Troubleshooting

Tips & Tricks for

your GC Analyzer &
CFT Application

7890A/7890B GC
Overview

October 29, 2014

1
Definitions
Carrier Gas
• Pressurized gas used to transport the sample through the system.
Detector Support Gases
• Gases needed by specific detectors to operate, i.e. hydrogen and air.
Sample Introduction
• Method of “placing” the sample into the carrier gas stream.
Inlet
• Device that controls the carrier gas flow and sample introduction onto the column.
Column
• Device that separation of the components in the sample.
Detector
• Device that responds to sample components as they elute from the column.
Data Acquisition
• Collection, conversion, and storage of detector signal used for integration and generation of
chromatogram and reports.
Agilent 7890B & 7890 Front View
Agilent 7890A & 7890B Rear View
 Agilent 7890 Top View

Valve Box, Actuators

and Valves

Detectors
Inlets
Gas Supply Characteristics

Gases must be chosen with consideration of the type

of detector used:
Inert.
Dry.
Pure.
99.9995% pure.
Using Compressed Gases Safely

Obtain safety information from your

company's safety department or from your
local gas supplier.
Carrier Gas Plumbing

Stainless Steel Diaphragm

Tank Regulator.
1/8” Swagelok -
NPT Adapter.

1/8” Copper Tubing

P/N 5180-4196.
Moisture Trap
P/N 5060-9084.
Hydrocarbon Indicating O2 Trap
Trap P/N IOT-2-HP.
P/N 5060-9096.
Gas System Maintenance
Filters/Traps
• Re-condition or replace at manufacture’s recommended interval.
• Default replacement interval is every 3 cylinders.

Leaks
• Every 4 to 6 months check all external tubing and fittings for leaks.
• Electronic leak detector recommended for internal and external leak
detection.

Liquid leak detection (soap solution) is NOT recommended.

Troubleshooting Process
1. Know operation fundamentals.
2. Gather information about problem.
3. Verify symptoms.
4. Verify operational parameters.
5. Isolate the problem.
6. Fix the problem.
7. Verify fix.
8. Document fix.
9. Create PM task?

Reference: Troubleshooting the Troubleshooting Course by Robert F. Mager

Isolate the Problem
Inspect parts/assemblies.

Review common recurring fixes:

• Instrument Log book.
• ChemStation Logbook
• Instrument Utilities Logs if configured

Check site/environmental conditions.

7890 Keypad

GC & GC/MS User Manuals and Tools

Theorize a solution.

Isolate problem to assembly/functional area:

• Flow.
• Chemical.
• Electrical.
• Mechanical.
• Operational.
Reprinted with permission from Troubleshooting the Troubleshooting Course, ©. 1982
Published by The Center for Effective Performance, 4250 Perimeter Park South, Suite 311,
Atlanta, GA 30341. 1-800-558-4237.
Fix the Problem

Only try one “fix” at a time.

Try quick fixes and easy solutions first.

Perform related maintenance tasks:

• Make sure to reset EMF resource counters on GC.
• Instrument Utilities Software

Reprinted with permission from Troubleshooting the Troubleshooting Course, ©. 1982

Published by The Center for Effective Performance, 4250 Perimeter Park South, Suite
311, Atlanta, GA 30341. 1-800-558-4237.
Verify the Fix

Verify that system performance is restored:

• ChemStation method.
• 7890 Keypad method
• Instrument Utilities

Verify that parts replaced are bad.

Restore system to operational configuration.

Reprinted with permission from Troubleshooting the Troubleshooting Course, ©. 1982

Published by The Center for Effective Performance, 4250 Perimeter Park South, Suite 311,
Atlanta, GA 30341. 1-800-558-4237.
Document the Fix

Review troubleshooting and fix actions.

Update instrument logbook.

Update Instrument Utilities Software.

Reprinted with permission from Troubleshooting the Troubleshooting Course, ©. 1982

Published by The Center for Effective Performance, 4250 Perimeter Park South, Suite 311,
Atlanta, GA 30341. 1-800-558-4237.
Make a Preventive Maintenance Task

Has the problem occurred before?

Did consumables repair problem?

Should the repair action be made part of scheduled preventive

maintenance?

Instrument Utilities Software:

• For scheduled maintenance.

Service Mode:
• EMF Resource counters.
Reprinted with permission from Troubleshooting the Troubleshooting Course, ©. 1982
Published by The Center for Effective Performance, 4250 Perimeter Park South, Suite
311, Atlanta, GA 30341. 1-800-558-4237.
Chromatographic Troubleshooting

Use Chromatogram to:

• Evaluate system performance:

– Detector response.
– Baseline.
– Peak resolution.
– Retention times.

• Evaluate maintenance/repair steps.

• Verify “fix” actions.

Troubleshooting
Tips & Tricks for
your GC Analyzer &
CFT Application

Diagnostics

October 29, 2014

16
Reference Documentation
• GC and GC/MS User Manuals & Tools DVD

– Documentation
– Videos
– Calculator
– Parts finder
– Firmware update
– Instrument utilities

• www.chem.agilent.com
Chromatographic Troubleshooting Tools
• Reference points
– Chromatogram and report of “standard”
– Copy of method parameters

• Known good standard samples

– TCD Checkout PN: 18710-60170
– FID Checkout PN: 5188-5372
– ECD Checkout PN: 18713-60040
– FPD Checkout PN: 5188-5953
– NPD Checkout PN: 18789-60060

• New syringe

• Spare column

• Spare consumables and frequently replaced parts

– Ferrules
– Septa
– Inlet liners
– O-rings
Agilent website: www.chem.agilent.com
Common Tools
• Torx drivers (T10 and T20)
• Open-end wrenches (1/4", 1/2", 3/8", 5/8", 5/16", 7/16", 9/16")
• 1/4" hex nut driver
• 7 mm hex nut driver
• Tweezers
• Flashlight
• Volt-ohm meter
• Needle-nose pliers
• Spare fuses (check the instrument manual)
Instrument Tools and Supplies

• Electrostatic discharge (ESD) protective wrist strap

• FID cleaning kit (PN 9301-0985)
• FID flow meter adapter (PN 19231-60660)
• Column cutter
• Electronic leak detector
• Electronic flow meter or soap film bubble meter
• Solvents for cleaning parts
• Light weight cotton gloves
Error Messages and Logbooks

Keypad and Display

GC & GC/MS User Manuals and Tools

• Instrument Utilities

Open Lab ChemStation

Agilent 7890 Keypad
 7890B Features – Early Maintenance Feedback
EMF (Counters)
• Injection based
• Time based
• Track usage
• Replace parts before degradation impacts
chromatographic results.
• Two Warning Thresholds
- Service Due
• Service indicator lights
• Maintenance log created
- Service Warning
• Reminder that the component needs
maintenance
7890B Features – Resource Conservation
Resource Conservation, the system provides an instrument schedule to conserve resources such
as electricity and gases.
• Sleep Method
- Sets low flows and temperatures

• Wake Method
- Sets new flows and conditions, typically to restore operating
conditions

• Condition Method
- Sets flows and temperatures high enough to clean out contamination
if present for a specific time
GC and GC/MS User Manuals & Tools
• Parts Finder
- Interactive software
- Locate replacements parts for your Agilent instrument
- Add parts to Parts List and print
- Order parts

• Firmware Update
- Easily update firmware to your instrument

• Instrument Utilities
- Monitor instruments
- View all the instruments’ information
- Tests and diagnostics
- Status of instruments on the network
User Manuals
Parts Finder
Easily find parts through search
Selective to specific instrument
• 7693A, 7650A, 7890A, 7890B, 5975 MSD,
5977 MSD
Search by component area
Interactive image
Interactive
Can access Agilent Store to place an order
Can add to parts list
Can add parts to favorite folder
Component breakdown by areas
Method Developer Tools – The Vapor Volume Calculator from OpenLAB
C01.05
Method Developer Tools – The GC Method Translator from OpenLAB C01.05
Instrument Utilities – Configure
Instrument Utilities – Tests
Problem Chromatogram
Typical Chromatogram

Peak Peak

#7
#6

#8
#9
No. Width Area Type
#1
#2

#3
#4
#1 0.023 1639 BB

#5
#2 0.027 3291 BB
#3 0.032 3522 BB
#4 0.037 2750 BV
#5 0.03 1590 VB
#6 0.037 5473 BB
#7 0.034 3465 BB
#8 0.037 4932 BV
Problem Chromatogram
5
#9 0.036 5020 BB
Isolate the Problem to a Functional Area

Filters/Traps Data system

Regulators Syringe/Sampler

Inlets
• Gas system
Detectors • Inlet
• Column
Gas Carrier
Hydrogen

• Detector
Air

Column
• Data system

Know the purpose and function of the major component areas.

Functional Areas
Flow
• improper supply pressures
• leaks
Chemical
• contaminated or “aged” samples/standards
• contaminated supply gases/traps
• contaminated inlet, column, detector
Electrical
• cable connections
Mechanical
• auto sampler syringe condition or installation
• vial fill level and sampling depth settings
Operational
• incorrect method loaded
• method parameters modified but not saved
Solve the Problem
Fix the problem.

Verify the fix.

Document fix.

Add to PM schedule if consumable solve problem.

Do not forget
• Reset counters or EMF
- Open Lab ChemStation
- 7890B or 7890A Keypad
- Instrument Utilities
• Schedule maintenance.
SSI Injection Modes
Injection Mode Purpose

Split Major component analysis.

Pulsed-split Allows larger injection volume

without liner overload and faster
transfer to column.

Splitless Trace component analysis.

Pulsed-splitless Larger injection volume without

liner overload and faster transfer to
column.
 Agilent 7890 Split/Splitless Inlet

Split Vent Carrier Septum Purge

SSI Splitless Mode

• Trace analysis

• Nearly all of the analytes and solvent enter the column.

SSI Splitless Mode Flow Diagram
Gas Saver

Split Mode

Splitless Mode
Variable Septum Purge Septum Purge

EPC Module

Frit
Valve
Proportional Valve
PS

Septum

Pressure Sensor
 Septum Purge

Effects of Septum Purging

EPC Module

Frit
Valve
Cap off the
septum purge. S/SL inlet. PS

FID detector.

Turn on the Septum

septum purge.

Septum purge prevents septa volatiles from

getting into the column.
Used in four inlets: SSL, PP, COC,
and PTV.
SSI Problem #1

Before After
#1
#2
#3

#5

#7
#8
#4

#6

#9
Peak Peak Peak Before After
No. Width Width Area Area Type
Normal

#1 0.024 0.025 780 1099 BB

#2 0.024 0.026 1310 1630 BB
#3 0.018 0.035 1820 2140 BB
#4 0.022 0.022 1390 1899 BV
#5 0.022 0.022 705 889 VB
#6 0.025 0.024 2890 3680 BB
#7 0.027 0.027 2420 3088 BB
#1
#2
#3

#5

#7
#8
#4

#6

#9

#8 0.025 0.025 2430 3092 BB

#9 0.024 0.024 2615 3256 BB
Problem

• Manual split injection

• Narrow-bore capillary column

• FID.
SSI Problem #2 – Which Flow Was Adjusted?

#1

#5
#2

#8
#3

#7
#4

#6

#9
Normal

Before After
Peak Peak Peak Before After
No. Width Width Area Area Type

#1 0.024 0.023 530 242 BB

#2 0.024 0.023 804 371 BB
#3 0.018 0.017 1068 453 BB
#4 0.022 0.021 909 400 BV
#5 0.022 0.021 435 195 VB
#6 0.025 0.023 1826 790 BB
#1

#5
#2

#8
#3

#7
#4

#6

#9
Problem

#7 0.027 0.026 1535 698 BB

#8 0.025 0.024 1538 657 BB
#9 0.024 0.023 1687 713 BB
SSI Problem #3 – Which Flow Was Adjusted?

#1

#7
#2
#3

#5
#4

#8
#6

#9
Before After
Normal

Peak Peak Peak Before After

No. Width Width Area Area Type

#1 0.024 530 BB
#2 0.024 804 BB
#3 0.018 0.031 1068 332 BB
#4 0.022 0.028 909 238 BV
5
#5 0.022 435 VB
#6 0.025 0.031 1826 585 BB
#7 0.027 0.040 1535 505 BB
Problem

#8 0.025 0.033 1538 465 BB

#1

#7
#2

#3

#4
#5

#6

#8
#9

#9 0.024 0.034 1687 531 BB

SSI Problem #4

#3

#6

#9
#8
#7
#4
#1
#2

#5
Peak Peak
Normal

No. Width Area Type

#1 0.021 551 BV
#2 0.026 1214 BB
#3 0.018 2521 BV
#4 0.020 1037 BV
#5 0.019 511 VB
#6 0.022 2253 BB
#7 0.025 1737 BB
#8 0.024 1703 BB
Problem

#9 0.023 2104 BB
SSI Septa and Merlin Microseal

• High Temp Analysis. • Longer life alternative.

• Low Bleed. • Duckbill design.
• Lower Coring. • Inlet pressures: 3-100 psi.
• Packaged in glass to maintain • Inlet temperatures: 100-300˚C.
purity.
• 11-mm diameter.

Merlin microseal requires 23 gauge syringe

needle tapered tip.
SSI Assembly

Replacement Filter
Cartridge Kit
P/N G1544-80530
SSI Seals

Gold seal (original)

Thermal nut
Gold seal (cross)
Seal
Washer

Reducing nut
18740-20885 Gold-plated seal
5182-9652 Gold-plated (cross) seal
18740-20880 Stainless steel seal
5061 - 5869 Washer
Agilent 7890 – Split/Splitless Capillary Inlet

Replacement Filter
Cartridge Kit
P/N G1544-80530.

GLASS POSITIONING BEAD

Deactivated Split Liner High Split Flow Gold Seal.

P/N 5183-4647 P/N 5182-9652 - Use with liners
that introduce restriction.
Split Liner
Splitless Liner
SSI Liner Volume versus Sample Volume

Solvent Density Mol. Wt. Exp. Ratio

Isooctane 0.69 114 138:1

Hexane 0.66 86 174:1
Pentane 0.62 72 198:1
Ethyl acetate 0.90 88 233:1
Chloroform 1.48 119 284:1
Methylene Chloride 1.33 85 356:1
Methanol 0.79 32 563:1
Water 1.00 18 1261:1

Injection temperature = 250°C.

Column head pressure = 13 psi (90 kPa).
EPC Modules
Auxiliary Front Detector Front Inlet

EPC5 EPC3 EPC1

EPC6 EPC4 EPC2

Back

PCM Back Detector Back Inlet

SSI EPC Module
Septum Purge Vent Carrier Control Valve

Carrier Gas Inlet

Septum Purge Valve

EPC Module Constant Pressure versus
Constant Flow
Pressure (measured/controlled)

Constant Pressure Oven Temperature

Actual Column Flow

Actual Column Flow (calculated)

Pressure (measured/controlled)
Constant Flow
Oven Temperature
PPI Flow-Controlled Flow Diagram

Flow-controlled mode
recommended for packed
columns.
PPI Pressure-Controlled Flow Diagram

Pressure-controlled mode
recommended for
capillary columns.
PPI Problem #1

#1
#2

#9
#3

#5

#7
#4

#8
#6
Before After
Normal

Peak Peak Peak Before After

No. Width Width Area Area Type

#1 0.023 0.029 1639 2009 BB

#2 0.027 0.039 3291 4394 BB
#3 0.032 0.035 3522 3363 BB
#4 0.037 0.040 2750 3252 BV
#5 0.03 0.033 1590 2141 VB
#6 0.037 0.039 5473 6168 BB
#7 0.034 0.040 3465 4516 BB
#8 0.037 0.039 4932 5568 BV
Problem

#9 0.036 0.044 5020 6049 BB

PPI Column Installation

Bottom of inlet
2
cm
Column nut 0 1-2 mm

Insulation cup
Typical Injection Port Problems

• Discrimination
– Needle
– Inlet
• Sample decomposition
• Incorrect temperature
• Contamination
• Blockage
• Leaks
• Flashback
Detecting Leaks

• EPC “chirp” alarm and shutdown

• Electronic leak detector
• Pressure test
• Chromatographic changes
– Retention times
– Area counts
• Methanol

– Soap-film leak detection fluids

Routine Injection Port Maintenance

• Change septum.
• Clean or replace syringe.
• Perform pressure decay or leak test and repair any leaks.
• Clean or replace liners/inserts.
• Replace O-rings.
• Clean or replace seal and washer (SSI).
Questions?

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