds full scale. After the adjustment,
measurement will be repeated.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method Wizard (Page 5) Peak Time Parameters

The Peak Time Parameters window is used to set peak integration parameters.

Figure 4.88 Method Wizard (Page 5) Peak Time Parameters

Setting Item Description

Analysis Displays the previously selected analysis type.
Use default settings Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay The allowed peak start delay is the amount of time (in min-
utes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.

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 4.4 Sample Table Editor
4.4.2 File Menu

Method Wizard (Page 6) USP/EP

The USP/EP window is displayed only for TC or NPOC methods, and is used to enable
samples to be checked in accordance with USP standards. Select the check box to enable
the function.

Figure 4.89 Method Wizard (Page 6) USP/EP

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4.4.2 File Menu

Method Wizard (Page 7) History

The History window is used to enable the History Log. The History Log records all
modifications to the method. The History Log can be set to require users to enter comments
for each modification.
Note: Once the History function is enabled, it cannot be changed. All modifications to
the method will be tracked. If the mandatory comment option is selected, the user
will be required to enter a comment each time any method parameter is modified.

Figure 4.90 Method Wizard (Page 7) History

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the system. Once the history log is enabled, it
cannot be changed.
User has to comment all Select this option to require comments or approval for all
modifications method modifications. If the History Log is not required, it
need not be enabled, as the software operates properly with-
out it.

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4.4.2 File Menu

4.4.2.4 Open

The Open command is used to select and open a Sample Table, Method, Calibration Curve,
Parameter, or Control Sample Template file. Save the open Sample Table before executing
the Open command. More than one Sample Table can be opened at the same time.
Selecting the Open command displays the Open dialog box shown below.

Figure 4.91 Open Dialog Box

TIP » The Open dialog box can also be displayed by clicking the Open File button on the Toolbar.

Table 4.2 displays the types of files that can be opened using this function. No other file
types should be opened using this menu command.
Table 4.2 • Acceptable File Types for Open Function
File Extension Description
.t32 Sample Table
.met Method
.cal Calibration Curve
.tpl Control Sample Template
.trd Data Profile

The opened file replaces the currently displayed table or function, depending on the type of
file selected.
Dialog Box Options Description
File name Enter the name of the file to be opened.
Look in Find the file to be opened by choosing the appropriate folder
or accessing other directories. The selected file will appear in
the File name text box.
Files of type Select the type of file from the drop-down list. Choose only
files of type *.t32 when opening a Sample Table.
Open button Opens the selected file.
Cancel button Aborts the Open operation.

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4.4.2 File Menu

4.4.2.5 Close

The Close command is used to close the current window and is an option only when a file is
open. If the open file has not been saved and the Close command is selected, the Save As
dialog box is displayed. Refer to Section 4.4.2.7 "Save As". Enter a name for the file and
click the OK button to save the file. If the open file has been modified but not saved and the
Close command is selected, a dialog box is displayed as shown below. Click the Yes button
to save the file before closing. Click the No button to close the file without saving the
modified information. Click the Cancel button to abort the Close command.

Figure 4.92 Dialog box for Saving Modified Data

4.4.2.6 Save

The Save command is used to save data in the current active file. If the file has not yet been
saved and the Save command is selected, the Save As dialog box is displayed. Refer to
Section 4.4.2.7 "Save As".

TIP » The Save command can also be executed by selecting the Save File button on the Toolbar.

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4.4.2 File Menu

4.4.2.7 Save As

The Save As command is used to save the current active file with a new file name.
Selecting the command opens the Save As dialog box shown below. Button options in the
dialog box are similar to those in the Open dialog box. Refer to Section 4.4.2.4 "Open".
Click the Save button to save the data under the specified file name. Click the Cancel
button to abort the Save As operation.

Figure 4.93 Save As Dialog Box

Dialog Box Options Description

File name Enter a name for the file. The applicable file extension will
automatically be added if it is not entered.
Save in Select the directory in which the file is to be saved by choos-
ing the folder or accessing other directories from the drop-
down list. The currently selected directory appears in the
Save in text field.
Save as type Select the type of file from the drop-down list. A list of avail-
able file types is listed in Table 4.2.

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4.4.2 File Menu

4.4.2.8 ASCII Export Options

The ASCII Export function is used to export Sample Table data to an ASCII file. Open a
Sample Table that contains completed measurement data. Select ASCII Export from the
File menu. The Save As dialog box is displayed. Refer to Section 4.4.2.7 "Save As". Enter
a file name for the ASCII file to be created and confirm that the “Save as type” field
contains the ASCII file type (*.txt). If the entered file name matches a file that already
exists, a confirmation message is displayed.

Figure 4.94 Save As Confirmation Message

Click the Yes button to overwrite the existing file and close the dialog box. Click the No
button to redisplay the Save As dialog box and enter a new file name.
Select the ASCII Export Options command from the File menu. The ASCII Export Options
dialog box, which contains several tabs, is displayed. Each tab contains a list of export
options, as shown in the figures below. Note that on each tab, certain items are selected by
default. Individual options can be selected or deselected by clicking in the check box. Use
the Select All and Select None buttons to quickly select and deselect all options on a tab.
Use the Default button to select the default options on a tab. Click the Cancel button to exit
the ASCII Export Options dialog box without saving changes. Click the OK button to save
changes and exit the ASCII Export Options window.
Header Tab

Figure 4.95 ASCII Export Options Window: Header Tab

Setting Item Description

Export header information Select to enable export of the selected header options. This
option is selected by default.

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4.4.2 File Menu

System Tab

Figure 4.96 ASCII Export Options Window: System Tab

Setting Item Description

Export system information Select to enable export of the selected system options. This
option is selected by default.

Data Tab

Figure 4.97 ASCII Export Options Window: Data Tab

Setting Item Description

Export data Select to enable export of the selected data options. This
option is selected by default.

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4.4.2 File Menu

Miscellaneous Tab

Figure 4.98 ASCII Export Options Window: Miscellaneous Tab

The Miscellaneous tab contains additional options for the format of exported data. To
change data format, open a Sample Table, select File>ASCII Export Options, then select
the file to which changes should be made. On the Miscellaneous tab, select the desired type
of Separator from the drop-down list. The Separator is the type of delimiter that will be
used to separate items of data. Select the “Export strings in quotation marks” option to
enclose all of the character string items in quotation marks.

4.4.2.9 Database Export

The Database Export command is used to enable automatic export of data to an external
(Microsoft Access) database during analysis. Selecting the command displays the
Database Options window.

Figure 4.99 Database Options Window

Setting Item Description

Enable automatic database Select this option to enable the database export function
export
Database Enter the name and filepath of the database, or click the
Browse button to select the database using the File>Open
dialog box.

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4.4.2 File Menu

4.4.2.10 Print>Table

The Print>Table command is used to print the active Sample Table in a table format. Select
this command to open the Print dialog box, which may have a variable display depending
on the installed printer driver. Specify items to be included in the printout by using the Page
Setup command. Refer to Section 4.4.2.15 "Page Setup" for more information.

Figure 4.100 Print Dialog Box

The Name text field identifies the printer that will be used to print the table. Specify a
different printer by selecting it from the Name drop-down list.
Setting Item Description
Properties Modify the printer settings using standard Windows proce-
dures.
Print range Click the All radio button to print all pages of the table. Click
the Pages radio button and enter the page numbers to be
printed if all pages are not desired.
Number of copies Enter the number of copies to be printed.

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4.4.2 File Menu

4.4.2.11 Print>Sample Report

The Print>Sample Report command is used to open the Print dialog box to print the Sample
Table in report format. The print dialog box is the same as that described in Section
4.4.2.10 "Print>Table".

Figure 4.101 Print Dialog Box

4.4.2.12 Print Preview>Table

The Print Preview>Table option is used to display the sample table before printing. Use the
buttons at the top of the Print Preview window to change the display or print the table, as
described below.
Button Description
Next Page and Previous Page Click the Next Page button to display the next page of the
report. Click the Previous page button to display the previous
page of the report. Note that the Next Page button is disabled
when the last page of the report is displayed, and the Previous
Page button is disabled when the first page of the report is
displayed.
One Page/Two Page Click the One Page button to display one page at a time in the
Print Preview window. After selection, the button toggles to
the Two Page button. Click the Two Page button to display
two pages side by side.
Zoom In and Zoom Out Click the Zoom In and Zoom Out buttons to change the mag-
nification of the displayed pages. Three different zoom fac-
tors are available. Repeated selection of either option will
continue to increase or decrease the magnification, as appli-
cable.
Close Click the Close button to close the Print Preview window and
return to the previous window. Note that the Print Preview
window must be closed to edit the report.
Print Click the Print button to print the report.

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4.4.2 File Menu

4.4.2.13 Print Preview>Sample Report

The Print Preview>Sample Report option is used to display the sample report before
printing. Use the buttons at the top of the Print Preview window to change the display or
print the report, as described in Section 4.4.2.12 "Print Preview>Table".

Figure 4.102 Print Preview>Report Window

4.4.2.14 Print Setup

The Print Setup command is used to set print options. Select this command to open the
Print Setup dialog box, which may have a variable display depending on the installed
printer driver. Modifications to the Print Setup dialog box are saved until the TOC-Control
V software is exited.

Figure 4.103 Print Setup Dialog Box

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4.4.2 File Menu

4.4.2.15 Page Setup

The Page Setup command is used to select items to be printed on a report or table and to
specify format parameters such as margins, headers, and footers. Selecting the command
displays the Page Setup window, which consists of several tabs. Each tab contains a list of
page setup options shown in the figures below. On each tab, certain options are selected by
default. Individual options can be selected or deselected by clicking in the check box. Use
the Select All and Select None buttons to quickly select and deselect all options on a tab.
Use the Default button to select the default options for a tab. Click the Cancel button to exit
the Page Setup window without saving changes. Click the OK button to save changes and
exit the Page Setup window.
Instrument Tab
The Instrument tab displays a list of instrument information items that can be printed on the
report.

Figure 4.104 Page Setup Window: Instrument Tab

Calibrations Tab
The Calibrations tab displays a list of calibration information items that can be printed on
the report.

Figure 4.105 Page Setup Window: Calibrations Tab

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4.4.2 File Menu

Samples Tab
The Samples tab displays a list of sample information items that can be printed on the
report.

Figure 4.106 Page Setup Window: Samples Tab

Header Tab
The Header tab displays a list of header items that can be printed on the report.

Figure 4.107 Page Setup Window: Header Tab

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4.4.2 File Menu

Miscellaneous Tab
The Miscellaneous tab displays a list of format items for the report, as described below.

Figure 4.108 Page Setup Window: Miscellaneous Tab

Setting Item Description

Margins Use the spin controls to enter the page margins (in mm).
Footer, Page No. Select this option to print the page number in the footer of
each page.
Header Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
User: Select this option to print the current user name in the
page header.
Document name: Select this option to print the document file
name in the page header.

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4.4.2 File Menu

4.4.2.16 Exit

The Exit command is used to exit the Sample Table Editor. If the active file has been
modified but not saved and the Exit command is selected, a dialog box is displayed as
shown below. Click the Yes button to save the file before exiting. Click the No button to
exit without saving the modified information. Click the Cancel button to abort the Exit
command.

Figure 4.109 Prompt to Save Data Changes

If the software is connected to an instrument and the Exit command is selected, a dialog
box is displayed as shown below. Click the OK button to disconnect the instrument before
exiting the software. Click the Cancel button to abort the Exit command.

Figure 4.110 Prompt to Disconnect Instrument

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 4.4 Sample Table Editor
4.4.3 Edit Menu

4.4.3 Edit Menu

The Edit menu contains functions that allow a user to modify data. To change data using the
Edit menu functions, a user must have the appropriate access rights. Options such as Cut,
Copy, and Paste are available only when a content selection from an open file is made.

Figure 4.111 Edit Menu

4.4.3.1 Undo

The Undo function is used to reverse the last change made in the active Sample Table and is
only available after the user changes the content of a cell in the table. The Undo function is
not available during actual measurement or when the user has inserted or deleted completed
samples, calibration curves, or control samples.

4.4.3.2 Cut/Copy/Paste

The Cut, Copy, and Paste functions are used to edit selected Sample Table cells and rows.
The Cut command deletes selected information from rows or cells and stores it on the
clipboard. Note that the Cut command cannot be used to delete entire samples after
measurement is completed. The Copy command copies selected data from rows or cells and
stores it on the clipboard. The Paste command copies the contents of the clipboard to the
selected cells or rows of the table. When pasting an entire row, click the destination row
number to highlight the entire destination row, then execute the Paste command.
Note: • When pasting, do not select a destination row that currently contains data.
The data will be overwritten!
• The Cut, Copy, and Paste commands can also be accessed by clicking the
icons on the Toolbar.

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4.4.3 Edit Menu

4.4.3.3 Replace

The Replace function is used to replace text in Sample Table cells with specified text.
Select the Replace function to open the Replace dialog box. The Replace command can be
used to replace data in the Sample Name, Sample ID, Dilution, and Comment fields of the
Sample Table. The command cannot be used to replace data for samples after measurement
is complete.

Figure 4.112 Replace Dialog Box

Setting Item Description

Find what Enter the text to be searched for.
Replace with Enter the text that the searched-for text should be replaced
with.
Match case Select to perform a case-sensitive text search.
Find Next Select to begin the search and to continue a search that has
already begun.
Replace Select to replace the found text with the text in the “Replace
with” field.
Replace All Select to replace all occurrences of found text with the text in
the “Replace with” field.
Cancel Select to close the Replace dialog box.

4.4.3.4 Find

The Find function is used to search for specified text. Selecting the Find command opens
the Find dialog box, which is similar to the Replace dialog box.and displays the options
described below. Refer to Section 4.4.3.3 "Replace".
Setting Item Description
Find what Enter the text to be searched for.
Match case Select to perform a case-sensitive text search.
Direction Click the Up radio button to search the table backwards from
the current location. Click the Down radio button to search
the table forward from the current location.
Find Next Select to begin the search and to continue a search that has
already begun.
Cancel Select to close the Find dialog box.

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4.4.3 Edit Menu

4.4.3.5 Exclude

The Exclude function is used to exclude selected injections from the calculations. A user
must have access rights for updating data to use the Exclude function. To exclude data,
highlight the desired injection shown in the Sample Window Injection Table and select
Exclude from the Edit menu. A confirmation dialog box is displayed. Click the Yes button
to exclude the selected data. Click the No button to abort the operation.

Figure 4.113 Exclude Confirmation Dialog Box

4.4.3.6 Recalculate>All

The Recalculate>All function is used to recalculate the data for all measured samples in a
Sample Table after applying a new calibration curve or excluding injections. To execute the
command, open the appropriate Sample Table and select Recalculate All from the Edit
menu. A message is displayed in the Notify folder of the Notification Bar when the
recalculation is complete.

4.4.3.7 Recalculate>Highlighted

The Recalculate>Highlighted function is used to recalculate the data for selected samples
after applying a new calibration curve or excluding injections. The function is similar to the
Recalculate All function described in Section 4.4.3.6 "Recalculate>All". To execute the
command, open the appropriate Sample Table, highlight the samples to be recalculated, and
select Recalculate Highlighted from the Edit menu.

4.4.3.8 Delete Data>All

The Delete Data>All function can only be used if the GLP conformity was disabled during
system installation. The function is used to delete all measurement data in the Sample
Table. The Sample Table structure can then be used to enter new data. A user must have
access rights for updating data to use the Delete Data>All function.
To use the Delete Data>All function, open a Sample Table that contains measurement data
and select Delete Data>All from the Edit menu. A confirmation dialog box is displayed, as
shown in the figure below. Click the Yes button to delete the data. Click the No button to
abort the operation. A message is displayed on the Notifications tab in the Notification Bar
when the data has been deleted.

Figure 4.114 Delete Data Confirmation Dialog Box

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 4.4 Sample Table Editor
4.4.3 Edit Menu

4.4.3.9 Delete Data>Highlighted

The Delete Data>Highlighted function is used to delete the measurement data for selected
samples. To execute the command, open the appropriate Sample Table, highlight the
samples to be deleted, and select Delete Data>Highlighted from the Edit menu. A message
is displayed on the Notifications tab in the Notification Bar when the selected data has been
deleted.

4.4.3.10 Import

The Import function is used to import data from an ASCII file into a Sample Table. Note
that the Import function is not available during sample analysis. To import data, open the
destination Sample Table and place the cursor in the row of the table into which data will be
imported. Select the Import function from the Edit menu. The Open dialog box is
displayed. Select the ASCII file from which data will be imported. The data is inserted in
the current position of the active Sample Table.

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 4.4 Sample Table Editor
4.4.4 View Menu

4.4.4 View Menu

The View menu contains options for viewing calibration, method, and sample information,
and for selecting settings for the display screen.

Figure 4.115 View Menu

4.4.4.1 Calibration Curve

The View>Calibration Curve command is used to view the calibration curve information
associated with a sample. Place the cursor in the desired row of the Injection Table and
select the Calibration Curve command from the View menu. The Calibration Curve
Properties window is displayed. Refer to Section 4.4.4.5 "Properties".

TIP » The Calibration Curve Properties window can also be displayed by clicking the
Calibration Curve (View) button on the Toolbar.

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4.4.4 View Menu

4.4.4.2 Method

The View>Method command is used to view the properties associated with a method.
Selecting the command displays the Sample/Method Properties window, which consists of
several tabs, including a separate tab for each applicable method. Each tab lists options for
method properties, as shown in the figures below. Individual options can be selected,
deselected, or edited by clicking in the check boxes or entering information into the text
fields. Note that certain options will be disabled if sample analysis is complete. Each tab
contains the same command buttons: OK, Cancel and Apply. Click the OK button to save
changes and exit the Sample/Method Properties window. Click the Cancel button to exit the
Sample/Method Properties window without saving changes. Click the Apply button to save
changes without exiting the Sample/Method properties window.

Figure 4.116 Sample/Method Properties Window: Common Tab

Common Tab
Setting Item Description
System Displays the system currently in use. Changes cannot be
made to this field.
User Displays the name of the user who created the method.
Changes cannot be made to this field.
Date of Creation Displays the date on which the method was created. Changes
cannot be made to this field.
Comment Enter a comment (512 characters maximum).

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4.4.4 View Menu

Parameter Tab

Figure 4.117 Sample/Method Properties Window: Parameter Tab

Setting Item Description

Analysis Displays analysis type. Changes cannot be made to this field.
Dilution Displays the preparation dilution factor, which will be used to
calculate sample concentrations. This field can be edited.
Sample Name Displays the default sample name (64 characters maximum).
This field can be edited.
Sample ID Displays the default sample ID (64 characters maximum).
This field can be edited.
No. of Determinations Displays the number of times (1-10) the sample is to be mea-
sured. Note that determinations and injections are different;
each determination is made up of one or more injections. This
field can be edited.
Perform sample checking Select to enable USP sample checking.
according to USP/EP
Current Method Displays the file name of the current method. Changes cannot
be made to this field.

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4.4.4 View Menu

TC Tab

Figure 4.118 Sample/Method Properties Window: TC Tab

Setting Item Description

Analysis Parameters Units: Displays the concentration units. This field can be edited by selecting
another option from the drop-down list.
No. of Injections: Displays the minimum/maximum number of injections for the
samples analyzed with this method. This field can be edited.
No. of Washes: Displays the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilution option was
selected, the sample will be diluted and the syringe will then be washed with the
diluted sample. This field can be edited.
SD Max: Displays the maximum standard deviation. If this value is met, no
additional injections are required. However, if both this value and the CV Max
value are exceeded, the samples are automatically reinjected up to the maxi-
mum number of times specified in the No. of Injections field. This field can be
edited.
CV Max: Displays the maximum coefficient of variation. If this value is met, no
additional injections are required. However, if both this value and the SD Max
value are exceeded, the samples are automatically reinjected up to the maxi-
mum number of times specified in the No. of Injections field. This field can be
edited.
Acid Addition: Displays the quantity of acid to be added to each sample. This
value is expressed as a percent or the sample volume and is available only for
NPOC and related analyses. This field can be edited.

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4.4.4 View Menu

Setting Item Description

Peak Time Parameters Use default settings: Select this option to use the default settings for peak inte-
gration.
Allowed peak start delay: Displays the amount of time (in minutes) that can
elapse before the analysis is stopped because a peak is not detected. This field
can be edited by entering a number between 0 and 20:00. This option is disabled
when Use default settings is selected.
Total integration time: Displays the amount of time (in minutes) that analysis
continues after the end of the peak is detected. This field can be edited by enter-
ing a number between 4:50 and 20:00. This option is disabled when Use default
settings is selected.
Multiple Injections Select this option to enable the syringe to draw up a single sample aliquot with a
volume equal to that required for all injections of the sample. When this option
is not selected, the syringe will draw up a separate sample aliquot for each
injection; as a result, selecting this option reduces analysis time.
Auto correction of inj. Select this option to enable the instrument to automatically adjust the injection
volume and dilution volume and dilution factor when the peak height for the initial injection exceeds
full scale. After the adjustment, measurement will be repeated.
Auto Dilution Displays the factor by which the instrument will automatically dilute the sam-
ple. This field can be edited.
Inj. Volume Displays the injection volume. This field can be edited.
Expected Conc. Range Enter the expected concentration if it is known.
Use area retrieved from Select to include blank check result in the concentration calculation.
the blank check
Calibration Curve 1/2/3 Displays the name(s) of calibration curve(s) used to quantitate samples ana-
lyzed by the method. These fields can be edited by entering a calibration curve
file name or clicking the Browse button to search for the file.

IC Tab
The IC tab options are similar to those described above for the TC tab.

Figure 4.119 Sample/Method Properties Window: IC Tab

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4.4.4 View Menu

NPOC and POC Tabs

The NPOC and POC tab options are similar to those described above for the TC tab.

Figure 4.120 Sample/Method Properties Window: NPOC Tab

TN Tab
The TN tab options are similar to those described above for the TC tab, except that some
options (such as Use area retrieved from blank check) are not available for TN
measurements.

Figure 4.121 Sample/Method Properties Window: TN Tab

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4.4.4 View Menu

History Tab
If the History Log was enabled when the method was created, the History tab displays a list
of changes made to the method parameters. If the History Log was not enabled previously,
it can be enabled on the History tab.

Figure 4.122 Sample/Method Properties Window: History Tab

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the system. If the History Log is not required, it
need not be enabled, as the software operates properly with-
out it. Once this is enabled, it cannot be disabled.
User has to comment all Select this option to require comments or approval for all
modifications modifications. If the History Log is not required, it need not
be enabled, as the software operates properly without it. Once
this is enabled, it cannot be disabled.
ACSII Export The displayed items in the list are exported as tab-delimi-
nated text files.

A list of the Comment dialog box contents is shown below:

Table 4.3 • Comment dialog box contents
Item Description
Date/Time Displays the date and time of the modification.
User Displays the user who made the modification.
Changed item Describes the parameter that changed.
From Displays the previous parameter value.
To Displays the new parameter value.
Comment Lists the reason for the modification.

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4.4.4 View Menu

4.4.4.3 Sample Window

The Sample Window is used to display detailed measurement information. The information
displayed in the Sample Window varies based on the type of analysis performed. To view
the Sample Window, open a Sample Table, place the cursor in the row of the Sample Table
that contains the desired sample, and select Sample Window from the View menu. The
Sample Window is displayed.

TIP » To view measurement data in real time, place the cursor in the row of the Sample Table that
contains the current sample, then open the Sample Window.
The Sample Window is divided into 3 sections: the Graph, the Parameter Table, and the
Injection Table. Note that the sections can be resized by dragging the dividers between
sections.

Figure 4.123 Sample Window

Graph
The upper left section of the Sample Window displays the peak profile graph. Change the
graph type by choosing from the options on the drop-down list.
Setting Items Description
Current Peak Displays the peak profile of the highlighted injection.
All Peaks Displays all injection peaks for the selected sample.
Calibration curve Displays calibration curves (for calibration standards only).
This function is not available during real-time analysis

Note: To view the peak profile of the measurement in progress, click the row with the
asterisk in the Sample No. column. To view a previous measurement, click the
desired row.
Parameter Table
The upper right section of the Sample Window displays sample parameters.
Setting Item Description
Sample Name Displays the name of highlighted sample.
Sample ID Displays the sample identification from the Sample Table.
Analysis Displays the analysis method used for the sample.
Result Displays the sample concentration.
Dilution Factor Displays the dilution factor. The result will be multiplied by
this factor to calculate the final concentration. If the sample
was not diluted, do not change the default value of 1.

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 4.4 Sample Table Editor
4.4.4 View Menu

Injection Table
The lower section of the Sample Window displays the Injection Table, which contains
detailed information about the injections performed for the selected sample. Asterisks are
displayed in the Injection Table for the injection that is currently being measured. Some
columns in the Injection Table use the Merge Cell function to display information that is
common to all the injections of a particular sample. If the sample has been analyzed by
more than one analysis method, the Injection Table contains several folders displayed as
tabs at the bottom of the window. The columns in the Injection Table are described below.
Setting Items Description
Spl. No. Displays the sample number.
Inj. No. Displays the injection number.
Area Displays the area value.
Mean area Displays the mean area value for all injections of the sample.
Conc. Displays the concentration obtained for the injection.
Mean Conc. Displays the mean concentration obtained for all injections of
the sample.
Result Displays the analysis result.
Notes Displays any analysis flags or notations associated with that
sample.
SD Area Displays the standard deviation calculated from the area.
CV Area Displays the coefficient of variation calculated from the area.
SD Conc. Displays the standard deviation calculated from the concen-
tration.
CV Conc. Displays the coefficient of variation calculated from the con-
centration.
Status Displays the analytical status, either “measuring” or “fin-
ished”.
Vial Displays the vial number (for ASI samples only).
Excluded Displays the exclusion flag, denoted as “E” for user exclusion
of the sample, “ES” for exclusion by the system, or “Not
Excluded”.
Modified Displays the modification flag of “M” if the sample was
modified.
Inj. Volume Displays the injection volume for each injection.
Dilution Factor Displays the dilution factor used in measurement.
Calibration curve Displays the calibration curve used.

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4.4.4.4 Outlier Test

The Outlier Test (also known as the Grubb test) is used to determine whether a selected
injection is an outlier. The test also determines whether the injection with the highest
deviation from the mean value is still within an acceptable range. The Outlier Test can only
be performed if the sample contains at least three non-excluded injections.

Figure 4.124 Outlier Test Window

To perform the Outlier Test, open the Sample Window and select the cells containing the
data to be tested. From the View menu, select Outlier Test. The Outlier Test window is
displayed. Select either Conc. or Area (CNV) for the data source. Exclude the injection that
is suspected of being an outlier, then select OK to close the dialog box.
If the sample does not contain enough injections for the test to be performed, an error
message is displayed and the Outlier Test window will not open.
The Outlier Test window contains the parameters listed below.
Setting Items Description
Result List Displays the result of the Outlier Test.
Conc. radio button Select to indicate that test calculations are to be performed
based on the concentration data.
Area (CNV) radio button Select to indicate that test calculations are to be performed
based on the area data.
Result Displays the result of the test.
Exclude button Click this button to exclude a suspect sample and recalculate
the test result.
Suspicious inj. Indicates the injection suspected of being an outlier, which is
identified as the sample with the highest deviation from the
mean value.
SD Displays the standard deviation for all of the injections.
CV Displays the coefficient of variation for all of the injections.
Grubb Value Displays the corresponding value from the Grubb table.
Test Value Displays the calculated Outlier Test value.

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4.4.4 View Menu

4.4.4.5 Properties

The View>Properties function displays various windows. The display depends on the
content of the cell selected in the Sample Table. If a range of cells is selected, the upper left
cell is considered the active cell. The table below shows the possible selections and the
corresponding Properties windows.
Table 4.4 • Properties Windows
Content of Active Cell Properties Window
Calibration Curve Calibration Curve Properties window
Method Sample/Method Properties window
Any other cell for a sample Sample/Method Properties window
Any other cell of a control Control Sample Properties window
sample

The Properties window contains options for viewing and modifying the method, calibration
curve, and sample properties. Each Properties window consists of several tabs. The
Calibration Curve Properties window tabs are shown and described below.
Calibration Curve Properties Window

Figure 4.125 Calibration Curve Properties Window: The Common Tab

Common Tab
The Common tab of the Calibration Curve properties window contains the following
information about the calibration curve.
Setting Item Description
System Displays the system used to create the calibration curve. This
field cannot be edited.
User Displays the name of the user who created the calibration
curve.
Date of Creation Displays the date and time the calibration curve was created.
Comment A comment regarding the calibration curve may be entered
here.
Print Prints the calibration curve information.

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Parameter Tab

Figure 4.126 Calibration Curve Properties Window: Parameter Tab

Setting Item Description

Analysis Displays the analysis method used to create the calibration curve. This field can-
not be edited.
Unit Displays the concentration units. This field cannot be edited.
Sample Name Displays the default sample name used for the calibration standards (64 characters
maximum). This field can be edited.
Sample ID Displays the default sample ID (64 characters maximum). This field can be edited.
No. of Cal. Points Displays the number of calibration standards used. This field cannot be changed.
Catalyst Type Displays the type of catalyst used.
Calibration Curve Displays the calibration curve type. This field cannot be changed.
Type
Calculation Method Displays the calibration curve calculation method. This field can be edited by
selecting a different option from the drop-down list. Two calculation methods are
available: point-to-point and linear regression. For both types, a curve represent-
ing the relationship between detector response and concentration is displayed.
The point-to-point curve fit draws a straight line between adjacent data points and
considers each line segment to be a separate calibration line governed by its own
equation. A linear regression statistically determines the line that best fits the pat-
tern of all data points. The number used to describe the agreement between the
calculated line and the data points is called the Coefficient of Determination (r2).
A coefficient of 1 indicates that the line fits the data points perfectly.
The general equation for a straight line is:
Y = mX + b
where: Y = Y-axis data point
X = X-axis data point
m = slope of line
b = Y-axis intercept point

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Setting Item Description

Zero Shift Select Zero Shift to shift the regression curve through the origin. Note that this
option does not change the slope of the line. Use this option as a correction when
the TC content in the Zero water used to prepare the calibration standards is too
large to ignore.
Multiple Injections Select to enable the syringe to draw up a single aliquot with a volume equal to that
required for all injections of the standard. When this option is not selected, the
syringe will draw up a separate aliquot for each injection; as a result, selecting this
option reduces analysis time.
Calibration Curve Displays the file name of the calibration curve. This field cannot be changed.
File

Analysis Tab
The Analysis tab displays additional analysis parameters.

Figure 4.127 Calibration Curve Properties Window: Analysis

Analysis Parameters
Setting Item Description
No. of Washes Displays the number of times (0-10) the syringe is washed with standard
prior to the first injection. Note that if the Auto Dilution option was
selected, the standard will be diluted and the syringe will then be washed
with the diluted standard. This option is not available for SSM. This field
can be edited.
Acid Addition Displays the quantity of acid to be added to each standard prior to injec-
tion. This value is expressed as a percent of the sample volume and is
available only for NPOC or related analyses. This field can be edited.
Sparge Time Displays the pre-sparge time (0-20 minutes). This option is only avail-
able when the external sparge kit is installed and the analysis type is
NPOC. This field can be edited.
Density: Displays the sample density. This option is available only for SSM.
By Weight/Volume: Displays the basis (Weight or Volume) for sample calculations. This
option is available only for SSM.

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Peak Time Parameters

Setting Item Description
Use default settings This option is selected if the default settings are used for peak
integration.
Allowed peak start delay Displays the amount of time (in minutes) that can elapse
before the analysis is stopped because a peak is not detected.
Total integration time Displays the amount of time (in minutes) that analysis contin-
ues after the end of the peak is detected.

Data Tab
The Data tab displays information about each calibration standard used in the calibration
curve.

Figure 4.128 Calibration Curve Properties Window: Data Tab

Setting Item Description

Auto Dilution Displays the auto dilution factor.
Inj. Volume Displays the injection volume, which varies depending on the
analysis type.

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Columns of data are displayed in a window below the Inj. Volume selection, as described
below.
Table 4.5 • Data Tab Columns
Column Name Description
Auto Dilution Displays the dilution factor for auto dilution.
Standard Solution Concentra- Displays the concentration of the standard solution used for
tion analysis.
No. Displays the calibration point number.
Conc. Displays the concentration of calibration point.
Mean Area Displays the mean area value from all non-excluded injec-
tions
No. of Injections Displays the minimum and maximum number of injections.
Excluded “E” indicates calibration point has been excluded.
SD Max Displays the maximum standard deviation.
CV Max Displays the maximum coefficient of variation.
SD Displays the standard deviation.
CV Displays the coefficient of variation.

Additional buttons are displayed, below the data columns and can be used to manipulate the
calibration parameters. The buttons are described below. Refer to Section 4.4.2.2
"Calibration Curve" for more detailed descriptions.
Button Function
Edit Edit the parameters for the selected calibration point.
Add Add a new calibration point.
Delete Delete the selected calibration point.
Delete All Delete all calibration points.
Exclude Exclude the selected calibration point.

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Graph Tab
The Graph tab displays the calibration curve in a graphic format.

Figure 4.129 Calibration Curve Properties Window: Graph Tab

Setting Item Description

Slope/Intercept/r^2 The values for Slope, Intercept, and r2 are displayed for the
selected calibration curve.

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History Tab
If the History Log was enabled when the calibration curve was created, the History tab
displays a list of changes made to the calibration curve parameters. If the History Log was
not enabled previously, it can be enabled on the History tab.

Figure 4.130 Calibration Curve Properties Window: History Tab

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the system. If the History Log is not required, it
need not be enabled, as the software operates properly with-
out it. Once this is enabled, it cannot be disabled.
User has to comment all Select this option to require comments or approval for all
modifications modifications.f the History Log is not required, it need not be
enabled, as the software operates properly without it. Once
this is enabled, it cannot be disabled.
ACSII Export The displayed items in the list are exported as tab-delimi-
nated text files.

A list of the Comment dialog box contents is shown below:

Table 4.6 • Comment dialog box contents
Item Description
Date/Time Displays the date and time of the modification.
User Displays the user who made the modification.
Changed item Describes the parameter that changed.
From Displays the previous parameter value.
To Displays the new parameter value.
Comment Lists the reason for the modification.

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4.4.4.6 Customize

The View>Customize window contains two tabs, one that displays or hides the toolbars and
one that customizes the toolbar content.

Figure 4.131 Customize Window: Toolbars Tab

Toolbars Tab
Select the desired toolbars from the list. All items are selected by default.
Option Description
Show Tooltips Displays tooltips when the mouse cursor is positioned over
the toolbar button.
Cool Look Select this option to display the toolbar buttons as flat but-
tons. This item is selected by default.
Large Buttons Select this option to display the toolbar buttons in a larger
size.
New button Click this button to create a user-defined toolbar button.
Reset/Delete button Click this button to reset the toolbar display to its original
state or delete a user-defined toolbar button.

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Command Tab

Figure 4.132 Customize Window: Command Tab

Option Description
Categories Displays the available toolbars.
Buttons Displays the buttons in the selected toolbar. The buttons can
be moved by dragging them to another toolbar.
Description Displays a description of the selected button.

4.4.4.7 Toolbar

The View>Toolbar function is used to select or deselect individual toolbars for display.
Toolbar display options (such as button size or appearance) can also be set using this
command.

Figure 4.133 Toolbar Window

4.4.4.8 Status Bar

The View>Status Bar function toggles the display state of the status bar between Show and
Hide. If the status bar is currently displayed, selecting this option will hide the status bar. If
the status bar is not displayed, selecting this option will display the status bar.

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4.4.4.9 ASI / 8-Port Sampler Vials

This function displays the ASI or 8-Port Sampler dialog box, and allows the user to enter
vial numbers for measurement using the ASI or the 8-Port Sampler. To access this
command, either create or open a sample table, and select View > ASI / 8-Port Sampler
Vials. The Sparge / Acid Addition dialog box opens automatically when the Start command
is made. The OK button saves the changes and closes the dialog box.
Using the Autosampler

Figure 4.134 Sparge / Acid Addition Dialog Box for the ASI-V Autosampler

Using One 8-Port Sampler

Figure 4.135 Sparge / Acid Addition Dialog Box for One 8-Port Sampler

Using Two 8-Port Samplers

Figure 4.136 Sparge / Acid Addition Dialog Box for Two 8-Port Samplers

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When the mouse is positioned over a vial in the drawing of the of ASI or 8-Port Sampler, a
tool-tip showing the vial number is displayed. Click the vial to display the following items.
Parameter Description
Vial No. Displays the currently selected vial number.
Acid Addition rate Displays the acid addition rate for each vial.
Sparge time Displays the sparge time for each vial.
Total injection volume Displays the total injection volume for each vial.

TIP » The desired vial position for a sample can be entered either directly into the Vial column or
by placing the cursor in the appropriate row of the Sparging/Acid Addition window and
then double-clicking the desired position in the tray diagram.

4.4.4.10 Data Profile

Displays the raw measurement data. The data profile is never modified or processed
following the initial collection. It includes the corresponding measurement parameters. The
files which were created and named using the object ID, each occupy a row in the sample
table, and are stored within the RawData folder in folders named using the date of creation.
The View>Data Profile function is used to view the data profile for a sample. Highlight the
desired row of the Sample Table, then select the command.

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4.4.5 Insert Menu

The Insert menu contains options for inserting sample groups, calibration curves,
individual samples, and control samples into the Sample Table.

Figure 4.137 Insert Menu

4.4.5.1 Auto Generate

The Auto Generate command opens the Sample Group Wizard, which is used to create a
group of unknown samples, control samples, and calibration standards, and then insert the
group into the active position of the Sample Table.
Sample Group Wizard (Page 1) Sample Source
The Sample Source window is used to specify the source of sample measurement
parameters.

Figure 4.138 Sample Group Wizard (Page 1) Sample Source

Setting Item Description

Method radio button Click this option to analyze the samples using the measure-
ment parameters from a specified method. This is the default
option.
Method text field Enter the desired method or select the method using the
Browse button.
Calibration curve radio but- Click this option to analyze the samples using the measure-
ton ment parameters from a specified calibration curve.
Calibration curve text field Enter the desired calibration curve or select the curve using
the Browse button.

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Sample Group Wizard (Page 2) Sample Parameter

The Sample Parameter window is used to enter basic information about the sample group.

Figure 4.139 Sample Group Wizard (Page 2) Sample Parameter

Setting Item Description

No. of Samples Enter the number of samples in the group. Enter an integer
ranging from 1 to 200. The default value is 1.
Start Vial Enter the starting vial position for the sample group. Enter an
integer ranging from 0 to 9 or 1 to 100, depending on the
sample tray size. The default value is 1. This field is disabled
if an autosampler is not a component of the configured sys-
tem.
Sample Name/Sample ID The default designations for these fields are obtained from
the method or calibration curve identified in Page 1 of the
Sample Group Wizard. Enter other names if desired.
Index Start Select this option to start the counting index. Each sample
added receives an increased counting index number.

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Sample Group Wizard (Page 3) Calibration Curves

The Calibration Curves window is used to identify the calibration standards in the sample
group and to specify their placement in the group. The window is also used to revise the list
of calibration curves that will be used to quantitate samples in the group.

Figure 4.140 Sample Group Wizard (Page 3) Calibration Curves

Setting Item Description

Perform Calibration Select one of the available options for when calibration
should be performed: At the beginning of the sample group or
Always, after (a selected number of) Samples have been ana-
lyzed.
Add button Use this button to add a calibration curve.
Delete button Highlight a calibration curve listed in the window and click
the Delete button to remove the curve from the sample group.
Calibration Curves No.: Displays the number of the calibration point.
File name: Displays the name of the calibration curve.
Analysis: Displays the analysis type.

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Sample Group Wizard (Page 4) Controls

The Controls window is used to identify the control samples in a sample group and to
specify their placement in the sample group.

Figure 4.141 Sample Group Wizard (Page 4) Controls

Insert Control Samples

Use the options listed below to insert individual control samples in the sample group.
Setting Items Description
At the beginning of the sam- Select this option to add control samples at the beginning of
ple group the sample group.
Always, after (number of) Select this option to add control samples at defined intervals
samples between unknown samples.
At the end of the sample Select this option to add control samples at the end of the
group sample group.

Control Templates
The Control Templates table displays a list of the control sample templates currently
assigned to the sample group. The templates specify measurement parameters, evaluation
criteria, and failure actions for the control samples. This table is empty by default. Use the
options listed below to revise the list of control sample templates associated with the
sample group.
Option Description
Add Select this option to add a control template to the sample
group.
Delete Select this option to delete a highlighted control template
from the list.

After all four pages of the Sample Group Wizard are complete, click the Finish button to
save changes and add the sample group to the Sample Table. If invalid parameter values
were entered, an error message will be displayed and the sample group will not be inserted
into the Sample Table until after the error is corrected.

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4.4.5.2 Sample

The Sample command opens the Sample Wizard, which is used to insert sample
measurement parameters into an existing Sample Table. The Sample Wizard is not
accessible during an analysis.
Sample Wizard (Page 1) Parameter Source
The Parameter Source window is used to specify the source of the sample measurement
parameters. The source can either be a method file or a calibration file. When one of these
sources is selected, the sample will be analyzed using the same measurement parameters as
those in the specified method or calibration file. Some of the source parameters can be
edited in subsequent pages of the Sample Wizard. Note that a sample can also be added to
the Sample Table without specifying a source, an option that is desirable when a sample is
to be analyzed using different parameters than those specified in the method or calibration
files. In this case, unique measurement parameters for the sample will be entered on
subsequent pages of the Sample Wizard.

Figure 4.142 Sample Wizard (Page 1) Parameter Source

Parameter Description
Method radio button Select this option to use the sample measurement parameters from a specified
method. This is the default option. Enter the method name in the text field, or
use the Browse button to select the file using the File>Open dialog box
Calibration Curve radio Select this option to use the measurement parameters from a specified cali-
button bration curve. Enter the calibration curve name in the text field, or use the
Browse button to select the file using the File>Open dialog box.
Edit parameters manually Select this option to insert a sample without defining a source. Sample mea-
radio button surement parameters will be entered in subsequent pages (1-12) of the Sam-
ple Wizard.
Skip remaining Wizard Select this option to accept all measurement parameters from the source file.
pages and use measure- The Next button will become a Finish button, and subsequent pages of the
ment parameters from the Sample Wizard will not be displayed. This option is disabled if Edit parame-
source ters manually is selected.

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Sample Wizard (Page 2) Analysis Information

Figure 4.143 Sample Wizard (Page 2) Analysis Information

Parameter Description
Analysis Select the analysis type from the drop-down list.
Default Sample Name Enter the sample name.
Default Sample ID Enter the sample identification.
Dilution Enter the preparation dilution factor.
No. of Determinations Use the spin controls to enter the number of times the sample
is to be measured. Note that determinations and injections are
different; each determination is made up of one or more
injections. Enter an integer from 1 to 10.

Note: For combined analyses such as TC/TN or POC+NPOC, subsequent Sample Wiz-
ard windows may appear more than once so that parameter modifications spe-
cific to each analysis type can be made. The analysis type that is associated with
each Sample Wizard window can be found in the Analysis box at the top of the
window.

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Sample Wizard (Page 3) Calibration Curve

The Calibration Curve window is used to identify the calibration curve(s) that will be used
to calculate the sample concentration. If more than one curve is identified, the software
automatically selects the curve to be used in calculating sample concentration. Refer to
Section 6.2.5 "Automatic Selection of Optimum Calibration Curve".

Figure 4.144 Sample Wizard (Page 3) Calibration Curve

Parameter Description
Analysis Displays the analysis type. This field cannot be changed.
Calibration Curve 1/2/3 Enter the name of the calibration curve or click the Browse
button to select a file using the File>Open dialog box.
Skip the injection parameter Select this item to skip the Measurement Parameters window
pages of the wizard of the Sample Wizard. Use this option when the sample mea-
surement parameters will be the same as those used for cali-
bration curve measurements.

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Sample Wizard (Page 4) Injection Parameters

Figure 4.145 Sample Wizard (Page 4) Injection Parameters

Parameter Description
Analysis Displays the analysis type. This field cannot be changed.
Units Enter the concentration units.
Injection Volume Enter the injection volume.
Expected Conc. Range Enter the maximum expected sample concentration.
No. of Injections Enter the minimum and maximum number of injections for
the sample.
SD Max Enter the maximum standard deviation. If this value is met,
no additional injections are required. However, if both this
value and the CV Max value are exceeded, the sample is
automatically reinjected up to the maximum number of times
specified in the No. of Injections field. The SD Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
CV Max Enter the maximum coefficient of variation. If this value is
met, no additional injections are required. However, if both
this value and the SD Max value are exceeded, the sample is
automatically reinjected up to the maximum number of times
specified in the No. of Injections field. The CV Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
No. of Washes Enter the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilu-
tion option was selected, the sample will be diluted and the
syringe will then be washed with the diluted sample.

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Parameter Description
Auto Dilution Enter a dilution factor for the sample. The instrument will
automatically dilute the sample by this factor, and the result
will be multiplied by the factor to obtain the final concentra-
tion. The default Auto Dilution value is 1.
Sparge Time Enter the sparge time.
Acid Addition Enter the desired quantity of acid to be added. This value is
expressed as a percent of the sample volume and is available
only for NPOC or related analyses.
Multiple Injections Select this option to enable the syringe to draw up a single
sample aliquot with a volume equal to that required for all
injections of the sample. When this option is not selected, the
syringe will draw up a separate sample aliquot for each injec-
tion. Selecting this option reduces analysis time.
Use blank check area Select this option to subtract the blank check area from the
measured area of the sample. This option is only available for
TC and NPOC analyses that use the high sensitivity catalyst.
Auto. correction of inj. vol. Select this option to enable the instrument to automatically
and dilution adjust the injection volume and dilution factor when the peak
height for the initial injection exceeds full scale. After the
adjustment, measurement will be repeated.

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Sample Wizard (Page 5) Peak Time Parameters

Figure 4.146 Sample Wizard (Page 5) Peak Time Parameters

Parameter Description
Analysis Displays the analysis type. This field cannot be changed.
Use default settings Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay The allowed peak start delay is the amount of time (in min-
utes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.

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Sample Wizard (Page 6) Calibration Curve

A second Calibration Curve window is only displayed when more than one analysis type
has been specified. This window is the same as Page 3 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.

Figure 4.147 Sample Wizard (Page 6) Calibration Curve Window (Second Analysis)

Sample Wizard (Page 7) Injection Parameters

A second Injection Parameters window is only displayed when more than one analysis type
has been specified. This window is the same as Page 4 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.

Figure 4.148 Sample Wizard (Page 7) Injection Parameters Window (Second Analysis)

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Sample Wizard (Page 8) Peak Time Parameters

A second Peak Time Parameters window is only displayed when more than one analysis
type has been specified. This window is the same as Page 5 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.

Figure 4.149 Sample Wizard (Page 8) Peak Time Parameters Window (Second Analysis)

Sample Wizard (Page 9) USP/EP

The USP/EP window is displayed only for TC or NPOC methods, and is used to enable
samples to be checked in accordance with USP/EP standards. This window is the same as
Page 6 of the Sample Wizard, which is described above. Select the check box to enable this
function.

Figure 4.150 Sample Wizard (Page 9) USP/EP

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4.4.5.3 Control

The Control command is used to insert a control sample into an existing Sample Table.
Note: A control sample template must be created before a control sample can be
inserted into a Sample Table. A control sample template has a file extension of
*.tpl and specifies measurement parameters for the Control Sample.
The following subsections describe the procedures for creating a control sample template
and for inserting a control sample into a Sample Table.

¬Creating a Control Sample Template

Control sample templates are created using the Control Sample Wizard. To access the
Control Sample Wizard select New>Control Sample Template from the File menu. The
Control Sample Wizard consists of several windows, each of which defines specific
parameters for the control sample template, as described below.
Control Sample Wizard (Page 1) System Information

Figure 4.151 Control Sample Wizard (Page 1) System Information

Parameter Description
System Select the instrument.
Operator Displays the current operator name. This field cannot be
changed.
Date of Creation Displays the current date and time. This field cannot be
changed.
Comment Enter a comment (512 characters maximum).

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Control Sample Wizard (Page 2) Control Sample Type

The Control Sample Type window is used to identify the type of control sample.

Figure 4.152 Control Sample Wizard (Page 2) Control Sample Type

Parameter Description
Control Sample Select this option to define individual sample parameters.
This is the default option.
Control Chart Sample Select this option to add the control sample to a defined con-
trol chart. Enter the file name or use the Browse button to
select the control chart file from the File>Open dialog box.
System Suitability Test for Select this option to check the control sample using USP/EP
USP/EP criteria.
Save the data in a control Enter a file name for the control sample template.
sample template

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4.4.5 Insert Menu

Control Sample Wizard (Page 3) Parameter Source

The Parameter Source window is used to specify the source of the control sample
measurement parameters. The source can either be a method file or a calibration file. When
one of these sources is selected, the control sample will be analyzed using the same
measurement parameters as those in the specified method or calibration file. Some of the
source parameters can be edited in subsequent pages of the Control Sample Wizard. Note
that a control sample can also be added to the Sample Table without specifying a source, an
option that is desirable when a control sample is to be analyzed using different parameters
than those specified in the method or calibration files. In this case, unique measurement
parameters for the sample will be entered on subsequent pages of the Control Sample
Wizard.

Figure 4.153 Control Sample Wizard (Page 3) Parameter Source

Parameter Description
Method radio button Select this option to use the measurement parameters from a
specified method. Enter the method name in the text field, or
use the Browse button to select the file using the File>Open
dialog box. This is the default option.
Calibration Curve radio but- Select this option to use the measurement parameters from a
ton specified calibration curve. Enter the calibration curve name
in the text field, or use the Browse button to select the file
using the File>Open dialog box.
Edit parameters manually Select this option to insert a control sample without defining
radio button a source. Control sample measurement parameters will be
entered in subsequent pages of the Control Sample Wizard.
Skip remaining Wizard pages Select this option to accept all measurement parameters from
and use measurement param- the source file. The Next button will become a Finish button,
eters from the source and subsequent pages of the Control Sample Wizard will not
be displayed. This option is disabled if Edit parameters man-
ually is selected.

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4.4.5 Insert Menu

Control Sample Wizard (Page 4) Analysis Parameters

Figure 4.154 Control Sample Wizard (Page 4) Analysis Parameters

Parameter Description
Analysis Select the analysis type from the drop-down list. If a source
method or calibration file was specified on Page 3 of the
Control Sample Wizard, this field is disabled and the applica-
ble analysis type is displayed.
Default Sample Name Enter the sample name. If a source method or calibration file
was specified on Page 3 of the Control Sample Wizard, the
default sample name from the source is displayed.
Default Sample ID Enter the sample identification. If a source method or calibra-
tion file was specified on Page 3 of the Control Sample Wiz-
ard, the default sample identification from the source is
displayed.
Dilution Enter the dilution factor. If a source method or calibration file
was specified on Page 3 of the Control Sample Wizard, the
default dilution factor is displayed.
Calibration Curve Enter the calibration file name that is to be used to calculate
control sample concentration. If a source method or calibra-
tion file was specified on Page 3 of the Control Sample Wiz-
ard, the default calibration curve name from the source is
displayed.

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4.4.5 Insert Menu

Control Sample Wizard (Page 5) Injection Parameters

Figure 4.155 Control Sample Wizard (Page 5) Injection Parameters

Parameter Description
Analysis Displays the analysis type. This field cannot be changed.
Units Select the concentration units.
Injection Volume Enter the injection volume.
Expected Conc. Range Enter the maximum expected concentration.
No. of Injections Enter the minimum/maximum number of injections for the control sample.
The setting range is from 1-20.
SD Max Enter the maximum standard deviation that is acceptable for the injections. If
this value is met, no additional injections are required. However, if both this
value and the CV Max value are exceeded, the control sample is automatically
reinjected up to the maximum number of times specified in the No. of Injec-
tions field. The SD Max field is disabled if the No. of Injections is 1 or if the
minimum is equal to the maximum.
CV Max Enter the maximum coefficient of variation that is acceptable for the injec-
tions. If this value is met, no additional injections are required. However, if
both this value and the SD Max value are exceeded, the control sample is
automatically reinjected up to the maximum number of times specified in the
No. of Injections field. The CV Max field is disabled if the No. of Injections is
1 or if the minimum is equal to the maximum.
No. of Washes Enter the number of times the syringe is to be washed with sample prior to the
first injection. Note that if the Auto Dilution option was selected, the sample
will be diluted and the syringe will then be washed with the diluted sample.
Auto Dilution Enter a dilution factor for the samples. The instrument will automatically
dilute the control sample by this factor, and the result will be multiplied by the
factor to obtain the final concentration. The default Auto Dilution value is 1.
Acid Addition Enter the desired quantity of acid to be added. This option is available only for
NPOC and related analyses.
Sparge Time Enter the sparge time.

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4.4.5 Insert Menu

Parameter Description
Multiple Injections Select to enable the syringe to draw up a single sample aliquot with a volume
equal to that required for all injections of the sample. When this option is not
selected, the syringe will draw up a separate sample aliquot for each injection;
as a result, selecting this option reduces analysis time.
Use area retrieved from Select this option to subtract the blank check area from the measured area of
the blank check the control sample. This option is only available for TC and NPOC analyses
that use the high sensitivity catalyst.

Control Sample Wizard (Page 6) Peak Time Parameters

The Peak Time Parameters window is used to set peak detection parameters for the control
samples.

Figure 4.156 Control Sample Wizard (Page 6) Peak Time Parameters

Setting Item Description

Use default settings Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay The allowed peak start delay is the amount of time (in min-
utes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time The total integration time is the amount of time (in minutes)
peak detection continues. Enter a number between 4:50 and
20:00.

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4.4.5 Insert Menu

Control Sample Wizard (Page 7) History

The History window is used to enable the History Log. The History Log records all
modifications to the control sample template properties. The History Log can be set to
require users to enter comments for each modification.
Note: Once the History Log is enabled, it cannot be disabled. All modifications to the
control sample template will be tracked. If the mandatory comment option is
selected, the user will be required to enter a comment each time any parameter in
the control sample template is modified.

Figure 4.157 Control Sample Wizard (Page 7) History

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the control sample template. Once the History
Log is enabled, it cannot be disabled. If the History Log is not
required, it need not be enabled, as the software operates
properly without it.
User has to comment all Select this option to require comments or approval for all
modifications modifications.

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4.4.5 Insert Menu

Control Sample Wizard (Page 8) Control Checking

The Control Checking window is used to select options for control checks and control
limits. This window is not displayed if the USP/EP system suitability criteria are used
because the control limits are already defined.

Figure 4.158 Control Sample Wizard (Page 8) Control Checking

Setting Option Description

Recovery Select this option to check recovery amounts in control sam-
ples.
Spiked Select this option to use an original and a spiked sample to
calculate the recovery amount. This option is enabled only
when the Recovery option is selected.
Original Concentration Enter the original concentration of the spiked sample. This
field is enabled only when the Recovery option is selected.
Spiked Concentration Enter the concentration of the spiked sample. This field is
enabled only when the Recovery and Spiked options are
selected.
Mean Value (Concentration) Select this option to check the mean value of the measured
concentrations.
Blind Value (Area) Select this option to check the mean value of the measured
area values.
Spanwidth (Concentration) Select this option to check the deviation of the measured con-
centrations.
Max. Dev. Enter the maximum acceptable deviation. This field is
enabled only when the Spanwidth option is selected.
Low Enter the lower limit of the valid control range, if the Blind
Value option is selected.
Up Enter the upper limit of the valid control range, if the Blind
Value option is selected.

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4.4.5 Insert Menu

Control Sample Wizard (Page 9) Failure Action

The Failure Action window is used to specify the actions taken when a control sample
exceeds the specified control limits.

Figure 4.159 Control Sample Wizard (Page 9) Failure Action

Setting Item Description

Action when the failure event Select the action to be taken the first time a control sample
occurs the first time exceeds the control limits. Options available from the drop-
down list are:
Continue (notify): Select this option to allow the analysis
sequence to continue normally and display a failure message
in the Notification Bar.
Stop (Whole Sample Run): Select this option to stop the sam-
ple run and display a failure message in the Notification Bar.
Repeat (From last control or calibration): Select this option
to automatically reanalyze all samples analyzed after the pre-
vious valid control sample or calibration curve (whichever
occurred most recently) and display a failure message in the
Notification Bar.
Action when the failure event Select the action to be taken the second time a control sample
occurs the second time exceeds the control limits. The options available from the
drop-down list are Continue and Stop. The Repeat option is
not available.

Save the control sample template and close the Control Sample Wizard by clicking the
Finish button.

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 4.4 Sample Table Editor
4.4.5 Insert Menu

¬Inserting a Control Sample into the Sample Table

Once the control sample template has been created, a control sample can be entered into the
Sample Table by following the procedure below.

Procedure
1. Open the Sample Table and place the cursor in the row where the control sample will
be inserted.
2. From the Insert menu, select Control.
The Open dialog box displays the available control sample template files.
3. Select the appropriate control sample template and click the Open button.
The Open dialog box closes and the Sparging/Acid Addition window is displayed.
4. Enter the ASI vial position for the control sample into the appropriate cell in the
Sparging/Acid Addition window.
5. Click the OK button.
The Sparging/Acid Addition window closes.
6. Scroll through the Sample Table to verify that the control sample has been inserted at
the correct location.

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 4.4 Sample Table Editor
4.4.6 Instrument Menu

4.4.6 Instrument Menu

The Instrument menu contains commands for connecting, starting, and stopping the
instrument, and for instrument maintenance functions.

Figure 4.160 Instrument Menu

4.4.6.1 Background Monitor

The Background Monitor command is used to open the Background Monitor window,
which displays the status of the autosampler and all installed instrument detectors. The real
time signal and ready status for various detectors can be viewed by toggling between the
individual instrument tabs. The command is available only when an instrument is
connected to the software. Instrument and communication errors are displayed in the
Notification Bar. The Background Monitor window cannot be open during measurement.
TOC Tab

Figure 4.161 Background Monitor Window: TOC Tab

Parameter Description
Furnace Displays the temperature of the TC furnace.
Dehumidifier Displays the temperature of the dehumidifier.
NDIR Baseline Pos.: Displays the status of the NDIR detector baseline position.
Baseline Fluc.: Displays the status of the NDIR detector baseline fluctuation.
Baseline Noise: Displays the status of the NDIR detector baseline noise.

The bottom portion of the TOC tab window displays a graph of the selected items.

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 4.4 Sample Table Editor
4.4.6 Instrument Menu

TN Tab

Figure 4.162 Background Monitor Window: TN Tab

Parameter Description
TN Reactor Displays the temperature of the TN reactor.
Chemiluminescence Baseline Pos.: Displays the status of the chemiluminescence detector baseline
position.
Baseline Fluc.: Displays the status of the chemiluminescence detector baseline
fluctuation.
Baseline Noise: Displays the status of the chemiluminescence detector baseline
noise.

The bottom portion of the TN tab window displays a graph of the selected items.
ASI Tab
The ASI tab is available only if the ASI is connected to the instrument. The ASI Power
indicator displays the power status of the ASI. The ASI Cover indicator displays the status
of the ASI cover.

Figure 4.163 Background Monitor Window: ASI Tab

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 4.4 Sample Table Editor
4.4.6 Instrument Menu

4.4.6.2 Connect

The Connect command is used to connect or disconnect the instrument and the software. If
the instrument is not connected, selecting the Connect command opens the communication
port, initializes the instrument, and downloads and checks the instrument parameters.
During this process, the Sequence window displays the progress of the connection. To abort
the Connect operation while it is in progress, click the Cancel button.

Figure 4.164 Sequence Window

The bottom portion of the Sequence window displays a list of tasks that are performed
during the Connect process. The progress of each task and the result after completing the
task are shown in columns to the right of the task list. The Sequence window closes when
the connection process is complete. If an error occurs during the Connect process, an error
message is displayed in the Notification Bar and the result column, and the Sequence
window remains open.
If the instrument is already connected to the software, the Connect command is used to
disconnect the instrument. A confirmation request dialog box is displayed when the
command is selected, as shown below.

Figure 4.165 Disconnect Confirmation Request Dialog Box

Click the OK button to disconnect the instrument, or the Cancel button to abort the
operation.

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 4.4 Sample Table Editor
4.4.6 Instrument Menu

4.4.6.3 Standby

The Standby function is used to shut down the instrument. To access the Standby function,
open a Sample Table, then select Standby from the Instrument menu. The Standby window,
which lists options for the shut down operation, is displayed. Select the desired options and
click the Standby button. Click the Escape button to abort the Standby operation and
maintain the instrument in Ready mode.

Reference: To end measurement, refer to Section 4.3.3 "Ending Measurement".

CAUTION
Do not turn off the TOC-V main instrument switch for at least 30 minutes after
initiating the shut down procedure.

Figure 4.166 Standby Window

Setting Item Description

Shut down instrument Select this option to begin a 30-minute countdown to instru-
ment shutdown. During the shutdown process, the carrier gas
is turned off and the furnace cools down. The power to the
instrument is automatically turned off when the countdown is
complete.
Auto restart Select this option to shut down the instrument but automati-
cally restart it at a specified time. Set the restart time using
the spin controls for Auto start time. The default settings are
the current system date and time.
Keep TC furnace heating Select this option to keep the TC furnace on during the
Standby mode. This option is available only when the Auto
restart option is selected.
Keep carrier gas flowing Select this option to keep the carrier gas flowing during the
Standby mode. This option is available only when the Auto
restart option is selected.

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 4.4 Sample Table Editor
4.4.6 Instrument Menu

4.4.6.4 Measurement Start

Click the Measurement Start command to open the Standby dialog box if the ASI is
included in the system configuration. If the ASI is not included, the Measurement Mode
dialog box is displayed. To start measurement, open the Sample Table, define a new
sample, and connect to the instrument.

Figure 4.167 Measurement Mode Dialog Box

Item Setting Description

Normal Mode Select this option to conduct analysis sample-by-sample.
Between samples, the instrument waits for the user command
before starting the next measurement.
Multiple Row Continuous Select this option to perform continuous, uninterrupted mea-
Mode surement of multiple rows until the user stops the measure-
ment sequence.
Continuous Mode Select this to perform measurement using multiple measure-
ment modes, without stopping measurement between modes.

Select OK to continue on to the measurement, or select Cancel to cancel the start of

measurement.

4.4.6.5 Stop>Peak Stop

The Stop>Peak Stop command is used to interrupt the current measurement. The peak
measured up to the stopping point is considered a complete peak. After the Stop>Peak Stop
command is executed, the next injection listed in the Sample Table is made and analysis
continues normally.

4.4.6.6 Stop>Finish Current Sample

The Stop>Finish Current Sample command is used to interrupt measurement after all
injections of the current sample are complete. After the Stop>Finish Current command is
executed, the instrument remains in Ready mode.

4.4.6.7 Stop>Halt

The Stop>Halt command is used to immediately interrupt the current measurement, discard
data from the current injection, and return the instrument to Ready mode.

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 4.4 Sample Table Editor
4.4.7 Maintenance Menu

4.4.7 Maintenance Menu

Instrument maintenance procedures are described in Section 5.6 "Software-Controlled
Maintenance Functions". All maintenance functions can be initiated using the options
displayed in the Instrument>Maintenance menu.

4.4.8 Tools Menu

Figure 4.168 Tools Menu

4.4.8.1 Control Charts

The Control Charts function is used to create control charts. Refer to Appendix B for a
detailed description of the function.

4.4.8.2 Method Validation

The Method Validation function is used to validate analytical methods. Refer to Appendix
A for a detailed description of the function.

4.4.8.3 Administration

The Administration function is used to access the Administration program of the TOC-
Control V software. Refer to Section 3.1 "Introduction to System Administration
Functions" for a detailed description of the Administration program.

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 4.4 Sample Table Editor
4.4.8 Tools Menu

4.4.8.4 Screen Lock

If the user must temporarily leave the PC he/she is logged into, the screen can be locked by
using the password function to prevent another individual from performing operations in
TOC-Control V. This function can be used only if the User ID / Password item is checked
in the Security dialog box.
To lock the screen, select Screen Lock in the Tools menu. The screen will then be locked
and the Re-enter Password dialog box is displayed. To release the screen lock, enter the
user ID and password into the designated fields. If the user ID and password entered are not
the same as those used up to that point, the screen lock will not be released.

Figure 4.169 Re-enter Password Dialog Box

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9 Options Menu

The Options menu contains commands for viewing and displaying system information and
for setting default measurement parameters.

Figure 4.170 Options Menu

4.4.9.1 General Information

The General Information command is used to view information about the system. The
General Information window contains two tabs, one that displays System parameters and
one that displays History information. Most of the fields in the General Information
window are disabled because they were set previously. After changing an active field, click
the OK button to close the window and save the changes or click the Apply button to save
the changes without closing the window. Click the Cancel button to close the window
without saving changes.

Figure 4.171 General Information Window: System Tab

System Tab
The System tab displays general parameters.
Parameter Description
System Displays the instrument identification.
File Version Displays the instrument file version.
User Displays the name of the user who set up the system.
Date of Creation Displays the date the system was set up.
Comment Enter a comment (512 characters maximum), if desired.

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 4.4 Sample Table Editor
4.4.9 Options Menu

History Tab

Figure 4.172 General Information Window: History Tab

The History tab is used to view the system’s History Log or to enable the log if it was not
previously selected.
Note: Once the History Log is enabled, it cannot be disabled.

Setting Item Description

Enable history log Select this option to enable the software to monitor all modi-
fications to the system. Once the History Log is enabled, it
cannot be disabled. If the History Log is not required, it need
not be enabled, as the software works properly without it.
User has to comment all Select this option to require comments or approval for all
modifications modifications.

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9.2 Default Measurement Parameters

The Default Measurement Parameters command is used to enter the default values for
samples, methods, and calibration curves. The Default Measurement Parameters window
contains a separate tab for each analysis type, into which the default values are entered. The
SSM-TC and SSM-IC tabs are items associated with the installation of SSM-5000A. For
details, refer to the SM-5000A User's Manual

Figure 4.173 Default Measurement Parameters: TC Tab

Figure 4.174 Default Measurement Parameters: TN Tab

The parameters shown on each of the tabs are similar and are described below.
Parameter Description
Units Select the default concentration units.
No. of Injections Enter the default minimum/maximum number of injections.
No. of Washes Enter the default number of times the syringe is to be washed
with sample prior to the first injection. Note that if the Auto
Dilution option was selected, the sample will be diluted and
the syringe will then be washed with the diluted sample.

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 4.4 Sample Table Editor
4.4.9 Options Menu

Parameter Description
Max SD Enter the default maximum standard deviation that is accept-
able for the injections. If this value is met, no additional
injections are required. However, if both this value and the
Max CV value are exceeded, the samples are automatically
reinjected up to the maximum number of times specified in
the No. of Injections field. The SD Max field is disabled if
the No. of Injections is 1 or if the minimum is equal to the
maximum.
Max CV Enter the default maximum coefficient of variation that is
acceptable for the injections. If this value is met, no addi-
tional injections are required. However, if both this value and
the Max SD value are exceeded, the samples are automati-
cally reinjected up to the maximum number of times speci-
fied in the No. of Injections field. The CV Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.

4.4.9.3 Display Settings>Display Font

The Display Settings>Display Font function is used to select font options for both the
general screen display (such as in the Sample Table and Print Preview screens) and printed
reports. Select a font type, style, size, and color from the lists in the Font dialog box. A
preview of the font appearance is displayed in the Sample field.

Figure 4.175 Font Dialog Box

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9.4 Display Settings>Table Settings

The Display Settings>Table Settings function is used to select the parameters that will be
displayed in the Sample Table window. The Table Options window contains two tabs, one
that lists Sample Table parameters and one that lists Injection Table parameters. Note that
on each tab, certain options are selected by default. Individual options can be selected or
deselected by clicking in the check box. Use the All and None buttons to quickly select and
deselect all options on a tab. Use the Default button to select the default options.
Sample Table Tab
Select the parameters that will be displayed in the Sample Table.

Figure 4.176 Table Options Window: Sample Table Tab

Samples Tab
Select the parameters that will be displayed in the Injection Table.

Figure 4.177 Table Options Window: Samples Tab

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9.5 Display Settings>Notification Bar Settings

The Display Settings>Notification Bar Settings function is used to set options for the
Notification Bar, where error messages and other notices are displayed. The Notification
Bar is located at the bottom of the Sample Table Editor window.
Four folders can be displayed in the Notification Bar: Notifications, System Folders,
Errors, and Events. When a folder is selected for display, a tab appears for that folder in the
Notification Bar. When more than one folder is selected for display, the contents of a
specific folder can be displayed by clicking the appropriate tab.

Figure 4.178 Notification Bar Settings Window

Setting Item Description

Folder List Lists the folders that can be displayed in the Notification Bar.
Display Folder Place a check in this box to display the folder.
Max. Number of Displayed Enter the maximum number of lines to be displayed in the
Lines Notification Bar. Acceptable values range from 0 to 200.
Font Displays the selected font. Modify the font by selecting the
Browse button to open the Font dialog box.

To select a folder for display in the Notification Bar, click the folder in the Folder List, then
select the Display Folder option. Set the Max. Number of Displayed Lines field to a value
greater than 0. To change the color or appearance of the text displayed in the folder, use the
Font option. Note that the Display Folder check box, Max. Number of Displayed Lines
field, and Font option apply only to the selected folder; as a result, these options must be set
separately for each folder.
Note: A folder will not be displayed in the Notification Bar unless the Display Folder
option is selected and the Max. Number of Displayed Lines field is set to a value
greater than 0.

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9.6 Display Settings>Floating Point Number Formats

The Display Settings>Floating Point Number Formats command is used to select display
options for numeric results in the Sample Table. Note that these options apply only to the
manner in which numbers are displayed; internal data retain their original values.

Figure 4.179 Floating Point Format Window

Select settings for both common numbers and percent values, as described below.
Common Floating Point Numbers
Setting Item Description
Number of significant digits Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the Select this option to display common floating point numbers
decimal point using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the deci-
mal point. The default value is 2.

Percent Values
Setting Item Description
Number of significant digits Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the Select this option to display percent values using a specified
decimal point number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.

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 4.4 Sample Table Editor
4.4.9 Options Menu

4.4.9.7 Directories

The Directories function is used to modify system directories. Select Options>Directories

to display the Folder window.

Figure 4.180 Folder Window

Show all directories for

Use the drop-down list to access various directories. Available directories are listed in the
Folder text field.
Add
Click the Add button to add a new directory to the list for a specified topic, and the Folder
dialog box is displayed. Highlight the desired directory from the drop-down Drive and
Directory lists, then select it by clicking the OK button. Click the Network button to access
at network drive.

Figure 4.181 Folder Dialog Box

Delete
Click the Delete button to delete a selected directory from the list.
Up
Click the Up button to move the selected directory up one line in the list. The order of the
directories in the list is the order in which the directories will be searched during instrument
operation.
Down
Click the Down button to move the selected directory down one line in the list. The order of
the directories in the list is the order in which the directories will be searched during
instrument operation.

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 4.4 Sample Table Editor
4.4.10 Window Menu

4.4.10 Window Menu

Figure 4.182 Window Menu

4.4.10.1 Cascade

The Cascade command is used to stack all open windows so that the title bars are visible.

4.4.10.2 Tile

The Tile command is used to size all open windows so that each window occupies an equal
portion of the screen.

4.4.10.3 Arrange Icons

The Arrange Icons command is used to neatly organize windows that have been minimized
or reduced to icons.

4.4.11 Help Menu

Figure 4.183 Help Menu

About
The About command is used to view copyright, software registration, and software version
information.

218 TOC-VCPH/CPN
 4.5 Application Operations
4.5.1 Manual Injection Analysis

4.5 Application Operations

4.5.1 Manual Injection Analysis

Samples can be injected manually to perform analysis without the sample injector syringe,
when the optional manual injection kit is installed.

4.5.1.1 Analysis Preparation

Installing the Manual Injection Kit

1. Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider.

Knurled Thumbscrew

Figure 4.184 Removing the Slider

2. Install the TC/TN block provided in the kit.

TC/TN Block

Figure 4.185 Installing the TC/TN Block

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 4.5 Application Operations
4.5.1 Manual Injection Analysis

3. If the IC reactor kit is being used, remove the IC injector slider, and install the IC
block provided in the manual injection kit.

IC Block

Figure 4.186 Installing the IC Block

Note: When installing the block, be sure that it is aligned with the
injection port.

Software Settings
Select the Manual Injection Kit option in the Instrument Setup Wizard Options window
during System Setup. Refer to Section 3.2.2 "Options Window".
Note: Selecting the Manual Injection Kit option disables operation of the TOC-V injec-
tor syringe.

220 TOC-VCPH/CPN
 4.5 Application Operations
4.5.1 Manual Injection Analysis

4.5.1.2 Measurement

Measurement procedures using the manual injection kit are similar to those described in
Section 4.3 "Measurement Procedures and Tutorial".

¬Calibration Curve Measurement

Procedure
1. From the File menu, select New. The New dialog box is displayed.

Figure 4.187 New Dialog Box

2. Double-click the Calibration Curve icon. The Calibration Curve Wizard opens. The
System Information window of the wizard is displayed.

Figure 4.188 Calibration Curve Wizard (Page 1) System Information

3. From the System drop-down list, select the system that was configured with the
Manual Injection Kit during setup.
4. Select the desired options on pages 2 and 3 of the Calibration Curve Wizard, which
list calibration curve type and analysis information settings, respectively. Enter the
name of the new calibration curve in the text box at the bottom of page 3 of the
wizard.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".

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4.5.1 Manual Injection Analysis

5. Enter the desired number of injections on page 4 of the Calibration Curve Wizard
(Calibration Measurement Parameters).
6. Enter the injection volume on page 5 of the Calibration Curve Wizard (Calibration
Points List).
Note: An injection volume is displayed automatically. The displayed
value is based on the volume of the last injection that was per-
formed using the sample injector. This value can be changed by the
user as appropriate.
7. Select the desired options on pages 6 and 7 of the Calibration Curve Wizard, which
list peak time parameter and history settings, respectively. Click the Finish button to
create the new calibration curve.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".
8. Create a Sample Table for the calibration curve. From the Insert menu, select
Calibration Curve. Select the newly created calibration curve from the list of files in
the Open dialog box.
9. Connect the instrument by selecting Connect from the Instrument menu. Then select
Start from the Instrument menu. The Manual Injection Parameter dialog box is
displayed.
10. Draw an appropriate amount of sample into the syringe.
Note: Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
11. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
12. Verify that the instrument is ready for measurement, and click the Start button.
13. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
14. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
The results are displayed when measurement is complete.
15. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.

222 TOC-VCPH/CPN
 4.5 Application Operations
4.5.1 Manual Injection Analysis

¬Sample Measurement

Procedure
1. From the File menu, select New. The New dialog box is displayed.

Figure 4.189 New Dialog Box

2. Double-click the Method icon. The Method Wizard opens. The System Information
window of the wizard (page 1) is displayed.

Figure 4.190 Method Wizard (Page 1) System Information

3. Select the system that was configured with the Manual Injection Kit and used to
create the calibration curve. Advance to page 2 of the Method Wizard (Analysis
Information) and enter the new method name in the text box at the bottom of the
window.
4. Advance to page 3 of the Method Wizard (Calibration Curves). Select the appropriate
calibration curve file.
5. Enter “1” in the No. of Injections field on page 4 of the Method Wizard (Injection
Parameters).

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4.5.1 Manual Injection Analysis

6. Select the desired options on pages 5, 6, and 7 of the Method Wizard, which list peak
time parameter, USP/EP check, and history settings, respectively. Click the Finish
button to create the new method.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".
7. From the Insert menu, select Sample to open the Sample Wizard. Select the newly
created method from the list of files in the Open dialog box. Complete the remaining
wizard pages.
8. From the Instrument menu, select Start. The Manual Injection Parameter dialog box is
displayed.
9. Draw an appropriate amount of sample into the syringe.
10. Draw in and discharge the sample 3 or 4 times before filling the syringe for
measurement.
11. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
12. Verify that the instrument is ready for measurement, and click the Start button.
13. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
14. Remove the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
15. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.

224 TOC-VCPH/CPN
 4.5 Application Operations
4.5.1 Manual Injection Analysis

4.5.1.3 Measurement Precautions for Low Concentration Samples

In manual injections of sample concentrations lower than 1µg/mL, it is necessary to take

the following precautions to prevent contamination of the sample and the measurement
process.

Injecting Sample into the Injection Port

Use a separate micro syringe (500µL) for high sensitivity measurement. Any
contamination on the sample injection port may affect the result for high sensitivity
measurement.The inside of the injection port can be contaminated by sample solution that
adheres to the tip of the micro syringe needle. When inserting the micro syringe into the
injection port, use extreme care to avoid touching the tapered portion of the inside of the
sample injection port. After filling the syringe, wipe the excess solution from the needle
surface with soft tissue paper. Prevent excess drops of solution from forming on the tip of
the needle by gently pulling back on the plunger.

Cleaning the Sample Injection Port

Under normal operating conditions, fill a 500µL micro syringe with pure water and insert it
into the injection port. Keep the bottom of the syringe barrel 8-10mm above the injection
port. Under normal operation, the bottom of the syringe barrel is inserted until it comes into
contact with the injection port allowing the needle tip to protrude from the needle guide
pipe by about 5-6mm. With the needle 8-10mm higher than normal operation, the tip of the
needle inside the needle guide pipe. Slowly dispense the pure water. The pure water does
not flow into the combustion tube. It is driven out of the injection port by the carrier gas
flowing through the needle guide pipe. Wipe off the water coming out of the injection tube
with soft tissue paper. The internal injection port and inside of the needle guide pipe are
now clean.
Measurement of service water or contamination free environmental water, such as river
water, often reveals that IC is the major part of TC when the TOC content is around 1ppm.
For these types of samples it is preferable to remove the IC content before measuring TOC
through the TC channel.
Errors for TC and IC analyses are additive. For samples that have a comparatively high IC
content relative to the TOC content, the TOC analysis error will be large if it is determined
by the difference between TC and IC results.

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 4.5 Application Operations
4.5.1 Manual Injection Analysis

4.5.1.4 Maintenance

Replacing the IC Injection Port Septum (Cushion O-Ring)

The septum used with the IC injection port is a consumable item. The septum typically can
be used for 200 or more injections; however, it should be replaced if there is deterioration
in reproducibility or peak shapes.
Part number for replacement cushion O-ring (20 pcs.): P/N 630-01559-01

Replacement Procedure
1. Loosen and remove the injection port bushing.
2. Remove the old septum, and insert a new one.
3. Replace the bushing and tighten it.

CAUTION
IC reaction solution may spatter close to the injection port septum and injection
port; however, this poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.

Gas-tight Syringe
For analysis, use a needle length of 50mm, or a 2 inch gas-tight syringe. The following gas-
tight syringes are available from Shimadzu. Order replacement syringes as necessary.

Table 4.7 • Gas-Tight Syringes (Option)

Part Name P/N Capacity
Gas-tight syringe set 25uL 638-60733-02 25uL
Gas-tight syringe set 50uL -03 50uL*
Gas-tight syringe set 100uL -04 100uL*
Gas-tight syringe set 250uL -05 250uL*
Gas-tight syringe set 500uL -06 500uL*
Gas-tight syringe 1mL 046-00026-02 1mL
Gas-tight syringe set 5mL -03 5mL
Gas-tight syringe set 10mL -04 10mL
* Set comprises one replacement gas-tight syringe needle and one plunger.

226 TOC-VCPH/CPN
 4.5 Application Operations
4.5.2 Gas Sample Analysis

4.5.2 Gas Sample Analysis

If the optional manual injection kit is installed, analysis of TC and IC in gaseous samples
can be performed by using gas-tight syringes or other applicable injectors to inject the
gaseous samples.

¬Precautions for Gas Sample Analysis

CAUTION
• Do not inject a large quantity of sample at one time when measuring combustible
or explosive gases. The combustion tube could break. The injection volume
should not exceed 10mL.
• Use caution when measuring combustible or explosive gases.
• Do not analyze samples that can release toxic substances during combustion. The
exhaust gas released during analysis passes through the CO2 detector to the CO2
absorber, after which it is used as NDIR purge gas, and then is vented inside the
instrument. Take appropriate countermeasures if there is a possibility that toxic
substances could be included in the exhaust gas. If appropriate countermeasures
cannot be taken, do not perform such analyses.

• The sample analysis results are displayed according to the gas concentration used in cal-
ibration. For example, if CO2 is used to generate the calibration curve, the sample anal-
ysis result is displayed based on a conversion using the CO2 gas concentration.
• Gaseous samples have certain properties such as adsorption, condensation and reactiv-
ity, and some gaseous samples are partially liquid or contain a solid component.
Depending on the properties, certain conditions may occur that cannot be ignored. Some
of these conditions are residual substances and contamination in the flow line, which
may result in peak tailing, carryover, baseline fluctuation, or other analytical problems.
• High concentrations of NOx or SOx in the sample or in the post combustion-oxidized
sample can interfere with the NDIR activity. To evaluate the degree of the interference,
combine the analysis of the base gas without the TOC component together with the
sample analysis.

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 4.5 Application Operations
4.5.2 Gas Sample Analysis

4.5.2.1 Analysis Preparation

¬Installation of the Manual Injection Kit

Installation Procedure
1. Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider, and install the TC/TN block provided in the kit.
2. If the IC reactor kit is being used, remove the IC injector slider, and install the IC
block provided in the manual injection kit.
Note: When installing the block, be sure that it is aligned with the
injection port.

Software Settings
Select the Manual Injection Kit option in the Instrument Setup Wizard Options window
during System Setup. Refer to Section 3.2.2 "Options Window".
Note: Selecting the Manual Injection Kit option disables operation of the
TOC-V injector syringe.

Reference: Refer to 4.5.1.1 "Analysis Preparation".

228 TOC-VCPH/CPN
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4.5.2 Gas Sample Analysis

4.5.2.2 Measurement

The procedure for setting the various parameters is the same as described in Section 4.2
"Setting General Measurement Parameters", Section 4.3 "Measurement Procedures and
Tutorial" and Section 4.4.2.2 "Calibration Curve".

¬Calibration Curve Measurement

Procedure
1. Prepare standard gas containing a known concentration of carbon.
Note: For IC (carbon dioxide) analysis, prepare a standard gas with a
known carbon dioxide concentration. For TC analysis, another
organic gas (for example, methane) of known concentration can be
used.
2. From the File menu, select New. The New dialog box is displayed.

Figure 4.191 New Dialog Box

3. Double-click the Calibration Curve icon. The Calibration Curve Wizard opens. The
System Information window of the wizard (page 1) is displayed.

Figure 4.192 Calibration Curve Wizard (Page 1) System Information

4. From the System drop-down list, select the system that was configured with the
Manual Injection Kit during setup.

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 4.5 Application Operations
4.5.2 Gas Sample Analysis

5. Select the desired options on pages 2 and 3 of the Calibration Curve Wizard, which
list calibration curve type and analysis information settings, respectively. Enter the
name of the new calibration curve in the text box at the bottom of page 3 of the
wizard.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".
6. Enter the desired number of injections on page 4 of the Calibration Curve Wizard
(Calibration Measurement Parameters).
7. Enter the injection volume on page 5 of the Calibration Curve Wizard (Calibration
Points List).
Note: An injection volume is displayed automatically. The displayed
value is based on the volume of the last injection that was per-
formed using the sample injector. This value can be changed by the
user as appropriate.
8. Select the desired options on pages 6 and 7 of the Calibration Curve Wizard, which
list peak time parameter and history settings, respectively. Click the Finish button to
create the new calibration curve.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".
9. Create a Sample Table for the calibration curve. From the Insert menu, select
Calibration Curve. Select the newly created calibration curve from the list of files in
the Open dialog box.
10. Connect the instrument by selecting Connect from the Instrument menu. Then select
Start from the Instrument menu. The Manual Injection Parameter dialog box is
displayed.
11. Draw an appropriate amount of sample into the syringe.
Note: Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
12. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
13. Verify that the instrument is ready for measurement, and click the Start button.
14. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
15. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
The results are displayed when measurement is complete.
16. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.

230 TOC-VCPH/CPN
 4.5 Application Operations
4.5.2 Gas Sample Analysis

¬Sample Measurement

Procedure
1. From the File menu, select New. The New dialog box is displayed.

Figure 4.193 New Dialog Box

2. Double-click the Method icon. The Method Wizard opens. The System Information
window of the wizard (page 1) is displayed.

Figure 4.194 Method Wizard (Page 1) System Information

3. Select the system that was configured with the Manual Injection Kit and used to
create the calibration curve. Advance to page 2 of the Method Wizard (Analysis
Information) and enter the new method name in the text box at the bottom of the
window.
4. Advance to page 3 of the Method Wizard (Calibration Curves). Select the appropriate
calibration curve file.
5. Enter “1” in the No. of Injections field on page 4 of the Method Wizard (Injection
Parameters).

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 4.5 Application Operations
4.5.2 Gas Sample Analysis

6. Select the desired options on pages 5, 6, and 7 of the Method Wizard, which list peak
time parameter, USP/EP check, and history settings, respectively. Click the Finish
button to create the new method.
Note: Select the settings described in Section 4.2 "Setting General Mea-
surement Parameters".
7. From the Insert menu, select Sample. Select the newly created method from the list of
files in the Open dialog box. Complete the remaining pages of the Sample Wizard.
8. From the Instrument menu, select Start. The Manual Injection Parameter dialog box is
displayed.
9. Draw an appropriate amount of sample into the syringe.
Note: Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
10. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
11. Verify that the instrument is ready for measurement, and click the Start button.
12. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
13. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
14. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.

¬Maintenance
Replacing the IC Injection Port Septum (Cushion O-Ring)
The septum used with the IC injection port is a consumable item. The septum typically can
be used for 200 or more injections; however, it should be replaced if there is deterioration
in reproducibility or peak shapes.
Part number for replacement cushion O-ring (20 pcs.): P/N 630-01559-01

Replacement Procedure
1. Loosen and remove the injection port bushing.
2. Remove the old septum, and insert a new one.
3. Replace the bushing and tighten it.

232 TOC-VCPH/CPN
 4.5 Application Operations
4.5.2 Gas Sample Analysis

CAUTION
IC reaction solution may spatter close to the injection port septum and injection
port; however, this poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.

Gas-tight Syringe
For analysis, use a needle length of 50mm., or a 2-inch gas-tight syringe. The following
gas-tight syringes are available from Shimadzu. Order replacement syringes as necessary.

Table 4.8 • Gas-Tight Syringes (Option)

Part Name P/N Capacity
Gas-tight syringe set 25uL 638-60733-02 25uL*
Gas-tight syringe set 50uL -03 50uL*
Gas-tight syringe set 100uL -04 100uL*
Gas-tight syringe set 250uL -05 250uL*
Gas-tight syringe set 500uL -06 500uL*
Gas-tight syringe 1mL 046-00026-02 1mL
Gas-tight syringe set 5mL -03 5mL
Gas-tight syringe set 10mL -04 10mL
* Set comprises one replacement gas-tight syringe needle and one plunger.

Table 4.9 • Relationship Between Appropriate Peak Height and (CO2) Gas
Concentration / Injection Volume *
Gas Concentration (CO2) Gas Injection Volume
TC 100ppm 10mL
1000ppm 1mL
1% 500uL
10% 300uL
100% 30uL
IC 100ppm 6uL
1000ppm 600uL
1% 300uL
10% 200uL
100% 20uL

*The values indicated in this table are reference values only. Data will vary slightly among
instruments.

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 4.5 Application Operations
4.5.2 Gas Sample Analysis

234 TOC-VCPH/CPN
 5

5 Maintenance
Inspection and maintenance of the TOC-V instrument are required to ensure normal
operation and reliable and accurate data acquisition.

5.1 Daily Inspection

Describes the daily inspection procedures that should be performed before
instrument startup.

5.2 Periodic Inspections

Describes periodic inspection procedures for the TOC-V.

5.3 Autosampler (ASI-V) Maintenance

Describes periodic inspection procedures for the autosampler.

5.4 8-Port Sampler (OCT-1) Maintenance

Describes periodic inspection procedures for the 8-Port Sampler.

5.5 TN Unit (TNM-1) Maintenance

Describes periodic inspection procedures for the TN unit.

5.6 Software-Controlled Maintenance Functions

Describes maintenance functions controlled by the TOC-Control V software.

5.7 Troubleshooting
Describes the error messages and troubleshooting procedures.
 5.1 Daily Inspection
5.1.1 Checking Dilution Water

5.1 Daily Inspection

Check the levels of dilution water, acid, drain vessel water, and humidifier water each day
before starting the instrument.

5.1.1 Checking Dilution Water

Verify that the dilution water volume is sufficient for analysis. If necessary, replenish the
dilution water as described in Section 4.1.6 "Preparation of Dilution Water".

5.1.2 Checking Acid

Verify that the acid volume is adequate for analysis. If necessary, replenish the acid as
described in Section 4.1.7 "Acid Preparation". Any container such as a small-mouth glass 1
liter bottle can be used.

5.1.3 Checking Drain Vessel Water Level

Overflow Tube

Drain
Vessel

Pure Water

Figure 5.1 Drain Vessel Water Level

Verify that the water level in the drain vessel inside the instrument is within 10mm of the
overflow tube on the side of the drain vessel. Replenish as necessary with purified water
(ion-exchange water).

Reference: Refer toSection 4.1.4 "Water Supply to the Cooler Drain Container", for details on adding
purified water,.

Confirm that the carrier gas does not leak from the tip of the drain tubing when the flow
rate is 150mL/min.

236 TOC-VCPH/CPN
 5.1 Daily Inspection
5.1.4 Checking Humidifier Water Level

5.1.4 Checking Humidifier Water Level

Supply Port

Pure Water

“Lo” Mark

Figure 5.2 Humidifier Water Level

Verify that the water level in the humidifier is above the “Lo” mark. If the level is below the
“Lo” mark, replenish by adding purified water through the water supply port on top of the
vessel. Add water until the level reaches the “Hi” mark.

TOC-VCPH/CPN 237
 5.2 Periodic Inspections
5.2.1 Catalyst Regeneration

5.2 Periodic Inspections

Periodically inspect the items listed in this section to maintain instrument performance
quality.

5.2.1 Catalyst Regeneration

Inorganic substances contained in the samples accumulate in the catalyst as salts and
oxides. Buildup of these residues decreases the sensitivity and reproducibility of analyses.
(Catalyst performance can be checked by measuring a standard solution.) This type of
catalyst contamination occurs when measuring alkaline samples and samples that contain
high concentrations of IC compounds. When catalyst contamination occurs, performance
can be restored by regenerating the catalyst. Catalyst regeneration is also an effective
means of reducing the system blank peaks that are present when using new catalyst or
catalyst that has not been used for a long time. The catalyst regeneration procedure has little
effect on TN analysis.
Catalyst is regenerated by injecting dilute hydrochloric acid onto the catalyst. The acid used
in the procedure is 2M hydrochloric acid obtained from the instrument reservoir (acid used
during IC and NPOC analysis). The catalyst regeneration process is the same for both TOC
standard catalyst and TOC high sensitivity catalyst. If performance is not restored after the
regeneration process has been conducted, replace the catalyst. Refer to Section 5.2.2
"Washing or Replacing Catalyst".

Regeneration Procedure
The procedure for regenerating the TC catalyst is controlled by the TOC-Control V
software, as described below.
1. From the Instrument menu in the Sample Table Editor, select
Maintenance>Regeneration of the TC Catalyst.
The Regeneration of TC-Catalyst dialog box is displayed.

Figure 5.3 Regeneration of TC-Catalyst Dialog Box

2. Click the Start button to begin the procedure. A progress bar is active until the TC
catalyst has been regenerated.
3. Click the Close button.

238 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.2 Washing or Replacing Catalyst

CAUTION
Dilute hydrochloric acid is the only type of acid that can be used to regenerate
TC catalyst. Other acids, particularly phosphoric acid, cause abnormally high
peaks and scattered peak values to occur. If this happens, the catalyst must be
replaced.

5.2.2 Washing or Replacing Catalyst

Large quantities of salts accumulate in the catalyst when measuring samples with high salt
concentrations. If sensitivity and reproducibility do not improve after catalyst regeneration,
wash or replace the catalyst. Refer to Section 5.2.1 "Catalyst Regeneration".

5.2.2.1 Washing Catalyst

Standard catalyst can be washed and reused several times using the following procedure.
High sensitivity catalyst cannot be washed and reused.

WARNING
Due to the danger of burn injury, allow the oven temperature to cool to room
temperature before starting any maintenance procedure involving the
combustion tube or catalyst.

Procedure
1. Thoroughly wash the catalyst with tap water to remove any accumulated salts.
2. Neutralize the alkalis with dilute hydrochloric acid (5:1).
3. Thoroughly wash the catalyst with tap water to remove the hydrochloric acid.
4. Rinse with pure water (ion exchange water acceptable) and then dry.

CAUTION
• Dry the catalyst at a temperature lower than 700°C to avoid the degradation of
catalyst activity that occurs at higher temperatures.
• A large quantity of steam is produced when the regenerated catalyst is placed in
the oven and heated. Due to the danger of burn injury, leave the outlet of the
combustion tube open until no more steam is released.

TOC-VCPH/CPN 239
 5.2 Periodic Inspections
5.2.2 Washing or Replacing Catalyst

5.2.2.2 Replacing Catalyst

If performance is not restored after washing the catalyst, it must be replaced. Replace the
catalyst with new platinum catalyst (alumina spherical support). Keep extra platinum
catalyst on hand for such a contingency. One bottle of platinum catalyst is enough for one
replacement.
Use the following procedure to replace the platinum catalyst.

Procedure
1. Wash the platinum mesh and the inside of the combustion tube with (1:2)
hydrochloric acid (1 part concentrated HCl and 2 parts water).
2. Rinse with water.
3. Dry, and reuse these items.
4. Fill the combustion tube as described in Section 4.1.1 "Catalyst Filling".

TOC High Sensitivity Catalyst

TOC high sensitivity catalyst cannot be washed and reused like standard catalyst. If
analysis sensitivity and reproducibility are not restored after catalyst regeneration, replace
the deteriorated high sensitivity catalyst with new high sensitivity catalyst. The platinum
mesh and combustion tube can be washed with hydrochloric acid and reused.

Disposal of Catalyst
Used catalyst should be disposed of according to local industrial waste disposal regulations.
It must be clearly disclosed using an industrial waste manifest that the used catalyst
contains platinum.

5.2.2.3 Replacing the Carrier Gas Purification Tube and Catalyst

The carrier gas purification tube burns the carrier gas and oxidizes carbon-based impurities,
converting them to carbon dioxide. The carbon dioxide is absorbed and eliminated by the
CO2 absorber. The carrier gas purification tube is filled with oxidation catalyst (same as
TOC standard catalyst).
The procedure for replacing the purification tube and catalyst is as follows.

Removal of Carrier Gas Purification Tube

WARNING
Before attempting to remove the carrier gas purification tube, be sure to allow
the oven temperature to cool to room temperature. There is a danger of burn
injury if this procedure is performed while the oven is hot.

240 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.2 Washing or Replacing Catalyst

Removal Procedure
1. Remove the compression fitting joints at the top and bottom of the carrier gas
purification tube.
2. Detach the TC/TN sample injection block from the combustion tube. Refer toSection
4.1.2 "Connecting the Combustion Tube".
3. Extract the carrier gas purification tube from the electric oven by pulling upward.

Replacing Catalyst

CAUTION
The top nut of the compression fitting joint is hand-tightened. Do not use tools to
tighten or loosen this nut. Because the tube is constructed of quartz glass,
over-tightening or aggressive handling may result in damage.

Procedure
1. Remove the catalyst from the carrier gas purification tube through the opening at the
top.
2. Remove the quartz wool using a thin tube or other instrument.
3. Insert a small amount of new TOC standard catalyst into the combustion tube from
the bottom (straight end).
4. Pack a small amount of quartz wool into the tube from the bottom.
Note: The quartz wool is inserted to prevent the catalyst from falling out
of the bottom. Packing too much quartz wool into the tube will
greatly impede airflow, so do not use too much quartz wool. To
prevent contamination of the catalyst or the inclusion of foreign
particles, use the same precautions used when filling the
combustion tube with TOC platinum catalyst.
5. Insert the straight end of the carrier gas purification tube down into the front 8mm
diameter hole in the oven.
6. Using the compression fitting joints, restore the tubing connections to their original
condition.

TOC-VCPH/CPN 241
 5.2 Periodic Inspections
5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes

5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes

The inner surface of the combustion tube devitrifies (becomes crystalline in texture and
turns white) when it reacts with salts contained in the samples. The tube can continue to be
used in this condition until it breaks or cracks.
During the catalyst washing or replacing process, wash the interior of the combustion tube
and carrier gas purification tube with (1:2) hydrochloric acid (1 part concentrated HCl and
2 parts water) to remove the contaminants and accumulated salts. Rinse with water, dry,
and then reuse the tube(s).

5.2.4 Replacing the High-Purity Air Cylinder

A 47-liter cylinder of high-purity air used as the carrier gas will last for approximately three
months using the H Type instrument, and two months using the N Type.
• Replace the cylinder when the residual pressure diminishes to a few hundredkPa. Do
not wait until it is completely empty.
• When connecting a new cylinder, clean the connections thoroughly. After connecting
the cylinder, do not allow dust or other matter to enter the instrument.
• Keep a spare cylinder available at all times.

5.2.5 Replacing the CO2 Absorber

Once a year, replace each of the CO2 absorbers (P/N 630-00999), which are located in the
holder behind the instrument.

CO2 Absorber Disposal Procedure

Used CO2 absorbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the used
CO2 absorber contains soda lime.

Reference: For details on replacing the CO2 absorbers, refer to Section 4.1.8 "Installation of the CO2
Absorber".

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 5.2 Periodic Inspections
5.2.6 Replacing the Halogen Scrubber

5.2.6 Replacing the Halogen Scrubber

The absorbent inside the halogen scrubber turns black as it absorbs chlorine. The
discoloration band advances toward the outlet as the amount of chlorine absorbed
increases. Replace the scrubber with a new halogen scrubber when the front of the
discoloration band reaches the position shown in Figure 5.4 "Halogen Scrubber".

Replacement Procedure
1. Unclip the upper and lower clips that secure the halogen scrubber.
2. Remove the upper and lower connection clamps.
3. Disconnect the Viton connectors and remove the halogen scrubber.

Replace Scrubber When

Discoloration Band Reaches
Gas Flow Direction this Point

Dehumidifier To Sample
Cell Inlet

Halogen Reactant-filled Cylinder

Figure 5.4 Halogen Scrubber

The baseline may fluctuate immediately after replacement. Allow the instrument to run for
a short time until the baseline stabilizes. Stabilization normally occurs within one hour.
Used halogen scrubbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the halogen
scrubber contains copper.

Clamps

Clips

Viton Connectors

Figure 5.5 Halogen Scrubber Replacement

TOC-VCPH/CPN 243
 5.2 Periodic Inspections
5.2.7 Replacing the Syringe Plunger Tip

5.2.7 Replacing the Syringe Plunger Tip

The syringe plunger tip is constructed of fluororesin and wears with use. Gaps will
eventually form between the plunger and the inner wall of the syringe barrel (glass tube),
causing leaks. When leaks occurs, bubbles are produced near the syringe tip when sample
is drawn into the syringe or sample may leak from the bottom of the barrel when the sample
is discharged. When these problems are observed, replace the plunger tip.

Replacement Procedure
1. Remove the syringe referring to Section 4.1.3 "Installing the Syringe".
2. Use a sharp knife to make two or three incisions at the bottom of the plunger tip, as
shown in Figure 5.6 "Removing the Old Plunger Tip".
3. Grasp the plunger tip with a pair of pliers and remove it from the plunger. The O-ring
that is held in place by the plunger tip also comes off. DO NOT reuse this O-ring.

Figure 5.6 Removing the Old Plunger Tip

4. Pushing down on the plunger, press the leading edge of the new plunger tip straight
into the plunger tip seat, as shown in Figure 5.7 "Installing the New Plunger Tip
(cross-section)". Save the syringe for future use since the plunger tip seat is enclosed
inside the syringe.

Plunger Tip

Plunger Tip Seat

Figure 5.7 Installing the New Plunger Tip (cross-section)

Note: • Do not scratch the perimeter of the plunger tip. This could cause leaks.
• Use only Shimadzu-specified plunger tips. Use of unspecified parts may
result in malfunction and/or diminished performance.

244 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.8 Replacing Ferrules at the Combustion Tube Outlet Connection

5.2.8 Replacing Ferrules at the Combustion Tube Outlet Connection

For High Sensitivity Analysis Kit

The front and rear Teflon ferrules used in the compression fitting connections at the
combustion tube outlet gradually become deformed and scratched with repeated use, and
may cause gas leakage. When this occurs, replace them with new ferrules. Keep a 6F-T
Sleeve set on hand as replacement parts.

Reference: For details on the replacement procedure, refer to Section 4.1.2 "Connecting the
Combustion Tube".

5.2.9 Replacing the Sliding Sample Injector O-rings

Two types of O-rings are stacked between the injection block and the slider of the sample
injector. If a gas leak develops in this area, replace both O-rings.
• White Upper O-ring: O-ring, Teflon P10 (P/N 036-11408-84)
• Black Lower O-ring: O-ring, 4DP10A (P/N 0936-11209-84)

White O-ring

Black O-ring

Figure 5.8 Replacing the Sliding Sample Injector O-rings

If a gas leak develops between the injector block and the combustion tube, replace the
O-ring there as well.

CAUTION
Do not scratch the O-rings or the O-ring seat when replacing the O-rings.

TOC-VCPH/CPN 245
 5.2 Periodic Inspections
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor

5.2.10 Replacing the Syringe Pump 8-port Valve Rotor

The fluororesin rotor of the syringe pump 8-port valve gradually becomes worn and
scratched after prolonged use due to suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate that
rotor replacement is necessary.
• Droplets of liquid around the 8-port valve (especially around the upper shaft)
• Decreased analysis reproducibility
• Presence of bubbles in the syringe
If the leakage is great, sample remaining in the tubing after it is drawn into the syringe may
flow back into the sample container. This is most likely due to a sampling tubing flange or
connection problem.

CAUTION
Switch OFF the instrument before replacing the 8-port valve rotor.

Procedure
1. Shut down the instrument and turn OFF the power.
2. Verify that the O mark on the 8-port valve interrupt plate is directed toward the No. 1
port. If not, the instrument was not shut down using the appropriate procedure. In this
case, switch the instrument back ON, and follow the correct shutdown procedure.

Reference: For the correct shutdown procedure, refer to Section 4.3.3 "Ending Measurement".
3. Remove the nut using the provided wrench.

Nut

Figure 5.9 Removing the Nut

4. Pull up to remove the rotor drive component. Hang it on the screw on the right side of
the plunger.

246 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor

5. Loosen the retaining nut using the provided wrench.

Spring-equipped Rod

Retaining Nut

Figure 5.10 Removing the Retaining Nut

6. Note the orientation (toward port No. 1) of the flat surface of the spring-equipped rod.
Remove the spring-equipped rod and retaining nut.
7. Note the orientation of the rotor hole position. Grasp the rotor with forceps and
remove by pulling up.

Rotor

Figure 5.11 Removing the Rotor

8. Insert a new rotor, taking care that the rotor hole matches original orientation.
9. Reinsert the retaining nut and spring-equipped rod, with the flat surface directed
toward port No. 1. Tighten the retaining nut.
10. Replace the rotor drive component, and tighten the nut.
11. Switch the instrument ON.
Note: Perform the syringe pump zero detection procedure before analysis.
Refer to Section 4.1.3.1 "Syringe Pump Zero Point Detection".

TOC-VCPH/CPN 247
 5.2 Periodic Inspections
5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier

5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier
The NDIR baseline becomes unstable with a decrease in the carbon dioxide absorption in
the carrier gas purifier CO2 absorber. The baseline position rises and reproducibility
diminishes, making analysis impossible. The soda lime must be replaced when this occurs.
The frequency with which soda lime must be replaced depends on the frequency of
analysis, quantity of organic impurities in the carrier gas, and the TOC content of the
samples. It is recommended that soda lime be replaced once every four months.

Soda Lime Replacement Procedure

CAUTION
The carrier gas pressure applied to the carrier gas purifier CO2 absorber is
approximately 200kPa. It is dangerous to perform this maintenance procedure
under these conditions. Before replacing the soda lime, lower the carrier gas
pressure in the instrument to normal as follows:
• Turn the supply valve of carrier gas source OFF.
• Switch OFF the instrument.

Procedure
1. Remove the elbow joints of the carrier gas purifier CO2 absorber, which are behind
the instrument.
2. Invert the CO2 absorber and remove the screw cap.
3. Remove the used soda lime.
4. Refill the absorber container with about 500g of new soda lime until it reaches about
5mm from the interior screw threads.

CAUTION
Do not allow any soda lime to enter the tube in the center of the container when
refilling the CO2 absorber.

5. Fill the hollow in the screw cap with quartz wool and screw the cap back on the
container.

CAUTION
To maintain an airtight seal, a rubber O-ring is placed between the container and
the screw cap. Inspect the O-ring to verify that it is not scratched or twisted, then
attach the cap.

248 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.12 Replenishing IC Reaction Solution

6. Using the elbow joints, connect the carrier gas purifier CO2 absorber to the two tubes
exiting the back of the instrument as follows:
• Tubing labeled “L”: Affixed to the connection port of the CO2 absorber container
labeled “L”
• Tubing labeled “S”: Affixed to the connection port of the CO2 absorber container
labeled “S”

CAUTION
Tighten the nut by hand only. Do not use tools.

7. Place the carrier gas purifier CO2 absorber container on the stand behind the
instrument.
Used soda lime should be disposed of according to local industrial waste disposal reg-
ulations. It must be clearly disclosed using an industrial waste manifest that the mate-
rial contains soda lime.

CAUTION
Soda lime is a corrosive chemical substance. Be careful not to touch it with bare
hands. For details, refer to Section 6.9 "Material Safety Data Sheets".

5.2.12 Replenishing IC Reaction Solution

For the H Type, verify that there is sufficient IC reaction solution in the IC reaction solution
vessel before performing IC analysis. If not, replenish the IC reaction solution referring to
Section 4.1.11 "IC Analysis Preparations".

CAUTION
The IC reaction solution is acidic. Use care not to spill or touch the fluid when
handling it. For details, refer to Section 6.9 "Material Safety Data Sheets".

TOC-VCPH/CPN 249
 5.2 Periodic Inspections
5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump

5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump

The IC reaction solution pump is a roller type pump that uses a rotating roller to flatten the
rubber tube carrying the IC reaction solution, thereby feeding solution into the system. This
rubber tubing gradually deteriorates, requiring periodic replacement of the pump head.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
dialog box. Refer to Section 4.2.4 "Maintenance History Settings".

CAUTION
The pump head and rubber tubing inside the IC reagent pump are filled with IC
reagent solution. This solution is acidic. Use care to avoid touching or spilling
the solution when changing the pump heads. For details refer to Section 6.9
"Material Safety Data Sheets".

Replacement Procedure
Use the following procedure to replace the rubber tubing of the pump head.
1. Grasp the front and rear stops of the pump head by hand. Pull the white pump head
from the black pump body.
2. Disconnect both of the yellow rubber tubes on the left side of the pump head from the
Teflon tubes.
3. Connect the new rubber tubing to the Teflon tubes of the pump head.
4. Replace the pump head by following the above procedure in reverse.

Figure 5.12 Replacing the Pump Head of the IC Reaction Solution Pump

250 TOC-VCPH/CPN
 5.2 Periodic Inspections
5.2.14 Replacing the Filler of the Optional POC Analysis CO2 Absorber

5.2.14 Replacing the Filler of the Optional POC Analysis CO2 Absorber
The CO2 absorber for POC analysis is filled with about 6 grams of lithium hydroxide,
which is sufficient to absorb carbon dioxide gas for several hundred analyses under normal
conditions. Airflow resistance gradually increases with use and may become excessive
irrespective of adequate carbon dioxide absorbency.
Replace the lithium hydroxide in the CO2 absorber with a new batch if analysis values
become unstable or carrier gas flow is impeded. For the procedure on filling the CO2
absorber with lithium hydroxide, refer to Section 4.1.12 "Preparation for POC analysis".

CAUTION
• Lithium hydroxide is a corrosive (strongly alkali) powder. Be carefuel not to spill
or touch it during handling. For details, refer to Section 6.9 "Material Safety
Data Sheets".
• Used lithium hydroxide should be disposed of by a certified industrial waste
handler according to local industrial waste disposal regulations. It must be clearly
disclosed using an industrial waste manifest that the waste is lithium hydroxide.
• Lithium hydroxide crystal is found in both anhydrous and hydrated forms.
Because the carbon dioxide gas absorbance properties of the hydrated form are
slightly inferior to those of the anhydrous form, use anhydrous lithium hydroxide
to fill the CO2 absorber.
• The life of the CO2 absorber will be shortened by performing POC analysis on
samples with high concentrations of IC.

TOC-VCPH/CPN 251
 5.3 Autosampler (ASI-V) Maintenance
5.3.1 Rinse Bottle Inspection

5.3 Autosampler (ASI-V) Maintenance

Maintenance of the autosampler includes periodic inspection of the rinse bottle, sample
catcher and rinse pump.

5.3.1 Rinse Bottle Inspection

Perform the following inspections before conducting analysis with the autosampler. If the
following inspections are not properly conducted, air will be drawn into the autosampler
injection pump, preventing the delivery of rinse water.
• Check the rinse water level
Verify that the water in the rinse bottle is above the 2-liter level mark. Add water if nec-
essary.
• Check the rinse tubing
Verify that the tip of the rinse tubing reaches nearly to the bottom of the rinse bottle.
Adjust the tubing position if necessary.
Rinse Tubing

Rinse Bottle

Figure 5.13 Rinse Bottle Inspection

5.3.2 Sample Catcher Inspection

Examine the turntable (black plate) and the sample catcher tray below the turntable when
installing or removing the autosampler vial rack. If they are wet or dirty, wipe them clean.

CAUTION
Corrosion of the instrument may occur if spilled sample is allowed to remain in
the sample catcher. Keep the sample catcher clean.

252 TOC-VCPH/CPN
 5.3 Autosampler (ASI-V) Maintenance
5.3.3 Replacing the Pump Head of the Rinse Pump

5.3.3 Replacing the Pump Head of the Rinse Pump

The rinse pump is located inside the autosampler and supplies rinse water to the rinse port.
The rinse pump is a roller type pump that uses a rotating roller to flatten the rubber tubing
carrying the rinse water, thereby feeding rinse water into the system. This rubber tubing
gradually deteriorates, requiring periodic replacement.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
dialog box. For details, refer to Section 4.2.4 "Maintenance History Settings".

Replacement Procedure
Use the following procedure to replace the pump head.
1. Remove the rectangular pump access cover on the back left side of the autosampler.
2. Grasp the latch on the pump head by hand and pull the white pump head from the
black pump body.
3. On the left side of the pump head, disconnect both of the yellow rubber tubes from the
Teflon tubes.
4. Connect the new rubber pump head tubing to the Teflon tubes.
5. Replace the pump head by following the above procedure in reverse and then replace
the pump access cover.

Pump
Head

Figure 5.14 Replacing the Pump Head of the Rinse Pump

TOC-VCPH/CPN 253
 5.4 8-Port Sampler (OCT-1) Maintenance
5.3.3 Replacing the Pump Head of the Rinse Pump

5.4 8-Port Sampler (OCT-1) Maintenance

5.4.1 Replacing the 8-Port Valve Rotor

The OCT-1 uses a fluororesin 8-port valve rotor. The valve rotor may become worn or
scratched after prolonged use due to the suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate
that it is necessary to replace the rotor.
• Droplets of liquid around the 8-port valve (especially, around the upper shaft)
• Decreased analysis reproducibility.
• Presence of bubbles in the TOC-V syringe.
If the leak is large, sample remaining in the tubing after the syringe has been filled may
flow back into the sample container. This is most likely due to a sample tubing or
flange connection problem.

CAUTION

Switch OFF the power before replacing to the 8-port valve rotor.

Replacement Procedure
1. Shut down the TOC-V unit and switch OFF the power.
Reference: Refer to Section 4.3.3 "Ending Measurement" for details on shutting down the TOC-V unit.
2. Remove the 4 screws at the top of the 8-Port Sampler, and take OFF the cover.
3. Verify that the O mark on the 8-port valve cover is directed toward port No.1.

Note: If the O mark is not directed toward port No.1, the instrument was not
shut down properly. If this is the case, turn the TOC-V on again, and
shut it down properly.

254 TOC-VCPH/CPN
 5.4 8-Port Sampler (OCT-1) Maintenance
5.3.3 Replacing the Pump Head of the Rinse Pump

4. Remove the nut using the wrench supplied with the TOC-V.

Nut

Figure 5.15 Removing the Nut

5. Remove the 8-port valve by pulling it downward.

6. Loosen the retaining nut using the provided wrench.
Retaining Nut

Figure 5.16 Removing the Retaining Bracket

7. Note the orientation (toward port No. 1) of the flat surface of the spring-equipped rod.
Remove the spring-equipped rod and retaining nut.
8. Note the orientation of the rotor hole position. Grasp the rotor with forceps, and
remove by pulling upwards.
Rotor

Figure 5.17 Removing the Rotor

9. Insert a new rotor, positioning the rotor hole to the original position.
10. Reinsert the spring-equipped rod and retaining nut with the flat surface directed
toward port No. 1. Tighten the retaining nut.
11. Replace the 8-port valve in its original position, and secure it using the nut.
12. Replace the cover of the 8-Port Sampler and secure it with four screws.
13. Switch on the TOC-V unit.
TOC-VCPH/CPN 255
 5.5 TN Unit (TNM-1) Maintenance
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit

5.5 TN Unit (TNM-1) Maintenance

Maintenance of the TN unit includes periodic inspection of the ozone treatment unit
catalyst, chemiluminescence detector and ozone generator.

5.5.1 Replacing the Catalyst in the Ozone Treatment Unit

The ozone treatment unit breaks down ozone gas produced by the ozone generator. The
catalyst inside the ozone treatment unit must periodically be replaced. Replace the catalyst
once a year for an instrument that runs 8 hours a day and 5 days a week.
Perform maintenance to the ozone treatment unit only after stopping the instrument as
described inSection 4.3.3 "Ending Measurement".

CAUTION
The interior of the ozone treatment unit is heated to 50°C. Perform maintenance
only after cooling for at least two hours.

Replacement Procedure
Use the following procedure to replace the catalyst in the ozone treatment unit.
1. Remove the knurled screw at the bottom of the unit, and remove the installation
bracket.
Ozone
Treatment Unit

Knurled Screw

Installation Bracket

Figure 5.18 Removing the Ozone Treatment Unit Screw and Bracket

256 TOC-VCPH/CPN
 5.5 TN Unit (TNM-1) Maintenance
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit

2. Remove the hose clamp at the bottom of the ozone treatment unit and pull off the
Viton tubing.

Hose Clamp

Viton Tubing

Figure 5.19 Removing the Viton tube

3. Remove the hose clamp at the top of the unit and remove it from the Viton coupling.

Hose Clamp

Viton Coupling

Figure 5.20 Removing the Ozone Treatment Unit

TOC-VCPH/CPN 257
 5.5 TN Unit (TNM-1) Maintenance
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit

4. Remove the cap from the ozone treatment unit and take out the used catalyst and
polypropylene packing material.

Figure 5.21 Emptying and Removing the Ozone Treatment Catalyst

5. Pack a small amount of new polypropylene packing material into the bottom of the
ozone treatment unit, then fill with approximately 60 grams of catalyst.
6. Insert a small amount of new polypropylene packing material on top of the catalyst.
7. Place the cap back on the container.
8. Remove the Viton coupling connecting the detector exhaust opening to the inlet of the
ozone treatment unit.
Replace this Viton coupling with a new one whenever the catalyst is replaced. Inspect
the Viton tubing at the outlet of the ozone treatment unit and replace it if cracked or
damaged.
9. Reconnect the Viton tubing and Viton coupling, and reinstall the ozone treatment unit.

CAUTION
Used catalyst should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that
the catalyst contains manganese dioxide.

258 TOC-VCPH/CPN
 5.5 TN Unit (TNM-1) Maintenance
5.5.2 Chemiluminescence Detector

5.5.2 Chemiluminescence Detector

The light receiving window of the chemiluminescence detector may become soiled by
components in the samples. Inspect and clean the window and gasket at least once a year.

Maintenance Procedure
Perform maintenance on the detector only after shutting down the instrument.
1. After removing the tubing from the reactor, as shown in the figure below, loosen the 4
mounting screws, and detach the reactor.
Detector

Reactor

Mounting
Screws

Gasket

Figure 5.22 Removing the Reactor

2. Remove the gasket and confirm that it is not dirty or cracked. Replace it if necessary.
3. Confirm that the detector window is not dirty. If necessary, gently wipe the window
clean with a cloth.
4. Place the flat side of the gasket facing the detector window, sandwiching it between
the window and the reactor.
5. Secure the gasket in place with the 4 mounting screws, tightening them uniformly.
6. Reconnect the tubing.

CAUTION
Recheck the tubing after completing the maintenance work to make absolutely
certain that there are no mistakes in the line connections and that everything has
been properly tightened.

TOC-VCPH/CPN 259
 5.5 TN Unit (TNM-1) Maintenance
5.5.3 Ozone Generator Replacement

5.5.3 Ozone Generator Replacement

Replace the ozone generator with a new one after 8000 hours of operation. Set a warning
generation value of 8000 hours in the Maintenance History dialog box. For details, refer to
Section 4.2.4 "Maintenance History Settings".
Ozone generator replacement must be carried out by an authorized Shimadzu service
engineer, or someone who has been properly trained in the procedure. Contact your
Shimadzu representative to request replacement at the appropriate time.

Confirming Operation Time

The ozone generator operating time is displayed in the Maintenance History window,
which is accessed through the Sample Table Editor. From the Instrument menu, select
Maintenance>Maintenance History.

CAUTION
If the ozone generator is used after 8000 hours of operation, ozone generation
may not be sufficient for analysis, or ozone may leak from inside the generator.
Replace the ozone generator without fail.

5.5.4 Replacing the NOx Absorber

The NOx absorber absorbs NOx gas generated in the TN unit. A CO2 absorber is used for
the NOx absorber. The CO2 absorber was previously used for purging the NDIR detector
optical system Section 5.2.5 "Replacing the CO2 Absorber" and is still effective for this
application.
During the annual replacement of the CO2 absorber used to purge the optical system of the
NDIR detector, replace the NOx absorber for the TN unit with the used CO2 absorber from
the TOC-V.

Discarding the NOx Absorber (CO2 Absorber)

Place a request to an authorized industrial waste contractor to process the used NOx
absorber (CO2 absorber). Clearly indicate in the industrial waste material manifest that the
absorber contains soda lime.

260 TOC-VCPH/CPN
 5.6 Software-Controlled Maintenance Functions
5.6.1 Zero Point Detection

5.6 Software-Controlled Maintenance Functions

Maintenance functions that can be performed using the TOC-Control V software are
described below. These functions can be accessed through the Instrument>Maintenance
menu.

Figure 5.23 Instrument>Maintenance Menu

To access the menu, select Instrument>Maintenance in the Sample Table Editor.

5.6.1 Zero Point Detection

Use this function to determine the zero point of the syringe. Click the Start button to begin
the procedure, during which a progress bar is active. The progress bar becomes inactive
after the syringe zero point is determined. Click the Close button.

Figure 5.24 Zero Point Detection Dialog Box

TOC-VCPH/CPN 261
 5.6 Software-Controlled Maintenance Functions
5.6.2 Regeneration of the TC Catalyst

5.6.2 Regeneration of the TC Catalyst

Use this function to restore the sensitivity and efficiency of the TC catalyst, which decrease
over time as inorganic substances are deposited on the catalyst surface. During the
procedure, dilute hydrochloric acid is injected onto the catalyst. Be sure to verify that
sufficient hydrochloric acid is in the instrument acid reservoir before starting the procedure.

Figure 5.25 Regeneration of TC Catalyst Dialog Box

Click the Start button to begin the procedure. A progress bar is active until the TC catalyst
is regenerated. Click the Close button.

5.6.3 Regeneration of the IC Solution

Use this function to restore the acidity of the IC solution, which decreases over time as the
acid reacts with IC sample constituents. During the procedure, IC reagent is automatically
pumped to the IC reaction vessel. This option is available only if an IC unit is connected to
the system.

Figure 5.26 Regeneration of IC Solution Dialog Box

Click the Start button to begin the procedure. A progress bar is active until the IC solution
is regenerated. Click the Close button.

262 TOC-VCPH/CPN
 5.6 Software-Controlled Maintenance Functions
5.6.4 Residue Removal

5.6.4 Residue Removal

Use this function to remove residue from the flow lines and syringe.

Figure 5.27 Residue Removal Dialog Box

Click the Start button to begin the procedure. A progress bar is active until the residue
removal procedure is complete. Click the Close button.

5.6.5 Replace Flowline Content

Select this command to replace the contents of the flow lines connected to the 8-port valve
from the dilution solution bottle and the hydrochloric acid bottle.

Figure 5.28 Replace Flow Line Content Dialog Box

Click the Start button to begin the procedure. A progress bar is active until the flow line
content has been replaced. Click the Close button.

TOC-VCPH/CPN 263
 5.6 Software-Controlled Maintenance Functions
5.6.6 Flowline Washing

5.6.6 Flowline Washing

Use this function to wash the selected flow lines.

Figure 5.29 Washing Dialog Box

To perform flow line washing, click the Select Flow Lines button to open the Wash Flow
Lines dialog box. Select the flow lines to be washed, and click the Washing button. The
ports for the 8-Port Sampler 1 (2) can be selected if the 8-Port Sampler 1 (2) is being used.

Figure 5.30 Wash Flow Lines Dialog Box

While this process is being executed, the buttons in the Washing dialog box are disabled,
and progress bar activity is displayed.

264 TOC-VCPH/CPN
 5.6 Software-Controlled Maintenance Functions
5.6.7 Mechanical Check

5.6.7 Mechanical Check

Select this function to check mechanical components of the instrument or to make
adjustments. The Mechanical Check window consists of several tabs, one for each
connected instrument.

¬TOC Tab

Figure 5.31 Mechanical Check Window: TOC Tab

Syringe Pump
Use the buttons to move the syringe pump to the Zero, Home, or Sparge posi-
tions. Click the Reset button to move the plunger to the highest position.
Solenoid Valves
Use the buttons to open or close the various solenoid valves. Different options
are available depending on the instrument configuration and oxidation method.
Port Select
Open the line between the syringe and an injection port by clicking the button for
the desired port.
TC Inj. Port
Specify whether the port should be set to drain or measure by clicking the appro-
priate button.
IC Inj. Port
Specify whether the port should be set to drain or measure by clicking the appro-
priate button.
Acid Pump
Use the buttons to open or close the IC acid pump lines.

TOC-VCPH/CPN 265
 5.6 Software-Controlled Maintenance Functions
5.6.7 Mechanical Check

¬ASI / 8-Port Sampler Tab

Figure 5.32 ASI / 8-Port Sampler Tab of Operation Verification Dialog Box

Rinse
Use the On and Off buttons to start and stop the ASI flow line rinsing option.
Move Tray
Use the directional arrows to move the ASI tray to the desired position. Click the
Reset button to return the tray to its home position.
Arm
Use the directional arrows to move the arm vertically. Use the drop-down list to
move the arm horizontally.
Vial Position
Use the spin controls to enter a vial position, then click the Move button to verify
that the arm moves to the specified vial position. This is the only option that is
enabled for systems using the OCT-1 8-port sampler.
Magnetic Stirrer
Use the On and Off buttons to start and stop the magnetic stirrer.

266 TOC-VCPH/CPN
 5.6 Software-Controlled Maintenance Functions
5.6.8 ASI / 8-Port Sampler Initialization

5.6.8 ASI / 8-Port Sampler Initialization

Use this function when first connecting the instrument to establish communication between
the TOC-Control V software and the ASI or 8-Port Sampler. This option is disabled if an
ASI or 8-Port Sampler is not connected to the system.

Figure 5.33 Initialize ASI / 8-Port Sampler Window

Click the Start button to begin the procedure, during which a progress bar is active. The
progress bar becomes inactive after the ASI or 8-Port Sampler is initialized. Click the Close
button.

5.6.9 ASI Rack Change

Use this function to change the ASI rack. This option is disabled if an ASI is not connected
to the system.

Figure 5.34 ASI Rack Change Window

Click the Preparation Start button to begin the procedure. A progress bar is active while the
rack moves to the position where it can be replaced. When the progress bar begins blinking,
replace the rack. Click the Finish Replacement button to initialize the ASI and complete the
rack change process. Click the Close button.

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 5.6 Software-Controlled Maintenance Functions
5.6.10 ASI Needle Change

5.6.10 ASI Needle Change

Use this function to change the ASI needle. This option is disabled if an ASI is not
connected to the system.

Figure 5.35 ASI Needle Change Window

Click the Preparation Start button to begin the procedure. A progress bar is active while the
needle moves to the position where it can be replaced. When the progress bar begins
blinking, replace the needle. Click the Finish Replacement button to initialize the ASI and
complete the needle change process. Click the Close button.

5.6.11 Change Syringe

Use this function to replace the syringe.

Figure 5.36 Syringe Change Window

Click the Preparation Start button to begin the procedure. A progress bar is active while the
syringe moves to the position where it can be replaced. When the progress bar begins
blinking, replace the syringe. Verify that the syringe moves smoothly between the upper
and lower positions by clicking the directional arrows. Click the Finish Replacement button
to move the syringe to its initialization position, then click the Close button.
Note: Perform the zero point detection procedure whenever a new syringe is installed
or the syringe is replaced. Refer to Section 4.1.3.1 "Syringe Pump Zero Point
Detection".

268 TOC-VCPH/CPN
 5.6 Software-Controlled Maintenance Functions
5.6.12 Blank Check

5.6.12 Blank Check

Use this function to automatically determine the background TC level of the instrument.
Conducting the Blank Check procedure is recommended prior to performing high
sensitivity measurements and after loading high sensitivity catalyst. Open a blank Sample
Table, connect the instrument, and select the Blank Check option from the Instrument
menu. Refer to Section 4.1.15.2 "TC Blank Check Analysis" for details. Set the injection
volume using the spin controls, then click the Start button to begin the procedure.

Figure 5.37 Blank Check Parameters Window

Note: Do not insert a sample into the Sample Table. The Blank Check procedure only
works in a blank Sample Table.

5.6.13 Maintenance Log

Refer to Section 4.2.4 "Maintenance History Settings" for more details.

5.6.14 History
Use this option to view the operational history of various instrument components and to set
limits for various parameters of the components. When a limit is exceeded for an
instrument component, a warning message will be generated on the PC screen to remind the
user to perform maintenance on the component. Refer to Section 4.2.4 "Maintenance
History Settings" for a detailed description of this function.

5.6.15 Sparge Gas Valve

Select this option to start and stop the flow of sparge gas when the external sparge kit is
used.

5.6.16 Adjust Sparging Flow Rate (Wet Chem.)

Use this function to adjust the sparge gas flow rate. This option is available only when the
wet chemical oxidation method is used.

TOC-VCPH/CPN 269
 5.7 Troubleshooting
5.7.1 Error Messages

5.7 Troubleshooting

This section describes the error messages displayed by the TOC-Control V software and
the actions recommended to resolve the underlying causes.

5.7.1 Error Messages

The following error messages are displayed on the PC screen when setting or operation
errors are made, or when problems with instrument operation occur. Take the corrective
actions indicated in the table below.

Table 5.1• Error Message List 1

Error Message Description Corrective Action
WARNING: Dilution water Actual amount of dilution water used Replenish the water in the dilution water con-
depleted exceeds value set in the Maintenance tainer. Then, reset the Dilution Water amount in
History Settings. the Maintenance History Settings.
WARNING: Acid depleted Actual amount of hydrochloric acid Replenish the hydrochloric acid in the acid con-
used exceeds value set in the Mainte- tainer. Then, reset the Total Acid Volume in the
nance History Settings. Maintenance History Settings.
ERROR: Combustion tube Actual volume of sample injected into Either regenerate the catalyst or replace the cata-
sample injections exceeded. combustion tube exceeds value set in lyst and combustion tube. Then, reset the Total
the Maintenance History Settings. TC Injection Volume in the Maintenance History
Settings.
ERROR: Syringe stroke num- Actual number of syringe strokes per- Replace the plunger tip. Then, reset the Syringe
ber exceeded formed exceeds value set in the Mainte- Stroke value in the Maintenance History Set-
nance History Settings. tings.
WARNING: IC pump tube Actual IC pump tubing operation time Replace the IC pump tubing. Then, reset the IC
operating hours exceeded. exceeds value set in the Maintenance Unit Pump time in the Maintenance History Set-
History Settings. tings.
WARNING: ASI pump tube Actual ASI pump tubing operation time Replace the ASI pump tubing. Then, reset the
operating hours exceeded. exceeds value set in the Maintenance ASI Rinse Pump time in the Maintenance His-
History Settings. tory Settings.

270 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.1 Error Messages

Table 5.2• Error Message List 2

Error Message Description Corrective Action
Information entered is incorrect. The user name and password entered are not Enter the correct user name and
Re-enter user name and password. valid. password. These fields are
case-sensitive. If the user account
has not been set up, contact the
system administrator.
Database path not found. The specified file does not exist in the specified Check the file name and path.
path. Check if the specified file has been
deleted or moved, or if the system
used for the file has been deleted.
Opening of communication port The process of opening the communication port Verify that the instrument is
has timed out. Check instrument has timed out. switched on, and that the instru-
connection and transmission set- ment connection and communica-
tings. tion port settings are correct.
Closing of communication port has The process of closing the communication port Verify that the instrument is
timed out. Transmission will be has timed out. switched on, and that the instru-
ended. ment connection and communica-
tion port settings are correct.
Communication is automatically
closed in that condition.
Instrument initialization has timed The process of initializing the instrument has Check if there is a problem with
out. timed out. the instrument operation, or if there
is a problem with communication
between the PC and the instrument.
The selected communication port An attempt was made to open a communication Check if the selected port is being
is already open. Verify that it is not port that has already been opened. used with another connection.
used with another connection.
Cannot open communication port. The communication port failed to open. Verify that the instrument is
Check instrument status and trans- switched on, and that the instru-
mission settings. ment connection and communica-
tion port settings are correct.
Mode error: Check instrument con- The operation was not accepted due to the instru- Verify the instrument operation. If
dition. If necessary, restart instru- ment condition. necessary, restart the instrument.
ment.

TOC-VCPH/CPN 271
 5.7 Troubleshooting
5.7.1 Error Messages

Table 5.3• Error Message List 3

Error Message Description Corrective Action
ERROR: Syringe Zero Point Syringe zero point detection could Properly mount the syringe. Then select Zero
Detection. not be performed. Syringe is not Point Detection from the Maintenance menu.
properly installed.
WARNING: TC furnace temper- TC furnace temperature is too low to Wait for the furnace temperature to rise before
ature is too low to regenerate cat- perform the catalyst regeneration executing the catalyst regeneration procedure.
alyst. procedure.
ERROR: Vial rack not present. Operation cannot continue because Mount a vial rack, and then execute the operation
there is no vial rack in the turntable. again.
ERROR: Vial rack has been Measurement cannot be performed Verify the type of vial rack mounted in the
exchanged. because the vial rack specified in the ASI-V, and then set the vial rack type in the soft-
settings differs from the type actu- ware.
ally detected.
ERROR: Vial rack type not set. The measurement parameters cannot Set the vial rack type in the software.
be validated because the vial rack
type is not specified in the software.
ERROR: ASI Cover is open. The ASI-V cover is open. The Close the ASI-V cover.
ASI-V operation has stopped as a
safety measure.

The following messages indicate that an error has occurred that prevents measurement
from continuing. Take the appropriate corrective actions as indicated in the following table.
If the cause of the problem cannot be discovered, or if the same error message appears after
taking the indicated corrective actions, contact your Shimadzu representative.
Note: When the following errors are generated, power to the instrument oven is auto-
matically stopped. When power to the oven is switched on again, wait until the
temperature rises before starting measurement.

272 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.1 Error Messages

Table 5.4• Error Message List 4

Error Message Description Corrective Action
ERROR: ROM Write An error occurred while writing to Switch off power to the instrument. Contact your Shi-
Error memory. madzu representative.
ERROR: Electric Fur- The electric furnace overheated. With the power ON, wait approximately 20 minutes for
nace Overheating the oven temperature to decrease then switch OFF the
instrument. After switching on the power and running
the instrument again, see if the same error is generated.
ERROR: Electric Fur- The oven temperature does not rise. Switch off power to the instrument. After switching on
nace Sensor the power and running the instrument again, see if the
ERROR: Syringe Posi- The syringe is not operating normally. same error is generated.
tion Detection
ERROR: Syringe Opera- The syringe is not operating normally Switch off the instrument, and remove any foreign parti-
tion due to clogging of the tubing connected cles from the line. After switching on the power and
to the 8-port valve. running the instrument again, see if the same error is
generated.
ERROR: Syringe Zero The syringe is not operating normally. Switch off the instrument. After switching on the power
Point Detection and running the instrument again, see if the same error
is generated.
ERROR: 8-Port Valve The 8-port valve is not operating nor- Switch off the instrument, and remove the rotor from the
Position Detection mally due to clogging inside of the sam- 8-port valve. Remove any particles found in the 8-port
ple injector 8-port valve. valve and wash valve.
ERROR: TC Slider The TC slider is not operating normally Switch off the instrument, inspect the slider and remove
due to particles wedged between the any foreign particles from the slider mechanism. Then
moving parts. switch on the power again.
ERROR: IC Slider The IC slider is not operating normally
due to particles wedged between the
moving parts.
ERROR: ASI Arm Verti- The ASI-V arm is not operating nor- Switch off power to the TOC-V main instrument. After
cal Position Detection mally in the vertical direction. switching on the power and running the instrument
ERROR: ASI Arm Verti- The ASI-V arm is not operating nor- again, see if the same error is generated.
cal Movement mally in the vertical direction. Since the problem is unrelated to the TOC-V main unit,
ERROR: ASI Arm Hori- The ASI-V arm is not operating nor- disconnect the ASI-V from the main unit, and perform
zontal Position Detection mally in the horizontal direction. operations using the TOC-V main unit alone until nor-
mal operation of the ASI-V is restored.
ERROR: ASI Arm Hori- The ASI-V arm is not operating nor-
zontal Movement mally in the horizontal direction.
ERROR: ASI Turntable The ASI-V turntable position could not Switch off power to the TOC-V main unit. Make sure
Position Detection be detected. Either the rack is not prop- the rack is properly seated, and remove any objects that
erly seated in the turntable, or some may be blocking the position detection notch on the
object may be blocking a position detec- periphery of the rack. After eliminating the cause of the
tion notch on the periphery of the rack. problem, place the cover on the ASI-V, and switch on
the power to the instrument again.
ERROR: TN Reactor The TNM-1 reactor temperature does Switch off power to the TOC-V main unit. After switch-
Temperature not rise. ing on the power and running the instrument again, see
if the same error is generated.

TOC-VCPH/CPN 273
 5.7 Troubleshooting
5.7.2 Troubleshooting

Table 5.4• Error Message List 4

Error Message Description Corrective Action
8-Port Sampler 1 posi- 8-Port Sampler 1 operation error Switch off instrument. Remove 8-port valve rotor from
tion detection occurred due to foreign matter infiltra- 8-Port Sampler 1, remove debris, etc., and wash valve.
8-Port Sampler 1 opera- tion into 8-port valve, etc.
tion
8-Port Sampler 2 posi- 8-Port Sampler 2 operation error Switch off instrument. Remove 8-port valve rotor from
tion detection occurred due to foreign matter infiltra- 8-Port Sampler 2, remove debris, etc., and wash valve.
8-Port Sampler 2 tion into 8-port valve, etc.
operation

5.7.2 Troubleshooting

5.7.2.1 TOC-V

(1) An error message is displayed.

→Refer to error message.
(2) The Ready lamp will not light.
→ Access the Background Monitor screen by selecting Background Monitor from the
Instrument menu. Refer to the screen to see which parameters are not satisfied.
(3) The baseline stays over the auto zero range. Baseline position never reaches the ready
state.

Does carrier
gas flow normally NO
to the analysis
cell?
Carrier gas leak.

YES Repair the leak.

Is dehumidifier
within the specified NO
temperature?
The dehumidifier temperature
setting is bad.
YES Contact your Shimadzu
representative.
The infrared gas
analyzer is bad.
Contact your Shimadzu
representative.

274 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.2 Troubleshooting

(4) The baseline is unstable.

Is carrier gas
NO
flowing normally?

Carrier gas leak.

YES
Repair the leak.

Was
the catalyst NO
replaced?
Accumulated obstructing
substance.
YES
Replace the catalyst.

Is the
dehumidifier NO
operating
normally?
The dehumidifier is bad.
YES
Contact your Shimadzu
representative.

Are
external
conditions (vibration, NO
temperature, power
voltage)
normal? External conditions are
adverse.
YES
Eliminate the adverse
condition.
The infrared gas analyzer
is bad.
Contact your Shimadzu
representative.

TOC-VCPH/CPN 275
 5.7 Troubleshooting
5.7.2 Troubleshooting

(5) Poor reproducibility with standard solution.

Is the NO
standard solution
normal?
Bad standard solution.

YES Prepare new standard

solution.

Is the
sample injected NO
normally from injection
tube?
Poor injection condition.

YES Adjust injector.

Do
bubbles remain
in syringe? (especially YES
in dilution
analysis)
Poor injection volume
repeatability.

NO Eliminate bubbles.

Was plunger tip NO

replaced recently?

Backlash of plunger tip.

YES Replace plunger tip.

Does
carrier gas YES
sometimes leak from
the drain
bottle?
Low water level.

NO Replenish the water.

Does the
poor reproducibility IC
occur in the
TC or IC
circuit? IC reaction solution has
deteriorated.

TC Regenerate the IC reaction

solution.

Was the NO
TC catalyst
regenerated?
Insufficient regeneration of
theTC catalyst .
YES
Regenerate the TC catalyst.

TC catalyst deteriorated.

Replace the TC catalyst.

276 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.2 Troubleshooting

(6) No peaks appear after sample injection.

Is
sample
injected into TC
NO
combustion tube or IC
reaction vessel?
(confirm
visually) Poor injection.

YES Correct the injection

condition.

Is carrier gas
always flowing from YES
the drain
bottle?

Is the
level of the water NO
normal in the
drain bottle?
Low water level.

YES Replenish water.

Was membrane filter NO

replaced?
Clogged membrane filter.

YES Replace the membrane filter.

Bad infrared gas analyzer. Large resistance downstream

of dehumidifier.
Contact your Shimadzu
representative. Contact your Shimadzu
representative.

TOC-VCPH/CPN 277
 5.7 Troubleshooting
5.7.2 Troubleshooting

5.7.2.2 ASI-V

(1) The ASI-V does not operate.

Is
connection
cable and power cable NO
properly connected?
Improperly connected cable.

YES Properly connect the cables.

Bad electrical system.

Contact your Shimadzu

representative.

(2) Rinse water is not delivered from the rinse port.

Is there
sufficient NO
rinse water in rinse
water bottle?
Insufficient rinse water.

YES Replenish the rinse water.

Is the
rinse tubing NO
properly inserted into
the rinse water
bottle? The rinse tubing is not properly
inserted into rinse water bottle.
YES
Properly insert the tubing into
the rinse water bottle.
The rinse pump is bad.

Contact your Shimadzu

representative.

278 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.2 Troubleshooting

(3) Reproducibility is poor.

Is there
any material YES
adhering to the
sample
needle?
Poor reproducibility due to
foreign matter.
NO Remove the obstruction from
the opening at the tip of the
sample needle.
Is there
a leak at the
connection of sample YES
needle and ASI
sample
tubing? Air is drawn in at the
connection.
NO
Properly reconnect the tubing.
Poor reproducibility due to
a problem with the TOC-V.
Refer to Troubleshooting #1.
TOC-V item (5)

5.7.2.3 8-Port Sampler OCT-1

(1) 8-Port Sampler does not operate.

Are the signal and NO

power cables properly
connected?
Cables are not properly
connected.

YES Connect the cables properly.

Electrical system is defective.

Contact your Shimadzu
representative.

TOC-VCPH/CPN 279
 5.7 Troubleshooting
5.7.2 Troubleshooting

(2) Reproducibility is poor.

Is any foreign material YES

adhering to the sample
tubing?
Reduced reproducibility due to
foreign material.
Eliminate blockage at the tip of the
NO sample tubing.

Is the leakage
present at the 8-port valve YES
and sample tubing
connection?
Connection is leaking.

NO Connect the tubing properly.

Poor reproducibility is due to the

TOC-V unit.
Refer to the TOC-V User Manual.

5.7.2.4 Corrective Actions for Poor Reproducibility

Corrective Action for Poor Sample Injection

The manner in which sample is discharged from the TC or IC sample injection tubing has a
large influence on reproducibility. The sample should be injected as vertically as possible
onto the TC catalyst or into the IC reaction vessel. If the sample is scattered or injected
obliquely, detach the sample injection tubing from the slider, and remove any obstruction
that may be adhering to the opening at the tip of the sample tubing.
Unacceptable Unacceptable
Appropriate (oblique spray) (scattered spray)

Figure 5.38 Sample Injection Patterns from Sample Tubing

Ensure that the tip of the tubing does not protrude beyond the bottom surface of the slider.
The O-ring or other seal parts will be scratched if the tubing protrudes, resulting in gas
leaks. The sample is not properly injected unless the tip of the tubing extends into the
depression in the bottom of the slider.
Check the state of the injection for TC analysis by looking through the TC combustion tube
while it is attached to the instrument. The sample injection tubing can be detached from the
slider, and water can be injected for inspection using the functions available in the
Instrument>Maintenance>Mechanical Check screen.

280 TOC-VCPH/CPN
 5.7 Troubleshooting
5.7.2 Troubleshooting

Salt or other substances adhering to the tip of the tubing after rinsing can allow large
droplets of sample to remain on the tip of the tubing after injection. A deformed tip on the
sample injection tubing (a beard-like protrusion, for example) may cause the sample to be
injected obliquely. In either case, reproducibility is adversely affected and the sample
injection tubing should be replaced. Another option available only if there is sufficient
length of tubing remaining is to use a sharp cutting tool at a 90° angle to cut off 2 - 3mm
from the tip of the currently used sample injection tubing.
Tube

Bushing

Packing (spacer,
washer, gasket)

Approximately
2 - 2.5mm

Figure 5.39 Slider Assembly

Corrective Action to Eliminate Bubbles Inside the Syringe

Small bubbles that adhere to the inside of the syringe by the plunger tip will have little
effect on analysis values. Larger bubbles inside the syringe will affect values and result in
poor reproducibility. Large bubbles form easily inside a dirty syringe. This is evident when
sample is mixed with dilution water in the syringe and when sparging with carrier gas
inside the syringe for IC removal pretreatment for NPOC analysis. In this case, detach the
syringe from the syringe pump. Repeatedly draw in and discharge laboratory glassware
detergent to wash the inside of the syringe. Then draw in a full-stroke volume of the
cleaning agent and let it sit for about 20 minutes, or overnight if the syringe is extremely
dirty. Thoroughly rinse away all of the detergent and reattach the syringe to the syringe
pump.

Decreased Reproducibility Due to Plunger Tip Backlash

The plunger tip is a consumable item and, as it is used, wears in the following ways:
(1) The surface of the plunger tip becomes worn and the seal between the plunger tip and
the inside of the glass syringe barrel deteriorates, allowing slight amounts of water to
leak out with vertical movements of the plunger.
(2) The contact site of the plunger tip and plunger becomes loose, causing a slight
backlash with vertical movement of the plunger.
As the above conditions start to occur, repeatability of sample injection volume decreases,
resulting in diminished analysis reproducibility. Item (2) above rapidly leads to decreased
reproducibility. Since it is very difficult to determine backlash by inspecting movement of
the plunger tip, inspect as follows.
Before sample injection, observe the wash injection used to replace the previous sample in
the syringe and flow line with the new sample. After injection, if a droplet forms at the tip
of the injection tubing and increases in size, there is a strong possibility that backlash has
increased. The corrective action in this case is to replace the plunger tip.
Note: The effect of backlash increases with smaller sample injection volumes. Poor
results might be obtained with a sample injection volume of 10µL, while the
effect might be negligible with a 100µL sample injection volume.

TOC-VCPH/CPN 281
 5.7 Troubleshooting
5.7.2 Troubleshooting

282 TOC-VCPH/CPN
 6
6 Reference Information
This chapter describes the principles of analysis and lists instrument specifications,
accessories, and parts. This chapter also includes installation procedures, for use in the
event that the instrument is relocated.

6.1 Principles of Analysis

The principles for TC, IC, POC, NPOC, TOC and TN analysis are described in
this section.
6.2 Analysis-Related Technical Information
This section summarizes technical information related to analysis, including
peak area analysis and calibration curve selection.
6.3 Specifications
This section lists specifications for the TOC-VCPH/CPN main unit, autosampler,
TN unit and the various optional kits.
6.4 Standard Accessories
The standard accessories are listed in this section.
6.5 Special Accessories
The optional accessories are listed in this section.
6.6 Consumable Parts List
The consumable parts are listed in this section.
6.7 Maintenance Parts List
The maintenance parts are listed in this section.
6.8 Installation
The installation site requirements and installation procedures for future
relocation of the instrument are described here.
6.9 Material Safety Data Sheets
Material Safety Data Sheets are provided in this section.
 6.1 Principles of Analysis
6.1.1 Principles of TC (Total Carbon) Analysis

6.1 Principles of Analysis

Two types of carbon are present in water: organic carbon and inorganic carbon. Organic
carbon (TOC) bonds with hydrogen or oxygen to form organic compounds. Inorganic
carbon (IC or TIC) is the structural basis for inorganic compounds such as gas carbonates
and carbonate ions. Collectively the two forms of carbon are referred to as total carbon
(TC) and the relationship between them is expressed TOC=TC-IC.
Nitrogen is also present in water in two types: organic and inorganic. The sum of these is
referred to as total nitrogen (TN).
The principles underlying TC and TN analysis are explained in the following sections.

6.1.1 Principles of TC (Total Carbon) Analysis

Sample is introduced into the TC combustion tube, which is filled with an oxidation
catalyst and heated to 680°C. The sample is burned in the combustion tube and, as a result,
the TC components in the sample are converted to carbon dioxide. Carrier gas, which flows
at a rate of 150mL/min to the combustion tube, carries the sample combustion products
from the combustion tube to an electronic dehumidifier, where the gas is cooled and
dehydrated. The gas then carries the sample combustion products through a halogen
scrubber to remove chlorine and other halogens. Finally, the carrier gas delivers the sample
combustion products to the cell of a non-dispersive infrared (NDIR) gas analyzer, where
the carbon dioxide is detected. The NDIR outputs an analog detection signal that forms a
peak; the peak area is measured by the TOC-Control V software.
The peak area is proportional to the TC concentration of the sample. A calibration curve
equation that mathematically expresses the relationship between peak area and TC
concentration can be generated by analyzing various concentrations of a TC standard
solution. The TC concentration in a sample can be determined by analyzing the sample to
obtain the peak area and then using the peak area in the calibration curve equation.

284 TOC-VCPH/CPN
 6.1 Principles of Analysis
6.1.2 Principles of IC (Inorganic Carbon) Analysis

6.1.2 Principles of IC (Inorganic Carbon) Analysis

Two methods for measuring IC using the TOC-V are available: analysis within the injection
syringe and analysis using the optional IC reactor. In both methods, the measured IC
consists of carbon derived from carbonates, hydrogen carbonates and dissolved carbon
dioxide.

Defining IC
The IC measured by TOC analysis consists of the carbon contained in carbonates and in
carbon dioxide dissolved in water. By acidifying the sample with a small amount of
hydrochloric acid to obtain a pH less than 3, all carbonates are converted to carbon dioxide
(CO2) by the following reactions:
Me2CO3 + 2HCl --> CO2 + 2MeCl + H2O

MeHCO3 + HCl --> CO2 + MeCl + H2O

Carbon dioxide and dissolved carbon dioxide in the sample are volatilized by bubbling
(sparging) air or nitrogen gas that does not contain carbon dioxide through the sample.

Analysis Using the IC Reaction Vessel (H Type Instrument)

The TOC-V IC reactor kit is used to sparge the IC reaction solution (acidified reaction
liquid) with carrier gas. Sample is injected into the IC reaction vessel and the IC in the
sample is converted to carbon dioxide, which is volatilized by the sparging process and
detected by the NDIR.

Analysis Within the Syringe (N Type Instrument)

The sample is acidified to pH 3 or lower in the syringe, using hydrochloric acid. The
sample is sparged with carrier gas and the IC in the sample is converted to carbon dioxide
and detected by the NDIR.

TOC-VCPH/CPN 285
 6.1 Principles of Analysis
6.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis

6.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis

After acidifying the sample to pH 2 to 3, sparge gas is bubbled through the sample to
eliminate the IC component. The remaining TC is measured to determine total organic
carbon, and the result is generally referred to as TOC. However, in the TOC-V, this analysis
value is referred to NPOC to distinguish it from the TOC value obtained by calculating the
difference between TC and IC. NPOC stands for non-purgeable organic carbon and refers
to organic carbon that is present in a sample in a non-volatile form.
NPOC and TOC (obtained by IC elimination) described in the TOC-related standard
methods and referred to in water quality-related test methods (JIS, ASTM, EPA, EN) are
identical. Purgeable organic substances in the sample can be lost during the sparging
process. Consequently, when the sample contains purgeable organic substances, TOC
should not be measured by the NPOC method. If the dissolved purgeable organic
component in the water sample is large, the amount volatilized during sparging is relatively
small. Generally, the amount of purgeable organic substances in natural environmental,
public and purified water is small; as a result, NPOC can be referred to as TOC.

Table 6.1 • Residual Rate of Volatile Organic Substances using Sparging (Nitrogen Gas)
Organic Substance Pre-Sparging Conc. Post-Sparging Conc. Residual Rate (%)
(ppm) (ppm)
Methanol 117. 5 116 98.6
Ethanol 106.5 105 98.5
Isopropyl alcohol 129 127 98.5
n-butyl alcohol 117 115 98.3
Acetone 106 101 95.3
Acetaldehyde 130 117 90.0
Ethyl acetate 102 88 86.3
Tyrosine 117 116.5 99.5
Benzene 85 2.5 2.9
Cyclohexane 79 2 2.5

286 TOC-VCPH/CPN
 6.1 Principles of Analysis
6.1.4 Principles of POC (Purgeable Organic Carbon) Analysis

6.1.4 Principles of POC (Purgeable Organic Carbon) Analysis

POC analysis is used to measure the volatilized component of TOC, which is produced
during the NPOC sample sparging process. As a result, NPOC+POC is equivalent to TOC.
POC analysis is performed as follows.
Sparge gas containing the volatilized CO2 and POC components of the sample is carried to
the lithium hydroxide-filled CO2 absorber to eliminate the CO2 that was converted from the
IC in the sample. The gas, which now contains only the POC component of the sample,
then passes through the combustion tube to be oxidized. The POC component is converted
to CO2 during oxidation and the CO2 is detected by the NDIR. Data processing is
conducted in the same manner as for TC.
POC is not precisely defined. Factors that determine whether or not, or to what degree, a
volatile organic carbon component is volatilized during sparging include the type of
organic compound, the gas/liquid contact with the sparge gas, and the ambient temperature
during sparging. The target of POC analysis is the organic component present in the
aqueous phase. As a result, organic compounds that are highly soluble in water (such as
methanol or ethanol) and not easily volatilized by sparging produce almost no peaks in
POC analysis.
Organic compounds with low solubility in water (such as methylene chloride or
chloroform) produce sharp peaks in POC analysis. Over a long period of time, compounds
such as acetone and methyl isobutyl ketone generate extremely broad, tailing peaks with no
specific end time.
The lithium hydroxide-filled CO2 absorber eliminates the carbon dioxide that was
generated along with the POC substances. Therefore, POC components that are easily
caught in the CO2 absorber (such as esters) produce low values in POC analysis. POC
results obtained using this technique are not absolute. The user should take all the above
factors into consideration when measuring POC using this instrument.

TOC-VCPH/CPN 287
 6.1 Principles of Analysis
6.1.5 Principles of Measuring TOC

6.1.5 Principles of Measuring TOC

TOC can be measured using the following 3 methods:
• TC-IC Method
• NPOC Method
• POC+NPOC Method

TC-IC Method
In the TC-IC method, TOC is measured as the difference between the TC and IC analysis
values. The TC-IC method is not recommended for samples that contain more IC than TOC
(samples where TC consists almost entirely of IC); the NPOC method is recommended for
such samples. The TOC value determined using the TC-IC method includes errors
associated with each of the individual TC and IC measurements, and can therefore result in
a large error in the TOC value.
Because detection accuracy decreases with increasing IC concentration, the NPOC method
is also recommended for samples containing IC concentrations exceeding 10ppm for TOC/
TN catalyst and 5ppm for high sensitivity catalyst.

NPOC Method
The NPOC method is the most widely used TOC analysis method. The NPOC method is
not recommended for samples that foam during sparging. Samples that become foamy
during sparging tend to form bubbles that flow out of the syringe, which removes the
concentrated TOC sample components and leaves a small amount of TOC in the syringe.
The TC-IC method is recommend in this situation.

POC+NPOC Method
The POC+NPOC method should be used when the amount of POC present in the sample
cannot be disregarded.

6.1.6 Principles of Measuring TN (Total Nitrogen)

When a sample is introduced into the combustion tube (furnace temperature 720°C), the
TN in the sample decomposes to nitrogen monoxide. Nitrogen gas does not become
nitrogen monoxide under these circumstances. The carrier gas, which contains the nitrogen
monoxide, is cooled and dehumidified by the electronic dehumidifier. The gas then enters a
chemiluminescence gas analyzer, where the nitrogen monoxide is detected. The detection
signal from the chemiluminescence gas analyzer generates a peak and the TN concentration
in the sample can then be measured.
Note: TN Detection Rate
In TN analysis, the state (crystalline state) in which TN exists in the sample
greatly affects the TN detection rate. Nitrogen contained in nitrates, nitrites,
ammonia and the majority of other organic nitrogen compounds exhibit high
detection rates. Conversely, some organic nitrogen-containing compounds (such
as hydrazines, pyrazolones, and azide compounds) have detection rates ranging
from 10% to 60%, depending on the concentration.

288 TOC-VCPH/CPN
 6.2 Analysis-Related Technical Information
6.2.1 Peak Area Analysis

6.2 Analysis-Related Technical Information

6.2.1 Peak Area Analysis

When a sample is analyzed, the TOC-Control V software automatically detects the
beginning and end of each peak produced, and calculates the peak areas. Detection of the
beginning and end of each peak is based on the slope of the tangent, which changes from
moment to moment. Peak detection begins when that slope exceeds a predetermined value
and ends when a negative slope falls below a specified value.
Note: • Separated Peaks: In TC analysis, multiple peaks may occur when a large
quantity of sample is injected. Only the end of the last peak is detected. The
total area of the multiple peaks is calculated.
• Baseline Correction: Baseline correction is performed for peaks produced
with fluctuating baseline to obtain the correct peak area.

Figure 6.1 Determining Peak Area

6.2.2 Peak Shape

Multiple peaks are especially prominent when using the high sensitivity catalyst with
sample injections greater than 100µL. As sample is injected onto the catalyst, the easily
volatilized organic substances and the crystalline organic substances are combusted at
different rates. As a result, carbon dioxide is generated multiple times, resulting in the
formation of multiple peaks. Easily volatilized organic substances are organic compounds
that are volatilized with water when an aqueous solution of the compounds is heated;
ethanol is one example of such a compound. Crystalline organic compounds remain in a
solid form following the heating of an aqueous solution of the compound; glucose is one
example of such a compound.
The manner in which the sample is injected also has an effect on peak shape. If a portion of
the sample is injected into the center of the combustion tube while another portion is
injected at the periphery, combustion may occur at different times, resulting in multiple
peaks.
Peak shape does not affect the analysis results. Even if multiple peaks occur due to the type
of organic substance or injection manner described above, the TOC-Control V calculates
the total area of the peaks generated to determine the TOC (or TC) accordingly.

TOC-VCPH/CPN 289
 6.2 Analysis-Related Technical Information
6.2.3 Calibration Curves

6.2.3 Calibration Curves

6.2.3.1 Types of Calibration Curves

1-Point and 2-Point Calibration Curves

The output signals of the TOC-V are linearized. As a result, there are almost no factors in
the reaction systems of the TC/TN combustion and IC reaction components that might
cause the concentration-output characteristic to deviate from linearity. Consequently,
calibration curves are commonly generated as 1-point curves consisting of 1 span point, or
2-point curves consisting of 1 span point and the zero point.
The concentration of TC and IC, or of TN, varies with standard solutions prepared with
pure water. A calibration curve generated using concentrations greater than 50 - 100mg/L
will pass very close to the zero point. In this case, it is practical to generate a 1-point
calibration curve.
Use a 2-point calibration curve when the concentration of TC and IC or TN in the pure
water used to prepare the standard solutions cannot be disregarded with respect to the
standard solution concentration. For information on handling of this type of curve, refer to
Section 6.2.3.2 "Shifting of Calibration Curves".

Multi-Point Calibration Curves

Calibration curves can be generated using up to 10 points. Calibration curves consisting of
3 or more points can be generated as a point-to-point curve or as a regression line using the
least squares method. With the least squares regression curve, a correlation coefficient is
displayed.

6.2.3.2 Shifting of Calibration Curves

Shift to Origin
The “shift to origin” function is used when the amount of TC and IC or TN in the pure
water used for standard solution preparation cannot be ignored with respect to the standard
solution concentration. A correction must be made by shifting the calibration curve in a
parallel fashion so that it passes through the origin. This corrects for the TC and IC or TN
concentration in the water used for standard solution preparation. An example of a situation
in which the “shift to origin” function is useful is described below.
When water containing 0.5mg/L TC is used to prepare a 10mg/L TC standard solution, the
actual TC concentration in the standard solution will be 10.5mg/L (0.5mg/L from the water
+ 10mg/L from the standard solution). The 2-point calibration curve generated using such a
solution is shown by the solid line in Figure 6.2 "Shifting of Calibration Curve". If this
curve is used without correction, the sample analysis values will always be 0.5mg/L less
than the true value. By shifting the calibration curve so that it passes through the origin, as
shown by the broken line in Figure 6.2 "Shifting of Calibration Curve", the calibration
curve is effectively corrected.

290 TOC-VCPH/CPN
 6.2 Analysis-Related Technical Information
6.2.3 Calibration Curves

A system blank is water that contains absolutely no carbon (zero water). When
measurement of a system blank produces a peak, the TC concentrations measured in
samples will be biased high by the amount of TC in the system blank. In most cases (with
the exception of high sensitivity analysis), this bias is not significant. Measurement error
resulting from the TC or TN content in the water used to prepare standard solutions is
typically much greater than measurement error resulting from the system blank value.
Correcting the calibration curve based on the TC or TN content in the standard solution
preparation water will produce satisfactory analyses. Using this correction method, the
value obtained for a system blank would be greater than zero by the amount of the blank
value.
The instrument allows shifting of calibration curves only to the extent of the system blank
value. The system blank peak height varies with such factors as the system configuration
and the type of catalyst used.

Shift to Blank Point

The “shift to blank point” procedure is performed for high sensitivity analyses when the
system blank value could have a significant effect on the measurement value.
By selecting the “shift to blank point” option, a TC blank check analysis is performed using
the same injection volume that will be used for sample measurement. The calibration curve
zero point is shifted to the TC blank check value.
Peak Area Value

0 TC Concentration (mg/L) 10
(0.5) (10+0.5)

Figure 6.2 Shifting of Calibration Curve

TOC-VCPH/CPN 291
 6.2 Analysis-Related Technical Information
6.2.4 Sparging During Standard Solution Analysis

6.2.4 Sparging During Standard Solution Analysis

Standard solutions that have TC concentrations so low as to be affected by the amount of
dissolved carbon dioxide in the solution should be sparged with carrier gas prior to
measurement. Sparging eliminates the dissolved carbon dioxide, thereby preventing it from
affecting the concentration of the standard solution.
The amount of dissolved carbon dioxide in water used for standard solution preparation is
affected by factors such as water purification method, length and condition of storage, and
the concentration of carbon dioxide in the atmosphere. Concentrations of dissolved carbon
dioxide increase when the water is exposed to the atmosphere during the standard solution
preparation process. Refer to “Table 6.2 • CO2 Content (ppm) in Distilled Water
Equilibrated with Atmosphere Temperature (°C)” for the dissolution rates of atmospheric
carbon dioxide in water.
It is important to consider both the concentration of the standard solution and the
concentration of TOC contained in the preparation water when deciding whether to use the
sparging function. Use of sparging is appropriate if the TOC contained in the water is low
enough to not substantially affect the standard solution concentration, but not low enough
to be ignored.
Note: Do not use sparging with IC standard solutions, as sparging decreases the IC con-
centration.

Table 6.2 • CO2 Content (ppm) in Distilled Water Equilibrated with Atmosphere
Temperature (°C)
Atmospheric CO2 0 5 10 15 20 25 30
(vol%)
0.030 1.00 0.83 0.79 0.59 0.51 0.44 0.38
0.033 1.10 0.91 0.76 0.65 0.56 0.48 0.42
0.044 1.47 1.22 1.02 0.87 0.74 0.64 0.56

The above CO2 content can be converted to IC using the following equation.
IC (ppm) = CO2 (mg/L) x 0.27

6.2.5 Automatic Selection of Optimum Calibration Curve

Up to three different calibration curves can be selected for use in a method. The curves are
specified in the “Calibration Curve 1”, “Calibration Curve 2” and “Calibration Curve 3”
fields on page 3 of the Method Wizard when the method is being created. Refer to Section
4.4.2.3 "Method Wizard" for more information. When more than one calibration curve is
specified, the TOC-Control V software automatically selects the optimum calibration curve
to be used for calculating measurement results.

292 TOC-VCPH/CPN
 6.2 Analysis-Related Technical Information
6.2.5 Automatic Selection of Optimum Calibration Curve

The automatic selection process occurs on a measurement-by-measurement basis.

Measurement values are always calculated first using Calibration Curve 1. The TOC-
Control V software then evaluates the result, applies the optimum calibration curve, and
recalculates the value if necessary. The calibration curve with a concentration range that is
greater than and closest to the measured value is used. Examples are shown below:
(1) If the measured value is less than the concentration of Calibration Curve 1 and greater
than the concentration of Calibration Curve 2 and Calibration Curve 3, Calibration
Curve 1 is used.
Conc. of Calibration Curve 1 > Measured Value > Conc. of Calibration Curves 2 and 3 →
Calibration Curve 1 is used

(2) If the measured value is less than the concentrations of Calibration Curve 1 and
Calibration Curve 2, and if the concentration of Calibration Curve 2 is less than that of
Calibration Curve 1, Calibration Curve 2 is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Measured Value →
Calibration Curve 2 is used

(3) If three calibration curves are specified, the calibration curve that is greater than and
closest to the measured value is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 3 > Measured Value > Conc. of Calibration
Curve 2 →
Calibration Curve 3 is used

(4) If the measured value is greater than the concentration of all curves and the
concentration of Calibration Curve 1 is greater than the concentration of Calibration
Curves 2 and 3, Calibration Curve 1 is used.
Measured Value > Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Conc. of Calibration
Curve 3 →
Calibration Curve 1 is used

Note: By setting the concentration ratio between calibration curves to a factor of

approximately 10, the automatic selection function can be effectively utilized for
analyses covering a wide range of concentrations. For example, use a concentra-
tion of 10ppm for Calibration Curve 1, 100ppm for Calibration Curve 2, and
1000ppm for Calibration Curve 3.

Considerations for the Automatic Selection Function

• The automatic selection process rules do not change when multi-point calibration
curves are included.
• When more than one injection is performed, the calibration curve is selected based
on the measured value of the first injection.
• Because the measured value is always calculated first using Calibration Curve 1,
specify the most commonly used calibration curve in this field.
• The priority of the second and third calibration curves is determined based on the
calibration curve concentrations and the sample concentration.

TOC-VCPH/CPN 293
 6.3 Specifications
6.3.1 TOC-VCPH/CPN

6.3 Specifications

6.3.1 TOC-VCPH/CPN

Analyte TC, IC, TOC (TC-IC), NPOC

Measurement principle 680°C catalytically-aided combustion oxidation/non-dispersive
infrared detection (NDIR)
Measuring range TC: 0 - 25000mg/L
IC:
• TOC-VCPH: 0 - 30000mg/L
• TOC-VCPN: 0 - 3000mg/L
Detection limits TC:
• TOC-VCPH: 4µg/L
• TOC-VCPN: TC: 50µg/L
IC: 4µg/L
Measurement time TC: Approx. 3min
IC:
• TOC-VCPH: Approx. 3min
• TOC-VCPN: Approx. 4min
Repeatability CV within 1.5%
Sample introduction Auto injection using syringe pump/slider
Sample injection volume 10 - 2000µL (variable)
Sample dilution function Dilution within syringe, dilution factor 2 - 50 times
Pretreatment for IC Automatic acid addition and sparging
Carrier gas High purity air (from cylinder)
Carrier gas pressure Approx. 300 - 600kPa
Carrier gas flow rate TOC-VCPH: 150mL/min (230mL/min when performing in-syringe
sparging)
TOC-VCPN: 230mL/min
Ambient temperature 5 - 35°C
Power requirements AC 100-120V ±10% or AC 220-240V ±10%, 6 A, 50/60Hz (power
consumption: approx. 230VA)
Fuse 8A.T (100V Systems) 15A.T (200V Systems)
Approximate dimensions (W) 440 x (D) 560 x (H) 460mm (excluding projections)
Weight Approx. 40kg

294 TOC-VCPH/CPN
 6.3 Specifications
6.3.2 ASI-V

6.3.2 ASI-V

Sample containers 24mL vial rack: 24mL (External diameter 23 x Height 85mm), 100
vials, 100 septum-equipped caps
40mL vial rack: 40mL (External diameter 27 x Height 9mm), 72
vials, 72 septum-equipped caps
Vial rack capacity 24mL vial rack: 93nvials
40mL vial rack: 68 vials
Sample pretreatment • Acid addition and sparging possible for NPOC analysis
• Needle rinse possible
• Stirring with magnetic stirrer (with optional magnetic stirrer)
Ambient temperature 5 - 35°C
Approximate dimensions (W) 370 x (D) 540 x (H) 490mm (excluding projections)
Weight Approx. 13kg

6.3.3 OCT-1 8-Port Sampler

No. of sample containers 8 containers

accommodated 16 containers (using 2 OCT-1 units)
Ambient temperature 5 - 35° C
External dimensions Approx. (W) 245 x (D) 245 x (H) 440mm (excluding protruding
parts)
Weight Approx. 3.5 kg

6.3.4 TNM-1

Analyte TN (total nitrogen)

Measurement principle Thermal decomposition / NO detection (chemiluminescence
method)
Measuring range 0 - 4000mg/L
Measurement time Approx. 4min
Repeatability CV within 3%
Ambient temperature 5 - 35°C
Power requirements AC 100-120V ±10% or AC 220-240V ±10%, 6 A, 50/60Hz (power
consumption: approx. 230VA)
Approximate dimensions (W) 160 x (D) 235 x (H) 400mm (excluding projections)
Weight Approx. 8kg

TOC-VCPH/CPN 295
 6.3 Specifications
6.3.5 POC Kit

6.3.5 POC Kit

Analyte POC
Measurement method Sparging / CO2 removal / combustion oxidation
CO2 removal method Absorption via lithium hydroxide, removal
Measuring range 0 - 500mg/L
Measurement time Approx. 4min
Repeatability CV within 5%

6.3.6 Carrier Gas Purifier Kit

Gas purification method Combustion oxidation / CO2 removal

Carrier gas supply Pressurized air or oxygen (free of dust, oil mist, water droplets, etc.)
Carrier gas supply pressure 300 - 600kPa

6.3.7 Manual Injection Kit (Gas Sample Injection Kit)

Analyte Liquid samples: TC, IC, TOC (TC-IC)

Gas samples: TC, carbon dioxide, TOC (determined by TC-carbon dioxide;
Carbon monoxide and other inorganic carbon containing gases aside from
carbon dioxide are also measured as TOC)
Measurement of IC, TOC and carbon dioxide is possible with the TOC-VCPH
Measurement principle 680°C catalytically-aided combustion oxidation/non-dispersive infrared
detection (NDIR)
Measuring range Liquid sample:
• TC: 0 - 20000mg/L
• IC: 0 - 20000mg/L
Gas sample:
6ppm - 100% CO2
Sample injection volume Liquid sample: 1 - 150µL
Gas sample: 20µL - 10mL
Measuring time Liquid sample:
• TC: Approx. 3min
• IC: Approx. 3min
Gas sample: 2 - 4min
Repeatability Liquid sample: CV within 2% (CV is within 3% when sample concentration
is 8000mg/L or greater)
Gas sample: CV within 2%
Sample introduction Manual injection using microsyringe

296 TOC-VCPH/CPN
 6.3 Specifications
6.3.8 PC Hardware Requirements

6.3.8 PC Hardware Requirements

PC IBM-PC/AT or compatible, with 9-pin RS-232C connector

CPU 233MHz or better
Memory 32 MB or greater
Hard drive 2 GB or greater
OS Windows95, Windows98, Windows2000, WindowsNT 4.0 (SP3 or
later), WindowsXP (*For compliance with FDA 21 CFR Part 11, use
Windows2000)
The User Authentication function cannot be used with WindowsXP.
Monitor resolution 800 x 600 or better, 1024 x 768 suggested

TOC-VCPH/CPN 297
 6.4 Standard Accessories
6.3.8 PC Hardware Requirements

6.4 Standard Accessories

Table 6.3 • Standard Accessories List 1 (TOC-VCPH/CPN)

Part Number Part Name TOC-VCPH TOC-VCPN
638-41323 Combustion tube, in case 2 1
638-92069-02 TOC regular catalyst set 1 1
638-92070-01 TOC high sensitivity catalyst set 1 -
638-16023 Catalyst filling rod 1 1
630-00999 CO2 absorber 1 1
630-00315-09 Plastic tube 9mm ID x 12mm OD 2m 2m
071-60813 Adapter, ground 1 1
071-60814-01 Power cord set (100-127V) 1 1
071-60814-06 Power cord set (220-240V) 1 1
638-59213-01 Plunger tip 1 1
630-00635-01 Potassium biphthalate, 2g 1 1
630-00962-01 Sodium carbonate, 25g 1 1
638-59213 Syringe 1 1
017-30812-01 Silicone grease 1 1
072-60359-01 Wiring band 2 2
630-00963-01 Sodium bicarbonate, 25g 1 1
072-02004-25 Fuse, 218 008 (100-127V) 2 2
072-02004-27 Fuse, 218 015 (220-240V) 2 2
631-20265 Plug, 35154 1 1
631-78002 Wrench, for 8-port valve 1 1
638-52337 Rinse water bottle 1 1
638-20072 Cap 1 -
638-60074 Ceramic fibers 1 1
638-64727 CD-ROM “TOC-Control V” 1 1
638-74029 Cable, (RS-232C) 1 1
631-81214 Plate, for CO2 absorber 1 1
035-55026-02 Half union 1 1
038-00292-04 Plastic bottle 2 1
638-94241 Instruction manual 1 1

298 TOC-VCPH/CPN
 6.4 Standard Accessories
6.3.8 PC Hardware Requirements

Table 6.4 • Standard Accessories List 2 (ASI Unit)

Part Number Part Name 24mL 40mL
638-41462 Vials, 24mL 100
038-00165-21 Vials, 40mL (with cap, septum) 72
638-20074-01 Cap, 24mL 100
038-00165-48 Septum, 24mL 100
638-52337 Rinse water bottle 1 1
072-60310-03 Wiring band, TM-53M 2 2
631-51869-20 Name plate, SAMPLE 1 1
631-51869-21 Name plate, GAS 1 1
072-60301 Wiring band, Nylon TY-23M 1 1
638-74027 Cable ASSY, ASI, signal 1 1
638-41448-01 Needle, regular type 24, 40 1 1

TOC-VCPH/CPN 299
 6.4 Standard Accessories
6.3.8 PC Hardware Requirements

Table 6.5 • Standard Accessories List 3 (OCT-1 8-Port Sampler)

Part Number Part Name 8-Port 8-Port Details
Sampler 1 Sampler 2
631-20265 Plug 35154 1 1 Rotor (for replacement
maintenance)
638-41443-03 Common Tubing C 1 Common port connection
tubing**
638-41443-04 Additional Common 1 Common port connection
Tubing C2 tubing****
638-41443-05 Common Tubing W 1 Common port connection
tubing**
638-41443-06 Additional Common 1 Common port connection
Tubing W2 tubing****
638-41337-03 Flanged Tubing C* 1 1 Sample tubing for combustion
analyzers (CSH/CSN/CPH/
CPN)
631-41660 Flanged Tubing W*** 1 1 Sample tubing for wet
chemical analyzers (WS/WP)
638-74004-01 Power Cable 1 Cable for connection to the
main unit
638-74028-01 Power Cable 1 Cable for connection to the
main unit
638-74028-02 Power/Signal Cable 1 Cable for connecting 8-Port
Sampler 1 to 8-Port Sampler 2
M393-E228 User Manual 1

* Flanged tubing in C sets have an inner diameter of 1.0 mm. This set is provided for use
with the combustion type TOC-V.
** Connect this tubing to the common (COM) port of the 8-Port Sampler and port No. 2 on
the TOC-V unit.
*** Flanged tubing in W sets have an inner diameter of 1.5 mm. This set is provided for use
with the wet chemical type TOC-V.
**** Connect this tubing to the common (COM) port of the 8-Port Sampler and port 1on the
TOC-V unit.

300 TOC-VCPH/CPN
 6.4 Standard Accessories
6.3.8 PC Hardware Requirements

Table 6.6 • Standard Accessories List 4 (TN Unit)

Part Number Part Name Qty
630-00999 CO2 absorber 1
638-60074 Ceramic fibers 1
017-40533-01 Potassium nitrate 1
072-02004-19 Fuse, 218 002 1
020-46547 SS screw pan head M 4 x 8 5
631-81157 Mounting plate TNM 1
072-60301 Wiring band, TY-23M 5
630-00315-05 Plastic tubing 5mm ID x 7mm OD 5m
631-41200-02 Viton tubing 5mm ID x 8mm OD 0.45
638-52353-03 Ozone treatment unit ASSY 1
035-60690-97 Tee 2
016-43284-01 Tube 0.1m
072-60338-03 Clip 2
638-42035 Capillary 1
071-60813 Adapter 1
071-60814-01 Power cord set (100-127V) 1
071-60814-06 Power cord set (220-240V) 1

Table 6.7 • Standard Accessories List 5 (Manual [Gas Sample] Injection Kit)
Part Number Part Name Qty
638-10194 Block, M-INJ TC ASSY 1
638-10195 Block, M-INJ IC ASSY 1
631-43291 Syringe packing 10

Table 6.8 • Standard Accessories List 6 (POC Measurement Kit)

Part Number Part Name Qty
630-00557 Quartz wool 1

TOC-VCPH/CPN 301
 6.4 Standard Accessories
6.3.8 PC Hardware Requirements

Table 6.9 • Standard Accessories List 7 (Carrier Gas Purifier Kit)

Part No. Part Name Qty
638-42013 L-shaped combustion tube (in case) 1
638-60116 TOC regular catalyst 1
630-00557 Quartz wool 1
638-52578-01 CO2 absorber container 1
630-00556 Soda lime 1
638-40168 Compression fitting, elbow 4
016-37504 Teflon tube (3×4) 2.9m
040-82074-03 Filter 1
035-65104 Union 2
016-43284-01 Nylon tube 0.1m

302 TOC-VCPH/CPN
 6.5 Special Accessories
6.3.8 PC Hardware Requirements

6.5 Special Accessories

Table 6.10 • Special Accessories List

Part Number Part Name CommentComment
638-93141-04 Autosampler ASI-V (24mL) 24mL vials
638-93141-08 Autosampler ASI-V (40mL) 40mL vials
638-93150-01 8-Port sampler OCT-1 For TOC-VCPH/CPN/CSH/CSN
638-93150-11 8-Port sampler OCT-2 (second For TOC-VCPH/CPN/CSH/CSN
unit)
638-91065-01 TN unit TNM-1 For AC 100-127V
638-91065-02 TN unit TNM-1 For AC 220-240V
638-91066 POC measurement kit
638-72596 Option wiring kit Required to install the POC kit or
external sparge kit for the TOC-VCPH
638-41447 Carrier gas purifier kit
638-77152 External sparge kit
638-93149-03 Manual injection kit
638-41460 Suspended solids kit (when used
with TOC-V alone)
638-93151 Suspended Solids Kit (when
autosampler is used)
638-53044-01 Sample rack and vial sets for 24mL sample rack
24mL sample vials 24mL sample vials
Vial caps
Septa
638-53044-02 Sample rack and vial sets for 40mL sample rack
40mL sample vials 40mL sample vials
Vial caps
Septa
638-67075 Stirrer (for 24mL vials) For autosampler 24mL vials
638-67076 Stirrer (for 40mL vials) For autosampler 40mL vials
046-00617-02 Stirrer bar (for 24mL vials) Stirrer bar for 24mL vials, 1 required for
sample measurement
046-00617-03 Stirrer bar (for 40mL vials) Stirrer bar for 40mL vials, 1 required for
sample measurement
630-00960 High purity air cylinder Recommended that user provide this
item.
630-08585-05 Cylinder pressure regulator User can provide this item.
638-41204 Air supply tubing set (with 20 User can provide this item.
meters of tubing)
630-02525-01 High speed homogenizer
638-52344 Drain bottle (for ASI)

TOC-VCPH/CPN 303
 6.6 Consumable Parts List
6.3.8 PC Hardware Requirements

6.6 Consumable Parts List

Table 6.11 • Consumable Parts List 1 (TOC-VCPH)

Part Number Part Name Comment
638-41323 Combustion tube, in case
638-60116 TOC regular catalyst
630-00105-01 Platinum mesh To support catalyst, 2
included
630-00557 Quartz wool To support catalyst, 1g
630-00996 TOC high sensitivity catalyst
638-41308-01 Cooling coil
630-00999 CO2 absorber
630-00992 Halogen scrubber
036-11209-84 O-ring, 4D P 10A For slider, 5pcs.
036-11408-84 O-ring, Teflon P10 For slider, 5pcs.
036-11222-84 O-ring, 4D P22 For IC reaction tube, 5pcs.
036-11219-84 O-ring, 4D P20 For TC reaction tube, 5pcs.
035-62994-03 Sleeve set 6F-T
042-00405-11 IC reaction solution supply
pump head
630-00635-01 Potassium biphthalate, 25 g
630-00962-01 Sodium carbonate, 25 g
630-00963-01 Sodium bicarbonate, 25 g
046-00044-11 Membrane filter
017-30812-01 Silicone grease, H.V.G.
630-08913-01 Chart paper 10 rolls
638-60074 Ceramic fibers
631-20265 8-port valve rotor
638-59213-01 Plunger tip
638-92206-01 Consumables set Refer to Table 6.13 for
contents

304 TOC-VCPH/CPN
 6.6 Consumable Parts List
6.3.8 PC Hardware Requirements

Table 6.12 • Consumable Parts List 2 (TOC-VCPN)

Part Number Part Name Comment
638-41323 Combustion tube, in case
638-60116 TOC regular catalyst
630-00105-01 Platinum mesh To support catalyst, 2
included
630-00557 Quartz wool To support catalyst, 1g
630-00999 CO2 absorber Contains 500mL
630-00992 Halogen scrubber
036-11209-84 O-ring, 4D P 10A For slider, 5pcs.
036-11408-84 O-ring, Teflon P10 For slider, 5pcs.
036-11219-84 O-ring, 4D P20 For TC reaction tube, 5pcs.
630-00635-01 Potassium biphthalate, 25 g
630-00962-01 Sodium carbonate, 25 g
630-00963-01 Sodium bicarbonate, 25 g
046-00044-11 Membrane filter
017-30812-01 Silicone grease, H.V.G.
638-60074 Ceramic fibers
631-20265 8-port valve rotor
638-59213-01 Plunger tip
638-92206-02 Consumables set Refer to Table 6.13 for
contents

TOC-VCPH/CPN 305
 6.6 Consumable Parts List
6.3.8 PC Hardware Requirements

Table 6.13 • Consumable Parts List 3 (TOC-VCPH/CPN)

Part No. Description Qty Remark
TOC- TOC-
VCPH VCPN
638-41323 Combustion tube (in case) 2 2
638-60116 TOC regular catalyst 2 2
630-00996 TOC high sensitive catalyst 1 0
630-00557 Quartz wool 1 1
630-00999 CO2 absorber 1 1
630-00992 Halogen scrubber 2 2
036-11209-84 O-ring, 4D P 10A 1 1 5 pcs
036-11408-84 O-ring, Teflon P10 1 1 5 pcs
036-11219-84 O-ring, 4DP 20 1 1 5 pcs
630-00635-01 Potassium hydrogen 1 1
phthalate, 25g
630-00962-01 Sodium carbonate,25g 1 1
630-00963-01 Sodium bicarbonate, 25g 1 1
638-60074 Ceramic fiber 1 1
042-00405-11 IC reagent supply pump head 1 0
631-20265 8-port valve rotor 1 1
638-59213-01 Plunger tip 2 2

Table 6.14 • Consumable Parts List 4 (ASI-V)

Part Number Part Name Comment
038-00165-21 Vial set 40mL, 72 vials, septa and
caps
638-41462 Vial 24mL, 100pcs
038-00165-48 Septum 24mL, 100pcs.
038-00165-50 Septum 40mL, 100pcs.
638-20074-01 Cap 24mL, 100pcs.
038-00165-40 Cap 40mL, 200pcs.
042-00405-11 Rinse pump head

Table 6.15 • Consumable Parts List 5 (8-Port Sampler OCT-1)

Part Number Part Name Comment
631-20265 8-Port valve rotor

306 TOC-VCPH/CPN
 6.6 Consumable Parts List
6.3.8 PC Hardware Requirements

Table 6.16 • Consumable Parts List 6 (TNM-1)

Part Number Part Name Comment
638-65232 Ozone treatment - catalyst 300g included
638-71162 Ozone treatment unit ASSY
631-43818 Reactor packing
631-40316 Viton joint, reactor outlet
036-19004-19 O-ring, Ozone treatment unit 1pc.
017-40533-01 Potassium nitrate, 25 g

Table 6.17 • Consumable Parts List 7 (Carrier Gas Purifier Kit)

Part Number Part Name Comment
638-42013 L-shaped combustion tube,
in case
630-00556 Soda lime Carrier gas purifier kit, 500g
included
638-60116 TOC regular catalyst

TOC-VCPH/CPN 307
 6.7 Maintenance Parts List
6.3.8 PC Hardware Requirements

6.7 Maintenance Parts List

Table 6.18 • Maintenance Parts List 1 (TOC-VCPH)

Part Number Part Name Comment
638-56135 8-port valve
638-59213 Syringe
638-41337-03 Flared tubing
631-41660 Flared tubing, for dilution
water
638-65383 Tandem cell (in case)

Table 6.19 • Maintenance Parts List 2 (TOC-VCPN)

Part Number Part Name Comment
638-56135 8-port valve
638-59213 Syringe
638-41337-03 Flared tubing
631-41660 Flared tubing, for dilution
water
638-65383 Tandem cell (in case)

Table 6.20 • Maintenance Parts List 3 (ASI-V)

Part Number Part Name Comment
638-41472-01 Needle, sampling For 24mL and 40mL, 1pc.
638-41448-01 Needle, sparging For 24mL and 40mL, 1pc.
638-41449-01 Needle, simultaneous sparge For 24mL, 40mL, 1pc.
type
638-41450-01 Needle, suspended solids kit, For 24mL, 40mL, 1pc.
0.8mm
638-42029-04 Tubing set (sampling) 1 sampling tube, with
retainer and tube seal
638-42029-05 Tubing set (sparge) 1 sparge tube, with retainer
and tube seal
638-42029-03 Tubing set (sampling + 1 each of sampling and
sparge for simultaneous sparge tube for simultaneous
sparge) sparging, with retainers and
tube seals

308 TOC-VCPH/CPN
 6.7 Maintenance Parts List
6.3.8 PC Hardware Requirements

Table 6.21 • Maintenance Parts List 4 (OCT-1 8-Port Sampler)

Part Number Part Name Comment
631-20265 8-port valve rotor Spare rotor
638-41337-03 Flared tubing C Sampling tube; for
combustion type TOC-V
638-41443-03 Common tubing C Main unit - OCT-1
connection tube; for
combustion TOC-V, 1 unit
638-41443-04 Common tubing C2 Main unit - OCT-1
connection tube; for
combustion TOC-V, add-on

Table 6.22 • Maintenance Parts List 5 (Manual Injection Kit)

Part Number Part Name Comment
630-00261 Open / Close valve, TC
injection port
638-60733-01 Microsyringe, MANU10 10µL
638-60733-02 Microsyringe, MANU25 25µL
638-60733-03 Microsyringe, MANU50 50µL
638-60733-04 Microsyringe, MANU100 100µL
638-60733-05 Microsyringe, MANU250 250µL
638-60733-06 Microsyringe, MANU500 500µL

TOC-VCPH/CPN 309
 6.8 Installation
6.8.1 Before Installation

6.8 Installation

6.8.1 Before Installation

Parts Inspection
Confirm that all of the components listed in Section 6.4 "Standard Accessories" have been
included in the shipping package.

6.8.2 Installation Site

Be sure to take into account the size of the instrument, how it will be used, and the
installation conditions indicated below when selecting an installation site. Instrument
damage or measurement errors may occur based on the conditions of the installation site.

6.8.2.1 Installation Site Selection

The instrument is designed for use on a desk or bench.

The external dimensions of the instrument are shown in Figure 6.3 "External Dimensions
of Instrument with ASI-V". A space of at least 200mm is required on either side of and
behind the instrument to enable unhindered operation and maintenance.
635mm

TOC-V Main Unit

Autosampler TOC-V Main Unit TN Unit

100
370mm mm 440mm 160mm

Figure 6.3 External Dimensions of Instrument with ASI-V

310 TOC-VCPH/CPN
 6.8 Installation
6.8.2 Installation Site

Figure 6.4 External Dimensions of Instrument with OCT-1 8-Port Sampler

CAUTION
When lifting the instrument, lift from the bottom and at both sides of the
instrument.
Do not lift the instrument by the front access door, as this may cause damage.

6.8.2.2 Installation Site Conditions

Select an installation site with the following conditions:
• A clean environment free of corrosive gases, organic gases, and dusts.
Note: Contamination in the atmosphere will cause analysis errors, especially for high
sensitivity analyses.
• A strong, level bench, free of vibration and shock.
• A location with a stable ambient temperature.
• A location with access to a completely grounded, stable power supply.

CAUTION
Avoid locations where flames are prohibited. Some internal parts reach high
temperatures and could cause a fire hazard.

Avoid the following kinds of locations:

• Locations close to heat sources, windows in direct sunlight, or in direct contact with
drafts from air conditioning vents.
• Near equipment that generates intense magnetic fields, electrical fields, or high
frequency waves.

TOC-VCPH/CPN 311
 6.8 Installation
6.8.3 Installation Procedure

6.8.3 Installation Procedure

6.8.3.1 Connecting Power Supply and Ground

¬Connecting Power Supply

Connect the instrument to a stable, AC 100-127V (100V System) or AC 220-240V (200V
System), 50Hz or 60Hz (single phase) power supply with sufficient capacity to
accommodate 6A or greater current.

CAUTION
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127V ±10% or AC 220-240V ±10%. Unstable voltage may
cause problems during high sensitivity analysis.

Note: The instrument is compatible with both 50 Hz and 60 Hz power supplies and can
be used with either frequency.

¬Grounding
The included power cord is a three-conductor cable including a ground wire, and a 2P plug
(with ground) at the end. If the power outlet does not have ground receptacle, use the
included 2P (no ground) adapter. Connect the external ground terminal to the ground.
The voltage terminals (AC) and ground terminal (ACC) on the power plug of this
instrument are arranged as shown in Figure 6.5 "Power Plug". Connect them so that they
match the power outlet being used.

Voltage terminal (AC) Ground terminal (ACC)

Ground terminal (G)

(Be sure to ground completely.)

Figure 6.5 Power Plug

312 TOC-VCPH/CPN
 6.8 Installation
6.8.3 Installation Procedure

CAUTION
• In addition to the consideration of safety, complete grounding is necessary to
prevent as much as possible the occurrence of signal noise. A Type-3 ground
(ground resistance: 100W or less, see Electrical Facilities Engineering Standards
for details) is recommended.
• Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.

6.8.3.2 Changing the Power Supply Voltage

The instrument is set up before shipment to match the power supply voltage in the locale
where it will be used. In the event that it becomes necessary to change the power supply
voltage, please contact your Shimadzu representative. Depending on the voltage change,
an authorized Shimadzu service engineer may be required to rewire connections to the
terminal block to change the power supply voltage and/or perform changes to the main
board.

6.8.3.3 Connecting Gas

Use one of the following as the carrier gas supply for this instrument.
• Cylinders filled with high purity air
• Compressed air or instrumentation air (Requires special Carrier Gas Purifier Kit
accessory)

¬High Purity Air Cylinders

High purity air is synthetic air manufactured from pure nitrogen and pure oxygen. It must
be guaranteed to contain less than one 1ppm of each of the following impurities: carbon
dioxide, carbon monoxide, and hydrocarbons.
The cylinder must be equipped with a pressure regulator to supply it at 300kPa to the gas
connection inlet of the instrument.
Note: If the carrier gas contains excessive impurities, analysis accuracy is diminished
and good results will not be obtained.

TOC-VCPH/CPN 313
 6.8 Installation
6.8.3 Installation Procedure

Precautions for Handling Gas Cylinders

The handling and safety management of high-pressure gases is strictly regulated
by high-pressure gas control laws, general high-pressure gas safety codes, and
fire laws.
The gas used in the instrument is not dangerous, but mistakes in handling of
high-pressure gas cylinders can be extremely hazardous. Carefully read and
obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40°C.
• Make sure there are no open flames anywhere within 2 meters of a gas cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• Turn OFF, immediately and completely, all valves on the cylinder, when finished
using gas.
• Inspect the operation of the pressure gauge at least once every three (3) months.

¬Compressed Air or Instrument Air Purified with the Carrier Gas Purification
Kit
Using the Carrier Gas Purification Kit enables air from a compressor or instrumentation air,
or high-impurity pressurized air in a cylinder, to be used as the carrier gas.
Since there are limits to the capabilities of the Carrier Gas Purification Kit, the following
conditions must be met when supplying compressed air.
• Provide an air filter in the supply line to remove dust, oil mist, water drops, and other
contaminants. Place an air filter in the tubing near the gas connection inlet of the
instrument when a compressor is used.
• Select the Oil-less Carrier Gas Purification Kit when a compressor is used.
• There are cases where the organic gas concentration is too high to be removed
completely by the gas purifier. Analysis accuracy is poor in atmospheres containing
high concentrations of volatile gases from exposed organic solvents and gasoline, or
high concentrations of automobile and diesel engine exhaust. If the possibility of the
presence of these kinds of gases cannot be avoided, use a filter to remove organic
particles and/or gases.

¬Gas Supply Pressure

Ensure that the gas supplied to the gas inlet of the instrument maintains a constant, stable
pressure of 300kPa. When using compressed air or instrumentation air, verify that the gas
supply pressure is greater than 300kPa and less than 600kPa.
Note: Do not allow the carrier gas supply pressure to exceed 600kPa.

¬Gas Tubing Connections

The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two [2]
half unions).

314 TOC-VCPH/CPN
 6.8 Installation
6.8.3 Installation Procedure

Procedure

Connection Inlet

Half Union

Nylon Tubing

Figure 6.6 Gas Tubing Connection

1. Connect the half unions to the carrier gas inlet on the instrument and the connection
outlet (¼” NPT) of the gas supply source.
2. Connect the nylon tubing (4mm OD, 2.5mm ID) between the gas supply source and
the instrument.
Note: To connect the nylon tubing, firmly insert it into the half union. To
disconnect the tubing, pull the tubing off while pushing down
firmly on the blue ring of the half union with a screwdriver.
3. Verify that there are no gas leaks.

CAUTION
• Do not allow acute bends in the tubing.
• Clean the tubing and connectors to remove any oils or other contaminants on
their inner surfaces.
• Copper tubing or stainless steel tubing may also be used.

TOC-VCPH/CPN 315
 6.8 Installation
6.8.3 Installation Procedure

6.8.3.4 Connecting the Drain Tubing

Drain tubing is connected to provide for external discharge of measured samples and other
liquid waste. If a nearby drainage pit is not available, use a 10 to 20 liter polypropylene
container as the drain receptacle.

Figure 6.7 Connect the Drain Tubing

The drain tubing from the dehumidifier drain port is located inside the right panel. Connect
it to the external drain tubing using two of the provided wiring bands so that there are no
leaks.

CAUTION
• Drainage occurs on a gravity basis. Keep resistance to a minimum. Ensure that
the drain tubing is never higher than the drain discharge port. Do not allow the
tip of the drain tubing to come in contact with the surface of the liquid in the
container. If resistance is high, insufficient drainage could cause the drainage liq-
uid to overflow inside the instrument.
• Corrosive substances such as acids may be present in the drainage liquid. Avoid
touching or spilling these liquids.

316 TOC-VCPH/CPN
 6.8 Installation
6.8.4 Installing the Autosampler

6.8.3.5 PC Cable Connections

This section describes the procedure for connecting the TOC-V to the PC using the
supplied RS-232C cable.

Procedure

1. Insert the supplied RS-232C cable into the RS-232C-1 connector on the back of the
TOC-V, and tighten the retaining screws on both sides. Figure 2.4 "Rear View"
2. Insert the plug at the other end of the RS-232C cable into the RS-232C connector of
the PC, and tighten the retaining screws on both sides.

6.8.4 Installing the Autosampler

This section describes procedures for installing the ASI-V autosampler.

¬Positioning the Autosampler

The autosampler is placed to the left of the TOC-V, as shown in Figure 6.8 "Installing the
Autosampler".

Figure 6.8 Installing the Autosampler

Note: Keep the distance between the autosampler and main unit to a minimum to allow
a free range of motion of the autosampler. If the autosampler tubing becomes
stretched taut, it may impede the movement of the autosampler arm, resulting in
operation errors and damage.

¬Removing the Shipping Screw

The ASI arm is secured with a shipping screw to prevent damage during shipment. Before
connecting power to the instrument, remove the ASI cover to access the shipping screw,
which is located on the retaining bracket. Remove the shipping screw and replace the cover.
Label the shipping screw and store it for future use.

TOC-VCPH/CPN 317
 6.8 Installation
6.8.4 Installing the Autosampler

CAUTION
To prevent instrument damage, verify that the ASI arm is firmly attached to the
retaining bracket with the shipping screw before shipping the instrument or
moving it to another location.

¬Connecting Cables
The TOC-V and ASI-V are connected using cables, as described below.

CAUTION
Verify that the TOC-V is switched OFF before performing the following
procedure.

Procedure
1. Connect the ASI-V power cord at the rear of the ASI-V to the ASI-V power connector
at the rear of the TOC-V.
2. Connect the provided signal cable to the ASI-V signal connectors at the rear of the
TOC-V and the ASI-V.

Figure 6.9 Connecting the Cables (TOC-V to ASI-V)

318 TOC-VCPH/CPN
 6.8 Installation
6.8.4 Installing the Autosampler

¬Connecting the Sample Tubing and Sparge Tubing (External Sparge Kit)
The procedure for connecting the ASI-V sample tubing and sparge tubing for the External
Sparge Kit is as follows.

Procedure
1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>ASI Needle Change.
3. Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
4. Remove the screw at the lower left side of the needle replacement window, and detach
the window cover by pulling downward.
5. Install the tubing clamp.

Needle Replacement Window

Sample Catcher

Figure 6.10 Tubing Installation

6. Install the bushing at the end of the sample tubing to the Number 2 port of the TOC-V
sample injector 8-port valve.

TOC-VCPH/CPN 319
 6.8 Installation
6.8.4 Installing the Autosampler

7. Draw the sparge tubing out through the joint and connect the sparge tubing.
Sparge Tubing
(External Sparge Kit)

External Sparge Unit

Advance Sparge Sampling Needle

Needle

Sparge Tubing

Tubing Installation Label

(External Sparge Kit)

Sparge Tubing
(External Sparge Kit)

ASI-V Cover

Installation figure using the anvance

sparge needle and the sampling needle.

Figure 6.11 Installing the External Sparge Kit

Note: Do not use the flow controller knob to turn off the sparge gas flow.

¬Installing the Needle

This section describes installation of the ASI-V needle. There are two types of needles, the
sample needle (same as the sparge needle) and the coaxial needle, which is a combined
sample/sparge needle.
When installing the needle, remove the needle replacement window cover. Refer to Figure
6.11 "Installing the External Sparge Kit", for the removal procedure.

320 TOC-VCPH/CPN
 6.8 Installation
6.8.4 Installing the Autosampler

Installation Procedure for the Sample Needle and Sparge Needle

1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>ASI Needle Change.
3. Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
4. Remove the screw, and then detach the needle holder from the arm.
5. Insert the needle into the opening in the needle holder.
6. Secure the needle by turning the retaining bracket and tightening the screw at the top
of the needle holder.
Note: There are two openings; the left opening is for the sample tubing
and the right opening is for the sparge tubing.

Retaining Bracket

Needle Holder

Sample Needle

Figure 6.12 Installing the Needle - 1

7. Securely fit the sample tubing or sparge tubing onto the upper end of the needle.
Note: Verify that the bushing is in position to secure the sample tubing
onto the sample needle.
8. Insert the lower tip of the needle into the needle guide opening, thrusting the needle
holder into the pin of the arm, and then tighten the screw.

TOC-VCPH/CPN 321
 6.8 Installation
6.8.4 Installing the Autosampler

9. Reinstall the needle replacement window cover, and tighten the screw.

Figure 6.13 Installing the Needle - 2

Installing the Coaxial Needle

1. Open the TOC-Control V Sample Table Editor and connect the instrument.
2. From the Instrument menu, select Maintenance>ASI Needle Change.
3. Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
4. Detach the needle holder from the arm.
5. Insert the needle into the opening in the needle holder.
6. Secure the needle by turning the retaining bracket, and tightening the screw at the top
of the needle holder.
7. Install the provided 3-way joint on the top of the needle.
8. Connect the sample tubing to the top of the 3-way joint, and the sparge tubing to the
side of the joint.
9. Insert the tip of the needle into the needle guide opening, thrusting the needle holder
into the pin of the arm, and then tighten the screw.
10. Reinstall the needle replacement window cover, and tighten the screw at the lower left
of the cover.

322 TOC-VCPH/CPN
 6.8 Installation
6.8.4 Installing the Autosampler

¬Installing the Turntable, Vial Rack and Cover

Installing the Turntable

1. Place the turntable on the ASI-V.
Note: There is no distinction between front and rear of the turntable, so
placement orientation is irrelevant.
2. Place the turntable so that the 3 guides on the ASI-V pass through the 3 holes at the
center of the turntable.

Three Holes at
Turntable Center of Turntable

Figure 6.14 Installing the Turntable

Installing the Vial Rack

1. Place the vial rack on top of the turntable.
2. Rotate the vial rack until the guides of the turntable fit into the vial rack. This secures
the vial rack in place.

Installing the Cover

1. Place the cover on the ASI-V.
Note: There is a magnet at the left rear of the cover. Verify that the cover
and ASI-V are in contact at the magnet.

¬Install the Rinse Bottle and Drain Tank

Installation of the rinse bottle and drain tank is explained below.
Rinse and drain tubing are attached to the autosampler, and are respectively labeled
“RINSE” and “DRAIN.” Use the rinse water tubing as is, and cut the drain tubing to an
appropriate length.

TOC-VCPH/CPN 323
 6.8 Installation
6.8.4 Installing the Autosampler

CAUTION
• Verify that the drain tubing remains lower than the drain port of the ASI-V, and
that the end of the drain tubing remains above the surface of the liquid in the
drain tank.
• Corrosive substances such as acids may be present in the drainage liquid. Avoid
touching or spilling these liquids.

Preparation
• The rinse bottle is provided as a standard accessory.
• The drain bottle is a special accessory (P/N 638-52344). A suitable substitute may be
used as the drain container.

Procedure
1. Place the rinse bottle on the bench with the TOC-V and the autosampler.
2. Place the drain container on the floor.
3. To minimize resistance, keep the tip of the drain tubing above the surface of the drain
liquid and as close to the instrument as possible.

CAUTION
Do not allow any slack or bends in the tubing that could cause a buildup of water
pressure.

Before Starting Analysis

Check the following before starting analysis.
• The rinse water bottle is filled to above the 2 L mark.
• The tip of the rinse tubing reaches nearly to the bottom of the rinse water bottle.

CAUTION
Perform the checks described above to ensure that rinse water will be delivered
and air will not be taken into the TOC-V injection pump.

324 TOC-VCPH/CPN
 6.8 Installation
6.8.5 OCT-1 8-Port Sampler Installation

6.8.5 OCT-1 8-Port Sampler Installation

The OCT-1 8-port sampler is installed as described below.

6.8.5.1 Installation Procedure

This section describes the procedure for installing the OCT-1 8-Port Sampler.
The unit is set up to the left of the TOC-V main body as shown in Figure 6.15“Installation
of the 8-Port Sampler”.

TIP » When 2 OCT-1 8-Port Samplers are to be used, place both units to the left of the TOC-V
main unit as shown in the overhead view of Figure 6.4“External Dimensions of Instrument
with OCT-1 8-Port Sampler”.

8-Port Sampler TOC-V Main Unit

Figure 6.15 Installation of the 8-Port Sampler

Cable Connections
The cable is connected between the main unit of the TOC-V and the 8-Port Sampler.

CAUTION
Confirm that the power to the TOC-V main unit is switched OFF before
performing this procedure.

Connection Procedure
1. Remove the 4 screws at the top of the 8-Port Sampler, and take off the cover.
2. Connect the power and signal cable to the circuit board of the 8-Port Sampler.
3. Connect the ground wire of the power cable to the grounding terminal on the circuit
board of the OCT-1.
4. Pass the cable through the rear panel, and replace the cover of the 8-Port Sampler.

TOC-VCPH/CPN 325
 6.8 Installation
6.8.5 OCT-1 8-Port Sampler Installation

Rear Panel

8-Port Sampler Power Cable

8-Port Sampler Signal Cable

Figure 6.16 Cable Connections (TOC-V and 8-Port Sampler)

5. Connect the power cable to the power receptacle on the back of the TOC-V.
6. Connect the signal cable to the 8-Port Sampler connection on the back of the TOC-V.

Installing Two 8-Port Sampler Units

When installing two 8-Port Sampler units, a signal cable (standard accessory) is connected
between 8-Port Sampler 1 and 8-Port Sampler 2.

Installation Procedure

1. Remove the covers from both 8-Port Sampler units.

2. Connect the signal cable exiting 8-Port Sampler 2 to the connector of 8-Port Sampler
1.

8-Port Sampler 2

Signal Cable

8-Port Sampler 1

Figure 1.17 Connecting Two 8-Port Samplers

326 TOC-VCPH/CPN
 6.8 Installation
6.8.5 OCT-1 8-Port Sampler Installation

3. Remove the port number label from the 8-Port Sampler 2 unit and replace it with the
port number label provided with the unit.
Note: The port that was originally labeled as port No. 1 should be labeled
as port No. 9.
4. Replace the covers on the 8-Port Samplers.

Connecting the Sample Tubing

Use the following procedure to connect the sample tubing of the 8-Port Sampler.

Tubing Connection Procedure

1. The sample tubing differs according to the TOC-V model that is used with the 8-Port
Sampler
Note: Refer to Table 6.21 •“Maintenance Parts List 4 (OCT-1 8-Port Sam-
pler)” for the appropriate part numbers.
2. Connect the fitting at one end of the tubing to the common (COM) port of the 8-Port
Sampler.
3. Pass the sample tubing through the hole in the left side panel of the TOC-V main unit.
Connect the fitting at the other end of the sample tubing to port No. 2 of the 8-port
valve of the TOC-V sample injector. Connect to port No. 1 when installing 8-Port
Sampler 2.
4. Connect the sample tubing to ports 1 - 8 (ports 9 - 16 for 8-Port Sampler 2) of the 8-
Port Sampler.

Sample Tubing

Figure 6.18 Tubing Connections

Note: Connection to the TOC-V Main Unit
• 8-Port Sampler 1
Connect the COM tubing to the common (COM) port of 8-Port Sampler 1 and
port No. 2 on the TOC-V unit.
• 8-Port Sampler 2
Connect the COM tubing to the common (COM) port of 8-Port Sampler 2 and
port No. 1 on the TOC-V unit

TOC-VCPH/CPN 327
 6.8 Installation
6.8.6 Installing the TN Unit

6.8.6 Installing the TN Unit

6.8.6.1 Connecting the Power and Installation

¬Connecting the Power Supply

Connect the TN unit to a stable, AC100V±10 V, 50Hz or 60Hz (single phase) power supply
with sufficient capacity to accommodate 2A or greater current. The symbol “~” on the
name plate indicates alternating current.

CAUTION
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127V ±10% or AC 220-240V ±10%. Unstable voltage may
cause problems during high sensitivity analysis.

Note: The instrument is compatible with both 50Hz and 60Hz power supplies and can
be used with either frequency.

¬Grounding
The included power cord is a three-conductor cable including a ground wire and a 2P plug
(with ground) at the end. If the power outlet does not have ground receptacle, use the
included 2P (no ground) adapter and ground the external ground tap terminal.
The voltage terminals (AC) and ground terminal (ACC) on the power plug of this
instrument are arranged as shown in Figure 6.19 "Power Plug". Connect them so that they
match the power outlet being used.
Voltage Terminal (AC) Ground Terminal (ACC)

Ground Terminal (G)

(Be sure to ground completely.)

Figure 6.19 Power Plug

328 TOC-VCPH/CPN
 6.8 Installation
6.8.6 Installing the TN Unit

CAUTION
• In addition to the consideration of safety, complete grounding is necessary to
prevent as much as possible the occurrence of signal noise. A Type-3 ground
(ground resistance: 100W or less, see Electrical Facilities Engineering Standards
for details) is recommended.
• Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.

6.8.6.2 Connecting Ozone Source Air

The TNM-1 incorporates an internal ozone generator, requiring a source of air gas
(supplied at about 500mL/min) separate from the carrier gas supplied to the TOC-V. While
it is possible to use TOC-V high purity carrier gas by providing branch tubing, the
consumption of the combined-use carrier gas would increase to about 150 - 250mL/min.
Assuming operation at the rate of 8 hours/day, 5 days/week, the 47 L, 12MPa air cylinder
would require monthly replacement (as compared to every 3 months when used for carrier
gas alone).
Because air gas for ozone generation is not required to be the high purity air used as carrier
gas, it is recommended to use instrumentation air or compressor-supplied air for ozone
generation, separate from the carrier gas.

¬Using Compressor Air or Instrumentation Air

When using compressor air or instrumentation air for generation of ozone, be sure that the
following conditions are satisfied.
• Install an air filter in the air supply line to eliminate dust, oil mist and water droplets
from the air. If a compressor is used, install the air filter (equipped with drain separation
and discharge branch) close to the tubing connection at the instrument.
• If a compressor is used, select an oil-less type air compressor. The oil-less air compres-
sor SLP-5D-2 SVF (P/N 638-59203-01) is available as an option.

¬Using a High Purity Air-Filled Cylinder (Via Branch Tubing from Carrier Gas)
High purity air is synthesized air using pure nitrogen and pure oxygen. Ensure that
contaminants, including carbon dioxide, carbon monoxide and total hydrocarbons, are
guaranteed not to exceed 1ppm each.
Install a pressure regulator on the gas cylinder and supply gas to the instrument so that the
pressure is 300kPa at the instrument gas connection port.
Note: If there are excessive contaminants in the carrier gas, measurement results will be
adversely affected due to low measurement reproducibility, etc.

TOC-VCPH/CPN 329
 6.8 Installation
6.8.6 Installing the TN Unit

Precautions in Handling Gas Cylinders

The handling and safety management of high-pressure gases is strictly regulated
by high-pressure gas control laws, general high-pressure gas safety codes, and
fire laws.
The gas used in this instrument itself is not dangerous, but mistakes in the
handling of high-pressure gas cylinders can be extremely hazardous. Carefully
read and obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40°C.
• Make sure there are no open flames anywhere within 2 meters of a gas cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• When finished using gas, immediately and completely turn OFF all valves on the
cylinder.
• Inspect the operation of the pressure gauge at least once every three (3) months.

¬Gas Supply Pressure

Supply gas at a constant, stable pressure of 300kPa (44PSI)at the gas inlet connection of the
TNM-1.
Note: Keep the carrier gas supply pressure to the instrument from exceeding 600kPa
(87PSI).

¬Gas Tubing Connections

The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two (2)
half unions).

Connection Inlet
Half Union

Nylon Tubing

Figure 6.20 Gas Tubing Connection

330 TOC-VCPH/CPN
 6.8 Installation
6.8.6 Installing the TN Unit

Procedure

1. Connect the half unions to the carrier gas inlet on the instrument and the connection
outlet (¼” NPT) of the gas supply source.
2. Connect the nylon tubing (4mm O.D., 2.5mm I.D.) between the gas supply source and
the instrument.

Note: The nylon tubing can be connected simply by firmly inserting it

into the half union. When disconnecting the tubing, pull off the tub-
ing while pushing down firmly on the green-colored ring of the half
union using a screwdriver.

3. After connection, check to see that there are no gas leaks.

CAUTION
• Do not allow any acute bends in the tubing.
• When tubing and connectors are prepared by the user, be sure to use clean
components that are free of oils or other contaminants on their inner surfaces.
• Copper tubing or stainless steel tubing may also be used.

¬Low Ozone Air Supply Pressure Safety Mechanism

To ensure safety, the TN unit is equipped with an ozone air gas pressure sensor that will
automatically cause the ozone generator to be switched off when the ozone air gas pressure
decreases below 50kPa.
If this occurs, the red lamp labeled “PRESS” at the lower right of the TNM front panel will
illuminate. Take the appropriate measures to correct the low pressure problem.

TOC-VCPH/CPN 331
 6.8 Installation
6.8.6 Installing the TN Unit

6.8.6.3 Connecting Gas Exhaust Tubing

Because the unit uses a chemiluminescence system for the detection of TN components, it
is equipped with an internal ozone generator. The ozone and NOx generated are removed
by the ozone treatment unit and NOx absorber, and are then exhausted. However, in the
event that the performance of the ozone treatment catalyst and NOx absorber deteriorate,
ozone and NOx gas may be expelled in the exhaust gas. Be sure to discharge exhaust gas to
the outdoors or to an exhaust pit using a 5mm I.D. flexible vinyl hose.

CAUTION
• To minimize resistance, leave the gas exhaust tubing open to the atmosphere.
• Be sure to connect the gas exhaust tubing to the instrument and discharge the
exhaust gas to the outdoors or an exhaust pit.
• If the gas exhaust tubing is not connected, ozone and NOx gas may be exhausted
from the instrument, causing harm to the respiratory organs of individuals in the
vicinity.

332 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.1 Hydrochloric Acid (HCl)

6.9 Material Safety Data Sheets

6.9.1 Hydrochloric Acid (HCl)

Shimadzu Scientific Instruments, Inc. 957006
7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 November, 1995

MATERIAL SAFETY DATA SHEET

SECTION I PRODUCT IDENTIFICATION
CAT. NO.: 630-00998-00 CAS NO.: Hydrochloric Acid -7647-01-0
NAME: Hydrochloric Acid OTHER NAME: Muriatic Acid; Regeneration Liquid
PRODUCT USE: This product is for specific use in the regeneration of the catalysts of the Shimadzu TOC. Refer to the Instruction Manual of the
unit for proper use.
SECTION II PRECAUTIONS TO BE TAKEN IN HANDLING
Do not get in eyes, on skin or on clothing. Wear rubber or neoprene gloves and impervious boots, apron or coveralls, as needed, to prevent skin contact. Avoid
breathing mist. Use only with adequate ventilation; local and/or general exhaust is recommended to keep employee exposure below the Airborne Exposure Limits.
If TLV is exceeded, a full face piece chemical cartridge respirator may be worn, in general, up to 100 times the TLV or the maximum use concentration specified
by the respirator supplier, whichever is less. Store in tightly closed containers, in cool, dry, ventilated area. Protect from physical damage and direct sunlight. Iso-
late from incompatible substances. Protect from moisture. Remove and wash contaminated clothing promptly. Wash hands thoroughly after handling. This sub-
stance is classified as a POISON under the Federal Caustic Poison Act.
SECTION III PHYSICAL DATA
Melt Boil Point Density Vapor Vapor Evaporation Odor Color Phase Water Solubility
Point Pressure Density Rate
N/A N/A N/A N/A N/A N/A Pungent Colorless / Clear Fuming Infinite / slight
Liquid evolution / heat
SECTION IV REACTIVITY DATA
Stable under ordinary conditions of use and storage. Containers may burst when heated. When heated to decomposition, emits toxic hydrogen chloride fumes and
will react with water or steam to produce heat and toxic and corrosive fumes. Hazardous Polymerization will not occur. Incompatibilities: A strong mineral acid;
concentrated hydrochloric acid is highly reactive with strong bases, metals, metal oxides, hydroxides, amines, carbonates and other alkaline materials. Incompati-
ble with materials such as cyanides, sulfides, sulfites and formaldehyde.
SECTION V FIRE AND EXPLOSION HAZARD DATA
FIRE: Can react with metals to release flammable hydrogen gas.
EXPLOSION: Not considered to be an explosion hazard.
EXTINGUISHING MEDIA: If involved in a fire, use water spray. Special firefighting procedures: Use full protective clothing and NIOSH-approved self-
contained breathing apparatus with full face piece operated in the pressure demand or other positive pressure mode.
SECTION VI TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
900mg/kg(hydrocloric acid concentrated) N/A 5ppm (TWA) Ceiling 5ppm (TWA) Ceiling
SECTION VII HEALTH HAZARD DATA
Symptoms of overexposure: Inhalation: corrosive; can cause coughing, choking, inflammation of the nose, throat and upper respiratory tract. Inhalation of higher
concentrations may cause lung damage. Ingestion: corrosive; swallowing product can cause immediate pain and burns of the mouth, throat, esophagus and gas-
trointestinal tract; may cause nausea, vomiting and diarrhea. Contact with skin: corrosive; can cause redness, pain, and severe skin burns; deep ulcers and discol-
ored skin; severe burns and eye damage. Chronic exposure: long-term exposure to concentrated vapors may cause erosion of teeth; long-term exposure seldom
occurs due to the corrosive properties of the acid. Persons with preexisting skin disorders or eye disease may be more susceptible to the effects of this substance.
SECTION VIII FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER.
In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating eyelids with fingers. If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult,
give oxygen. If swallowed, wash out mouth with water provided person is conscious. CALL A PHYSICIAN. DO NOT INDUCE VOMITING. If conscious, give
large quantities of milk or water. Never give anything by mouth to an unconscious or convulsing person. Get medical attention immediately.
SECTION IX SPILL OR LEAK PROCEDURES
Cleanup personnel should wear protective clothing and respiratory equipment suitable for toxic or corrosive fluids or vapors. Isolate or enclose the area of the leak
or spill. Small spills: Flush with water and neutralize with alkaline material (soda ash, lime, etc.). Sewer neutralized material with excess water. Larger spills and
lot sizes: Neutralize with alkaline material, pick up with absorbent material (sand, earth, vermiculite). Provide forced ventilation to dissipate fumes. For disposal,
neutralize with alkaline materials (soda ash, lime, etc.). Dispose in a RCRA-approved waste facility or sewer the neutralized slurry with excess water if local ordi-
nances allow. Reportable quantity (RQ) (CWA/CERCLA): 5000 labs. Ensure compliance with federal, state and local regulations.
SECTION X SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the infor-
mation for their particular purposes.

TOC-VCPH/CPN 333
 6.9 Material Safety Data Sheets
6.9.2 Phosphoric Acid

6.9.2 Phosphoric Acid

Shimadzu Scientific Instruments, Inc. 957006

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT NO.: 630-00710-00 CAS NO.: 07664-38-2
NAME: Phosphoric Acid 25% Ultrapure SYNONYM: Phosphoric Acid, IC Reaction Liquid
SECTION II PRDUCT USE
This product is specifically for use in the IC channel of the TOC 500, TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction man-
ual for directions on proper use. Keep tightly sealed in a cool, dry, well ventilated place. Store separate form flammable and combustible materials. Wear appropri-
ate protective clothing and eye protection.
SECTION III PHYSICAL DATA
Melt Point Boil Point Density Vapor Pressure Color Phase Water Solubility
N/A N/A N/A N/A Colorless / Clear Liquid Completly Soluble
SECTION IV HAZARDS IDENTIFICATION
Corrosive, causes burns. Harmful if swallowed. Target organ(s): liver, blood. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Take off immediately all contaminated clothing. Wear suitable protective clothing, gloves and eye/face protection.
SECTION V TOXICITY DATA
UNR-MAN LDLO:220mg/kg ORL-RAT LD50:1530mg/kg
IHL-RAT LC50: >850mg/m3/1h SKN-RBT LD50:2740mg/kg
SECTION VI HEALTH HAZARD DATA
Acute Effects: Harmful if swallowed. May be harmful if inhaled. May be harmful if absorbed through the skin. Material is extremely
destructive to tissue of the mucous membranes and upper respiratory tract, eyes and skin. Inhalation may result in spasm,
inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema. Symptoms of exposure may
include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. May cause
cyanosis.
Chronic Effects: Target organ(s): liver, blood, bone marrow. To the best of our knowledge, the chemical, physical, and toxicological properties
have not been thoroughly investigated.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is diffi-
cult, give oxygen. If swallowed, wash out mouth with water provided person is conscious. Call a physician. Wash contaminated clothing before reuse. Discard con-
taminated shoes.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Carbon dioxide, dry chemical powder or appropriate foam.
SPECIAL FIREFIGHTING PROCEDURES: Wear self-contained breathing apparatus and protective clothing to prevent contact
with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Emits toxic fumes under fire conditions.
SECTION IX ACCIDENTAL RELEASE MEASURES
Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Cover with dry lime or soda ash, pick up, keep in a closed container
and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
INCOMPATIBILITIES: Strong bases, finely powdered metals
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS: Thermal decomposition may produce toxic fumes of phosphorus
oxides and/or phosphine.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

334 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.3 CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime

6.9.3 CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime

Shimadzu Scientific Instruments, Inc. 957003

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-00556-00 CAS NO. 80006-28-8
NAME: Soda Lime OTHER NAME: Soda Lime; Soda and Lime
PRODUCT USE: CO2 Scrubber in Shimadzu TOC Analyzers
SECTION II PRECAUTIONS TO BE TAKEN IN HANDLING
Protect skin, eyes and clothing. Avoid prolonged or repeated exposure. Wash thoroughly after handling. Safety shower and eye bath. Use 8" minimum face shield.
Store as a corrosive. Keep tightly closed and store in a cool, dry, place. Air and moisture sensitive. Use as directed in the TOC-4000 Instruction Manual.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Pressure Vapor Density Evaporation Odor Color Phase Water
Point Point Rate Solubility
N/A N/A N/A N/A N/A N/A N/A White Granules, various sizes N/A
SECTION IV REACTIVITY DATA
Incompatible with strong acids. Absorbs CO2, moisture inactivates.
SECTION V FIRE AND EXPLOSION HAZARD DATA
EXTINGUISHING MEDIA: Dry chemical fire extinguisher. Wear self-contained breathing apparatus and protective clothing to prevent skin and eye
exposure.
UNUSUAL FIRE HAZARD: Emits toxic fumes in a fire.
SECTION VI TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
N/A VX965000 N/A N/A
SECTION VII HEALTH HAZARD DATA
Acute effects: Harmful if swallowed, inhaled, or absorbed through skin. Material is extremely destructive to tissue of the mucous membranes and upper respiratory
tract, eyes and skin. Inhalation may be fatal as a result of spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema.
Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. To the best of our
knowledge, the chemical, physical, and toxicological properties have not been thoroughly investigated.
SECTION VIII FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER.

In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating eyelids with fingers. If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult,
give oxygen. If swallowed, wash out mouth with water provided person is conscious. CALL A PHYSICIAN. Wash contaminated clothing before reuse. Discard
contaminated shoes. For complete information, see actual entry in RTECS #VX965000.
SECTION IX SPILL OR LEAK PROCEDURES
Occupational spill: Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Absorb on sand or vermiculite and place in
closed containers for disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the infor-
mation for their particular purposes.

TOC-VCPH/CPN 335
 6.9 Material Safety Data Sheets
6.9.4 Lithium Hydroxide (monohydrate)

6.9.4 Lithium Hydroxide (monohydrate)

Shimadzu Scientific Instruments, Inc. 957002

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-00961-00 CAS NO. 1310-66-3
NAME: Lithium Hydroxide Anhydride, 99.95%OTHER NAME: Lithium Hydroxide Hydrate, Lithium Hydroxide Anhydride
(DOT,N2680(DOT)
TRADE NAME: IC Absorbent
PRODUCT USE: This product is for specific use with TOC instruments.
SECTION II PRECAUTIONS TO BE TAKEN IN HANDLING
Wear appropriate NIOSH/MSHA-approved respirator, chemical-resistant gloves, safety goggles, other protective clothing. Safety shower and eye bath. Use only in
a chemical fume hood. Face shield, 8-inch minimum. Do not breathe dust. Do not get in eyes, on skin, or on clothing. Avoid prolonged or repeated exposure. Wash
thoroughly after handling. Corrosive, harmful solid. Keep tightly closed. Hygroscopic. Store under nitrogen, in a cool, dry, place.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
N/A N/A 1.510 N/A N/A N/A N/A White Crystals N/A
SECTION IV REACTIVITY DATA
Substance is strongly alkali. In contact with or mixed with acid, reaction is extremely strong. Aluminum and zinc are corroded by this substance and not suitable as
containers. Corrosive effect is enhanced in presence of humidity or water. Absorbs CO2 from air. Containers made of steel, stainless steel, glass, ceramic and many
synthetic compounds are relatively durable. Nature of decomposition products not known.
SECTION V FIRE AND EXPLOSION HAZARD DATA
FIRE: This substance is nonflammable. Use water mist, powdered extinguishing reagents, foam or carbon dioxide gas. Cool container
using water mist, and move container to safe location.
EXPLOSION: Not considered to be an explosion hazard.
EXTINGUISHING MEDIA: Carbon dioxide, dry chemical powder, alcohol or polymer foam. Special Firefighting Procedures: Use full protective clothing
and NIOSH-approved self-contained breathing apparatus with full face piece operated in the pressure demand or other positive
pressure mode.
SECTION VI TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
N/A 0j6307080 Lithium hydroxide, Monohydrate N/A N/A
REVIEWS, STANDARDS, AND REGULATIONS: NOES 1983, HZD X6293000; TNF 60; NIS 6239; NOS 54; TNE 59941; TFE 6243
SECTION VII HEALTH HAZARD DATA
Acute Effects: Harmful if swallowed, inhaled or absorbed through skin. Material is extremely destructive to tissue of the mucous membranes and upper respiratory
tract, eyes and skin. Inhalation may be fatal as a result of spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema.
Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. Uncontrolled move-
ment, muscle spasms, and loss of consciousness may occur. To the best of our knowledge, the chemical, physical and toxicological properties have not been thor-
oughly investigated.
SECTION VIII FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER. In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15
minutes while removing contaminated clothing and shoes. Assure adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh
air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water, provided person is conscious. CALL
A PHYSICIAN. Wash contaminated clothing before reuse, discard contaminated shoes. Additional information: Large doses of lithium ion have caused dizziness
and prostration, and can cause damage if sodium intake is limited. Dehydration, weight loss, dermatological effects and thyroid disturbances have been reported.
Central nervous system effects that include slurred speech, blurred vision, sensory loss, ataxia and convulsions may occur. Diarrhea, vomiting and neuromuscular
effects such as tremor, clonus and hyperactive reflexes may occur as a result of repeated exposure to lithium ion.
SECTION IX SPILL OR LEAK PROCEDURES
Occupational Spill: Evacuate area. Wear protective footwear. Sweep up and place in a bag and hold for waste disposal. Waste Disposal Method: For small quanti-
ties, cautiously add to a large stirred excess of water. Adjust the pH to neutral, separate any insoluble solids or liquids and package them for hazardous-waste dis-
posal. Flush the aqueous solution down the drain with plenty of water. The hydrolysis and neutralization reactions may generate heat and fumes which can be
controlled by the rate of addition. Observe all federal, state and local environmental regulations. Water Contamination: Harmful to marine life. Change in pH will
result in alkaline damage to marine life.
SECTION X SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the infor-
mation for their particular purposes.

336 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.5 Halogen Scrubber

6.9.5 Halogen Scrubber

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-0092-00 CAS NO. 07740-50-8
NAME: Halogen Scrubber OTHER NAME: Copper Wool
PRODUCT USE: This product is for specific use with TOC instruments.
SECTION II PRODUCT USE
For use specifically with the Shimadzu TOC 500, TOC 5,000, and TOC 4,000 instruments. Consult the appropriate instrument manual for proper use.
SECTION III PHYSICAL DATA

Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
1083°C 2595°C N/A N/A N/A N/A N/A Reddish Solid Malleable N/A
Metal
SECTION IV HAZARDS IDENTIFICATION
Dust, mist or fumes may cause eye and skin irritation. Avoid contact.
SECTION V TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
N/A GL5325000 N/A N/A
SECTION VI HEALTH HAZARD DATA
Exposure to large amounts can cause gastrointestinal disturbances, nausea, vomiting, headaches, or dizziness.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. in case of skin contact, immediately wash skin with soap and
copious amounts of water. if ingested and subject is conscious, immediately give large amounts of water. get medical attention.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Appropriate to surrounding fire. Possible formation of toxic copper fumes. Use appropriate respiratory support.
SECTION IX ACCIDENTAL RELEASE MEASURES
N/A
SECTION X STABILITY AND REACTIVITY
INCOMPATIBILITIES: Strong acids, active halogens such as chlorine, fluorine, iodine, and bromine. ammonia.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

TOC-VCPH/CPN 337
 6.9 Material Safety Data Sheets
6.9.6 Quartz Wool

6.9.6 Quartz Wool

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-0557-00 CAS NO. 14808-60-7
NAME: Quartz Wool OTHER NAME: N/A
SECTION II PRODUCT USE
Support for catalyst in reaction tubes of TOC instruments. consult instrument manuals for proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
N/A N/A N/A N/A N/A N/A N/A Grey Fibrous N/A
SECTION IV HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION V TOXICITY DATA
INERT
SECTION VI HEALTH HAZARD DATA
INERT
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. In case of skin contact, immediately wash skin with soap and
copious amounts of water.
SECTION VIII FIRE FIGHTING MEASURES
N/A
SECTION IX ACCIDENTAL RELEASE MEASURES
N/A
SECTION X STABILITY AND REACTIVITY
N/A
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

338 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.7 High Sensitivity Catalyst

6.9.7 High Sensitivity Catalyst

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-00996-00 CAS NO. N/A
NAME: High Sensitivity TC Catalyst OTHER NAME: Platinum on Quartz Wool
SECTION II PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
N/A N/A N/A N/A N/A N/A N/A Grey Fibrous Solid N/A
SECTION IV HAZARDS IDENTIFICATION
FLAMMABLE: Possible sensitizer. Keep away from sources of ignition - NO SMOKING. Take precautionary measures against static
discharges. Keep container tightly closed and in a well-ventilated place.
SECTION V TOXICITY DATA
ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. May cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. Prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing. To the best of our knowledge, the chemical, physical, and toxicological
properties have not been thoroughly investigated.
SECTION VI HEALTH HAZARD DATA
SEE SECTION 5.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. IF
inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided
person is conscious. Call a physician. Remove and wash contaminated clothing promptly.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: CARBON dioxide, dry chemical powder or appropriate foam.
SECTION IX ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves.
Sweep up, place in a bag and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
INCOMPATIBILITIES: Strong oxidizing agents, organic materials.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Nature of decomposition products not known. Hazardous polymerization will not occur.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

TOC-VCPH/CPN 339
 6.9 Material Safety Data Sheets
6.9.8 Normal Sensitivity Catalyst

6.9.8 Normal Sensitivity Catalyst

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 017-42801-00 and 017-42801-01 CAS NO. 7440-06-4(Platinum) and 1344-28-1(Alumina)
NAME: Regular Sensitivity Catalyst OTHER NAME: Platinum on 1/8" Alumina Pellets
SECTION II PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
N/A N/A N/A N/A N/A N/A N/A Grey Solid Pellets N/A
SECTION IV HAZARDS IDENTIFICATION
FLAMMABLE: Possible sensitizer. keep away from sources of ignition - no smoking. Take precautionary measures against static discharges.
Keep container tightly closed and in a well-ventilated place. Harmful by inhalation. Irritating to respiratory system.
TARGET ORGAN(S): Lungs, bones, do not breathe dust. In case of insufficient ventilation, wear suitable respiratory equipment. Wear suitable
protective clothing.
SECTION V TOXICITY DATA

ACUTE EFFECTS: May be harmful by inhalation or ingestion. May cause eye irritation. may cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
EXPOSURE CAN CAUSE: Coughing, chest pains, difficulty in breathing, gastrointestinal disturbances.
CHRONIC EFFECTS: Prolonged exposure can cause damage to the lungs and bones. TO the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
TARGET ORGAN DATA: Lungs, thorax or respiration (tumors) tumorigenic (neoplastic by RTECS criteria) tumorigenic (equivocal tumorigenic agent by
RTECS criteria) tumorigenic (tumors at site of application) only selected registry of toxic effects of chemical substances
(RTECS) data is presented here. see actual entry in RTECS.
SECTION VI HEALTH HAZARD DATA
OSHA PEL: 8H TWA 5MG/ME respirable fraction; 8h TWA 10MG/M3 total dust
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. If inhaled,
remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is
conscious. Call a physician. Remove and wash contaminated clothing promptly. In case of skin contact, immediately wash skin with soap and copious amounts of
water.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Carbon dioxide, dry chemical powder or appropriate foam.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic
hydrochloric acid and phosgene.
SECTION IX ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste dis-
posal. Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
Stability: Stable.
Incompatibilities: Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halocarbons, oxygen difluoride, sodium nitrate, vinyl acetate,
strong oxidizing agents,organic materials. Protect from moisture. Hazardous combustion or decomposition products. Nature of
decomposition products not known. Hazardous polymerization will not occur.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

340 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.9 Potassium Nitrate

6.9.9 Potassium Nitrate

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. CAS NO. 7757-79-1
NAME: Potassium Nitrate OTHER NAME: Nitric Acid, Potassium Salt, Saltpeter
PRODUCT USE: This product is for specific use with TOC instruments.
SECTION II PHYSICAL DATA
Melt Boil Specific Vapor Vapor Evaporation Odor Color Phase Water
Point Point Gravity Pressure Density Rate Solubility
334°C N/A 2.11 N/A 3.0 N/A Odorless White Crystalline Pow- Appreciable
der (>10%)
SECTION III HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION IV HEALTH HAZARD DATA
TARGET ORGANS: Blood, Central Nervous System
SIGNS/SYMPTOMS OF OVEREXP: Chronic exposure can cause anemia, nephritis and methemoglobinemia.
SECTION V FIRST-AID MEASURES
INGESTION: If conscious, induce vomiting and call a physician.
SKIN: Flush with water.
EYES: Flush with water for 15 minutes and call a physician.
SECTION VI FIRE FIGHTING MEASURES
EXTUNGUISHING MEDIA Carbon dioxide, dry chemical, or appropriate foam.
SPECIAL. Use NIOSH/MSHA approved SCBA & full protective equipment. Move containers from fire area if it can be done without
risk. Use water to keep fire exposed containers cool.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS.Strong oxidizer. Contact with other materials may cause fire. When exposed to heat, closed containers may
explode.Emits toxic fumes under fire conditions.
SECTION VII ACCIDENTAL RELEASE MEASURES
Absorb on sand or vermiculite and place in closed containers for disposal. Ventilate area and wash spill site after material pickup is complete. Evacuate the area.
Wear self-contained breathing apparatus, rubber boots, and heavy rubber gloves.
SECTION VIII SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

TOC-VCPH/CPN 341
 6.9 Material Safety Data Sheets
6.9.10 Sodium Bicarbonate

6.9.10 Sodium Bicarbonate

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-00963-01 CAS NO. 144-55-8
NAME: Sodium Bicarbonate 100% OTHER NAME: Baking Soda
SECTION II PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
50°C N/A 2.16 N/A N/A N/A N/A White Solid Powders 10%
SECTION IV HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION V TOXICITY DATA
N/A
SECTION VI HEALTH HAZARD DATA
Exposure to large amounts can cause gastrointestinal disturbances.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. In case of skin contact, immediately wash skin with soap and
copious amounts of water.
SECTION VIII FIRE FIGHTING MEASURES
N/A
SECTION IX ACCIDENTAL RELEASE MEASURES
N/A
SECTION X STABILITY AND REACTIVITY
N/A
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

342 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.11 Sodium Carbonate

6.9.11 Sodium Carbonate

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-0092-01 CAS NO. 497-19-8
NAME: Sodium Carbonate, 100% OTHER NAME: N/A
SECTION II PRDUCT USE
This product is specifically for use in the IC channel of the TOC 500, TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction man-
ual for directions on proper use. Keep tightly sealed in a cool, dry, well ventilated place. Store separate form flammable and combustible materials. Wear appropri-
ate protective clothing and eye protection.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
N/A N/A 2.16 N/A N/A N/A N/A White Solid Powder or Completely
Crystals Soluble
SECTION IV HAZARDS IDENTIFICATION
Corrosive, causes burns, harmful if swallowed. Target organ(s): liver, blood. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Take off all contaminated clothing. Wear suitable protective clothing, gloves and eye/face protection.
SECTION V TOXICITY DATA
ORL-RAT LD50:4090mg/KG,IHL-RAT LC50:2300mg/M3/2H
ORL-MUS LD50:6600mg/KG,IHL-MUS LC50:1200mg/M3/2H
SCU-MUS LD50:2210mg/KG,IHL-GPG LC50:800mg/M3/2H
SECTION VI HEALTH HAZARD DATA
Harmful if swallowed, inhaled, or absorbed through skin.causes severe irritation. High concentrations are extremely destructive to tissues of the mucous mem-
branes and upper respiratory tract, eyes and skin. Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, head-
ache, nausea and vomiting. To the best of our knowledge, the chemical, physical, and toxicological properties have not been thoroughly investigated.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is diffi-
cult, give oxygen. If swallowed, wash out mouth with water provided person is conscious. Call a physician. wash contaminated clothing before reuse. Discard con-
taminated shoes.
SECTION VIII FIRE FIGHTING MEASURES
NONCOMBUSTIBLE. Use extinguishing media appropriate to surrounding fire conditions.
SPECIAL. Wear self-contained breathing apparatus and protective clothing to prevent contact with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS.Emits toxic fumes under fire conditions.
SECTION IX ACCIDENTAL RELEASE MEASURES
Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Wear disposable coveralls and discard them after use. Sweep up,
place in a bag and hold for waste disposal. Avoid raising dust.Ventilate area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
INCOMPATIBILITIES: Strong acids, aluminum, protect from moisture.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Carbon monoxide, carbon dioxide.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

TOC-VCPH/CPN 343
 6.9 Material Safety Data Sheets
6.9.12 Potassium Hydrogen Phthalate

6.9.12 Potassium Hydrogen Phthalate

Shimadzu Scientific Instruments, Inc.

7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:
MATERIAL SAFETY DATA SHEET
SECTION I PRODUCT IDENTIFICATION
CAT. NO. 630-00635-01 CAS NO. 877-24-7
NAME: Potassium Hydrogen Phthalate OTHER NAME: Phthalic Acid, Monopotassium Salt, Khp Primary Standard
SECTION II PRODUCT USE
Specifically for use as an organic carbon standard in the Shimadzu TOC 500, TOC 5,000, and TOC 4,000 instruments. Consult the appropriate instrument manual
for proper use.
SECTION III PHYSICAL DATA
Melt Boil Density Vapor Vapor Evaporation Odor Color Phase Water
Point Point Pressure Density Rate Solubility
295-300°C N/A N/A N/A N/A N/A N/A White Crystals N/A
SECTION IV HAZARDS IDENTIFICATION
Irritant, irritating to eyes, respiratory system and skin. Possible sensitizer. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Wear suitable protective clothing.
SECTION V TOXICITY DATA
RTECS #: CZ4326000
1,2-BENZENEDICARBOXYLIC ACID, MONOPOTASSIUM SALT
ORL-RAT LD50:>3200mg/KG KODAK* 21MAY1971
SKN-GPG LD50:>1 GM/KG KODAK* 21MAY1971
Only selected registry of toxic effects of chemical substances (RTECS) data is presented here. See actual entry in RTECS for complete information.
SECTION VI HEALTH HAZARD DATA
ACUTE EFFECTS: May be harmful by inhalation, ingestion, or skin absorption; causes skin irritation; vapor or mist is irritating to the eyes,
mucous membranes and upper respiratory tract.
EXPOSURE CAN CAUSE ASTHMATIC SYMPTOMS: Cough, hoarseness, rhinorrhea, wheezing, and conjunctivitis, nausea, or vomiting. Prolonged or repeated
exposure may cause allergic reactions in certain sensitive individuals. To the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
SECTION VII FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. If
inhaled, remove to fresh air. if not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided per-
son is conscious. Call a physician. wash contaminated clothing before reuse.
SECTION VIII FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA: Water spray, carbon dioxide, dry chemical powder or appropriate foam.
SPECIAL FIREFIGHTING PROCEDURES: Wear self-contained breathing apparatus and protective clothing to prevent contact with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS:Emits toxic fumes under fire conditions.
SECTION IX ACCIDENTAL RELEASE MEASURES
Wear respirator, chemical safety goggles, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste disposal. Avoid raising dust. Ventilate
area and wash spill site after material pickup is complete.
SECTION X STABILITY AND REACTIVITY
STABILITY: Stable.
INCOMPATIBILITIES: Strong oxidizing agent
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Toxic fumes of carbon monoxide, carbon dioxide
HAZARDOUS POLYMERIZATION:Will NOT occur.
SECTION XI SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

344 TOC-VCPH/CPN
 6.9 Material Safety Data Sheets
6.9.13 Water

6.9.13 Water
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046 Control No.
Tel: 1(800) 477-1227 Date:

MATERIAL SAFETY DATA SHEET

SECTION I PRODUCT IDENTIFICATION
CAT. NO. CAS NO. 7732-18-5
NAME: Water OTHER NAME: Dihydrogen Oxide
MOLECULAR WEIGHT: 18 CHEMICAL FORMULA:H2O
SECTION I HAZARDS IDENTIFICATION
EMERGENCY OVERVIEW: Not applicable.
HEALTH RATING: 0 - None FLAMMABILITY RATING: 0 - None
REACTIVITY RATING: 1 - Slight CONTACT RATING: 0 - None
LAB PROTECTIVE EQUIP: Goggles; lab coat STORAGE COLOR CODE: Orange (General Storage)
SECTION II HEALTH EFFECTS
POTENTIAL HEALTH EFFECTS: Water is non-hazardous.
INHALATION: Not applicable. INGESTION: Not applicable.
SKIN CONTACT Not applicable. EYE CONTACT: Not applicable.
CHRONIC EXPOSURE: Not applicable. AGGRAVATION OF PRE-EXISTING CONDITIONS: Not applicable.
SECTION III FIRST AID MEASURES
INHALATION: Not applicable. INGESTION: Not applicable.
SKIN CONTACT: Not applicable. EYE CONTACT: Not applicable.
SECTION IV FIRE FIGHTING MEASURES
FIRE: Not applicable. EXPLOSION: Not applicable.
FIRE EXTINGUISHING MEDIA: Use extinguishing media appropriate for surrounding fire.
SPECIAL INFORMATION: In the event of a fire, wear full protective clothing and NIOSH-approved self-contained breathing apparatus with full facepiece
operated in the pressure demand or other positive pressure mode.
SECTION V ACCIDENTAL RELEASE MEASURES
Non-hazardous material. Clean up of spills requires no special equipment or procedures.
SECTION VI HANDLING AND STORAGE
Keep container tightly closed. Suitable for any general chemical storage area. Protect from freezing. Water is considered a non-regulated product, but may react
vigorously with some specific materials. Avoid contact with all materials until investigation shows substance is compatible.
SECTION VII EXPOSURE CONTROLS/PERSONAL PROTECTION
AIRBORNE EXPOSURE LIMITS: Not applicable. VENTILATION SYSTEM: Not applicable.
PERSONAL RESPIRATORS (NIOSH APPROVED): Not applicable.
SKIN PROTECTION: None required. EYE PROTECTION: None required.
SECTION VIII PHYSICAL AND CHEMICAL PROPERTIES
Melt Boil Specific Vapor Vapor Evaporation pH Color Phase Water
Point Point Gravity Pressure Density Rate Solubility
0°C 100°C 1.00 17.5 @ 20°C N/A N/A 7.0 Clear, Liquid Complete
Colorless
SECTION IX STABILITY AND REACTIVITY
STABILITY: Stable under ordinary conditions of use and storage.
HAZARDOUS DECOMPOSITION PRODUCTS: Not applicable.
HAZARDOUS POLYMERIZATION: Will not occur.
INCOMPATIBILITIES: Strong reducing agents, acid chlorides, phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride.
SECTION X ECOLOGICAL INFORMATION
ENVIRONMENTAL FATE: Not applicable.
ENVIRONMENTAL TOXICITY: Not applicable.
SECTION XI DISPOSAL CONSIDERATIONS
Whatever cannot be saved for recovery or recycling should be flushed to sewer. If material becomes contaminated during use, dispose of accordingly. Dispose
of container and unused contents in accordance with federal, state and local requirements.
SECTION XII TRANSPORT INFORMATION
Not regulated.
SECTION XIII OTHER INFORMATION
NFPA RATINGS: Health: 0 Flammability: 0 Reactivity: 0
LABEL HAZARD WARNING: Not applicable.
LABEL PRECAUTIONS: Keep in tightly closed container.
LABEL FIRST AID: Not applicable.
PRODUCT USE: Laboratory Reagent.
SECTION XIV SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.

TOC-VCPH/CPN 345
 6.9 Material Safety Data Sheets
6.9.13 Water

346 TOC-VCPH/CPN
 Appendix A
Appendix A Method Validation
The Method Validation function tests the variance and the linearity of the data. The
function also determines performance characteristics according to the requirements of DIN
38402-Part 51. The Method Validation function displays the data used for executing
method validation, performs the required calculations and displays the results. Data can
either be imported directly from the TOC-Control V Sample Table, or entered manually
into the data table. Data can also be exported to ASCII files, stored and printed.
 Method Validation
Main Window

A.1 Main Window

The Main Window is separated into three sections. The upper left section of the window
displays the calibration curve, the upper right section displays the calculated validation
results and the lower portion displays the data table, which contains all relevant data for
performing the validation. The toolbar options (such as Open, Save, Cut, Copy, and Paste)
are similar to those described in Section 4.4.2 "File Menu" and Section 4.4.3 "Edit Menu".

Figure A.1 Method Validation Main Window

The windows can be resized by dragging the dividers between the sections.

348 TOC-VCPH/CPN
 Method Validation
File Menu

A.2 File Menu

Figure A.2 File Menu

A.2.1 New
Use the New command to create a new, empty method validation file. A new file can also
be created by clicking the New toolbar button. If a file that contains modified and unsaved
data is open when the New command is selected, a prompt is displayed in a dialog box.
Select one of the options in the dialog box to determine if the unsaved data should be saved
before opening a new method validation file. Click the Yes button to save the document and
create a new method validation file. Click the No button to create a new document without
saving previous data.

Figure A.3 Prompt for Saving Data

TOC-VCPH/CPN 349
 Method Validation
File Menu

A.2.2 Open
Use the Open command to open a saved method validation file (*.val). A file can also be
opened by clicking the Open toolbar button.
Start the method validation process by selecting a.cal file; application of DIN 38402 will
begin. The process can also be started by selecting the calibration curve row in the Sample
Table and opening the method validation function using the Tools>Method Validation
command.

Figure A.4 Open Dialog Box

When the Open command is selected, the File>Open dialog box is displayed. To open an
existing file, select the filename and choose the Open button. To create a new method
validation file, type the filename into the File name text field, then select the New button.
For further information on the standard functions of the Open dialog box, refer to Section
4.4.2.4 "Open".
Note: An error message is displayed if a file that is not in a correct, TOC-Control V for-
mat is selected.

350 TOC-VCPH/CPN
 Method Validation
File Menu

A.2.3 Save
Use the Save command to save data in the current active file. If the file has not been saved,
selecting the Save command opens the Save As dialog box. The Save command can also be
executed by clicking the Save toolbar button.

A.2.4 Save As

Figure A.5 Save As Dialog Box

The Save As command saves the active, current data to a new file name. Enter the desired
name in the File Name field. Two different file types are available: validation files (*.val)
used for storing the data in binary files and ASCII files (*.txt) used for exporting the data.
Select the desired file type from the Save As Type drop-down list. Use the Save In window
to select the location where the file should be saved. For details about the Save As
command, refer to Section 4.4.2.7 "Save As".

A.2.5 Print
Use the Print command to print data from a method validation file. Executing the Print
command opens the Print dialog box; displayed options vary based on the installed printer
driver. The Print command can also be executed by clicking the Print toolbar button.

Figure A.6 Print Dialog Box

Use the Print Range option to specify the range to be printed. The All selection prints all
pages in the file. Specific pages can be printed by selecting the Pages option and entering
the desired page numbers. Use the Number of Copies field to select the number of copies to
be printed.

TOC-VCPH/CPN 351
 Method Validation
File Menu

A.2.6 Print Preview

Use the Print Preview command to view the method validation file before printing.

Figure A.7 Print Preview Window

Button Description
Next Page and Previous Page Click the Next Page button to display the next page of the
report. Click the Previous page button to display the previous
page of the report. The Next Page button is disabled when the
last page of the report is displayed, and the Previous Page
button is disabled when the first page of the report is dis-
played.
One Page/Two Page Click the One Page button to display one page at a time in the
Print Preview window. After selection, the button toggles to
the Two Page button. Click the Two Page button to display
two pages side by side.
Zoom In and Zoom Out Click the Zoom In and Zoom Out buttons to change the mag-
nification of the displayed pages. Three different zoom fac-
tors are available. Repeated selection of either option will
continue to increase or decrease the magnification, as appli-
cable.
Close Click the Close button to close the Print Preview window and
return to the previous window.The Print Preview window
must be closed to edit the report.
Print Click the Print button to print the report.

352 TOC-VCPH/CPN
 Method Validation
File Menu

A.2.7 Print Setup

Select Print Setup to open the Print Setup dialog box.

Figure A.8 Print Setup Dialog Box

The print options available vary based on the printer installed. Select the paper size and
source from the drop-down lists, and select Portrait or Landscape to change the orientation
of the printed pages. Click the OK button to save the selections, or click the Cancel button
to close the dialog box without saving changes.

A.2.8 Page Setup

Use the Page Setup command to select items to be printed and to select options for printing
format, such as margins, headers, and footers.

Figure A.9 Page Setup Window: Data Tab

The Page Setup window consists of several tabs. Use the OK button to save changes and
exit the Page Setup window. Click the Cancel button to exit the Page Setup window without
saving changes. Click the Apply button to update the parameters without closing the Page
Setup window.
Note: On each tab in the Page Setup window, certain items are checked (selected) by
default. To deselect these options, click the item.

TOC-VCPH/CPN 353
 Method Validation
File Menu

Data Tab
The Data tab displays a list of items that can be selected for printing. Select the desired
items and click the OK button.

Grid Tab

Figure A.10 Page Setup Window: Grid Tab

The Grid tab displays a list of format items for the report, as described below.
Option Description
Row Headers Prints row headers in the table.
Column Headers Prints column headers in the table.
Print Frame Prints a frame around the table.
Vertical Lines Prints vertical lines in the table.
Horizontal Lines Prints horizontal lines in the table.
Only Black and White Prints only in 2 colors, without gray backgrounds or other
colors.
First Rows, then Columns Prints rows first, followed by columns, when more than one
page is printed
First Columns, then Rows Prints columns first, followed by rows, when more than one
page is printed.
Vertical Prints the table on the vertical center of the page.
Horizontal Prints the table on the horizontal center of the page.

354 TOC-VCPH/CPN
 Method Validation
File Menu

Miscellaneous Tab

Figure A.11 Page Setup Window: Miscellaneous Tab

The Miscellaneous tab displays a list of format items for the report, as described below.
Setting Item Description
Margins Use the spin controls to enter the page margins (in mm.).
Footer, Page No. Select this option to print the page number in the footer of
each page.
Header Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
Operator: Select this option to print the current user name in
the page header.

A.2.9 Exit
Select Exit to close the Method Validation application. If an active file contains unsaved
information, a prompt to save changes is displayed. Select Yes or No, or select Cancel to
abort the exit function.

Figure A.12 Prompt to Save Data Changes

TOC-VCPH/CPN 355
 Method Validation
Edit Menu

A.3 Edit Menu

Options such as Cut, Copy, and Paste are available only if content is selected.

Figure A.13 Edit Menu

A.3.1 Undo
Use the Undo function to reverse the last change made in the data table. This function is
available only in documents that can be manually edited and when the user changes the
content of a cell in the data table.

A.3.2 Cut/Copy/Paste
Use the Cut, Copy, and Paste commands to edit highlighted table cells and rows. The Cut
command deletes information in rows or cells and stores it on the clipboard. The Copy
command copies data from rows or cells to the clipboard. The Paste command copies the
contents of the clipboard to the current row of the table. When pasting a whole row, select
the entire destination row first by clicking the row number.
Note: Do not select a row for pasting that currently contains data. The data will be over-
written!

TIP » The Cut, Copy and Paste commands have shortcut buttons on the toolbar.

A.3.3 Insert Row

Use the Insert Row command to add an additional row to the data table. This command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of rows equivalent to the number of calibration
points in the calibration curve.

356 TOC-VCPH/CPN
 Method Validation
Edit Menu

A.3.4 Delete Row

Use the Delete Row command to delete a row from the data table. The command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of rows equivalent to the number of calibration
points in the calibration curve. The Delete Row function is not available if the number of
rows is 4 or less. Once a row is deleted, the format of the remaining rows is updated. A
confirmation dialog box opens asking you to confirm the deletion.

Figure A.14 Delete Row Confirmation Dialog Box

A.3.5 Insert Column

Use the Insert Column command to add an additional column to the data table. The
command is available only for documents that can be manually edited. TOC-Control V
method validation documents have a fixed number of columns equivalent to the maximum
number of injections specified for the calibration points.

A.3.6 Delete Column

Use the Delete Column function to delete a column from the data table. The command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of columns equivalent to the maximum number
of injections specified for the calibration points. The Delete Column function is not
available if the number of columns is 3 or less. Once a column is deleted, the format of the
remaining columns is updated. A confirmation dialog box opens asking you to confirm the
deletion.

A.3.7 Recalculate
Use the Recalculate command to recalculate all method validation data. The results and
calibration curve sections of the Method Validation window are also updated when the
Recalculate command is selected. Errors that occur during the recalculation process are
displayed in message boxes. For example, an error message may be displayed if the data in
the table does not contain sufficient information, if there are not enough data points defined
in the table, if less than 3 injections are available, and if numeric data is incorrect and
results in an illegal mathematical operation (such as division by zero).

TIP » The Recalculate command has a shortcut button on the toolbar.

TOC-VCPH/CPN 357
 Method Validation
View Menu

A.4 View Menu

Figure A.15 View Menu

Toolbar
The Toolbar function displays or hides the toolbar.

Status Bar
The Status Bar function displays or hides the status bar.

358 TOC-VCPH/CPN
 Method Validation
Options Menu

A.5 Options Menu

Figure A.16 Options Menu

A.5.1 General Parameter

Select the General Parameter command to display the General Information dialog box.

Figure A.17 General Information Dialog Box

The General Information dialog box is used to view and edit information about the method
validation file, such as the system used to create the file, the file version, the operator who
created the file and the date on which the file was created. Some information fields may be
disabled. Comments about the file are displayed in the Comment field.

TOC-VCPH/CPN 359
 Method Validation
Options Menu

A.5.2 Method Validation Parameter

The Method Validation Parameter command displays the Method Validation Parameter
window, which contains detailed information about the method, as described below.

Figure A.18 Method Validation Parameter Window

Item Description
Enable manual editing Select to allow data tables to be edited manually. This option
is disabled for files linked to TOC-Control V calibration
curves. If this option is deselected, it is disabled and cannot
be selected again. This option is selected by default.
Unit Displays the calibration curve units. This option is disabled if
the Enable manual editing option is not selected.
Analysis Type Displays the analysis used to create the calibration curve.
This option is disabled if the Enable manual editing option is
not selected.
Date/Time Displays the date and time the file was created.
Title Displays the title of the method validation file.
Calibration curve file name Displays the name of the TOC-Control V calibration curve.

360 TOC-VCPH/CPN
 Method Validation
Options Menu

A.5.3 Font
Use the Font command to select fonts for printed reports and display screens. Selecting the
Font command opens the Font dialog box.

TIP » The Font command has a shortcut button on the toolbar.

Figure A.19 Font Dialog Box

Choose a font for printed reports by selecting options from the Font, Font Style, Size, Color
and Script drop-down lists. A preview of the font appearance is visible in the Sample field
on the lower portion of the Font dialog box.

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 Method Validation
Options Menu

A.5.4 Floating Point Numbering Format

Use the Floating Point Numbering Format command to select display options for numeric
results in the method validation tables. These options apply only to the manner in which
numbers are displayed; internal data retain their original values.

Figure A.20 Floating Point Format Window

Common Floating Point Numbers

Setting Item Description
Number of significant digits Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the Select this option to display common floating point numbers
decimal point using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the deci-
mal point. The default value is 2.

Percent Values
Setting Item Description
Number of significant digits Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the Select this option to display percent values using a specified
decimal point number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.

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 Method Validation
Options Menu

A.5.5 ASCII Export Options

Use the ASCII Export Options function to export method validation data to an ASCII file.

Figure A.21 ASCII Export Options Dialog Box

Setting Item Description

Header Select this option to export method validation file header.
Data Select this option to export method validation data.
Results Select this option to export method validation results.
Separator Select the type of separator to be used between items in the
ASCII file.
Export strings in quotation Select this option to add quotation marks to all exported
marks strings.

To export a file, create or open a method validation file. Select the desired options from the
ASCII Export Options dialog box and select OK. The File>Save As dialog box is
displayed. Enter a file name for the ASCII file and select the *.txt file type.

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 Method Validation
Options Menu

A.5.6 Validation Strictly Following DIN38402

Use the Validation Strictly Following DIN38402 option to conduct the validation
calculation by DIN 38402 requirements; that is, only the area obtained from the first
injection of every standard is used in the calibration calculation. When this option is not
selected, the mean value of the area counts from all injections of each standard is used in
the calibration calculation.
Perform method validation according to DIN regulations as follows:
Step 1 Select the estimated working range.
Step 2 Prepare 10 calibration standards, with concentrations distributed uniformly
over the complete working range.
Step 3 Create a Sample Table, with 10 injections of the highest and lowest standard
concentrations and a single injection for all other standards. If more than one
injection is made of the intermediate standards, the linearity test is calculated
with the results of the first replicates only.
Step 4 Analyze the standards. The results are saved in a.cal file.
Step 5 Select Method Validation from the Tools menu in the Sample Table Editor.
The Method Validation main window is displayed.
Step 6 Select the Validation Strictly Following DIN from the Options menu.
Step 7 Select Open from the File menu.
Step 8 Select.cal from the file type drop-down list.
Step 9 From the list of file names, select the.cal file where the measurement data was
saved. Then select OK.
Step 10 The calculations are automatically performed, and the validation data
displayed.
Step 11 Select Save from the File menu, assign a file name in the dialog box, and
select OK. The validation data is saved with a.val file name extension.
When the Validation Strictly Following DIN option is enabled, a check mark is displayed in
front of the menu item. After selecting this option, a confirmation message is displayed.

Figure A.22 Confirmation Message for Validation Strictly Following DIN 38402

Select Yes to execute recalculation. The calibration curve and result sections of the Method
Validation window are updated accordingly.

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 Method Validation
Help Menu

A.6 Help Menu

About Meth Val...

Use the About command to view copyright and version information.

TOC-VCPH/CPN 365
 Method Validation
Help Menu

366 TOC-VCPH/CPN
 Appendix B
Appendix B Control Charts
The Control Charts software monitors precision and accuracy of a defined data set. The
software supports five types of Control Charts:
•Mean Value Control Charts
•Recovery Control Charts
•Blind Value Control Charts
•Spanwidth Control Charts
•User Defined Control Charts
The Mean Value Control Chart checks the accuracy of an analytical method on an
instrument. Control value drifts may indicate a change in system performance.
The Recovery Control Chart tests an analytical method for matrix influences and provides a
restrictive control of accuracy by testing proportional system errors. Using certified
standards will test the accuracy of the system as well as the recovery rate.
The Blind Value Control Chart is a special form of the Mean Value Control Chart used for
quality assurance of the instrument and variable elements. Unlike the Mean Value Control
Chart, the control value is the information value (absorbance, peak height, peak area)
received from the analysis.
The Spanwidth Control Chart tests the precision of an analytical method and monitors the
accuracy under actual conditions (Drift Control). For this type of Control Chart, there are
several existing models for calculating the control and warning limits.
Each type of control chart can be used to create charts for different working range and
analysis methods. For each control chart, a file is created which contains general
information about the type, data structure and other global data.
 Control Charts
File Menu

B.1 File Menu

Figure B.1 File Menu

B.1.1 New
The New function is used to define new control charts and displays the Control Chart
Wizard. Follow the Control Chart Wizard process to enter a new control chart. The file
extension *.cc is used for all control charts.
Note: Control Chart parameters can be changed at a later time by selecting
Options>Control chart options from the main menu bar.

Control Chart Wizard System Information Window

The first page of the Control Chart Wizard is used to enter basic system information and is
similar to the System Information pages in the Method and Sample Wizards. Refer to
Section 4.4.5.2 "Sample" and Section 4.4.2.3 "Method Wizard".

Figure B.2 Control Chart Wizard: System Information Window

368 TOC-VCPH/CPN
 Control Charts
File Menu

Control Chart Wizard Control Chart Type Window

Select the type of control chart to be created and select the analysis type from the drop
down list.

Figure B.3 Control Chart Wizard: Control Chart Type Window

Control Chart Wizard Control Chart Parameters Window

Enter the control chart parameter values and limits as described below.

Figure B.4 Control Chart Wizard: Control Chart Parameters Window

Setting Item Description

Automatic calculation of the Select to enable automatic calculation of the control chart
control chart limits limits. The upper and lower warning and control limits are
calculated after the control samples for the preparation period
are added to the control chart.
No. of samples in the pre- Enter the number of samples in the preparation period. The
period default value is 12. This option is disabled if the Automatic
calculation of the control chart limits option is not selected.
No. of samples in the control Enter the number of samples in the control period. The
period default value is 50.

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 Control Charts
File Menu

Setting Item Description

Working range Enter the upper and lower limits of the working range. Match
the range with the concentration of samples used for control
tracking and the concentration range of the selected calibra-
tion curve. Use the drop-down list to select the units.
Rated Value Enter the rated value of the working range. This option is dis-
abled if the Automatic calculation of the control chart limits
option is not selected.
Control Limits Enter the upper and lower control limits. This option is dis-
abled if the Automatic calculation of the control chart limits
option is not selected.
Warning Limits Enter the upper and lower warning limits. This option is dis-
abled if the Automatic calculation of the control chart limits
option is not selected.
Exclusion Limits Enter the upper and lower exclusion limits.

Control Chart Wizard Recovery Control Chart Parameter Window

This window is only displayed if the Recovery Control Chart is selected in the Control
Chart Wizard, and Automatic calculation of the control chart limits is not selected.

Figure B.5 Control Chart Wizard: Recovery Control Chart Parameter Window

Setting Item Description

Use of certified standard Select this option to use a certified sample as a control sam-
ple.
Fixed theoretical concentra- Select this option if the standard has a fixed concentration.
tion Enter the concentration in the text box.
Use of real sample Select this option if the control sample is a real sample.
Fixed concentration of the Select this option if the spiked component has a fixed con-
spiked component. centration. Enter the concentration in the text box.

370 TOC-VCPH/CPN
 Control Charts
File Menu

Control Chart Wizard Spanwidth Control Chart Options Window

This window is only displayed if the Spanwidth Control Chart is selected in the Control
Chart Wizard.

Figure B.6 Control Chart Wizard: Spanwidth Control Chart Options Window

Setting Item Description

No. of inj. per sample Enter the number of injections for a sample used in the con-
trol chart. The default value is 3, and the range is 3-25.
Refuse control samples with Select this option to exclude from the control chart samples
different inj. no whose number of injections differs from those specified in
the No. of inj. per sample field.

TOC-VCPH/CPN 371
 Control Charts
File Menu

Control Chart Wizard History Window

The Control Chart Wizard History function is identical to other history functions in the
TOC-Control V system. Refer to Section 4.4.2.3 "Method Wizard" for more details about
the History function. The History window provides information on all control chart
changes when enabled.

Figure B.7 Control Chart Wizard: History Window

Setting Item Description

Enable history log Select this option to enable the History Log, which is used to
monitor all modifications to the control charts. Once the His-
tory Log is enabled, it cannot be turned off.
Operator has to comment on Select this option to require the user to enter comments or
all modifications obtain approval for modifications to the control charts.

B.1.2 Following Control Chart

Select the Following Control Chart menu item to create a Following Control Chart. It is
recommended that a new control chart be created after 50 samples have been entered in the
control period. The new control chart uses the calculated standard deviation from the
control period as the new control chart limits. Control chart options are:
Setting Item Description
File Name Displays the name of the currently active control chart.
Save the current control chart Enter a new file name in this field to save the currently active
as control chart to a new location or with a new file name. A
confirmation message is displayed to confirm the operation.
Create Select this option to create the Following Control Chart. The
new limits are calculated from the samples of the control
period stored in the previous control chart.
Parameter Select this option to display the parameters of the newly cre-
ated Following Control Chart. This function can also be
accessed using the Options>Control Chart Options command
in the main window.

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 Control Charts
File Menu

B.1.3 Open
The Open command is used to open files. Select a *.cc file to open a control chart file.
Refer to Section 4.4.2.4 "Open" for further information on the standard File>Open dialog
box.

B.1.4 Save
The Save command saves the current control chart.

B.1.5 Save As
Use the Save As command to save files for the first time, or to save a file using a new file
name. Files can be saved as file types *.cc or *.txt (ASCII format). For more information
on the Save As function, refer to Section 4.4.2.7 "Save As".

B.1.6 Print>Data
Use the Print>Data command to print data in spreadsheet format. For more information on
the Print function, refer to Section 4.4.2.10 "Print>Table".

B.1.7 Print>Graph
Use the Print>Graph command to print data in graphical format. For more information on
the Print function, refer to Section 4.4.2.10 "Print>Table".

B.1.8 Print Preview>Data/Print Preview>Graph

Use the Print Preview>Data function to display a preview of the data to be printed. Use the
Print Preview>Graph function to display a preview of the graph to be printed. For more
information on the Print Preview function, refer to Section 4.4.2.12 "Print Preview>Table".

TOC-VCPH/CPN 373
 Control Charts
File Menu

B.1.9 Print Setup

Use the Print Setup command to select the printing parameters.

Figure B.8 Print Setup Dialog Box

The print options available vary based on the printer installed. Select the paper size and
source from the drop-down lists, and select Portrait or Landscape to change the orientation
of the printed file. Select OK to save the selections, or Cancel to close the dialog box
without saving changes.

B.1.10 Page Setup

Use the Page Setup command to select items to be printed and to select options for printing
format, such as margins, headers, and footers.

Figure B.9 Page Setup Window: Data Tab

The Page Setup window consists of several tabs. Use the OK button to save changes and
exit the Page Setup window. Click the Cancel button to exit the Page Setup window without
saving changes. Click the Apply button to update the parameters without closing the Page
Setup window.
Note: On each tab in the Page Setup window, certain items are checked (selected) by
default. To deselect these options, click the item.

374 TOC-VCPH/CPN
 Control Charts
File Menu

Data Tab
The Data tab displays a list of items that can be selected for printing. Select the desired
items and click the OK button.

Grid Tab

Figure B.10 Page Setup Window: Grid Tab

The Grid tab displays a list of format items for the report.
Option Description
Row Headers Prints row headers in the table.
Column Headers Prints column headers in the table.
Print Frame Prints a frame around the table.
Vertical Lines Prints vertical lines in the table.
Horizontal Lines Prints horizontal lines in the table.
Only Black and White Prints only in 2 colors, without gray backgrounds or other
colors.
First Rows, then Columns Prints rows first, followed by columns, when more than one
page is printed
First Columns, then Rows Prints columns first, followed by rows, when more than one
page is printed.
Vertical Prints the table on the vertical center of the page.
Horizontal Prints the table on the horizontal center of the page.

TOC-VCPH/CPN 375
 Control Charts
File Menu

Miscellaneous Tab

Figure B.11 Page Setup Window: Miscellaneous Tab

The Miscellaneous tab displays a list of format items for the report, as described below.
Setting Item Description
Margins Use the spin controls to enter the page margins (in mm).
Footer, Page No. Select this option to print the page number in the footer of
each page.
Header Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
Operator: Select this option to print the current user name in
the page header.

B.1.11 Exit
Select Exit to close the Control Chart application.

376 TOC-VCPH/CPN
 Control Charts
Edit Menu

B.2 Edit Menu

Figure B.12 Edit Menu

Copy
Use the Copy command to copy the selected range from the data table to the clipboard.

Recalculate
Use the Recalculate command to recalculate the limits of the control chart. This function
should be performed after one or more control samples have been excluded or added to the
control chart.

Exclude
Use the Exclude command to exclude a selected range of control samples from the control
chart calculations. When Exclude is selected, the Exclude dialog box is displayed. Enter a
comment describing the reason for excluding the sample. The Exclude function is only
available when one or more control samples are selected. A dialog box displays a message
requesting confirmation that the sample be excluded. Select Yes to confirm and recalculate
the control limits, or No to abort recalculation.

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 Control Charts
View Menu

B.3 View Menu

Figure B.13 View Menu

B.3.1 Statistics
The Statistics command displays the Statistics window.

Figure B.14 Statistics Window

Setting Item Description

Type Displays the type of control chart.
No. of samples (pre-period) Displays the number of samples in the preparation period.
This value was entered in the Control Chart Wizard.
Total no. of samples Displays the total number of samples in the control chart.
Excluded samples are not included in the total number.
Control limits Displays the control limits.
Data from the control period Displays the Average Control Value, which is the mean value
of the samples in the control period. Also displays the calcu-
lated standard deviation and coefficient of variation.

378 TOC-VCPH/CPN
 Control Charts
View Menu

B.3.2 Comparison
After a control chart is completed, the results from the control period must be compared
with the results from the preparation period. For control charts without a preparation
period, the current values must be compared with the results of the preparation period or the
control period from the previous control chart. The View>Comparison command displays
the Comparison between control charts window.

Figure B.15 Comparison Between Control Charts Window

Setting Item Description

Previous control chart Displays the file name of the previous control chart, if appli-
cable.
Mean value t-test Displays the results of the T-test in the text box beneath the
Item and Value lists. The T-table value and the calculated test
value are also displayed in the Item and Value list. The test
value is calculated based on the mean values and variances
obtained from the control and preparation period. The T-test
result shows whether the long term deviation of the control
samples is significant.
F-test Displays the results of the F-test in the text box beneath the
Item and Value list. The F-table value and the calculated test
value are also displayed in the Item and Value list.

TOC-VCPH/CPN 379
 Control Charts
View Menu

B.3.3 Out of Control Events

The Out of Control Events window displays a list of all out of control events.

Figure B.16 Out of Control Events Window

Spl. No.
Displays the sample number for which the out of control event occurred.

Event
Describes the out of control event.

B.3.4 Toolbar/Status Bar

The View>Toolbar and View>Status Bar commands show and hide the Toolbar and Status
Bar, respectively.

380 TOC-VCPH/CPN
 Control Charts
Options Menu

B.4 Options Menu

Figure B.17 Options Menu

B.4.1 Control Chart Options

Use the Control Chart Options command to view and edit the control chart parameters
entered in the various pages of the Control Chart Wizard. Refer to Section B.1.1 "New".
Note: Some options within the Control Chart Options tabs (such as control chart type or
sample concentrations) may be disabled if the control chart contains data. The
disabled parameters are options that cannot be modified once data is entered.

B.4.2 Font
The Font command opens the standard Font dialog box. Refer to Section 4.4.9.3 "Display
Settings>Display Font" for detailed information about font options.

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 Control Charts
Options Menu

B.4.3 Floating Point Numbering Format

The Floating Point Numbering Format command is used to select display options for
numeric results in the control charts. These options apply only to the manner in which
numbers are displayed; internal data retain their original values.

Figure B.18 Floating Point Format Window

Common Floating Point Numbers

Setting Item Description
Number of significant digits Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the Select this option to display common floating point numbers
decimal point using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the deci-
mal point. The default value is 2.

Percent Values
Setting Item Description
Number of significant digits Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the Select this option to display percent values using a specified
decimal point number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.

382 TOC-VCPH/CPN
 Control Charts
Options Menu

B.4.4 ASCII Export Options

The ASCII Export Options function is used to export control chart data to an ASCII-
formatted file.

Figure B.19 ASCII Export Options Dialog Box

Setting Item Description

Header Select this option to export control chart file header.
Data Select this option to export control chart data.
Limits Select this option to export control chart limits.
Separator Select the type of separator to be used between items in the
ASCII file.
Export strings in quotation Select this option to add quotation marks to all exported
marks strings.

To export a file, create or open a control chart. Select the desired options from the ASCII
Export Options dialog box, and select OK. The File>Save As dialog box is displayed. Enter
a file name for the ASCII file and select the *.txt file type.

B.4.5 Enable Exclusion

Use the Enable Exclusion command to exclude a selected range of control samples from
the control chart calculations. When the Enable Exclusion command is executed, the
Exclude dialog box is displayed. Enter a comment describing the reason for excluding the
sample. This option is only available when one or more control samples are selected. A
dialog box displays a message requesting confirmation that the sample be excluded. Select
Yes to confirm and recalculate the control limits, or No to abort the process.

TOC-VCPH/CPN 383
 Control Charts
Help Menu

B.5 Help Menu

About ContrCharts...
Use the About command to view copyright and version information.

384 TOC-VCPH/CPN
 Index
Numerics
8-Port Sampler Installation .......................................................325
Analysis Using ...................................................80 Maintenance............................................ 254–255
Connecting Two Units .....................................326 Rear View .......................................................... 15
Connection .......................................................327 Sealing the Sample Containers ..........................80
Front View .........................................................15 8-Port Valve
High Sensitivity..................................................82 Replacing Rotor (8-Port Sampler) ...................254
Initializing ........................................................267 Replacing Rotor (Syringe Pump).....................246

A
Accessories...................................................... 298–303 Application Operations ................................... 219–233
Special..............................................................303 ASCII Export Options
Standard ...........................................................298 Data Tab...........................................................147
Acid Header Tab.......................................................146
Addition in NPOC..................................... 76, 189 Miscellaneous Tab ...........................................148
Addition Volume..............................................139 System Tab ......................................................147
Checking Volume ............................................236 ASCII File, Exporting Control Charts .....................383
Effect on Instrument...........................................71 ASI-V, See Autosampler
Hydrochloric ....................................................333 Auto Dilution ..........................................132, 139, 189
Phosphoric........................................................334 Auto Generate ..........................................................181
Preparation .........................................................51 Auto Regeneration of IC Solution ............................. 27
Add Event Log ...........................................................22 Auto Restart .............................................................121
Administration .................................................... 19–33 Autosampler.............................................................295
Air, Low Pressure Safety .........................................331 Cables, Connecting ................................. 318, 319
Alkaline Samples .......................................................71 Cover Installation.............................................323
Analysis Drain Tank Installation .................................... 323
Blank Check.......................................................66 Front View .........................................................14
Calibration Parameters.....................................128 High Sensitivity Analysis ..................................75
Calibration Run ................................................100 Initializing........................................................ 267
Control Sample Parameters..............................196 Installation .......................................................317
Creating New Method......................................135 Maintenance............................................ 252–253
Ending ..............................................................120 Needle Change.................................................268
Gas Sample ......................................................227 Needle Types .............................................. 28, 85
Group Of Samples............................................181 Needle, Coaxial................................................322
High Sensitivity..................................................75 Needle, Sample ................................................321
IC........................................................................56 NPOC Analysis..................................................76
Individual Sample ............................................185 Positioning .......................................................317
Manual Injection ..............................................219 Rear View .......................................................... 14
Method Parameters ..........................................136 Rinse Bottle Inspection.................................... 252
New ..................................................................125 Rinse Bottle Installation...................................323
New Catalyst ......................................................36 Rinse Pump Head Replacement.......................253
POC....................................................................58 Sample Catcher Inspection ..............................252
Preparation .................................................. 36–82 Shipping Screw ................................................317
Principles................................................. 284–288 Software Settings ........................................ 28, 84
Procedures................................................. 89–121 Specifications...................................................295
Sample Parameters...........................................186 Tray Type...........................................................28
Sample Run ......................................................108 Troubleshooting ...................................... 278–280
Suspended Solids ...............................................69 Turntable Installation.......................................323
Technical Information............................. 289–293 Vial Positions...................................................179
TN ......................................................................59 Vial Rack Change ............................................267
Viewing Data in Real Time .............................167 Vial Rack Installation ......................................323

B
Background Monitor ................................................203 Blank, System ..........................................................291
Base, Effect on Instrument.........................................71 Buzzer, Setting in Software .......................................84
Blank Check...................................................... 68, 269
Analysis..............................................................66
Using Area in Calculations ............ 139, 189, 198

Index-1
 Index
C
Cable Connections ................................................... 325 Setting Type ...................................................... 26
Cables, Connecting ......................................... 318, 319 Standard............................................................. 36
Calibration Curve .................................................... 290 TOC ................................................................... 37
1-Point and 2-Point .......................................... 290 TOC/TN............................................................. 39
Calculation Method ......................................... 171 Washing........................................................... 239
Creating .................................................. 126, 132 Ceramic Fiber ......................................................39, 42
Entering Calibration Standard Levels.............. 132 Change Password ...................................................... 21
Gas Sample Analysis ....................................... 229 Dialog Box ........................................................ 21
High Sensitivity Analysis .................................. 65 Chemiluminescence Detector.................................. 259
Inserting into Method ...................................... 137 CO2 Absorber .......................................................... 335
Inserting into Sample Table............................. 126 Disposal ........................................................... 242
Inserting Into Sample Wizard.......................... 187 Installation ...................................................52, 58
Manual Injection Kit........................................ 221 MSDS .............................................................. 335
Multi-Point....................................................... 290 Replacing........................................ 242, 248, 251
Optimum .......................................................... 292 Used as NOx Absorber...................................... 59
Options............................................................. 128 Coaxial Needle ........................................... 28, 85, 320
Points List ........................................................ 131 Com Port.................................................................... 30
Points Parameters ............................................ 132 Combustion Tube
Shifting To Blank Point ................................... 291 Connecting......................................................... 40
Shifting to Origin............................129, 172, 290 Filling with Catalyst ............................. 37, 38, 39
Types ...................................................... 128, 290 Installating H Type ............................................ 40
Viewing Data ................................................... 160 Installating N Type ............................................ 43
Viewing Properties .......................................... 170 Replacing......................................................... 242
Calibration Curve Wizard............................... 100, 126 Replacing Ferrules........................................... 245
Analysis Information Window ........................ 128 Washing........................................................... 242
Analysis Options.............................................. 102 Comment ................................................................... 22
Calibration Points List ..................................... 103 Communication Settings ........................................... 30
Calibration Points Window ............................. 131 Configured System, Deleting .................................... 33
Curve Type ...................................................... 101 Connecting Gas Tubing (TN Unit).......................... 330
Curve Type Window ....................................... 128 Connection
Default Measurement Parameters.................... 102 8-Port Sampler................................................. 327
History ............................................................. 104 Cables .............................................................. 325
History Window .............................................. 134 Two 8-Port Samplers....................................... 326
Measurement Parameters Window .................. 130 Consumable Parts ............................................304–307
Opening ........................................................... 125 Control Chart Wizard .............................................. 368
Peak Integration Parameters ............................ 103 Control Charts ........................................ 208, 367–384
Peak Time Parameters Window ...................... 133 Comparing ....................................................... 379
System Information Window........................... 127 Creating ........................................................... 368
Carrier Gas Editing .....................................................377, 381
Connecting....................................................... 313 Excluding Samples From ........................377, 383
Flow Rate........................................................... 90 Exporting To ASCII File ................................. 383
Pressure.............................................................. 89 Following Chart............................................... 372
Purification Tube ............................................. 240 Opening ........................................................... 373
Purifier ............................................................. 314 Out Of Control Events..................................... 380
Kit Specifications .................................... 296 Printing ............................................................ 373
Replacing CO2 Absorber ......................... 248 Recalculating Limits........................................ 377
Supply Pressure ............................................... 314 Saving .............................................................. 373
Tubing Connections......................................... 314 Setting Number Format ................................... 382
Catalyst Statistics........................................................... 378
Disposal ........................................................... 240 Types ............................................................... 367
Filling................................................................. 36 Control Checking .................................................... 200
Filling Rod .................................................. 37, 38 Control Sample
High Sensitivity ........................................ 37, 240 Identifying ....................................................... 184
New.................................................................... 36 Inserting Into Sample Table ............................ 202
Regenerating ........................................... 238, 262 Selecting Type ................................................. 194
Replacing ......................................................... 239 Template .......................................................... 193

Index-2
 Index
Control Sample Wizard Corrosion Warning ......................................................x
Analysis Parameters Window ..........................196 Cover, Installation....................................................323
Control Checking Window ..............................200 Creating
Control Sample Type Window ........................194 Calibration Curve.............................................126
Creating A Template........................................193 Control Charts..................................................368
Failure Action Window....................................201 Control Sample Template ................................193
History Window...............................................199 Method .............................................................135
Injection Parameters Window..........................197 Method Validation File.................................... 349
Opening............................................................126 Sample Table ...................................................125
Parameter Source Window...............................195 TC Calibration File ..........................................100
Peak Time Parameters Window.......................198 CV Max
System Information Window ...........................193 Setting in Method Wizard................................138
Cooler Drain Container..............................................48 Setting In Sample Wizard ................................188
Corrective Action
Eliminate Syringe Bubbles...............................281
Poor Reproducibility ........................................280
Poor Sample Injection......................................280

D
Data Determinations, No. of............................136, 162, 186
Deleting............................................................158 Dialog Box
Exporting to Database......................................148 Change Password...............................................21
Importing from ASCII .....................................159 Dilution Water
Recalculating....................................................158 Checking ..........................................................236
Replacing .........................................................157 Preparing............................................................50
Database, Exporting Data to ....................................148 Display Settings
Default Measurement Parameters ..................... 87, 212 Floating Point Number Formats ......................216
Default Measurement Parameters Dialog Box...........98 Notification Bar Settings .................................215
Deleting Table Settings ..................................................214
All Sample Table Data.....................................158 Disposal
Configured System.............................................33 Catalyst ............................................................240
Selected Sample Table Data ............................159 CO2 Absorber ..................................................242
Description, System .............................................. 7–18 Drain Tank, Installation ...........................................323
Detector Drain Tubing, Connecting .......................................316
Chemiluminescence .........................................259 Drain Vessel Water, Checking.................................236
Viewing Status .................................................203

E
Edit Menu, Sample Table Editor..............................156 Excluding
Editing Data from Sample Table ..................................158
Calibration Point Parameters ...........................132 Injections from Calculations............................158
Control Charts ......................................... 377, 381 Samples From Control Charts................. 377, 383
Method Validation File ....................................356 Exporting
Sample Table....................................................156 Control Charts..................................................383
Electric Shock Warning ........................................... viii Data to ASCII File ...........................................146
Ending Measurement ...............................................120 Data to Database ..............................................148
Error Messages................................................ 270–274 Method Validation Data...................................363

F
File Menu, Sample Table Editor ..............................125 Flow Diagrams.................................................... 11–13
Flow charts, Troubleshooting ..................................274 Flow Line
Flow Diagram Replacing Content............................................263
TOC-VCPH .........................................................11 Replacing Parts and Slider.................................54
TOC-VCPH+POC OPTION ..................................12 Residue Removal .............................................263
TOC-VCPH+TNM-1...........................................12 Setting Washes in Software ...............................86
TOC-VCPN .........................................................13 Washing ...........................................................264
TOC-VCPN+TNM-1...........................................13

Index-3
 Index
Flow Rate Front View
Carrier Gas......................................................... 90 8-Port Sampler................................................... 15
Ozone Source..................................................... 91 Autosampler ...................................................... 14
Sparge Gas ......................................................... 53 TOC-V................................................................. 8
Sparge Gas, Wet Chemical .............................. 269 Furnace ...................................................................... 90
Power................................................................. 90
Temperature.................................................27, 84

G
General Information Window.................................. 125 Ground, Connecting ................................................ 312
General Measurement Parameters ...................... 83–88 Grounding........................................................312, 328
Graph, in Sample Window ...................................... 167 Grubb Test, See Outlier Test

H
Halogen Scrubber History Log
MSDS .............................................................. 337 Calibration ....................................................... 134
Replacing ......................................................... 243 Control Sample................................................ 199
High Purity Air Cylinder ................................ 242, 313 Instrument.......................................................... 31
High Sensitivity Method............................................................. 142
Analysis ............................................................. 63 History Settings, Maintenance .................................. 88
Catalyst .............................................37, 240, 339 Humidifier
Combustion Tube .............................................. 40 Checking Water Level..................................... 237
Using 8-Port Sampler ........................................ 82 Filling with Water ............................................. 49
High Temperature Warning.......................................vii Hydrochloric acid .................................................... 333

I
IC ............................................................................. 285 Installation
Analysis Preparation.......................................... 56 8-Port Sampler................................................. 325
Injection Port Septum ...................................... 226 Autosampler .................................................... 317
Principles ......................................................... 285 Cover ....................................................... 323
Reaction Solution ..................................... 57, 249 Drain Tank............................................... 323
Reaction Solution Pump .................................. 250 Needle, Coaxial ....................................... 322
Reaction Solution Regeneration .........27, 84, 262 Needle, Sample........................................ 321
Removal Pretreatment ....................................... 68 Positioning............................................... 317
Standard Solution .............................................. 61 Rinse Bottle ............................................. 323
Injection Parameters Shipping Screw........................................ 317
Control Sample ................................................ 197 Turntable ................................................. 323
Method............................................................. 138 Vial Rack ...........................................74, 323
Sample ............................................................. 188 CO2 Absorber ..............................................52, 58
Injection Port Septum, Replacing ............................ 226 Combustion Tube
Injection Table, in Sample Window ........................ 168 High Sensitivity......................................... 40
Injection Volume, Setting............................... 138, 188 N Type....................................................... 43
Injury Warning ........................................................... ix Manual Injection Kit ....................................... 219
Inorganic Carbon, See IC Preparation....................................................... 310
Insert Menu, Sample Table Editor........................... 181 Procedure......................................................... 312
Inside Front View Site................................................................... 310
TN ...................................................................... 17 Suspended Solids Kit......................................... 54
TOC-V ............................................................... 10 Syringe............................................................... 45
Inside Top View TN Unit............................................................ 328
TOC-V ............................................................... 11 TOC-V.....................................................310–332
Inspection
Daily ....................................................... 236–237
Periodic ................................................... 238–251

Index-4
 Index
Instrument Instrument Setup Wizard
Auto Restart .....................................................121 ASI Window ............................................... 28, 95
Background Monitor ........................................203 Auto Regeneration of IC Solution .....................27
Connecting And Disconnecting .......................205 Autosampler Parameters ....................................28
Detector Status .................................................203 Buzzer ................................................................27
Effects of Acid, Base, and Salt ..........................71 Cell Length ........................................................26
History Log ........................................................31 Communication Window...................................30
Maintenance .....................................................261 Configuration .....................................................24
Menu, Sample Table Editor .............................203 Furnace Temperature .........................................27
Operation................................................... 35–233 History Log ........................................................31
Overview......................................................... 1–5 Needle ................................................................28
Power .................................................................89 Options Window ......................................... 24, 94
Setup............................................................ 23–33 Oxidation Method ..............................................24
Shut Down Procedure ......................................120 Ready Status Check ...........................................27
Standby Window..............................................206 SSM Window.....................................................29
Starting ...................................................... 89, 207 System Information Window...................... 23, 94
Viewing Properties.............................................32 TOC Window.....................................................26
Instrument Properties Dialog Box..............................32 Tubing Diameter ................................................26
Introduction.................................................................iii
System Administration ...................................... 20

L
Left Side View Lithium hydroxide, MSDS ......................................336
TOC-V .................................................................9

M
Maintenance .................................................... 235–281 Measurment
8-Port Sampler ........................................ 254–255 8-Port Sampler ...................................................80
Autosampler ............................................ 252–253 Mechanical Check....................................................265
Chemiluminescence Detector ..........................259 Method
Daily Inspection ...................................... 236–237 Creating New ...................................................135
Gas Sample Analysis .......................................232 Viewing Properties ..........................................161
History..............................................................269 Method Properties
History Settings..................................................88 Common Tab ...................................................161
Log ...................................................................269 History Tab ......................................................166
Manual Injection Kit ........................................226 NPOC and POC Tabs ......................................165
Mechanical Check............................................265 Parameter Tab ..................................................162
Menu ................................................................261 TC Tab .............................................................163
Parts......................................................... 308–309 TN Tab.............................................................165
Periodic Inspection.................................. 238–251 Method Validation ..................................208, 347–365
Software-Controlled................................ 261–269 According to DIN ................................... 347, 364
TN ........................................................... 256–260 Creating New File............................................349
Warning Message Limits ...................................88 Editing File ......................................................356
Manual Contents Overview .........................................v Exporting Data To ASCII ................................363
Manual Injection Kit ................................................296 Main Window ..................................................348
Analysis............................................................219 Opening File ....................................................350
Calibration........................................................221 Printing File .....................................................351
Installation........................................................219 Saving File .......................................................351
Maintenance .....................................................226 Setting Number Display Format ......................362
Specifications ...................................................296 Viewing Parameters.........................................359
Material Safety Data Sheets, See MSDS

Index-5
 Index
Method Wizard MSDS ..............................................................333–345
Acid Addition Volume .................................... 139 CO2 Absorber .................................................. 335
Analysis Information ....................................... 136 Halogen Scrubber ............................................ 337
Auto Dilution ................................................... 139 High Sensitivity Catalyst................................. 339
Calibration Curve ............................................ 137 Hydrochloric acid ............................................ 333
Creating New Method ..................................... 135 Lithium hydroxide........................................... 336
CV Max ........................................................... 138 Normal Sensitivity Catalyst............................. 340
Determinations................................................. 136 Phosphoric acid ............................................... 334
History Log...................................................... 142 Potassium hydrogen phthalate......................... 344
Injection Parameters ........................................ 138 Potassium nitrate ............................................. 341
Injection Volume ............................................. 138 Quartz Wool .................................................... 338
Multiple Injections........................................... 139 Sodium bicarbonate......................................... 342
Number of Injections ....................................... 138 Sodium carbonate ............................................ 343
Opening ........................................................... 126 Water ............................................................... 345
Peak Integration Parameters ............................ 140 Multiple Injections ................................. 129, 139, 189
SD Max............................................................ 138 Multi-Point Calibration Curve................................. 290
System Information ......................................... 135
Using Blank Check Area ................................. 139
USP/EP ............................................................ 141

N
Needle Notation Conventions................................................. vi
Change ............................................................. 268 Notification Bar ...............................................124, 215
Coaxial........................................................ 28, 85 NOx Absorber
Coaxial+Sparge .......................................... 28, 85 Connecting......................................................... 59
Installation, Coaxial......................................... 322 Replacement .................................................... 260
Installation, Sample ......................................... 321 Using a CO2 Absorber....................................... 59
Rinse .................................................................. 85 NPOC
Rinse after Acid Addition.................................. 86 Acid Addition .................................................... 76
Sample ........................................................ 28, 85 Analysis ............................................................. 76
Sample+Sparge........................................... 28, 85 Principles .................................................286, 288
Setting in Software ..................................... 28, 85 Number of Injections.......................................138, 188
Types ..................................................28, 85, 320

O
OCT-1/2, See 8-Port Sampler Options Menu, Sample Table Editor ....................... 210
Opening Outlier Test.............................................................. 169
Calibration Curve Wizard................................ 125 Oxidation Method, Selecting..................................... 24
Control Sample Wizard ................................... 126 Ozone
Method Validation File.................................... 350 Connecting Source .......................................... 329
Method Wizard ................................................ 126 Generator Replacement ................................... 260
Sample Group Wizard ..................................... 181 Generator, Low Air Supply Safety.................. 331
Sample Table ....................................96, 125, 143 Generator, Source Air Pressure ....................... 330
Sample Wizard ................................................ 185 Source Airflow Rate .......................................... 91
Sparge Gas Valve ............................................ 269 Treatment Unit ................................................ 256

P
Page Setup Parameter Source..................................................... 185
Calibrations Tab .............................................. 152 Parameter Table, in Sample Window...................... 167
Header Tab ...................................................... 153
Instrument Tab................................................. 152
Miscellaneous Tab ........................................... 154
Samples Tab .................................................... 153

Index-6
 Index
Parts Precautions...................................................................3
Consumable Gas Sample Analysis .......................................227
ASI-V .......................................................306 High Sensitivity Analysis ..................................63
Carrier Gas Purifier Kit............................307 Preparation
TNM-1 .....................................................307 Acid....................................................................51
TOC-VCPH ...............................................304 Analysis ...................................................... 36–82
TOC-VCPN ...............................................305 Dilution Water ...................................................50
Maintenance High Sensitivity Analysis ........................... 63, 65
ASI-V .......................................................308 Manual Injection Analysis ...............................219
Manual Injection Kit ................................309 Sample ..................................................63, 72–79
TOC-VCPH ...............................................308 Standard Solution...............................................60
TOC-VCPN ...............................................308 TN Analysis .......................................................59
Peak Pressure
Area..................................................................289 Ozone Generator Source Air............................330
Integration Parameters ...........133, 140, 190, 198 Principles
Shape................................................................289 IC .....................................................................285
Start Delay........................................................140 NPOC...................................................... 286, 288
Total Integration Time .....................................140 Of Analysis ............................................. 284–288
Phosphoric acid ........................................................334 POC..................................................................287
Plunger Tip Backlash ...............................................281 POC+NPOC.....................................................288
POC TN ....................................................................288
Analysis Preparation ..........................................58 TOC ................................................................. 284
kit .....................................................................296 Print
Principles..........................................................287 Control Charts..................................................373
Standard Solution...............................................61 Method Validation File.................................... 351
POC+NPOC Principles ............................................288 Options.............................................................151
Post Sale Service.........................................................iv Page Setup........................................................ 152
Potassium hydrogen phthalate, MSDS.....................344 Preview, Report ...............................................151
Potassium nitrate, MSDS .........................................341 Preview, Table .................................................150
Power Sample Report..................................................150
Furnace...............................................................90 Sample Table ...................................................149
Instrument ..........................................................89 Product Warranty........................................................iv
TN ......................................................................84 Purgeable Organic Carbon, See POC
Power Supply
Changing Voltage ............................................313
Connecting .............................................. 312, 328

Q
Quartz Wool.........................................37, 39, 58, 338

R
Ready Status Check ............................................ 27, 84 Regenerating
Rear View Catalyst ................................................... 238, 262
8-Port Sampler ...................................................15 IC Solution................................................ 27, 262
Autosampler .......................................................14 Replacing Sample Table Data..................................157
TN ......................................................................18 Replacing the NOx Absorber ...................................260
TOC-V .................................................................9 Residue Removal .....................................................263
Recalculating Right Side View, TOC-V.............................................8
All Sample Table Data.....................................158 Rinse
Control Chart Limits ........................................377 Bottle....................................................... 252, 323
Selected Sample Table Data ............................158 Needle ................................................................85
Reference Information .................................... 283–345 Needle, After Acid Addition..............................86
Pump Head.......................................................253

Index-7
 Index
S
Salt, Effect on Instrument .......................................... 71 Printing Sample Table ..................................... 149
Sample Recalculating Data .......................................... 158
Alkaline ............................................................. 71 Replacing Data ................................................ 157
Catcher............................................................. 252 Reversing Last Action ..................................... 156
Container ........................................................... 80 Sample Window ......................................114, 167
Containing Acid................................................. 71 Saving .............................................................. 144
Containing High IC Levels................................ 38 Saving As ........................................................ 145
Containing Salt .................................................. 71 Searching for Text ........................................... 157
Group ............................................................... 181 Sequence Window........................................... 205
High Sensitivity .......................................... 63, 65 Setting Vial Position................................106, 179
Loading .............................................................. 80 Sparging/Acid Addition Window.................... 106
Manual Injection.............................................. 223 Standby Window ............................................. 206
Needle .................................................28, 85, 320 Starting Instrument .......................................... 207
Preparation............................................63, 72–79 Status Bar ................................................124, 178
Report, Printing ............................................... 150 Stopping the Instrument .................................. 207
Suspended Solids ............................................... 69 Toolbar ....................................................122, 178
Sample Group Wizard Toolbar, Customize ......................................... 177
Calibration Curve ............................................ 183 View Menu ...................................................... 160
Controls ........................................................... 184 Viewing Calibration Curve .....................160, 170
Measurement Parameters................................. 182 Viewing Cell Properties .................................. 170
Opening ........................................................... 181 Viewing Data in Real Time............................. 167
Parameter Source ............................................. 181 Viewing Method Properties............................. 161
Sample Table Editor ....................................... 122–218 Viewing Vial Positions.................................... 179
Auto Restart ..................................................... 121 Window Menu ................................................. 218
Background Monitor........................................ 203 Sample Window ...................................................... 114
Closing a File................................................... 144 Graph ............................................................... 167
Connecting The Instrument ............................. 205 Injection Table................................................. 168
Creating New Sample Table..................... 98, 125 Parameter Table............................................... 167
Deleting All Data............................................. 158 Sample Wizard
Deleting Selected Data .................................... 159 Acid Addition .................................................. 189
Directories ....................................................... 217 Analysis Information Window ........................ 186
Edit Menu ........................................................ 156 Auto Dilution................................................... 189
Editing Rows and Cells ................................... 156 Calibration Curve ............................................ 191
Excluding Data ................................................ 158 Calibration Curve Window ............................. 187
Exiting ............................................................. 155 CV Max ........................................................... 188
Exporting Data to ASCII ................................. 146 Determinations ................................................ 186
Exporting Data to Database ............................. 148 Injection Parameters ........................................ 191
File Menu......................................................... 125 Injection Parameters Window ......................... 188
Finding Cell Content ....................................... 157 Injection Volume ............................................. 188
General Information Window.......................... 125 Multiple Injections .......................................... 189
Help Menu ....................................................... 218 Number of Injections....................................... 188
Importing Data from ASCII ............................ 159 Parameter Source Window .............................. 185
Insert Menu...................................................... 181 Peak Time Parameters Window ...................... 190
Inserting Calibration Curve ............................. 126 SD Max............................................................ 188
Inserting Control Samples ............................... 193 Units ................................................................ 188
Inserting Sample Group................................... 181 USP/EP Window ............................................. 192
Inserting Samples ............................................ 185 Screen Lock ............................................................... 20
Instrument Menu.............................................. 203 SD Max............................................................138, 188
Notification Bar ...................................... 124, 215 Sequence Window ................................................... 205
Opening File .................................................... 143 Shipping Screw........................................................ 317
Options Menu .................................................. 210 Sliding Sample Injector ........................................... 245
Outlier Test ...................................................... 169 Sodium bicarbonate, MSDS .................................... 342
Overview ......................................................... 122 Sodium carbonate, MSDS ....................................... 343
Page Setup Options.......................................... 152
Previewing Sample Report .............................. 151
Previewing Sample Table ................................ 150
Printing Options............................................... 151
Printing Sample Report ................................... 150

Index-8
 Index
Software Standard Solution.......................................................60
Connecting To Instrument ...............................205 Analysis ...........................................................100
Creating New Method......................................135 High Sensitivity .................................................64
Maintenance Functions ....................................261 Preparing............................................................60
Maintenance History Settings ............................88 Sparging ...........................................................292
Module .............................................................122 Storing................................................................62
Overview..................................................... 19–33 Standby Window............................................. 120, 206
Ready Status Check ...........................................84 Starting The Instrument ...........................................207
Setting Measurement Parameters................ 83, 87 Starting the Instrument...............................................89
Setting up a Sequence ......................................125 Status Bar........................................................ 124, 178
Source Air (TN Unit) Stirrer .................................................................. 78, 86
Pressure ............................................................330 Stopping the Instrument
Sparge Halt...................................................................207
Gas Flow Rate....................................................53 Stop Finish Current..........................................207
Gas Flow Rate, Wet Chemical.........................269 Stop Peak Stop .................................................207
Gas Valve.........................................................269 Suspended Solids ................................................ 54, 69
Needle ....................................................... 28, 320 Syringe
NPOC Analysis ..................................................77 Changing................................................. 226, 268
Time, Setting....................................................139 Installation .........................................................45
Sparging/Acid Addition Window ............................106 Manual Injection Kit........................................226
Special Accessories..................................................303 Plunger Tip ......................................................244
Specifications .................................................. 294–297 Plunger Tip Backlash.......................................281
Autosampler .....................................................295 Replacing ...........................................................45
Carrier Gas Purifier Kit....................................296 Residue Removal .............................................263
Gas Sample Injection Kit .................................296 Washing with Sample .....................138, 188, 212
Manual Injection Kit ........................................296 Washing with Standard........................... 130, 172
POC Kit............................................................296 Syringe Pump
TN ....................................................................295 8-Port Valve Rotor...........................................246
TOC-V .............................................................294 Zero Point Detection..........................................47
Standard Accessories System Administration
ASI ...................................................................299 Add Event Log...................................................22
Manual Injection Kit ........................................301 Change Password...............................................21
POC Kit............................................................301 Introduction........................................................20
TN ....................................................................301 Screen Lock .......................................................20
TOC-VCPH/CPN ................................................298 System Blank ...........................................................291
System Description ............................................... 7–18
System Information Window
Instrument Setup Wizard ...................................94

T
TC TN
Analysis, New Catalyst ......................................36 Analysis Preparation ..........................................59
Blank Check.............................................. 66, 269 Analysis, New Catalyst...................................... 36
Principles..........................................................284 Connecting Ozone Source Air .........................329
Standard Solution...............................................60 Front and Right Side Views...............................16
TC/TN, Standard Solution .........................................61 Gas Exhaust Tubing.........................................332
TC-IC .......................................................................288 Grounding ........................................................ 328
Technical Information..................................... 289–293 Inside Front View ..............................................17
Time, Sparge ............................................................139 Installation .......................................................328
Maintenance............................................ 256–260
Ozone Source Airflow Rate...............................91
Power Source .....................................................84
Power Supply...................................................328
Principles .........................................................288
Rear View .......................................................... 18
Specifications...................................................295
Standard Solution...............................................61
Turning On.........................................................91
Unit ..................................................................295

Index-9
 Index
TN Unit Toolbar, Sample Table Editor
Gas Tubing Connection ................................... 330 Customizing..................................................... 177
TOC Displaying ....................................................... 178
Principles ......................................................... 284 Functions ......................................................... 122
Setting Parameters ............................................. 83 Total Carbon, See TC
Setting Parameters in Software.......................... 26 Total Nitrogen, See TN
TOC window of the Instrument Setup Wizard .......... 94 Total Organic Carbon, See TOC
TOC/TN, Catalyst...................................................... 39 Troubleshooting...............................................270–281
TOC-Control V Autosampler ............................................278–280
Administration Tool .......................................... 21 Flow Charts ..................................................... 274
Administrator Window ...................................... 21 TOC-V.....................................................274–277
TOC-V Tubing Diameter........................................................ 83
Construction......................................................... 8 Turntable, Installation ............................................. 323
Front View ........................................................... 8 Tutorial ..............................................................92–119
Grounding ........................................................ 312 Calibration Runs.............................................. 100
High Sensitivity Catalyst ................................... 37 Configuring the Instrument ............................... 93
Inside Front View .............................................. 10 Connecting the Instrument ..........................96, 98
Inside Top View ................................................ 11 Creating a Sample Table ................................... 98
Installation .............................................. 310–332 Evaluating Results........................................... 114
Left Side View..................................................... 9 Measurement ................................................... 112
Rear View ............................................................ 9 Printing Report ................................................ 117
Right Side View................................................... 8 Unknown Run.................................................. 108
Specifications................................................... 294
Standard Catalyst ............................................... 37
Troubleshooting...................................... 274–277

U
Units....................... 87, 130, 138, 163, 171, 188, 212 USP/EP ............................................................141, 192

V
Vial View Menu, Sample Table Editor ........................... 160
Filling................................................................. 72 Viewing Measurement Data in Real Time .............. 167
Placing in Rack .................................................. 74
Rack Installation ....................................... 74, 323
Sealing ............................................................... 73
Setting Position....................................... 106, 179
Types ................................................................. 72

W
Warning Water
Corrosion ............................................................. x Dilution............................................................ 236
Electric Shock...................................................viii Drain Vessel .................................................... 236
High Temperature..............................................vii Humidifier ....................................................... 237
Injury .................................................................. ix MSDS .............................................................. 345
Warning Labels..........................................................vii Pure.................................................................... 50
Warning Message, Maintenance................................ 88 Supply to Cooler Drain Container..................... 48
Warranty ..................................................................... iv Zero ................................................................... 60
Washing
Catalyst ............................................................ 239
Combustion Tube ............................................ 242
Flow Lines ................................................ 86, 264
Syringe with Sample.......................138, 188, 212
Syringe with Standard ............................ 130, 172

Z
Zero Point Detection......................................... 47, 261 Zero Water................................................................. 60
Zero Shift ........................................................ 129, 172

Index-10