Operating Manual

multi EA 5100
C/N/S/X Analyzer
Manufacturer Analytik Jena GmbH
Konrad-Zuse-Straße 1
07745 Jena / Germany
Telephone: +49 3641 77 70
Fax: +49 3641 77 9279
E-mail: [email protected]

Technical Service Analytik Jena GmbH

Konrad-Zuse-Straße 1
07745 Jena / Germany
Phone: +49 3641 77 7407
Fax: +49 3641 77 9279
Email: [email protected]

For a proper and safe use of this product follow the instructions.
Keep the operating manual for future reference.

General Information http://www.analytik-jena.com

Documentation Number 11-0203-002-23

Edition A (01/2021)

Technical Documentation Analytik Jena GmbH

© Copyright 2021, Analytik Jena GmbH

multi EA 5100 Table of contents

Table of contents
1 About this user manual .................................................................................................................................................. 7

2 Intended use.................................................................................................................................................................... 8

3 Security ............................................................................................................................................................................ 10
3.1 Safety labeling on the device ........................................................................................................................... 10
3.2 Requirements for the operating personnel..................................................................................................... 11
3.3 Safety instructions, transport and commissioning ......................................................................................... 11
3.4 Safety instructions: during operation .............................................................................................................. 12
3.4.1 General safety instructions during operation.................................................................................................. 12
3.4.2 Safety instructions – protection against explosion and fire........................................................................... 12
3.4.3 Safety instructions: electrical equipment ........................................................................................................ 13
3.4.4 Handling of auxiliary and operating materials ............................................................................................... 13
3.4.5 Decontamination after soiling ......................................................................................................................... 14
3.4.6 Behavior during overpressure faults (0206, gas pressure fault) ................................................................... 14
3.5 Behavior during emergencies .......................................................................................................................... 14
3.6 Safety instructions – maintenance and repair ................................................................................................ 15

4 Function and design ....................................................................................................................................................... 16

4.1 multi EA 5100 basic module............................................................................................................................ 16
4.1.1 Principle of operation ....................................................................................................................................... 16
4.1.2 Design of the basic module.............................................................................................................................. 18
4.2 Sampling modules ............................................................................................................................................ 29
4.2.1 Auto-injector..................................................................................................................................................... 29

5 Installation and commissioning ..................................................................................................................................... 30

5.1 Installation conditions ...................................................................................................................................... 30
5.2 Installation location requirements................................................................................................................... 30
5.3 Power supply..................................................................................................................................................... 30
5.4 Gas supply ......................................................................................................................................................... 31
5.5 Device layout and space requirements ............................................................................................................ 31
5.6 Installing and commissioning the analysis system ......................................................................................... 34

6 Operation ........................................................................................................................................................................ 36
6.1 General notes for measuring operations......................................................................................................... 36
6.2 Selecting the measurement method ............................................................................................................... 37
6.3 Switching on the basic module and the modules ........................................................................................... 38
6.4 Switching off the basic module and the modules........................................................................................... 39
6.5 Recommissioning after emergency shutdown (Cl module 5100) ................................................................. 40

7 Nitrogen analysis with the N module 5100 ................................................................................................................. 42

7.1 Function and design ......................................................................................................................................... 42
7.1.1 Function and measuring principle ................................................................................................................... 42
7.1.2 Design................................................................................................................................................................ 42
7.1.3 Connection ........................................................................................................................................................ 43
7.2 Installation ........................................................................................................................................................ 45
7.3 Operation .......................................................................................................................................................... 47

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Table of contents multi EA 5100

8 Chlorine analysis with the Cl module 5100 .................................................................................................................. 48

8.1 Function and design ......................................................................................................................................... 48
8.1.1 Function and measuring principle ................................................................................................................... 48
8.1.2 Design................................................................................................................................................................ 48
8.1.3 Connection ........................................................................................................................................................ 56
8.2 Installation ........................................................................................................................................................ 59
8.3 Operation .......................................................................................................................................................... 63
8.3.1 Preparing the measuring cell ........................................................................................................................... 63
8.3.2 Operating the analysis system ......................................................................................................................... 65
8.3.3 Notes for measuring operations ...................................................................................................................... 66

9 Sulfur analysis with the S module 5100 (basic, MPO) ................................................................................................ 67

9.1 Function and design ......................................................................................................................................... 67
9.1.1 Function and measuring principle ................................................................................................................... 67
9.1.2 Design................................................................................................................................................................ 67
9.1.3 Connection ........................................................................................................................................................ 68
9.2 Installation ........................................................................................................................................................ 69
9.3 Operation .......................................................................................................................................................... 70

10 Sulfur analysis with the S module 5100 coulometric .................................................................................................. 71

10.1 Function and design ......................................................................................................................................... 71
10.1.1 Function and measuring principle ................................................................................................................... 71
10.1.2 Design................................................................................................................................................................ 71
10.1.3 Connection ........................................................................................................................................................ 77
10.2 Installation ........................................................................................................................................................ 77
10.3 Operation .......................................................................................................................................................... 80
10.3.1 Preparing the measuring cell ........................................................................................................................... 80
10.3.2 Operating the analysis system ......................................................................................................................... 81

11 Carbon analysis with the C module 5100 .................................................................................................................... 83

11.1 Function and design ......................................................................................................................................... 83
11.1.1 Function and measuring principle ................................................................................................................... 83
11.1.2 Design................................................................................................................................................................ 83
11.1.3 Connection ........................................................................................................................................................ 84
11.2 Installation ........................................................................................................................................................ 85
11.3 Operating the analysis system ......................................................................................................................... 85

12 Carbon analysis with the TOC module 5100 ................................................................................................................ 87

12.1 Function and design ......................................................................................................................................... 87
12.1.1 Function and measuring principle ................................................................................................................... 87
12.1.2 Design................................................................................................................................................................ 87
12.1.3 Connection ........................................................................................................................................................ 92
12.2 Installation ........................................................................................................................................................ 94
12.3 Operation .......................................................................................................................................................... 96
12.3.1 Operating the analysis system ......................................................................................................................... 96
12.3.2 Notes for measuring operations ...................................................................................................................... 97

13 Troubleshooting.............................................................................................................................................................. 98
13.1 General notes.................................................................................................................................................... 98
13.2 Remedying software message faults............................................................................................................... 98
13.3 Initializing the basic module and the system components ............................................................................104

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multi EA 5100 Table of contents

13.4 Displays in the window Status analyzer .........................................................................................................105

13.4.1 Overview ...........................................................................................................................................................105
13.4.2 Method..............................................................................................................................................................106
13.4.3 Sampling modules ............................................................................................................................................106
13.4.4 Detectors ...........................................................................................................................................................107
13.5 Device faults on the basic module ...................................................................................................................109
13.6 Analytical problems in the basic module.........................................................................................................111
13.7 Device faults on the N module 5100 ..............................................................................................................112
13.8 Analytical problems during TC determination ................................................................................................113
13.9 Device faults on the chlorine detector.............................................................................................................114
13.10 Analytical problems during AOX, EOX and TX determination .......................................................................115
13.11 Device faults on the S module 5100 basic and S module 5100 MPO ..........................................................116
13.12 Analytical problems during TS determination ................................................................................................116
13.13 Device faults on the coulometric sulfur detector ............................................................................................117
13.14 Analytical problems during coulometric TS determination............................................................................117
13.15 Device faults on the carbon detector...............................................................................................................119
13.16 Analytical problems during TC, EC/OC determination ...................................................................................119
13.17 Device faults on the TOC detector ...................................................................................................................120
13.18 Analytical problems during TC, EC/OC, TOC, NPOC and TIC determination .................................................121

14 Maintenance and care.................................................................................................................................................... 124

14.1 Overview of maintenance work .......................................................................................................................124
14.2 Maintenance of the multi-purpose combustion tube ....................................................................................126
14.2.1 Removing the combustion tube.......................................................................................................................127
14.2.2 Cleaning the combustion tube .........................................................................................................................128
14.2.3 Inserting the quartz wool plug.........................................................................................................................128
14.2.4 Installing the combustion tube ........................................................................................................................129
14.3 Maintenance of the auto-protection valve assembly .....................................................................................131
14.3.1 Installing/removing the auto-protection valve assembly ..............................................................................131
14.3.2 Check and replace the filter..............................................................................................................................132
14.3.3 Replacing the pneumatic seal ..........................................................................................................................133
14.4 Replacing the membrane dryer .......................................................................................................................134
14.5 Replacing the hose connections ......................................................................................................................136
14.6 Replacing the septum on the injection port....................................................................................................136
14.7 Replacing the check valves and particle filters................................................................................................137
14.7.1 Replacing the check valves on the gas box .....................................................................................................137
14.7.2 Replacing the particle filters in the gas inlets .................................................................................................138
14.8 Checking the system for leaks..........................................................................................................................139
14.8.1 System tightness for N/S/C methods ..............................................................................................................139
14.8.2 System tightness for Cl methods .....................................................................................................................139
14.8.3 System tightness for TOC methods .................................................................................................................141
14.9 Removing and installing the combustion furnace ..........................................................................................141
14.10 Maintenance of the N module 5100 nitrogen detector ................................................................................143
14.10.1 Replacing the ozone generator........................................................................................................................143
14.10.2 Replacing the absorber.....................................................................................................................................145
14.10.3 Replacing the chemical ozone decomposer ....................................................................................................146
14.11 Maintenance of the Cl module 5100 chlorine detector ................................................................................147

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Table of contents multi EA 5100

14.11.1 Replacing the sulfuric acid and cleaning the sulfuric acid container. ............................................................147
14.11.2 Maintenance of the measuring cell .................................................................................................................149
14.11.3 Maintenance and storage of the electrodes ...................................................................................................150
14.12 Maintenance of the S module 5100 basic and S module 5100 MPO sulfur detector ................................152
14.12.1 Replacing the UV lamp .....................................................................................................................................152
14.12.2 Replacing the chemical ozone decomposer ....................................................................................................154
14.13 Maintenance of the coulometric sulfur detector ............................................................................................155
14.13.1 Replacing the absorber.....................................................................................................................................155
14.13.2 Replacing the electrolyte solution ...................................................................................................................157
14.14 Maintenance of the TOC detector ...................................................................................................................158
14.14.1 Replacing the water traps ................................................................................................................................159
14.14.2 Replacing the halogen trap..............................................................................................................................159
14.14.3 Regenerating the TIC reactor...........................................................................................................................161
14.14.4 Cleaning the TIC reactor ...................................................................................................................................161
14.14.5 Replacing the pump hose of the condensate pump .......................................................................................163
14.14.6 Cleaning the condensation coil........................................................................................................................164
14.14.7 Replacing the catalyst in the TOC combustion tube .......................................................................................165

15 Transport and storage .................................................................................................................................................... 167

15.1 Transport...........................................................................................................................................................167
15.2 Moving the device in the laboratory................................................................................................................167
15.3 Storage ..............................................................................................................................................................167
15.4 Preparing the basic module for transport and storage ..................................................................................168
15.5 Preparing detection modules...........................................................................................................................168
15.5.1 Notes for the transport of the Cl module 5100 .............................................................................................169
15.5.2 Notes on transport of the S module 5100 coulometric ................................................................................170
15.5.3 Notes on transport of the TOC module 5100 ................................................................................................170

16 Disposal ........................................................................................................................................................................... 171

17 Specifications .................................................................................................................................................................. 172

17.1 Technical data for the multi EA 5100 ............................................................................................................172
17.2 Technical data of the N module 5100 ...........................................................................................................176
17.3 Technical data for the Cl module 5100 ..........................................................................................................176
17.4 Technical data for the S module 5100 (basic, MPO) ....................................................................................177
17.5 Technical data for the S module 5100 coulometric ......................................................................................178
17.6 Technical data for the C module 5100 ...........................................................................................................178
17.7 Technical data for the TOC module 5100 ......................................................................................................179
17.8 Standards and directives ..................................................................................................................................180

6
multi EA 5100 About this user manual

1 About this user manual

The multi EA 5100 analyzer is intended for operation by qualified personnel with the
aid of this user manual.
The user manual contains descriptions of the design and operation of the multi EA 5100
and provides personnel experienced in analysis with the necessary information for the
safe handling of the basic module and its components. The user manual also includes
notes on the maintenance and care of the equipment and potential causes and remedies
for any faults.

Conventions Instructions for actions which occur in chronological order are numbered and combined
in action units.
Warnings are indicated by a warning triangle and a signal word. The type, source and
consequences of the hazard are stated together with notes on preventing the hazard.
Elements of the control and analysis program are indicated as follows:
¡ Program terms are in bold (e.g., the System menu).
¡ Buttons are indicated by square brackets (e.g., [OK]).
¡ Menu items are separated by vertical lines (e.g., System | Device).

Symbols and signal words used The user manual uses the following symbols and signal words to indicate hazards or in-
in this manual structions. The warnings are always placed before an action.

WARNING
Indicates a potentially hazardous situation which can cause death or very serious (possi-
bly permanent) injury.

CAUTION
Indicates a potentially hazardous situation which can cause slight or minor injuries.

NOTICE
Provides information on potential material or environmental damage.

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Intended use multi EA 5100

2 Intended use
The multi EA 5100 is a modular analyzer for determining the sulfur, nitrogen, chlorine
and carbon content in solid, liquid, paste-like, viscous and gaseous samples. Sample di-
gestion is achieved via pyrolysis and subsequent thermal oxidation of the achieved result
of the pyrolysis. The various element contents are determined in accordance with na-
tional and international standards by subsequent selective detection systems.
Depending on the functionality, the basic module includes at least one detection module
and one sampling module. The basic module and any connected modules are controlled
by the multiWin control and analysis software, and the analysis of the measurement
data is performed in this as well.
The analyzer may only be used for the analyses listed in the user manual. Only this spec-
ified use is regarded as the intended use, ensuring the safety of the user and the device.

Suitable sample types for the The analyzer can be used for the following sample types:
multi EA 5100 ¡ Organic solids, e.g., wax, polymer
¡ Organic liquids, e.g., fuels, solvents
¡ High-viscosity organic liquids, gels and paste-like samples, e.g., crude oil, asphalt,
bitumen, tar
¡ Organic gases and gas mixtures, e.g., natural gas, methane
¡ Compressed liquefied gases, e.g., LPG, NPG, butane, propane, propylene
¡ Carbon modifications, e.g., coal, elemental carbon, soot, coke
¡ TC/TOC/TIC/NPOC in water analyses, e.g., waste water
¡ EC/OC determination in particulate emissions, e.g., air quality control, three-way
catalytic converter research
¡ AOX and EOX for water, sludge and soil via the column or batch method

Unsuitable samples The following sample types may not be analyzed with the multi EA 5100:
¡ Highly flammable organic compounds – risk of explosion!
¡ Self-reactive materials and explosives, e.g., peroxides, epoxides, azides
¡ Organic and inorganic phosphorous compounds, e.g., phosphoric acid ester
¡ Silico-organic and reactive or unstable inorganic silicium compounds, e.g., silane
¡ Metal organic compounds, e.g., nickel carbonyl
¡ Corrosive or highly-reactive substances, inorganic acids, HF, Cl2, H2SO4
¡ Materials with high inorganic or organic salt content, in particular Na+ und K+ ions,
e.g., soil, fertilizers, feed, construction material
¡ Inorganic compounds, e.g., minerals, inorganic halogens
¡ Samples requiring more than 1100 °C for complete oxidation or digestion, e.g., met-
als, alloys, N2
¡ Pure elements, e.g., sulfur, nitrogen
¡ Sample with element contents exceeding the permissible operating range.
¡ TOC, TIC or TC analyses of solids, e.g., soil, sediment
Alkali salts and alkaline earth salts lead to crystallization of all quartz glass components
This process is accelerated by increased salt concentrations and combustion tempera-
tures, i.e. reducing the service life of the quartz glass components.

Gases used The device must only be used with argon and oxygen of the required quality as a carrier
gas.

Sum parameters Attaching the corresponding detectors and sampling modules allows the multi EA 5100
analyzer to determine the following parameters as sum parameters.

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multi EA 5100 Intended use

Parameter Description
TS Total sulfur
Organically bound sulfur is detected. Inorganic sulfur compounds are
only digested partially or not at all.
TN Total nitrogen
Organically bound nitrogen is detected. Inorganic nitrogen compounds
and molecular nitrogen (N2) are only digested partially or not at all.
TC Total carbon
The total organic carbon and elementary carbon and contained CO2 is
detected. Inorganic carbon compounds are only digested partially or not
at all.
TX Total chlorine
The organically bound chlorine contained in the sample is detected.
Bromide and iodine compounds are only detected partially. Fluorine
compounds are not detected at all. The result is output as defined as to-
tal chlorine. Inorganic halogen compounds are only digested partially or
not at all.
EOX Extractable organically bound halogens
The EOX parameter is the sum of organically bound halogens (chlorine,
bromide, iodine) extracted under defined conditions from a water sam-
ple or from solids (sludge and sediment) using an organic solvent. Fluo-
rine is not detected.
AOX Adsorbable organically bound halogens
The AOX parameter is the sum of organically bound halogens (chlorine,
bromide, iodine) adsorbed under defined conditions (pH < 2 with
HNO3) from a water sample or a solid sample (sludge and sediment) in
active carbon using the vibration or column method. Fluorine is not de-
tected.
EC/OC Elementary carbon/organic carbon
The content of elementary carbon of a sample is detected directly after
the thermal desorption of the organic carbon. The amount of organic
carbon is then determined sequentially after thermal oxidation of the
remaining sample.
The following parameters can be determined from aqueous samples with the multi EA
5100:
Parameter Explanation
TC Total carbon
TIC Total inorganic carbon
The total inorganic carbon from carbonates, hydrocarbonates and dis-
solved carbon dioxide is determined.
TOC Total organic carbon
The total organic carbon content is determined mathematically by cal-
culating the difference: TOC = TC - TIC. Determination of the TC and TIC
content of the sample is required for this.
NPOC Non purgeable organic carbon
The total non-purgeable organic carbon content of a sample is de-
tected. Highly volatile organic compounds are not or only partially de-
tected.

9
Security multi EA 5100

3 Security
For your own safety and to ensure error-free and safe operation of the device, please
read this chapter carefully before commissioning.
Observe all safety instructions listed in this user manual and all messages and infor-
mation displayed on the monitor by the control and analysis software.

3.1 Safety labeling on the device

Warning and mandatory action labels have been attached to the device and must al-
ways be observed.
Damaged or missing warning and mandatory action labels can cause incorrect ac-
tions leading to personal injury or material damage. The labels must not be removed.
Damaged warning and mandatory action labels must be replaced immediately!
The following warning and mandatory action labels have been attached to the de-
vice:
Warning sym- Meaning Comment
bol
Warning against dan- In the device interior on the electronics
gerous electrical volt- cover
age Warning against electrical voltage. Be-
fore opening the electronics the device
must be disconnected from the mains.
Warning about hot In the device interior on the combus-
surface tion furnace
On the top cover of the combustion
furnace
On the heated gas transfer line from
the Cl module 5100
Touching the furnaces or the ends of
the gas transfer lines during operation
or shortly after shutdown of the device
can result in burn injuries.
Warning against cor- On the "high sensitive" measuring cell
rosive substances of the Cl module 5100
Exercise caution when handling the
electrolyte solution. It contains highly-
concentrated acetic acid.
On the sulfuric acid container and the
safety attachment of the Cl module
5100
Exercise caution when handling con-
centrated sulfuric acid
Warning against UV In the S module 5100 (basic, MPO)
radiation Switch off the detection module before
performing maintenance on the UV
lamp.

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multi EA 5100 Security

Warning sym- Meaning Comment

bol
Caution (GHS07) On the absorber and the chemical
ozone decomposer of the N module
5100
On the chemical ozone decomposer of
the S module 5100 MPO
The cartridges contain hazardous sub-
stances. Do not open the cartridges.
Only replace the entire cartridge.

Mandatory ac- Meaning Comment

tion labels
Disconnect the power On the rear panel of and/or the side
supply before open- panels of the basic module and the de-
ing the device cover. tector modules
In the device interior on the electronics
cover
Observe the operat- On the rear panel of and/or the side
ing manual panels of the basic module and the de-
tector modules

3.2 Requirements for the operating personnel

The device must only be operated by qualified specialist personnel instructed in the
use of the device. This instruction also include teaching the contents of this user
manual and of the user manuals of the connected system components. We recom-
mend training by qualified employees of Analytik Jena or its representatives.
In addition to the safety instructions in this user manual, the general applicable
safety and accident prevention regulations of the respective country the device is op-
erated in must be observed and adhered to. The operator must ensure the latest ver-
sion of these regulations.
The user manual must be accessible to the operating and service personnel.

3.3 Safety instructions, transport and commissioning

Incorrect installation can create serious hazards. This may result in electric shock and
explosion if the gases are not connected correctly.
¡ Only the Analytik Jena GmbH customer service or specialist personnel trained
and authorized by them is allowed to install and commission the device and its
system components.
¡ Unauthorized assembly and installation is not permitted.
Insufficiently secured components pose a risk of injury.
¡ During transport, secure the device components as specified in these operating
instructions.
¡ Loose parts must be removed from the system components and packed sepa-
rately.

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Security multi EA 5100

To prevent health damage, the following must be observed when moving the device
in the laboratory (lifting and carrying):
¡ For safety reasons, two persons are required to transport the device who must
hold the unit by either side of the equipment.
¡ The device does not have any carrying handles. Therefore the device must be
gripped firmly with both hands at the lower end.
¡ Risk of damage to health due to improper decontamination! Perform a profes-
sional and documented decontamination of the device before returning it to An-
alytik Jena. The decontamination report is available from Service when register-
ing the return. Service must refuse acceptance of contaminated devices. The
sender may be liable for damage caused by inadequate decontamination of the
device.

3.4 Safety instructions: during operation

3.4.1 General safety instructions during operation

The operator must make sure that the device and its safety equipment is in sound
condition each time before starting up the device. This applies in particular after
each modification or extension of the device or its repair.
Observe the following:
¡ The device may only be operated if all items of protective equipment (e.g. covers
in front of electronic components) are in place, properly installed and fully oper-
ational.
¡ The sound condition of the protection and safety equipment must be checked
regularly. Any defects must be corrected as soon as they occur.
¡ Protective and safety equipment must never be removed, modified or switched
off during operation.
¡ Free access to the power switch on the back of the enclosure must be ensured
during operation.
¡ The ventilation equipment on the device must be in good working condition.
Covered ventilation grilles or slots etc. may cause the device to break down or
may cause damage to it.
¡ The furnace operates at temperatures of 700 to 1100 °C. Hot components must
not be touched during or directly after the operation of the device.
¡ Caution when handling glass components. Risk of broken glass and therefore risk
of injury!
¡ Keep all combustible materials away from the analyzer.
¡ When operating the sampling modules (Autoinjector, MMS and ABD), there is a
crushing risk for hands and fingers. Maintain a safe distance.
¡ When handling the Autoinjector, there is a danger of stabbing yourself in the
hand or finger with the syringe. Exercise caution when handling the syringe.
¡ When operating the multi-matrix autosampler with temperature control func-
tion (MMS-T or Multi Matrix Sampler with Liquids kit TMP), the syringe holder
and the sample tablet achieve temperatures of up to 80 °C during heating. These
hot components present a risk of burn injuries.

3.4.2 Safety instructions – protection against explosion and fire

The device may not be operated in an explosive environment.

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multi EA 5100 Security

Smoking or handling open flames are prohibited in the room in which the device is
operated!

3.4.3 Safety instructions: electrical equipment

Lethal voltages may occur in the device! Contact with live components may cause
death, serious injury or painful electrical shock.
¡ The power plug must be connected to a proper power outlet to ensure that the
device meets protection class I (ground connector). The device may only be con-
nected to power sources whose nominal voltage is the same as that on the rating
plate of the equipment. Do not replace the removable power cable of the device
with a power cable that does not meet the specifications (with no protective
ground conductor). Extensions of the supply cable are not permitted!
¡ The basic module and the system components may only be connected to the
mains when they are switched off.
¡ Electrical connection cables between the basic module and the system compo-
nents may only be connected or disconnected when the device is switched off.
¡ Before opening the device, the device must be switched off at the main switch
and the power plug must be disconnected from the power outlet! The only ex-
ception is for instructions that explicitly indicate that the doors of the basic mod-
ule or of a detection module must be opened during operation. This is the case,
for example, during the end point routine of the Cl module 5100 or when
searching for a gas leak in the measuring gas connection between the basic
module and the Cl module 5100.
¡ Work on the electronics may only be carried out by the customer service of Ana-
lytik Jena and specially authorized technicians.

3.4.4 Handling of auxiliary and operating materials

The operator is responsible for the selection of substances used in the process as well
as for their safe handling. This is particularly important for radioactive, infectious,
poisonous, corrosive, combustible, explosive and otherwise dangerous substances.
When handling hazardous substances, the locally applicable safety instructions and
instructions in the safety data sheets from the manufacturers of the auxiliary and op-
erating materials must be complied with.
Hazardous substances are used during operation of the following detection modules:
Detection module Hazardous substance Use
Cl module 5100 Concentrated sulfuric Drying agent in the sul-
acid furic acid container
Acetic acid Preparing the electrolyte
Concentrated nitric acid solution

Methanol
Thymol
S module 5100 coulo- Acetic acid Preparing the electrolyte
metric solution
TOC module 5100 40 % orthophosphoric Reagent in the TIC reac-
acid tor
0.2 mol/l hydrochloric Reagent for NPOC de-
acid termination

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Security multi EA 5100

Acetic acid vapors causing strong irritation of the airways can occur in the measuring
cell of the Cl module 5100. Connect the measuring cell with the exhaust hose and
connect the detection module to the laboratory exhaust unit.

3.4.5 Decontamination after soiling

Observe the following:

¡ The operator is responsible for carrying out suitable decontamination should the
device become contaminated externally or internally with dangerous substances.
¡ Splashes, drops or larger liquid spillages should be removed using an absorbent
material such as cotton wool, laboratory wipes or cellulose.
¡ For biological contamination, wipe the affected area with a suitable disinfectant,
such as an Incidin Plus solution. Then wipe the cleaned areas so that they are
dry.
¡ The only suitable cleaning method for the housing is wipe disinfection. If the dis-
infectant has a spray nozzle, apply disinfectant to a suitable cloth before using it
on the device.
Particular care must be taken if infectious materials are analyzed with the device,
as the device cannot be decontaminated as a single unit.
¡ Before using a cleaning or decontamination procedure other than that pre-
scribed by the manufacturer, the user is required to check with the manufacturer
that the intended procedure will not damage the device. Safety labels attached
to the device must not have methanol applied.
¡ If a Cl module 5100 is used: Concentrated sulfuric acid is used as a drying agent
in the detection module. The electrolyte solution in the "high sensitive" measur-
ing cell has a high concentration of acetic acid. To decontaminate, rinse out the
sulfuric acid container with its safety attachment and the measuring cell with
distilled water.

3.4.6 Behavior during overpressure faults (0206, gas pressure fault)

Extreme caution is required during system overpressure! Incorrect operation can en-
danger the operating personnel and damage the analysis system. If an overpressure
fault is detected, a warning message will appear in the multiWin program.
Observe the following:
¡ Never switch off a device subject to overpressure!
¡ Do not introduce any samples.
¡ Do not close the program.
¡ Do not switch off the modules.
¡ Do not switch off the gas supply.
¡ N/S/C branch: Wait until the overpressure in the system has dropped to normal
pressure. The routine for reducing the overpressure in the N/S/C branch runs au-
tomatically.
¡ Chlorine branch: For devices with an operational Cl module 5100, ventilation
must be performed manually (→ "Recommissioning after emergency shutdown
(Cl module 5100)"  40).
¡ After relieving the overpressure remove the obstruction in the gas path.

3.5 Behavior during emergencies

Observe the following:

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multi EA 5100 Security

¡ If there is no immediate risk of injury, switch off the device and the connected
system components immediately in hazardous situations or in the event of an
accident and/or disconnect the power plugs from the power outlets.
¡ Close the oxygen gas supply as soon as possible after switching off the equip-
ment!
¡ When closing the argon gas supply, a return of the acid used can occur in the Cl
module 5100. For this reason, the measuring gas lines to this module must be
disconnected before closing the argon gas supply.
¡ When attaching the Cl module 5100: There is a risk of injury from sulfuric acid!
During an emergency shutdown the vacuum may draw sulfuric acid into the
transfer line and the auto-protection valve assembly during the cooling down pe-
riod. After an emergency shutdown, check that the transfer line and the auto-
protection valve assembly are not contaminated with sulfuric acid (→ "Recom-
missioning after emergency shutdown (Cl module 5100)"  40) before recom-
missioning.
¡ When closing the gas supply, a return of the slightly acidic electrolyte solution
and the phosphoric acid in the TIC reactor can occur in the S module 5100 coulo-
metric and the TOC module 5100. Check the measuring gas hoses for contami-
nation before recommissioning. Observe the safety instructions for handling
acidic solutions during cleaning.

3.6 Safety instructions – maintenance and repair

The device is generally maintained by the customer service department of Analytik

Jena or specialist personnel trained and authorized by them.
Unauthorized maintenance can damage the device. For this reason, only the activi-
ties described in the user manual in the "Maintenance and care" chapter may be per-
formed by the operator.
¡ Only clean the exterior of the device with a slightly moistened, non-dripping
cloth. Use only water and, if required, customary surfactants.
¡ Do not use any organic solvents or abrasives to clean the device. Exercise caution
when decontaminating the device with disinfectants containing alcohol. The al-
cohol can damage the safety labeling on the device.
¡ All maintenance and repair work on the device must only be carried out when
the device is switched off (unless specified otherwise).
¡ Maintenance work and the replacement of system components (e.g., the re-
moval of the combustion tube) must only be carried out when the device has
cooled down sufficiently.
¡ The gas supply must be shut off before performing any maintenance or repair
work (unless specified otherwise).
¡ All protective equipment must be reinstalled and checked for proper function
when the maintenance or repair work is complete.
¡ Ensure that all connections are gas-tight again after maintenance.
¡ Use only original spare parts, wear parts and consumables. They have been
tested and ensure safe operation. Glass part are wear parts and are not subject
to the warranty.
¡ During maintenance of the combustion tube and of the auto-protection valve as-
sembly, there is a risk of injury due to falling parts. Exercise extreme caution
when handling the two components.

15
Function and design multi EA 5100

4 Function and design

4.1 multi EA 5100 basic module

The multi EA 5100 analysis system is modular and can be adapted to each measuring
tasks by combining it with different detectors and sampling modules. The analysis sys-
tem is used to determine the sulfur, nitrogen, chlorine and carbon content in solid, liq-
uid, paste-like, viscous and gaseous samples. It can additionally analyze the AOX, EOX,
EC/OC or TOC, NPOC and TIC sum parameters.
The core of the analyzer system is the multi EA 5100 basic module, which performs
sample gas digestion and measuring gas drying. (As an exception, the measuring gas is
dried in the detection module for chlorine determination.)
The analysis system is controlled and the measurement data is evaluated via the multi-
Win control and analysis software.
A self-check system (SCS) is integrated into the analysis system. The SCS consists of a
combination of hardware components and software functions that automatically ensure
proper function of the entire analysis system. Depending on the system setup, the SCS
checks the important device safety and analysis quality parameters (e.g., gas flow, tem-
peratures, pressures, system integrity, baseline stability, signal drift, cooling time, flame
value, etc.) multiple times per second

4.1.1 Principle of operation

4.1.1.1 Vertical and horizontal operation

The basic module is equipped with a double furnace. This innovative technology enables
operation of the combustion furnace in vertical or horizontal mode. Switching between
the two operation modes is simple, and is performed by the user.

Vertical operation mode In vertical operation mode, the sample aliquot is injected directly into the multi-purpose
combustion tube via the injection port. The sampling module required is a multi-matrix
autosampler, an auto-injector, a GSS module or an LPG module.
Advantages of vertical operation mode:
¡ For gases, LPG, liquid samples with normal viscosity
¡ Best for N, A and Cl trace and ultratrace analyses
¡ Fast analysis
¡ Small bench space required

Horizontal operation mode In horizontal operation, solids and liquids are transferred to the multi-purpose combus-
tion furnace on boats with Automatic Boat Drive (ABD). Sample feeding can be auto-
mated with an autosampler in combination with the ABD. Liquids can alternatively be
transferred into the horizontal combustion furnace via the auto-injector.
Gases and LPG are injected directly via the injection port of the sample port of the ABD.
Advantages of horizontal operation mode:
¡ For gases, LPG, solids, liquid samples independent of viscosity
¡ Best for volatile liquids

16
multi EA 5100 Function and design

Sample feed
Liquid/LPG/gaseous

Sample feed
Solid/liquid/LPG/gaseous

C/N/S analysis Dryer

S detector
N detector
C detector

Flame sensor Quartz glass boat

Cooled sample port
Cl analysis - (EOX/TOX/AOX)
Coulometer

Figure 1 Operating modes of the multi EA 5100

4.1.1.2 Sample Digestion

TS, TN, TC, TX and EOX Sample digestion to determine TS, TN, TC, TX and EOX can be performed in vertical and
horizontal operation mode.
Digestion is a two-stage process at 1000 to 1100 °C via pyrolysis with subsequent ther-
mal oxidation. In the first phase, the sample components are pyrolyzed in an argon flow,
and the generated pyrolysis gases are incinerated in an oxygen flow. Next, the remain-
ing pyrolysis products are re-incinerated in a pure oxygen flow during the second phase.
This digestion is summed up via the following equations:
R*-H + O2 → CO2 + H2O
R*-N + O2 → NOx + CO2 + H2O
R*-S + O2 → SO2 + CO2 + H2O
R*-X** + O2 → HX** + CO2 + H2O
R* - carbonic substance
X** - F-, Cl-, Br-, I-

TOC Digestion for TOC determination is performed in vertical operation mode via thermal ox-
idation in an oxygen flow at 700 °C. The aqueous samples are injected directly into the
TOC combustion tube via the injection port.

TIC Digestion for TIC determination is performed in the TOC module via wet chemical oxida-
tion with phosphoric acid. The aqueous samples are injected into the TIC reactor manu-
ally.

AOX Digestion for AOX determination is performed in the horizontal operation mode. The
loaded active carbon is combusted in the oxygen flow at at least 950 °C and forms hy-
drogen halogen, carbon dioxide and water. The loaded active carbon is transferred to
the multi-purpose combustion tube with or without a quartz container in the quartz
glass boat with ABD.

17
Function and design multi EA 5100

EC/OC Digestion for EC/OC determination is performed in horizontal operation mode. Digestion
is performed in two phases. In the first process phase, the OC content adsorbed on the
filter samples is thermally desorbed in a pure argon flow. The gaseous products are then
re-incinerated in oxygen. In the second process phase, the remaining EC proportion in
pure oxygen is converted completely to CO2.
The filter samples are transferred to the combustion furnace via the ABD and a special
feed program.

4.1.1.3 Measuring gas dryer

After leaving the combustion tube, the mixture is dried before it is transferred to the de-
tectors.
Parameter Method
TS, TN, TC, EC/OC Membrane dryer (in the basic module)
TX, AOX, EOX Concentrated sulfuric acid (in the Cl module 5100)
TOC, NPOC, TIC Condensation through Peltier cooling (in the TOC module
5100)

4.1.2 Design of the basic module

4.1.2.1 Main components

Main components of the basic The multi EA 5100 basic module contains the following main components:
module ¡ Electronics/internal device control
¡ Gas supply
¡ Combustion system
¡ Measuring gas transfer
All basic module components that must be operated or maintained by the user can be
accessed via the 2 doors on the front side or via the removable side panels.
Electrical connection and gas connections) and the interfaces for connecting the system
components are on the rear of the device.
Double furnace device ¡ Vertical and horizontal operating mode possible
¡ Opening with maintenance flaps at the right-hand side panel
Vertical operation ¡ Furnace in vertical installation position
¡ Right side panel closed

18
multi EA 5100 Function and design

7 1

6
2

3
5

Figure 2 Front view in vertical operation mode

1 Ventilator 2 Control electronics
3 Membrane dryer unit 4 Tilt device
5 Pump connection for N/S/C mode 6 Combustion furnace
7 Knob for tilting the furnace

Horizontal operation ¡ Furnace in horizontal installation position

¡ Opening with maintenance flaps at the right-hand side panel

1
4

2
3

Figure 3 Basic module in horizontal operation mode

1 Control electronics 2 Combustion furnace
3 Auto-protection valve assembly 4 Gas box

19
Function and design multi EA 5100

4.1.2.2 Electrical components, display elements and connections

Internal device control The control electronics are found on the rear of the basic module behind the panel when
viewed from the front. The control electronics provides the power supply and control of
the individual components and the communication with the control PC and other con-
nected system modules.

Operational LED

Figure 4 Basic module with a sampling module and a detection module.

A green LED is installed on the left door of the basic module After loading the control
and analysis software, the LED lights up, indicating that the device is ready for opera-
tion.

Power switch, ports, connec- The power switch and the interfaces for connecting the system modules and for con-
tions necting the control PC can be found on the rear of the device.
The control PC can be connected via a USB port. The interfaces for connecting the sam-
pling modules and for connecting the detectors are RS 232 interfaces.

20
multi EA 5100 Function and design

1
2

Figure 5 Interfaces on the rear of the device

1 Gas connectors 3 USB port for PC
2 Power connection, power switch 4 Interfaces for detector modules and
sampling modules

Figure 6 Power connection, power switch

1 Power switch 2 Equipment fuse
3 Power connection

21
Function and design multi EA 5100

11

10 9 8 7 6 5 4
Figure 7 Interfaces for detector modules and sampling modules
1 "External" connection 2 Autoinjector connection
3 "Flame" flame sensor connection 4 S-coulometer connection
5 S-UVF connection 6 CI-coulometer connection
7 N-CLD connection 8 C-NDIR connection
9 Sampler connection (RS-232 bus) 10 Service connection
11 Control PC connection

Interfaces in the device The electrical connections for the combustion furnace, the flame sensor and the temper-
ature sensor can be found on the rear interior side of the device. The connections are
only accessible in the vertical installation position of the combustion furnace.

1 2 3
Figure 8 Connection for the sensors and the combustion furnace in the device
1 Temperature sensor 2 Combustion furnace
3 flame sensor
The connections for the auto-protect valve assembly and the heated transfer line (only if
the CI module is connected) can be found in the frame behind the door. The toggle
switch for opening and closing the pneumatic seal in the auto-protection valve assembly
is also located there.

22
multi EA 5100 Function and design

1 2 3
Figure 9 Connections for the auto-protection valve assembly and transfer line
1 Toggle switch for opening and clos- 2 Transfer line heating connection
ing the pneumatic seal in the auto-
protection valve assembly
3 Valve assembly connection

4.1.2.3 Gas supply/hose diagrams

Hose diagrams The connection between the individual components is made with labeled hoses. The
numbers circled in the hose diagram match the labels on the hoses in the multi EA
5100.

23
24
Function and design

to the N/S/C detector

9 Filter
Filter 1 2 16

N/S/C Exhaust
outlet
Ar O2 ABD
7 15 Gas box
MFM
main

bypass
inlet

seal

dryer
Pump

6 3
8 12 11 4
Cl system tightness
test
Rotary bearing

Combustion furnace
10

Figure 10Hose diagram for horizontal operation

Coupling
14 ABD

Rotary bearing
13
5
Membrane dryer
multi EA 5100
 to the N/S/C detector

9 Filter 1 2
multi EA 5100

N/S/C Exhaust
outlet
Ar O2 ABD 3
main
7 15
4
MFM inlet
Pump
11
6
seal
13
Membrane dryer

Cl system tightness

Gas box
12

Figure 11 Hose diagram for vertical operation

test
dryer

8
bypass

5
Combustion furnace

Rotary bearing
Rotary bearing

14
Coupling
10
to the Cl detector

25
Function and design
Function and design multi EA 5100

Gas connections at the rear of The gas connections are located on the rear of the device. The gas supplies for oxygen
the device and argon must be connected to the "IN O2" or "IN Ar" connection via the included con-
nection hoses (AD 6 mm, ID 4 mm.

5 1

Figure 12Gas connections at the rear of the device

1 Argon gas inlet (Ar) 2 Gas outlet to the N/S/C module
3 Purge gas outlet of the membrane 4 Oxygen gas inlet (O2)
dryer with "exhaust" filter
5 Gas outlet to the ABD

Gas connections on the gas box The two process gases, argon and oxygen, are controlled via the gas box in the basic
module. The gas box is located on the left side of the device.

26
multi EA 5100 Function and design

Figure 13Gas connections on the gas box

1 "main" – oxygen supply to the com- 2 "inlet" – argon supply to the combus-
bustion tube (hose 3) tion tube (hose 4)
3 "seal" – argon connection for the seal 4 "dryer" – dry gas flow (oxygen) for
of the auto-protection valve assem- the membrane dryer (hose 12)
bly (hose 11)
5 "bypass" – argon connection for the
safety purging (safety bypass) of the
chlorine branch (hose 8)

Connections on the combustion

tube

2
1

Figure 14Connections on the combustion tube

1 Flame sensor connection (only if ABD is connected in horizontal mode)
2 Ar hose 4 connection (in horizontal operation mode, no argon is supplied
here, argon is supplied via ABD)
3 O2 hose 3 connection

27
Function and design multi EA 5100

Gas supply control The composition of the gas mixture for optimum gas digestion is controlled via the flow
management system (FMS).

4.1.2.4 Combustion system

A resistance-heated combustion furnace for digestion temperatures of 700 to 1100 °C is

used in the basic module. Digestion with the multi-purpose combustion tube is per-
formed at temperatures of 950 °C or 1000 to 1100 °C, depending on the application.
The double furnace device can be switched to the required operating mode quickly via
the tilt device.

Figure 15 Combustion furnace in the vertical and horizontal operating mode

A multi-purpose combustion tube used for all standard applications, both in vertical or
horizontal operation mode, is installed in the combustion furnace. The combustion tube
is made of quartz glass. The auto-protection assembly group connects the combustion
tube to the measuring gas dryer or the further path of the measuring gas.

1
3

2
Figure 16 Multi-purpose combustion tube
1 Oxygen supply connection 2 Argon supply connection
3 Flame sensor connection 4 Screw cap with septum (only for vertical opera-
tion mode and operation with an auto-injector)

28
multi EA 5100 Function and design

4.1.2.5 Measuring gas dryer

Measuring gas is dried in accordance with the measuring method:

¡ To determine TS, TN, TC, EC/OC via membrane dryer:
The membrane dryer is mounted on the furnace. To increase drying effectiveness,
purge gas (O2) is drawn through the membrane dryer with a pump. The membrane
dryer is maintenance-free.

Figure 17Membrane dryer

¡ To determine TX, AOX, EOX via concentrated sulfuric acid:
Sulfuric acid is dried in the Cl module 5100. The measuring gas is routed to the sul-
furic acid container via a transfer line.
¡ To determine TOC, NPOC, TIC via condensation with Peltier cooling in the TOC mod-
ule 5100.

4.2 Sampling modules

4.2.1 Auto-injector

There are two types of auto-injector. The classic auto-injector is suitable for vertical and
horizontal operation mode, while the Autoinjector AI-EA is only used in vertical opera-
tion mode.
The auto-injectors are suitable for the following applications:
¡ In vertical operation mode for non-viscous liquids and colorless EOX extracts
¡ In horizontal operation mode only for volatile liquids
The auto-injectors are unsuitable for the following sample types:
¡ Viscous liquids and their solutions
¡ Solids suspended in solution
¡ Colored EOX extracts
¡ Water analyses (TC/NPOC determination)

29
Installation and commissioning multi EA 5100

5 Installation and commissioning

5.1 Installation conditions

5.2 Installation location requirements

Ambient conditions The climate conditions for the installation location are listed in the technical data (→
"Technical data for the multi EA 5100 "  172). If required, ensure that the room is
temperature-controlled.

Laboratory conditions The device is only approved for indoor use. The installation location should have the
characteristics of a chemical laboratory. It must meet the following conditions:
¡ Atmosphere free from hydrocarbons, halogens, sulfur compounds and nitrogen ox-
ides
¡ Atmosphere with low dust levels
¡ No vibrations
¡ No smoking in the operating room of the device

Installation location require- The requirements for the installation location of the device are as follows:
ments ¡ No caustic vapor in the immediate vicinity of the device and its system components.
These could corrode the device connections and modules.
¡ Free from draft air; do not install the device close to windows or doors
¡ Away from electromagnetic sources of interference
¡ No direct sunlight and away from radiant heaters
¡ The front door and air vents must not be obstructed by other equipment or furnish-
ings
¡ Maintain a safety distance of at least 20 cm from the rear of the device to other de-
vices or walls.

5.3 Power supply

WARNING
Danger due to electrical voltage
¡ Only connect the device to a properly grounded socket which complies with the volt-
age indicated on the device’s rating plate.
¡ Do not use an adapter in the feeder.

The device operates on single-phase alternating current.

The installation of the electrical equipment in the laboratory must comply with the DIN
VDE 0100 standard. At the connection point, an electrical current in accordance with the
standard IEC 38 must be available.
The electrical connection data can be found in the technical data (→ "Technical data for
the multi EA 5100 "  172).

30
multi EA 5100 Installation and commissioning

5.4 Gas supply

The operator is responsible for the gas supply and the corresponding connections and
pressure reducers.
The connection hoses with outer diameter (AD) 6 mm and inner diameter (ID) 4 mm
are provided with the device. Their lengths are 2 m. If other lengths are preferred,
please contact the Analytik Jena GmbH customer service department. The required gases
and their qualities are listed in the technical data (→ "Technical data for the multi EA
5100 "  172).

5.5 Device layout and space requirements

The space required for the modular analysis system depends on all the components that
make up the measuring station. The analysis station always includes:
¡ Basic module
¡ 1 sampling module (to the right of the basic device or on top of it)
¡ 1 detection module (to the left of the basic device)
Several modules may also be placed in a row.
Component Width x Height x Depth Mass [kg] Arrangement
[mm]
Basic module 510 x 470 x 550 mm 25 kg
multi EA 5100
Detection modules
N module 5100 300 x 500 x 550 mm 13 kg As last detector in a
row
S module 5100 300 x 470 x 550 mm 13 kg Left/right of other
basic detectors
S module 5100
MPO
Cl module 5100 300 x 470 x 530 mm 12 kg To the immediate left
of the basic module
S module 5100 300 x 470 x 530 mm 11 kg Left of the Cl module
coulometric 5100
C module 5100 300 x 470 x 530 mm 12 kg Left/right of other
detectors
TOC module 5100 300 x 470 x 530 mm 12 kg To the immediate left
of the basic module
or to the left of the Cl
module 5100
Sampling modules
ABD 520 x 210 x 500 mm 12 kg To the right of the
basic module
MBD 500 x 80 x 80 mm 0.35 kg To the right of the
basic module
Multi Matrix Sam- ca. 510 x 500 x 410 ca. 9.5 kg On the basic module
pler mm or on the ABD*

31
Installation and commissioning multi EA 5100

Component Width x Height x Depth Mass [kg] Arrangement

[mm]
Autoinjector 30 x 80 mm 0.5 kg Installed on the basic
(without syringe, module, or on the
⌀ x L) right of the basic
Auto injector cou- 80 x 110 mm module
pling (⌀ x L)
Autoinjector AI- 150 x 270 x 240 mm 1.5 kg On the basic module
EA
GSS/LPG combi 300 x 800 x 550 mm 11 kg/ To the right of the
module, GSS mod- 12 kg basic module or ABD
ule or LPG module
2.0
* For the temperature-controlled autosampler MMS-T and the Liquids kit TMP: There is
sufficient space provided for the inclusion of a thermostat (approx.
250 x 650 x 400 mm).

Figure 18Space required for the basic device and modules (vertical operation)

32
multi EA 5100 Installation and commissioning

Figure 19Space required for the basic device and modules (horizontal operation)

33
Installation and commissioning multi EA 5100

5.6 Installing and commissioning the analysis system

WARNING
Danger due to incorrect commissioning
¡ The analysis system may only be set up, mounted and installed by the Analytik Jena
GmbH customer service department.
¡ Any unauthorized access of the device can endanger the user and the operational
safety of the equipment and limits or completely voids any warranty claims.

NOTICE
Retain the transport packaging
Return transport for maintenance must be in the original packaging. This alone prevents
transport damage.

The basic module, the sampling modules and the detectors are unpacked and assembled
by the Analytik Jena GmbH customer service department or personnel trained and au-
thorized by them.
Check when unpacking the device for completeness and soundness of the delivery in ac-
cordance with the packing list included.
The customer service department tests the function of the analysis system after installa-
tion and documents the test.

Installing the basic module } Carefully remove the basic module and its components from the transport packaging.
Do not damage the transport packaging!
} Place the basic module at its intended location.
} Ensure adequate space for the additional system components (sampling modules,
detectors).
} Install the combustion furnace (→ "Removing and installing the combustion furnace"
 141).
} Install the auto-protection valve assembly (→ "Maintenance of the auto-protection
valve assembly"  131).
} Install the combustion tube in the combustion furnace (→ "Maintenance of the
multi-purpose combustion tube"  126).
} Place the additional system modules on their intended locations and connect them.

CAUTION
Danger of short circuit!
¡ Only connect the basic module and other system components when they are pow-
ered down and switched off.
¡ Before connecting the power supply cable, set the power switch of the rear of the
device to "0".
¡ Only use the IEC connection cable included in the scope of delivery for the connec-
tion to the power supply (VDE label, 1.5 m long). Extensions of the supply cable are
not permitted!

34
multi EA 5100 Installation and commissioning

NOTICE
Settled condensation and temperature differences can damage individual com-
ponents of the basic module during commissioning.
¡ If there is any temperature difference between the storage location and the operat-
ing location, allow the analyzer system to acclimatize for at least one hour in the
room it will operate in.

Connecting power and gases } Connect the power cable to the connection of the rear of the basic module.
} Connect the power plug to a grounded power outlet.
} Connect the supplied connection hoses to the pressure reducers of the gas supply
and the the O2 and Ar gas connections on the rear of the device (media connections
of the rear of the device).
} Set the inlet pressure on the pressure reducers (600 kPa (6 bar)).
} Connect the computer and connect it to the basic module via the supplied USB cable.
} Connect further system components (detectors, sampling modules) to the basic
module.
ü The basic module is now ready for operation and can be switched on.

3
2

Figure 20Media connections of the rear of the device

1 Power connection 2 USB port for computer
3 "O2" oxygen connection 4 "Ar" argon connection

35
Operation multi EA 5100

6 Operation

6.1 General notes for measuring operations

Only use the correct sampling modules for the corresponding matrix and installation po-
sition of the furnace for sampling.
Furnace installation Sample type Sampling
position
Vertical: Liquids ¡ Autoinjector
¡ Multi Matrix Sampler
MMS
Gas, non-pressurized ¡ GSS module
Gas, pressurized ¡ GSS/LPG combi module
¡ GSS module with GSS
adapterbox
LPG ¡ LPG module 2.0
¡ GSS/LPG combi module
Horizontal: Solids ¡ Automatic Boat Drive
ABD
¡ ABD with MMS
Liquids ¡ ABD with manual dosing
syringe
¡ ABD with MMS
¡ Autoinjector
Gas, non-pressurized ¡ GSS module
Gas, pressurized ¡ GSS/LPG combi module
¡ GSS module with GSS
adapterbox
LPG ¡ LPG module 2.0
¡ GSS/LPG combi module
Observe the following during analysis:
¡ To add samples of flammable substances in horizontal operation, always use ABD
with a flame sensor in automatic or automatic plus mode or an Autoinjector.
¡ To add samples of flammable substances, do not use the ABD in parameter mode,
or only use it with program parameters designed and tested for it (risk of soot!).
¡ Do not exceed the maximum permissible sample amounts (→ "Technical data for
the multi EA 5100 "  172).
¡ Adjust the dosing rate to the sample matrix and observe the maximum dosing
speeds (→ "Technical data for the multi EA 5100 "  172).
¡ Standard solutions with organic solvents can change composition rapidly due to the
volatility. Therefore, ensure that the clear space above the liquid in the sample cup
is small when preparing and storing samples. Store the solutions in the refrigerator.
The boiling points of the materials used should also not differ by more than 50 °C.
¡ Adjust the sample volume to the expected concentration to remain within the mea-
suring range of the detector.
¡ Begin the analysis with a standard solution and determine the daily factor. If the
value measured for the standard solution differs by more than 20 % from the target
value, repeat the measurement. If required, look for the source of the fault. If re-
quired, re-calibrate the analysis system.

36
multi EA 5100 Operation

¡ For examining very low element contents, examining a blind value is recommended
before the daily factor. The blind value measurement cleans the analysis system.

6.2 Selecting the measurement method

Select the proper measurement method for each sample with the following table.
Some parameters can only be analyzed with horizontally or vertically installed furnaces
¡ Horizontal: AOX, EC/OC
¡ Vertical: TOC, TIC, NPOC (in water)
For other samples, the recommended measurement method depends on the nature of
the sample.
Sample Furnace installation po- Comment
sition and sampling
TS, TN, TX, TC in:
Organic solids, e.g., wax, Horizontal for ABD with flame sensor
polymer ABD For trace analysis:
High-viscosity organic liq- ABD with MMS Use 1 quartz glass boat
uids, gels and paste-like for all samples
samples, e.g., crude oil, as- MMS with temperature-
phalt, bitumen, tar control unit in heating
Bio-Diesel mode for high-viscosity
Oils such as crude oil, paraf- liquids
fin oil and vegetable oil ABD without MMS for
Volatile liquids such as pe- non-homogeneous sam-
troleum ether, methanol, ples
naphtha
Liquids or solids with high
element content
(> 100 mg/l)
Organic liquids with normal Horizontal for ABD with flame sensor
viscosity, such as fuels, sol- Autoinjector
vents
ABD
ABD with Multi Matrix
Sampler
Vertical for For trace analysis: must
Autoinjector and Au- be vertical
toinjector AI-EA
MMS
EOX Horizontal for ABD with flame sensor
ABD Sample (colorless, col-
ABD with MMS ored) in n-hexane or pe-
troleum ether
Vertical for Only colorless samples in
MMS n-hexane

Autoinjector

37
Operation multi EA 5100

Sample Furnace installation po- Comment

sition and sampling
AOX Horizontal for Column method:
ABD Activated carbon in a
quartz container in a
ABD with MMS quartz glass boat
Batch method:
Activated carbon with no
quartz container in a
quartz glass boat with
holding-down clamp
EC/OC Horizontal for Filter in a quartz glass
ABD boat with hold-down
clamp
ABD with MMS
TC, TOC, NPOC in water Vertical for
Multi Matrix Sampler
or manual sampling
TIC in water Vertical (manual sam- Direct injection in the TIC
pling) reactor
Gas, non-pressurized Horizontal or vertical For trace analysis:
for Vertical + GSS module
GSS module recommended

with ABD (horizontal)

Gas, pressurized Horizontal or vertical
for
GSS/LPG combi mod-
ule
GSS module with GSS
adapterbox
with ABD (horizontal)
LPG Horizontal or vertical For trace analysis:
GSS/LPG combi mod- Vertical + GSS/LPG combi
ule module recommended

LPG module 2.0

with ABD (horizontal)

6.3 Switching on the basic module and the modules

Before switching on the basic module, always check:

¡ The other components (detection modules, sampling modules, PC) are connected to
the basic module.
¡ The gas supply is connected in accordance with instructions. The inlet pressure is ex-
actly 600 kPa (6 bar).
¡ The samples have been prepared.
Switch on the basic module as follows:
} Open the valves at the pressure reducers of the gas supply.

38
multi EA 5100 Operation

} Switch on all required components (detection modules, sampling modules, PC).

} Switch on the basic module via the power switch.
} The basic module boots up. The LED on the front lights up in green after approx 30
s.
} Start the multiWin program. Log in with user name and password.
} Click the [Initialize analyzer] button.
ü Initialization takes place after successful login.

NOTICE
Observe the run-in period
In the Status analyzer window, components that are not yet ready for operation are dis-
played in red. The heating time for 1050 °C is approx. 30 min. Measurement is not pos-
sible during the run-in period.
¡ If the analyzer is still not ready after approx. 30 min, perform a fault search (→
"Troubleshooting"  98).

6.4 Switching off the basic module and the modules

NOTICE
Risk of overheating
If the basic module is switched off too early, the electronics can overheat and become
damaged due to lack of cooling.
¡ Only switch off the basic module after a cooling time of 1 h.

Switch off the basic modules and its modules as follows:

} Exit the multiWin program.
} Switch off the connected modules via their respective power switches.
} Only switch off the basic module after a cooling time of 1 h.
If the system is switched off too early, the electronics inside the device can overheat
due to lack of cooling.
} If a Cl module 5100 is connected: Before closing the gas supply, remove the sulfuric
acid container from the module and completely drain the sulfuric acid.
} If a S module 5100 coulometric is connected: Before closing the gas supply, remove
the gas transfer line from the gas inlet tube of the measuring cell.
} After switching off the modules, close the gas supply.
} Exit the Windows operating system and switch off the PC.
ü Shutdown of the basic modules and its modules is complete.

39
Operation multi EA 5100

6.5 Recommissioning after emergency shutdown (Cl module 5100)

WARNING
Chemical burns due to concentrated sulfuric acid
If a Cl module 5100 is connected to the basic module, sulfuric acid can still be in the gas
transfer line and the auto-protection valve assembly after an emergency shutdown.
¡ Wear protective clothing when working on the sulfuric acid container.
¡ Exercise particular caution when checking the gas transfer line and the auto-protec-
tion valve assembly.
¡ Observe all specifications in the safety datasheet.

CAUTION
Risk of burns from the hot furnace and from the gas transfer line
¡ Allow the device to cool before recommissioning.

Observe the following when recommissioning the basic module and Cl module 5100.
Vent the analysis system after an overpressure fault (fault message"206 – gas pressure
fault") as described in the following:
} Carefully disconnect the measuring gas hose from the measurement cell.
} Carefully disconnect the gas transfer line from the sulfuric acid container and remove
the sulfuric acid container from the module.
} Disconnect the gas transfer line of the auto-protection valve assembly in the basic
module. Remove the heating cable plug from its socket.
} Carefully remove the gas transfer line and check it for contamination with sulfuric
acid.
} If necessary, clean the gas transfer line:
– Rinse the gas transfer line with distilled water and then with ethanol.
– Dry the gas transfer line (e.g. by blowing it through with an inert gas).
} Wait for the pressure in the system to decrease. Then switch off the basic module.
Shut off the gas supply.
} Open the seal for the auto-protection valve assembly in the basic module. To do this,
flip the toggle switch up. Remove the valve assembly plug from its socket.
} Carefully remove the auto-protection valve assembly from the basic module and
check it for contamination with sulfuric acid.
} If necessary, clean and dry the assembly. Replace the filter.
If cleaning is not possible or if the auto-protection valve assembly is damaged, it
must be replaced prior to recommissioning.
} Reinstall the auto-protection valve assembly in the basic module. Connect the as-
sembly via the cable. Ensure that a filter has been inserted in the auto-protect valve
assembly.
} Refill the sulfuric acid container with sulfuric acid and insert it in the detection mod-
ule. Connect the measuring gas hose with the sulfuric acid container.
} Refit the gas transfer line:

40
multi EA 5100 Operation

– Connect the gas transfer line with the auto-protection valve assembly. Plug the
heating cable plug into its socket.
– Route the gas transfer line through the wall of the basic module top the detection
module. Connect the gas transfer line to the sulfuric acid container.
ü The basic module and the detection module can be switched back on again.

41
Nitrogen analysis with the N module 5100 multi EA 5100

7 Nitrogen analysis with the N module 5100

7.1 Function and design

7.1.1 Function and measuring principle

Expansion of the basic module with the detection module allows the determination of
the nitrogen content in solids, liquids, and gases via chemiluminescence.
Organic nitrogen compounds can be determined as a TN sum parameter with the analy-
sis system. Inorganic nitrogen compounds are only detected if they can be digested in
the combustion furnace. Pure nitrogen cannot be analyzed.
The chemiluminescence of the reaction between nitrogen monoxide (NO) and ozone
(O3) is used for the determination. This reaction creates nitrogen dioxide in its excited
state (NO2*) for a short time. During the transition to the base state, the nitrogen diox-
ide emits electromagnetic radiation in the visible light spectrum. The light emitted is
proportional to the NO2* concentration. This allows measurement of the concentration
via light. NO is the only substance involved in the reaction, which means that this
method is very selective and not influenced by any other constituents of the measuring
gas.
NO + O3 → NO2* + O2
NO* → NO2 + hv
The measuring gas is created during incineration of organic nitrogen compounds in the
basic module. It contains a mixture of NO and NO2, generally known as NOx.
R-N + O2 → NOx + CO2 + H2O
R: Hydrocarbon residue, NOx: Mixture of NO and NO2
The measuring gas is passed through a converter which renders the NO2 portion usable
for the reaction and hence for detection purposes. The converter reduces NO2 to NO.
The ozone required for the reaction is created in the device from the supplied oxygen
(O2). Excess O3 is removed in the ozone decomposer after the reaction. The toxic gas is
not released into the ambient air.

7.1.2 Design

The detection module is used to determine the nitrogen content via chemiluminescence.
All components required for determination are mounted inside the sealed housing.

42
multi EA 5100 Nitrogen analysis with the N module 5100

Figure 21Basic module with detection module and sampling module

The detection module consists of the following components:
Component Function
Micro-plasma chamber Preparation of ozone (O3) from oxygen
Converter Transformation of nitrogen dioxide
(NO2) into nitrogen monoxide (NO)
Reactor with sensor Reaction of nitrogen monoxide (NO)
with ozone (O3) to produce nitrogen
dioxide (NO2*)
Detection of the amount of emitted light
Chemical and thermal ozone decom- Decomposition of excess ozone (O3)
poser
Diaphragm pump Conveyance of the measuring gas
through the detector
Differential pressure sensor Regulation of the pressure compensa-
tion between the variable measuring gas
flow and the fixed suction flow of the
membrane pump.
Absorber Cleaning of the aspirated air before en-
tering the diaphragm pump

7.1.3 Connection

The equipment door at the front is closed tightly and cannot be opened. An LED is in-
stalled on the door. The LED flashes during the run-in period of the detection module
and lights up permanently when the module is operational.
The following connections can be found on the rear of the detection module:
¡ Main switch, power connection, device fuses
¡ Media connections for gases and waste
¡ Interface for connection to a basic module
¡ Service interface with programming button.
A diagram at the center on the rear of the device explains the different connections.

43
Nitrogen analysis with the N module 5100 multi EA 5100

9
8
7

6 1

Figure 22Rear of the nitrogen detector

1 O2 gas inlet 2 Measuring gas inlet
3 Measuring gas outlet 4 Absorber
5 Service interface, 6 Interface to the basic module
programming button
7 Power connection 8 Fuse holder
9 Equipment switch
The device switch for switching the detection module on and off is located on the top
right of the rear of the device (when viewed from the front). The device fuse and power
connection are located beneath it.
Communication with the basic module is performed via a 9 pin interface cable. The in-
terface of the rear of the detector is marked with "N-CLD".
The gas for producing ozone is connected to the "O2/air" quick-release connector on the
rear of the detector. The hose for the measuring gas coming from the basic module is
connected to the "sample in" gas inlet.
In order to equalize pressure differences caused by differing gas flows, it is possible to
use an absorber to allow air to enter the device. The absorber filters constituents from
the air which may distort the analysis.
The "service" interface is for service purposes only (monitoring function only). The trans-
mission data log of the detection module is output via this interface. A null modem cable
is required to connect. The programming button is also only for service purposes
(firmware updates).

44
multi EA 5100 Nitrogen analysis with the N module 5100

7.2 Installation

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

NOTICE
The detection module is equipped with a pump that can disrupt the function of other
optical detection modules or lead to serious errors.
¡ Always connect the detection module as the last in any series of the detectors.

} Install the detection module as the last in any series of detectors.

} Install the absorber on the rear of the device:
– Fasten the two holding clamps with the supplied screws.
– First press the absorber into the upper holding clamp and then into the lower
one.
– Connect hose 6 to the absorber. Do not pull the hose out of the device!

Figure 23Absorber
1 Hose 6 connection 2 Holding clamp
3 Absorber
} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!

45
Nitrogen analysis with the N module 5100 multi EA 5100

} Insert the oxygen hose in the "O2" connector.

NOTICE! To release the hose, press the red ring into the connector and pull the
hose out of the connection.
} Connect the detection module with the basic module via the interface:
"N-CLD" interface on the rear of the detection module
"N-CLD" on the rear of the basic module.
} Connect the measuring gas hose of the basic module to the "sample in" gas inlet on
the rear of the module.
} Connect an approx. 50 cm long hose to the "out" connection. Route the hose away
from the device.
ü Connection of the detection module is complete.
The hose at the "out" connection prevents reaction gases from being sucked back into the
device by the absorber, disrupting the analysis. The hose does not have to be connected
to the laboratory exhaust unit.

Figure 24Connecting detection modules to the basic module

1 Detection module interfaces 2 Measuring gas outlet (for measur-
ing nitrogen, sulfur, carbon)

46
multi EA 5100 Nitrogen analysis with the N module 5100

7.3 Operation

CAUTION
Risk of respiratory problems due to leaking ozone
If the gas hoses have not been properly connected to the ozone generator, ozone may
leak out of the detection module.
¡ If you can smell ozone, switch off the device and check the connection of the gas
hoses on the ozone generator.

} Switch on the basic module and the detection module.

ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.
} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.
} Select Start |Start - Analysis in the menu.
} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.
} Enter the sample ID for all sample in the Name field.
} Release all sequence lines
} Confirm the entries with [OK].
} Click the [Start Measurement] button.
ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

47
Chlorine analysis with the Cl module 5100 multi EA 5100

8 Chlorine analysis with the Cl module 5100

8.1 Function and design

8.1.1 Function and measuring principle

Expansion of the basic module with the detection module allows determination of the
chlorine content in solid, liquid, paste-like, viscous and gaseous samples. When doing
so, the device will determine the bromine and iodine content as proportions of the total
chlorine of the sample as well. Fluorine is not detected.
Organic halogen compounds can be determined as TX, AOX and EOX sum parameters
with the analysis system. Inorganic halogen compounds are only determined if they can
be digested via the combustion furnace. Halogen hydracids or pure halogens cannot be
analyzed.
Organic halogen compounds are incinerated into hydrogen halogen, carbon dioxide and
water in the basic module.
The measuring gas flow is routed to the detection module via a transfer line and dried
there. The hydrogen halogens (HCl, HBr, Hl) are determined there via microcoulometric
titration. Hydrogen flouride (HF) is not determined.
In the first step, hydrogen chloride HCl* dissolves in the electrolyte, and dissociates to
hydrogen and chloride ions (H+, Cl-) In the measuring cell, the chloride ions react with
silver ions created via electrolysis to form silver chloride (AgCl). To achieve the most
complete reaction to AgCl, titration is carried out in a strong acetic acid electrolyte. The
solubility product of AgCl is reduced in the acetic acid electrolyte.
R-X + O2 → HX + CO2 + H2O
HX* → H+ + X-
Ag → Ag+ + e-
Ag+ + X- → AgX
R: Hydrocarbon residue, X: Cl, Br, I, * HBr und HI are determined as proportions of AgBr
and AgI.
The end point of the titration is displayed potentiometrically. In accordance with Fara-
day's law, the amount of chloride ions can be calculated from the amount of charge ex-
pended to create the silver ions.

8.1.2 Design

The detection module consists of the following main components:

¡ Wide-range coulometer for amperometry and potentiometry
¡ Stirrer/cooling block for the measuring cell (with automatic cell detection)
¡ Measuring cells with electrodes
¡ Sulfuric acid container with safety attachment and gas inlet
¡ Connections, interfaces
¡ Electrode containers

48
multi EA 5100 Chlorine analysis with the Cl module 5100

4 2

Figure 25Design of the chlorine detector (without measuring cell)

1 Safety attachment 2 Sulfuric acid container
3 Stirrer/cooling block 4 Connections for electrodes,
measuring cells
The wide-range coulometer has 3 application ranges. A special measuring cell is used
for each application range:
¡ "high sensitive" for low chlorine content (e.g., fuels, LPG, EOX)
¡ "sensitive" for medium chlorine content (e.g., waste oil, AOX)
¡ "high concentration" for high chlorine content (e.g., waste, polymers, waste oil)
The measuring cells are automatically detected when they are inserted into the stirrer/
cooling block. When the detection module is switched on, the magnetic stirring rod in
the measuring cell starts moving. The preset cell temperature is 18 °C and can be modi-
fied as a method parameter in the control and analysis software.

The "sensitive" measuring cell The "sensitive" measuring cell is used for chlorine contents between 1 to 100 µg.
The measuring cell consists of the electrode space, which holds the electrolyte solution,
and the stirrer block in the detection module. A generator anode in the form of a stable
silver plate (silver circle) is located on the bottom of the electrode space. The magnetic
stirring rod runs above the anode.
The cell is sealed airtight with a lid and three knurled head screws. The lid has two
openings:
¡ The opening marked "electrode" is for the amperometric combined electrode.
¡ The unmarked opening is used for direct injection into the measuring cell or to con-
nect to the exhaust.

49
Chlorine analysis with the Cl module 5100 multi EA 5100

2
1

Figure 26Measuring cell "sensitive" with lid

1 Opening for combined electrode 2 Opening for direct injection and ex-
haust connection

2
1

Figure 27Equipped measuring cell

1 Combined electrode 2 Olive for connecting to the exhaust
The combined electrode is used for the "sensitive" and "high concentration" measuring
cells. It combines the indicator electrodes (Ag), the generator cathode (Pt) and the gas
inlet. The measuring gas hose can be connected directly to the electrode.
The combined electrode is rinsed thoroughly after measurement and stored in a dry
place.

50
multi EA 5100 Chlorine analysis with the Cl module 5100

1 5
2 3 4
Figure 28Combined electrode
1 Connector plug 2 Generator cathode (Pt)
3 Indicator electrodes (Ag) 4 Gas inlet to measuring cell
5 Measuring gas connection
(hose 20)

The "high concentration" mea- The measuring cell has the same function as the "sensitive" measuring cell, but has a
suring cell higher electrolyte volume. It is suitable for a chlorine content of 10 to 1000 µg, and is
recommended in particular for TX determination of highly contaminated waste and of
polymer samples with high PVC content.
Here, as well, the maintenance-free combined electrode is used.

1 2 3 4 5 6

Figure 29Measuring cell "high concentration" with lid

1 Knurled head screw 2 Opening for combined electrode
(labeled)
3 Opening for direct injection and 4 Electrode space with silver anode
exhaust connection
5 Magnetic stirring rod 6 Electrical connection of the
measuring cell

51
Chlorine analysis with the Cl module 5100 multi EA 5100

The "high sensitive" measuring This measuring cell is used for very low chlorine content (0.01 to 10 µg). In particular, it
cell is recommended for use in EOX determination or for gaseous sample.
The measuring cell consists of the base element with a magnetic stirring rod and lid. The
positions of the required components are marked inside the lid of the measuring cell.
The central borehole is intended for an adapter that is connected to the exhaust hose. It
is used as an exhaust for the acetic acid vapors.
The small unmarked opening is used for direct injection into the cell. This opening is
closed with a plug when measuring gas is routed into the measuring cell from the com-
bustion furnace.

3 8

4
2
7
5

1
6

Figure 30Measuring cell "high sensitive" with lid

1 Opening for the platinum electrode 2 Opening for the silver electrode
3 Opening for the gas inlet tube 4 Opening for direct injection
5 Opening for the sensor electrode 6 Opening for the reference electrode
7 Opening for exhaust connection 8 Measuring cell base element with
magnetic stirrer rod

52
multi EA 5100 Chlorine analysis with the Cl module 5100

6
7

1 2

5 3

Figure 31Lid of the "high sensitive" measuring cell equipped with all electrodes
1 Platinum electrode 2 Silver electrode
3 Gas inlet tube with Teflon screw 4 Opening for direct injection, with
connection (for measuring gas) plug
5 Sensor electrode 6 Reference electrode
7 Adapter for exhaust connection

Sensor and reference elec- The sensor and reference electrode are always inserted into the measuring cell together.
trodes
The sensor electrode has a chlorinated sensor pin which is inserted into the measuring
cell, and a gold contact. The sensor pin is touch-sensitive. Scratch protection is applied
to it for storage.
The reference electrode is supplied dry, with no bridging electrolyte. The same acetic
acid electrolyte solution used for the measuring cell is used as a bridging electrolyte. The
bridging electrolyte is applied via the filling opening. The reference electrode is ready for
measurement after a run-in period of approx. 4 h in the measuring cell.
The filling opening of the reference electrode must be open during operation. For short-
term storage, close the filling opening and place the dry protective cap on the electrode.
The openings in the lid of the measuring cell are designed to align the sensor pin of the
sensor electrode toward the diaphragm of the reference electrode.
A pre-amplifier is applied to the reference electrode. Its connection cables connect the
reference electrode with the sensor electrode and with the connection on the detection
module.

53
Chlorine analysis with the Cl module 5100 multi EA 5100

1
5
2
3

Figure 32Reference electrode and sensor electrode

1 Electrical connection 2 Filling opening for bridging elec-
trolyte
3 Holder for the reference electrode in 4 Diaphragm
the measuring cell lid
5 Pre-amplifier 6 Sensor electrode
A short hose with a T piece can be found in the accessories of the measuring cell. The
hose and the T piece are applied to the adapter and connected to the exhaust hose. One
side of the T piece remains open. The acetic acid vapors can be drawn out of the detec-
tion module effectively without the electrolyte solution evaporating too rapidly.
1

Figure 33Exhaust connection

1 T piece 2 Short hose
3 Adapter

Generator electrodes A pair of generator electrodes generate the silver ions needed for chemical precipitation.
The pair of electrodes consist of a platinum cathode with a salt bridge and a silver an-
ode.

54
multi EA 5100 Chlorine analysis with the Cl module 5100

3
1

Figure 34Platinum electrode with salt bridge

1 Platinum electrode with salt bridge, 2 Salt bridge
complete
3 Platinum electrode with screw-on
cap and sealing ring

Figure 35Silver electrode

55
Chlorine analysis with the Cl module 5100 multi EA 5100

8.1.3 Connection

An LED is installed on the front of the detection module. The LED lights up when the
module is switched on.
The power switch, the device fuse and the power connection are located on the rear of
the module. The RS 232 interface for connection to the basic module ("CL-Coul" inter-
face) is also located on the rear of the module. The gas outlet for connection to the ex-
haust hose of the laboratory exhaust system is located at the bottom left of the rear
panel.

5
4
3

Figure 36Rear of the chlorine detector

1 Interface to the basic module 2 Gas outlet
3 Power connection 4 Fuse holder
5 Equipment switch
The electrical connections for the measuring cells and electrodes are located on the in-
side of the detection module's rear panel. They cannot be interchanged. Each connector
only fits into one terminal.

56
multi EA 5100 Chlorine analysis with the Cl module 5100

1 2

5 4 3

Figure 37Measuring cell connections

1 Combined electrode connection 2 Measuring cells "sensitive" and "high
concentration" connection
3 Platinum electrode connection 4 Silver electrode connection
5 Sensor and reference electrode con-
nection (via pre-amplifier)

Measuring gas transfer A heated gas transfer line is used to transfer the measuring gas. It connects the combus-
tion system of the basic module with the sulfuric acid container in the detection module.
The hose of the gas transfer line is connected to the sulfuric acid container connection
with a banjo bolt with a conical nipple. The other end of the gas transfer line is con-
nected to the auto-protection valve assembly in the basic device.

7 1

5 2

4
4 3

Figure 38Connection of the heated gas transfer lines to the sulfuric acid container
1 Safety attachment 2 Sulfuric acid container
3 Hose for measuring gas infeed 4 Connector
5 Banjo bolt 6 Heated gas transfer line
7 Measuring gas transfer to the mea-
suring cell with PTFE connector
The measuring gas is routed into the measuring cell via the safety attachment of the
sulfuric acid container.
¡ The measuring gas hose is connected directly to the combined electrode with the
"sensitive" and "high concentration" measuring cells.

57
Chlorine analysis with the Cl module 5100 multi EA 5100

¡ A cut glass tube is used to feed gas into the "high sensitive" measuring cell.

Figure 39Gas infeed tube with PTFE connector

In both cases, the measuring gas hose is fastened with the aid of a PTFE connector. En-
sure the proper fit of the sealing rings!

Figure 40Gas infeed to the "sensitive" measuring cell

58
multi EA 5100 Chlorine analysis with the Cl module 5100

8.2 Installation

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

} Place the detection module to the immediate left of the basic module.
} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!
} Connect the detection module with the basic module via the interface:
CL-Coul interface on the rear of the detection module
CL-Coul interface on the rear of the basic module
} Connect the "waste" outlet with the exhaust hose. Connect the hose with the exhaust
system, or route the hose into a vent.

59
Chlorine analysis with the Cl module 5100 multi EA 5100

Installing the detection module

7 1

5 2

4
4 3

Figure 41Connection of the heated gas transfer lines to the sulfuric acid container
1 Safety attachment 2 Sulfuric acid container
3 Hose for measuring gas infeed 4 Connector
5 Banjo bolt 6 Heated gas transfer line
7 Measuring gas transfer to the mea-
suring cell with PTFE connector
} Insert the sulfuric acid container in the holders.
} Route the gas transfer line through the top right opening of the detection module.
} Connect the gas transfer line to the sulfuric acid container:
– Insert the thin hose (3) into the sulfuric acid container.
– Connect the connector (4) to the sulfuric acid container.
– Connect the gas transfer line via the banjo bolt (5) on the connector.
NOTICE! Ensure the proper fit of the conical nipples!
} Place the safety attachment on the sulfuric acid container and attach the safety clip.
} Connect hose 20 with the safety attachment. Connect the hose to the measuring cell
later.
} Connect the gas transfer line in the basic module:
– Route the free end of the gas transfer line through the top left opening on the
basic module.
– Connect the gas transfer line to the auto-protection valve assembly.
– Connect the heating cable of the gas transfer line to its socket.

60
multi EA 5100 Chlorine analysis with the Cl module 5100

Figure 42Connection of the gas transfer line in the basic module

Left Connection to the auto-pro- Right Heating cable connection
tection valve assembly
ü Connection of the detection module is complete.

Inserting measuring cells The "sensitive" and "high concentration" measuring cells are inserted into the detection
module as follows:
} Insert the measuring cell with magnetic stirring rod and lid into the de-
tection module.
} Fill the measuring cell with electrolyte solution.
} Insert the combined electrode into the marked opening of the measuring
cell.
} Fasten hose 20 from the sulfuric acid container to the connection of the
combined electrode with the PTFE connector (1).
1 2 } Connect the olive (2) with the exhaust hose (hose 21) in the detection
module.

} Connect the combined electrode and the measuring cell to the inside of
1 2 the rear panel of the detection module:
Combined electrode connection (1)
Measuring cell connection (2)
5 4 3 Do not use connections (3) to (5).

61
Chlorine analysis with the Cl module 5100 multi EA 5100

The "high sensitive" measuring cell is inserted into the detection module as follows:

NOTICE
Risk of damage to the sensor electrode
The sensor pin and the gold contact of the sensor electrodes are sensitive to touch.
¡ Apply scratch protection to the sensor pin for storage.
¡ Rinse the sensor pin with ultrapure water before use or to clean it. Do not touch it
again after this. Do not dry the pin or wipe it dry!
¡ Before use or to clean it, wipe the gold contact with a cloth and some ethanol. Do
not touch it again after this.

} Insert the measuring cell with magnetic stirring rod and lid into the de-
6 tection module.
7
} Fill the measuring cell with electrolyte solution.
1 2 } Insert the components in the following openings:
Platinum electrode with salt bridge (1): "Pt" opening
Silver electrode (2): "Ag" opening
Gas inlet hose (1): "Inlet" opening
3 Sensor electrode (5): "Sens" opening
5
Reference electrode (6): large "ref" opening
Adapter (7): Center "outlet" opening
The openings on the lid align the sensor electrode and the reference
4
electrode toward each other.
} Close the opening for direct injection (4, "test") with a plug.
} Connect the short hose with the T piece to the adapter (7). Connect the
exhaust hose in the detection module (hose 21) with a limb of the T
piece.
} Place the pre-amplifier on the reference electrode. Connect the pre-am-
plifier with the sensor electrode.

} Connect hose 20 from the sulfuric acid container to the gas inlet tube via
the PTFE connector.
NOTICE! The conical nipples of the PTFE connector must be in the
proper position on the hose. Otherwise, gas leaks may ensue.

} Connect the electrode on the inside of the rear panel of the detection
1 2 module:
Platinum electrode connection (3)
Silver electrode connection (4)
5 4 3 Sensor and reference electrode connection (5)
Do not use connections (1) and (2).

62
multi EA 5100 Chlorine analysis with the Cl module 5100

8.3 Operation

8.3.1 Preparing the measuring cell

Preparing the measuring cell includes the following steps:

¡ Preparing the electrolyte solution
¡ Performing the end point routine

8.3.1.1 The "sensitive" and "high concentration" measuring cells

The measuring cells are similar in function. The "high concentration" measuring cell
works with a larger electrolyte solution volume.

Preparation of the electrolyte

solution

WARNING
Risk of chemical burns
100 % acetic acid (glacial acetic acid), concentrated nitric acid and thymol can cause se-
vere chemical burns. Methanol is a toxic, highly flammable material.
¡ Wear protective clothing when preparing the electrolyte solution. Work under an ex-
tractor.
¡ Observe all instructions and specifications in the safety data sheets.

ð Reagents required: 200 ml acetic acid 100 % (glacial acetic acid), 4 ml concentrated
nitric acid, 4 g gelatin, 1.0 g thymol, 0.3 g thymol blue, 500 ml methanol
} Solution A:
Fill 500 ml of water into a 1000-ml volumetric flask, add 4 ml of HNO3 (conc.), care-
fully add 200 ml of acidic acid and top up with water to the marking.
} Solution B1:
Mix 4 g of gelatin in a beaker with 400 ml of water, allow to swell for 3 hours and
then dissolve whilst heating to 35 to 45 °C.
The excess gelatin will sediment at the bottom of the beaker. Only use the clear su-
pernatant. Filter the solution, if necessary.
} Solution B2:
Dissolve 1.0 g of thymol and 0.3 g of thymol blue in a beaker with 500 ml of
methanol.
} Solution B:
After solution B1 has cooled down to 18 to 22 °C, slowly add it to solution B2 while
stirring, transfer into a 1000-ml volumetric flask and top up with water to the mark-
ing.
} Solution C, finished electrolyte:
Pipette 8 ml of solution B in a 100 ml measuring cylinder and fill with solution A to
100 ml, or
pipette 40 ml of solution B in a 500 ml measuring cylinder and fill with solution A to
500 ml.
ü The electrolyte solution is finished.
Storage and shelf life of the electrolyte solutions:
¡ When stored at 4 ±3 °C in well-sealed bottles, solutions A and B can be kept for ap-
prox. 6 months.

63
Chlorine analysis with the Cl module 5100 multi EA 5100

¡ The finished electrolyte solution (solution C) can be kept for approx. 30 days if kept
in a well-sealed glass container at 20 to 25 °C.

Performing the end point rou- An end point routine is necessary after every electrolyte change. The end point routine is
tine used to adjust the electrolyte to the optimal operating range of the measuring cell. The
operating point of the measuring cell is: 1500 to 5000 Counts .
} Start the end point routine via the System |End point routine menu item.
} Remove the olive from the lid of the measuring cell. Dose the HCl solution directly
into the measuring cell when instructed to by the software.
"sensitive" measuring cell: 200 µl of 0.01 N HCl
"high concentration" measuring cell: 200 µl of 0.1 N HCl
} Directly after dosing, activate the end point routine by clicking on [OK].
} The End point routine status is displayed in the Status analyzer window during this
routine. After the end point routine, the Stand-by titration and the current indicator
value is displayed.
ü The system is ready for measurements.
The determined operation point of the combined electrode is displayed in the System |
Component test menu item in the Chlorine tab.

Protecting the combined elec- Observe the following to protect the combined electrode against unnecessary wear:
trode ¡ Always add fresh electrolyte to the measuring cell before the end point routine.
¡ Do not carry out the end point routine several times in a row.

8.3.1.2 The "high sensitive" measuring cell

Preparation of the electrolyte Measurements with the "high sensitive" measuring cell require an electrolyte solution.
solution The electrolyte solution is also used as a bridge electrolyte for the reference electrode.

WARNING
Risk of chemical burns
100 % acetic acid (glacial acetic acid) can cause severe chemical burns. Gases may de-
velop during shaking.
¡ Wear protective clothing when preparing the electrolyte solution. Work under an ex-
tractor.
¡ Observe all instructions and specifications in the safety data sheet.

ð Reagents required: 800 ml acetic acid 100 % (glacial acetic acid), 2.7 g sodium ac-
etate p.a. (CH3COONa), anhydrous
} Dilute 2.7 g of sodium acetate in 200 ml of ultrapure water in a 1-liter volumetric
flask.
} Carefully add 800 ml of glacial acetic acid. Keep moving the flask while pouring the
acid. Carefully shake the mixture.
NOTICE! Do not exceed the specified amounts of water and glacial acetic acid. Do
not fill the flask up to the 1-liter mark (volume contraction).

Performing the end point rou- The end point routine is used to set the electrolyte to the optimum operating point of
tine the sensor electrode within the operating range of the titration cell.
¡ Operating range: 1000 to 10000 Counts
¡ Optimal operation range: 3000 Counts

64
multi EA 5100 Chlorine analysis with the Cl module 5100

Automatic end point routine As soon as the indicator value is outside the operating range of the titration cell, the sys-
tem automatically triggers an end point routine. This routine may also be triggered be-
tween two measurements of a multiple determination. The End point routine status is
displayed in the Status analyzer window during this routine.
Indicator value is higher than the operating range:
¡ Silver ions are automatically produced. The electrolyte is set to the optimum operat-
ing range of 3000 Counts.
Indicator value is lower than the operating range:
¡ The software prompts the user to add the following solution to the measuring cell:
100 µl hydrochloric acid (HCl, 10 mg/l HCl)
¡ If the indicator value rises above the operating range again, silver ions will be pro-
duced automatically. The electrolyte is set to the optimum operating range.
When working with a MMS, the addition of chloride ions to the measuring cells can be
performed automatically if the indicator value goes below the operating range while an
analysis sequence is in progress. For this, the user must have prepared a suitable organic
chlorine solution and placed it in the intended position (110) on the sample rack.
After the end point routine, the measuring cell requires approx 15 min to achieve a sta-
ble cell potential. During this time, a negative drift can occur with indicator values below
3000 Counts.

Manual end point routine For indicator values within the operating range, the end point routine can be started
manually via the System |End point routine menu item.
After the end point routine, the current indicator value is displayed in the Status ana-
lyzer window. If the current indicator value is within the operating range and the drift is
stable, the system is ready for measurements

8.3.2 Operating the analysis system

} Place the measuring cell with electrodes and electrolyte solution in the detection
module and connect it to electricity.
} Switch on the basic module and the detection module.
ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.
} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.
} Select Start |Start - Analysis in the menu.
} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.

65
Chlorine analysis with the Cl module 5100 multi EA 5100

} Enter the sample ID for all sample in the Name field.

} Release all sequence lines
} Confirm the entries with [OK].
} Click the [Start Measurement] button.
ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

8.3.3 Notes for measuring operations

CAUTION
Risk of respiratory problems due to leaking acetic acid vapors
The electrolyte solution of the "high sensitive" measuring cells contains high concentra-
tions of acetic acid.
¡ Ensure that the exhaust hose is connected to the measuring cell.
Check if the exhaust hose is connected to the "waste" outlet on the rear of the detec-
tion module, and that it is connected to the exhaust system.
¡ Before measurement operations, always close the front door of the detection mod-
ule and switch on the laboratory exhaust system.

WARNING
Risk of chemical burns
Concentrated sulfuric acid is used in the detection module as a drying agent. The con-
centrated acid can lead to severe chemical burns.
The 100 % acetic acid (glacial acetic acid), nitric acid and thymol used to create the elec-
trolyte solution can lead to severe chemical burns.
¡ Wear protective clothing when working with these hazardous substances.
¡ Observe all instructions and specifications in the safety data sheets.
¡ Fill the sulfuric acid container with fresh concentrated sulfuric acid every day (→
"Replacing the sulfuric acid and cleaning the sulfuric acid container."  147).

The "sensitive" and "high con- Fill the measuring cells with fresh electrolyte solution daily:
centration" measuring cells ¡ "sensitive" measuring cell: 15 to 20 ml
¡ "high concentration" measuring cell: 120 ml

The "high sensitive" measuring Fill the measuring cell daily with electrolyte solution: to approx. 65 ml
cell
Change the electrolyte solution:
¡ Once per week
¡ If analytical problems occur
¡ If crystalline deposits form
Open the refill opening of the reference electrode during operation.

66
multi EA 5100 Sulfur analysis with the S module 5100 (basic, MPO)

9 Sulfur analysis with the S module 5100 (basic, MPO)

9.1 Function and design

9.1.1 Function and measuring principle

Expansion of the basic module with the detection module allows determination of the
sulfur content in solid, liquid, paste-like, viscous and gaseous samples via UV floures-
cence.
The measuring gas is created during incineration of organic sulfur compounds in the ba-
sic module. It contains sulfur dioxide (SO2).
R-S + O2 → SO2 + CO2 + H2O
R: Hydrocarbon residue
The detection is performed using the UV fluorescence method. Sulfur dioxide (SO2) ex-
cited via UV light emits a characteristic flourescence (220 to 420 nm). This flourescence
is measured. The SO2 concentration is determined from the changes to the flourescent
intensity.

9.1.2 Design

The detection module allows determinations of the sulfur content via UV flourescence.
All components required for determination are mounted inside the sealed housing.

Figure 43Basic module with detection module and sampling module

This analysis gas containing SO2 is excited to flourescence via the radiation of a UV lamp.
The intensity of the fluorescence is determined with a photomultiplier (PMT).
To determine the sulfur content without interference from simultaneous increased ni-
trogen content the patented MPO (microplasma optimization) technology has been de-
veloped. The MPO technology removes the interfering nitrogen monoxide from the
measuring gas. This important, for example, during analysis of diesel fuels containing
cetane improvers.

67
Sulfur analysis with the S module 5100 (basic, MPO) multi EA 5100

The detection module is available with and without the MPO option. The MPO option is
not suited for multi-element methods that determine multiple elements simultaneously.
It can be switched on and off as needed via the control and analysis software.
Working with a method with the active MPO requires calibration performed with the
MPO active. Otherwise the measurement results will be too low. Conversely, use of cali-
bration with an active MPO for a method with no MPO can lead to false measurement
results that are too high.

9.1.3 Connection

The equipment door at the front is closed tightly and cannot be opened. An LED is in-
stalled on the door. The LED flashes during the run-in period of the detection module
and lights up permanently when the module is operational.
The device switch for switching the module on and off is located on the top right of the
rear of the device (when viewed from the front). The device fuse and power connection
are located beneath it.
Communication with the basic module is performed via a 9 pin interface cable. The in-
terface is labeled "S-UVF".
The hose for the measuring gas coming from the basic module is connected to the "sam-
ple in" gas inlet. The gas outlet is labeled "sample out".
The "Service" interface and the programming button are only required for service pur-
poses.

8
7
6

5 S-UVF

4
1

Figure 44Rear of the sulfur detector

1 Chemical ozone decomposer (MPO) 2 Measuring gas inlet
3 Measuring gas outlet 4 Service interface and programming
button.
5 Interface to the basic module 6 Power connection
7 Fuse holder 8 Equipment switch
The diagram on the rear explains the connector allocation.

68
multi EA 5100 Sulfur analysis with the S module 5100 (basic, MPO)

9.2 Installation

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

} Place the detection module to the left of the basic module. In the event of a series of
detection modules: place the detection module to the left or right of the others.
} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!
} Connect the detection module with the basic module via the interface:
S-UVF interface on the rear of the detection module
S-UVF interface on the rear of the basic module
} Connect the measuring gas hose of the basic module to the "sample in" gas inlet on
the rear of the module.
} Leave the "sample out" outlet unconnected or connect it to the measuring gas inlet of
the next detection module.
} For detection modules with MPO technology: Install the chemical ozone decomposer
on the rear of the module:
– Fasten the two holding clamps with the supplied screws.
– First press the chemical ozone decomposer into the upper holding clamp and
then into the lower one.
– Connect the hose from the "waste (MPO)" outlet to the ozone decomposer. Do not
pull the hose out of the device!
ü Connection of the detection module is complete.

Figure 45Chemical ozone decomposer

69
Sulfur analysis with the S module 5100 (basic, MPO) multi EA 5100

9.3 Operation

CAUTION
Risk of respiratory problems due to leaking ozone
If the gas hoses have not been properly connected to the ozone generator, ozone may
leak out of the detection module.
¡ If you can smell ozone, switch off the device and check the connection of the gas
hoses on the ozone generator.

} Switch on the basic module and the detection module.

ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.
} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.
} Select Start |Start - Analysis in the menu.
} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.
} Enter the sample ID for all sample in the Name field.
} Release all sequence lines
} Confirm the entries with [OK].
} Click the [Start Measurement] button.
ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

70
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

10 Sulfur analysis with the S module 5100 coulometric

10.1 Function and design

10.1.1 Function and measuring principle

Expansion of the basic module with the detection module allows the determination of
the sulfur content in solids, liquids, and gases via microcoulometric titration.
The organic sulfur compounds are incinerated into a mixture of sulfur dioxide (SO2) and
sulfur trioxide (SO3) in the basic module. Both oxides are created in a fixed relation. Car-
bon dioxide and water is also created during this incineration.
The amount of SO2 is proportional to the total sulfur amount in the sample.
The measuring gas flow is first dried and then routed to the detection module via a
transfer line. In the measuring cell, the sulfur oxides dissolve in the electrolyte and react
with iodine. This decreases the cell potential.
R-S + O2 → SO2 + SO3 + CO2 + H2O
2 H2O + SO2 + I2 → H2SO4 + 2 HI
R: Hydrocarbon residue
After a specified accumulation time dependent of the sulfur content of the sample, titra-
tion begins. The iodine ions are oxidized back to iodine at the anode. This increases the
cell potential. The end point of the iodometric titration has been reached when the
measuring cell has again reached its original potential.
With titration and end point routine: The electrode reactions consist of an anode reac-
tion (+) and a cathode reaction (-).
Anode (+): 2 I- → I2 + 2 e-
Cathode (-): 2 H+ + 2 e- → H2

10.1.2 Design

The detection module consists of the following main components:

¡ Measuring cell with electrodes
¡ NOx and HX absorbers for gas purification
¡ Gas inlet tube
¡ Magnetic mixer
¡ Interface to the basic module
A easily-opened door for changing the electrolyte solution is installed on the front of the
detection module. For maintenance purposes, the door can be removed.

71
Sulfur analysis with the S module 5100 coulometric multi EA 5100

8 1

2
6

5 4

Figure 46Coulometric sulfur detector with measuring cell (without door)

1 Indicator electrodes connection 2 Indicator electrode (black)
3 Gas inlet 4 Measuring cell
5 Port for manual dosing 6 Anode (yellow)
7 Cathode (red) 8 Generator electrodes connection

72
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

7 3

6
4

Figure 47Coulometric sulfur detectors without measuring cell

1 Measuring gas hose from the basic 2 Measuring gas hose to the measur-
module (hose 71) ing cell (hose 72)
3 HX absorber 4 Hose 73
5 Magnetic mixer with controls 6 Magnetic mixer connection
7 NOx absorber

Measuring cell The measuring cell is equipped with electrodes for generation and indication. The elec-
trodes are color-coded:
¡ Generation: Yellow anode, red cathode
¡ Indication: Black indicator electrodes
The measuring gas is routed into the measuring cell via the gas inlet tube. The solution
for the end point routine, the sodium sulfate solution (Na2SO3) and the solutions for the
cell measurements are dosed, for example, via the port for manual dosing.
The measuring cell must be filled with approx. 100 ml electrolyte solution (approx. to
the height of the manual dosing port).

73
Sulfur analysis with the S module 5100 coulometric multi EA 5100

7
1
6

3
4

Figure 48Coulometric measuring cell

1 Indicator electrodes (black) 2 Gas inlet tube
3 Port for manual dosing 4 Electrolyte solution filling height
5 Cathode (red) 6 Anode (yellow)
7 Gas outlet

Electrodes A diaphragm is located between the electrodes for generation (anode and cathode). The
diaphragm is only permeable for sulfations. This means that the diaphragm prevent
false analysis results due to undesired compounds.
The electrodes for indication are platinum electrodes.

74
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

6
1

5 3
4

Figure 49Generator and indicator electrodes, gas inlet tube

1 Generator electrodes (with union 2 Cathode (inside)
nut)
3 Diaphragm 4 Anode (outside)
5 Platinum electrodes 6 Gas inlet tube
7 Indicator electrodes

Absorber To clean the measuring gas, two absorbers are installed in the detection module. The
absorbers remove elements from the measuring gas that could disrupt the analysis.
The NOx absorber removes nitrogen oxides (NOx) from the measuring gas. High nitro-
gen oxide content has an influence on the analysis and leads to false results. The filling
of the absorber is normally green. If the color changes to yellow or light brown, the fill-
ing must be replaced.
The HX absorber removes hydrogen halogens (HX with X = Cl, Br, I) from the measuring
gas. Hydrogen halogens disrupt the analysis due to cross-sensitivities. The absorber con-
tains silver wool. The silver wool must be replaced if the color changes from metallic sil-
ver to dark gray.

75
Sulfur analysis with the S module 5100 coulometric multi EA 5100

2 1

Figure 50NOx absorber and HX absorber

1 NOx absorber 2 HX absorber

Hose diagram Labeled hoses connect the measuring cell with the other components in the detection
module. The numbers in the hose diagram correspond to the labels on the hoses.

71
72
NOx absorber

HX absorber

Measuring cell

73

Mixer

Figure 51Hose diagram

76
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

10.1.3 Connection

The electrical connection and the interface to the basic module can be found on the rear
of the detection module.
The device switch for switching the detection module on and off is located on the top
right of the rear of the device (when viewed from the front). The device fuse and power
connection are located beneath it.
Communication with the basic module is performed via a 9 pin interface cable. The in-
terface on the rear of the device is labeled "S-Coul".

Figure 52Rear of the coulometric sulfur detector

1 Power connection, fuse holder, de- 2 Interface to the basic module
vice switch

10.2 Installation

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

77
Sulfur analysis with the S module 5100 coulometric multi EA 5100

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

NOTICE
The detection module cannot be operated together with optical detectors.
¡ Do not connect the detection module together with an optical detector.

} Place the detection module to the left of the basic module.

} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!
} Connect the detection module with the basic module via the interface:
S-Coul interface on the rear of the detection module
S-Coul interface on the rear of the basic module
} Route the measuring gas hose (hose 71) from the basic module through the side
opening on the detection module. Connect the hose to the top of the NOx absorber.
} Connect the outlet of the HX absorber to hose 72.
Hose 72 is connected to the measuring cell later.
} Check that the NOx absorber and the HX absorber are connected via hose 73.
} Insert the electrodes into the measuring cell as displayed in the illustration.
} Insert the gas inlet tube into the measuring cell. Connect the gas inlet tube with hose
72 via the PTFE connector.
} Connect the electrodes to the "Generation" and "Indication" connections.
The connections cannot be mixed up.
ü Connection of the coulometric sulfur detector is complete.

78
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

8 1

2
6

5 4

Figure 53Coulometric sulfur detector with measuring cell (without door)

1 Indicator electrodes connection 2 Indicator electrode (black)
3 Gas inlet 4 Measuring cell
5 Port for manual dosing 6 Anode (yellow)
7 Cathode (red) 8 Generator electrodes connection

79
Sulfur analysis with the S module 5100 coulometric multi EA 5100

10.3 Operation

10.3.1 Preparing the measuring cell

Preparing the measuring cell includes the following steps:

¡ Preparing the electrolyte solution
¡ Performing the end point routine
Two further solutions are required for the end point routine and for the check of the
measuring cell. The creation of these solutions is also described in the following.

Preparation of the electrolyte

solution

WARNING
Risk of chemical burns
100 % acetic acid (glacial acetic acid) can cause severe chemical burns. Gases may de-
velop during shaking.
¡ Wear protective clothing when preparing the electrolyte solution. Work under an ex-
tractor.
¡ Observe all instructions and specifications in the safety data sheet.

ð Prepare the electrolyte solution one day before its use.

ð Reagents required: 10 ml acetic acid 100 % (glacial acetic acid), 10 g sodium ac-
etate, 5 g potassium iodide, 7.5 g potassium chloride
} Dissolve the given amounts of sodium acetate, potassium iodide and potassium chlo-
ride in a 1-liter volumetric flask. Wait until the salts have completely dissolved.
} Carefully add 10 ml of glacial acetic acid. Keep moving the flask while pouring the
acid. Carefully shake the solution.
} Fill the volumetric flask with ultrapure water up to the mark. Carefully shake the so-
lution.
} Fill the measuring cell with approx. 100 ml of electrolyte solution (to the level of the
port for manual metering).
ü The electrolyte solution has been prepared and added to the measuring cell.

Performing the end point rou- A sodium sulfite solution (1000 mg/l) is required for the end point routine:
tine
ð Reagents required: 393.9 mg sodium sulfite
} Fill a 100 ml volumetric flask with the specified quantity of sodium sulfite.
} Fill the volumetric flask with ultrapure water up to the calibration mark. Shake the
flask until the sodium sulfite has completely dissolved.
Storage and handling of the sodium sulfite solution:
¡ The solution is sensitive to atmospheric oxygen and may thus be stored in a refriger-
ator for no longer than 1 month.
¡ For the end point routine, only 2 – 10 μl of the master solution are required.
¡ For better metering, diluted solutions can be used.
For the end point routine, the cell potential is set to the optimum operating range of the
measuring cell.
¡ Operating range: 110 to 160 mV
¡ Optimal operation range: 120 mV

80
multi EA 5100 Sulfur analysis with the S module 5100 coulometric

As soon as the cell potential goes outside of the operating range, the software will auto-
matically start an end point routine.
Cell potential is lower than the operating range:
¡ Automatic generation start (iodine generation)
Cell potential is higher than the operating range:
¡ Add sodium sulfite solution when the software instructs.
¡ Titration runs automatically until the cell potential sinks to 120 mV.
An end point routine is also automatically started when electrolyte is replaced.
When working with a MMS, the addition of chloride ions to the measuring cells can be
performed automatically if the indicator value exceeds the operating range while an
analysis sequence is in progress. For this, the user must have prepared a suitable organic
sulfur solution and placed it in the intended position (110) on the sample rack.

Checking the measuring cell Only check the measuring cell if a defect of the detection module is suspected.
A sodium sulfate solution (1000 mg/l) is required for the check of the measuring cell.
ð Reagents required: 1.5482 mg sodium thiosulfate pentahydrate
} Weigh the indicated quantity of sodium thiosulfate into a 100 ml volumetric flask.
} Fill the volumetric flask with ultrapure water up to the calibration mark. Shake the
solution until the salt has dissolved completed.
The solution can be kept for approx. 1 month in a tightly-sealed container.
Standard solutions can be prepared by diluting the solution.
100 μl of the diluted solutions contain the following TS amounts:
¡ 10 mg/l standard: 1 μg S absolute
¡ 100 mg/l standard: 10 μg S absolute
After the function test of the measuring cell with the sodium thiosulfate solution, the
electrolyte must be replaced.

10.3.2 Operating the analysis system

} Place the measuring cell with electrodes and electrolyte solution in the detection
module and connect it to electricity.
} Switch on the basic module and the detection module.
ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.
} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.

81
Sulfur analysis with the S module 5100 coulometric multi EA 5100

} Select Start |Start - Analysis in the menu.

} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.
} Enter the sample ID for all sample in the Name field.
} Release all sequence lines
} Confirm the entries with [OK].
} Click the [Start Measurement] button.
ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

82
multi EA 5100 Carbon analysis with the C module 5100

11 Carbon analysis with the C module 5100

11.1 Function and design

11.1.1 Function and measuring principle

Expansion of the basic module with the detection module allows determination of the
carbon content in solid, liquid, paste-like, viscous and gaseous samples.
The detection module contains a wide-range NDIR detector. The carbon content in or-
ganic compounds can be determined as TC and EC/OC sum parameters with the detec-
tion module.
Carbon dioxide (CO2) and water (H2O) is created during thermal oxidation of the sam-
ples in the basic module. The gas mixture is dried and transferred to the NDIR detector.
R + O2 → CO2 + H2O
R: Hydrocarbon
The radiation sensor is CO2-sensitive. The double bond between carbon (C) and oxy-
gen(O) has a specific absorption range in the infrared wavelength band.
If a ray of light is projected through a cuvette arrangement, the CO2 content in the mea-
suring gas absorbs a proportion of the total radiation proportional to the CO2 concentra-
tion.

11.1.2 Design

The detection module is used to determine the carbon content in solids, liquids and
gases by measuring the IR IR absorption. All components required for determination are
mounted inside the sealed housing.
The device door is closed tightly and cannot be opened. An LED is installed on the front
of the detection module. The LED flashes during the run-in period and lights up perma-
nently when the module is operational.

Figure 54Basic module with detection module and sampling module

83
Carbon analysis with the C module 5100 multi EA 5100

The detection module can be used to determine TC and EC/OC.

¡ TC determination can be performed in both the multi-purpose combustion tube
(standard tube) and the special EC/OC combustion tube.
¡ EC/OC determination requires the use of the EC/OC combustion tube.
Analytik Jena GmbH also provides special boats with hold-down clamps for EC/OC deter-
mination, with which, for example, diesel exhaust particles can be examined on quartz-
fiber filters. The use of the ABD is required in horizontal operation mode.

11.1.3 Connection

The following components can be found on the rear of the device:

¡ Main switch, power connection and device fuses
¡ Inlet and outlet for the analysis gas
¡ Interface to the basic module

1
2
3

Figure 55Rear of the carbon detector

1 Equipment switch 2 Fuse holder
3 Power connection 4 Interface to the basic module
5 "Sample out" sample outlet 6 "Sample in" sample inlet
Communication with the basic module is performed via a 9 pin interface cable. The in-
terface is labeled "C-NDIR".
The hose for the measuring gas coming from the basic module is connected to the "sam-
ple in" gas inlet. The gas outlet is labeled "sample out". The module does not need to be
connected to the laboratory exhaust system.

84
multi EA 5100 Carbon analysis with the C module 5100

11.2 Installation

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

} Place the detection module to the left of the basic module. In the event of a series of
detection modules: place the detection module to the left or right of the others.
} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!
} Connect the detection module with the basic module via the interface:
"C-NDIR" interface on the rear of the detection module
"C-NDIR" on the rear of the basic module.
} Connect the measuring gas hose of the basic module to the "sample in" gas inlet on
the rear of the module.
} Leave the "sample out" outlet unconnected or connect it to the measuring gas inlet of
the next detection module.
ü Connection of the detection module is complete.

11.3 Operating the analysis system

} Switch on the basic module and the detection module.

ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.
} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.
} Select Start |Start - Analysis in the menu.
} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.
} Enter the sample ID for all sample in the Name field.
} Release all sequence lines
} Confirm the entries with [OK].

85
Carbon analysis with the C module 5100 multi EA 5100

} Click the [Start Measurement] button.

ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

86
multi EA 5100 Carbon analysis with the TOC module 5100

12 Carbon analysis with the TOC module 5100

12.1 Function and design

12.1.1 Function and measuring principle

The detection module contains a wide-range NDIR detector. Expansion of the basic
module with the detection module allow determination of the following sum parame-
ters:
Sum parameters Samples Basic module configuration
TC Organic liquids, solids and Vertical/horizontal opera-
gases tion
EC/OC Elemental and organically Horizontal operation
bound carbon from par- with:
ticulate emissions (fine ¡ Special combustion
particulate matter, diesel tube for EC/OC deter-
engine exhaust, smoke mination
gas
TC, TOC, NPOC, TIC Water samples Vertical operation with:
¡ TOC combustion tube
¡ Condensation coil
Carbon dioxide (CO2) and water (H2O) is created during thermal oxidation of the sam-
ples in the basic module. The gas mixture is dried and transferred to the NDIR detector.
R + O2 → CO2 + H2O
R: Hydrocarbon
The radiation sensor used in the TOC module is CO2-sensitive. The double bond between
carbon (C) and oxygen(O) has a specific absorption range in the infrared wavelength
band.
If a ray of light is projected through a cuvette arrangement, the CO2 content in the mea-
suring gas absorbs a proportion of the total radiation proportional to the CO2 concentra-
tion.
A proportion of the water sample is dosed manually into the TIC reactor to determine
the inorganically bound carbon (TIC) content. The sample reacts with phosphoric acid in
the TIC reactor. This creates CO2, which is determined via the NDIR detector.
The detection module determines the CO2 concentration multiple times per second and
generates an integral over time from the signals. The integral is proportional to the car-
bon concentration in the sample.

12.1.2 Design

All components of the module to be operated or serviced by the user can be access via
the door on the front of the module.
The module consists of the following main components:
¡ TIC condenser unit (with TIC reactor, gas-liquid separator, measuring gas dryer)
¡ Condensate pump
¡ Halogen trap and water traps for drying and cleaning the measuring gas.
¡ NDIR detector (in the rear part of the detector)
¡ Indicator and control elements, connections

87
Carbon analysis with the TOC module 5100 multi EA 5100

7
1

2
6

3
4

Figure 56TOC detector, door opened

1 Water traps 2 Measuring gas hose from the basic
module (hose 80)
3 Condensate pump 4 TIC reactor
5 Cooling block (measuring gas dryer) 6 Halogen trap
7 Hose 81
The basic module must be equipped with the following components to analyze aqueous
samples:
¡ TOC combustion tube
¡ Condensation coil

88
multi EA 5100 Carbon analysis with the TOC module 5100

Figure 57Components in the basic module

1 TOC combustion tube injection port 2 Spherical joint (fasten with forked
clamp)
3 Condensation coil

TOC combustion tube The TOC combustion tube (reactor) is used to determine the TC, TOC and NPOC param-
eters in water samples. The combustion tube is made of quartz glass and is filled with a
catalyst and additives. If the effectiveness of the catalyst decreases, the combustion tube
has to be filled again.

Figure 58TOC combustion tube (unfilled)

89
Carbon analysis with the TOC module 5100 multi EA 5100

Screw the screw cap with the septum on the top opening of the combustion tube. Con-
nect the condensation coil with the aid of a fork type clamp to the spherical joint on the
lateral outlet.
The oxygen gas supply (hose 3 of the basic module) is connected via a FAST connector
at the lateral outlet directly under the screw cap. The tube holder is used to fasten the
TOC combustion tube in the furnace.

Figure 59Tube holder for the TOC combustion tube

Sampling Water samples are dosed directly into the TOC combustion tube via the injection port
with microliter syringes. A syringe with scale is used for manual dosing. For automatic
sampling via the autosampler, special microliter syringes are used. The syringes have
special dimensions and therefore have no scale. They are unsuitable for manual opera-
tion for this reason. The syringes have a gas connection for analyses in NPOC mode. The
injection volume is: 50 to 500 µl. Optimum measurement results are achieved when 50
to 100 % of the volume of the microliter syringe is used.
The injection port is equipped with temperature-resistant septums with a high penetra-
tion tolerance.
A proportion of the sample is dosed directly into the TIC reactor of the TOC module with
a microliter syringe with a scale to determine the inorganic carbon content (TIC). Only
manual dosing is permitted for this.

Measuring gas drying and For the analysis of water samples, the basic module is equipped with a condensation coil
cleaning made of glass. The condensation coil is connected to the TOC combustion tube via the
spherical joint. Connect hose 80 to the other end of the condensation coil via the the
FAST connector.
The measuring gas cools quickly in the condensation coil and the water vapor con-
denses. The mixture of measuring gas and water is transferred to the TIC reactor in the
detection module via hose 80.

90
multi EA 5100 Carbon analysis with the TOC module 5100

2
1

Figure 60Condensation coil

1 FAST connector 2 Spherical joint
The detection module is equipped with the TIC condensation unit. The TIC condensation
unit consists of the following components:
Component Task
TIC reactor TIC determination
Gas-liquid separator Separation of the liquid phase (conden-
sate, waste solution from TIC determi-
nation)
Cooling block Water vapor condensation (measuring
gas drying)
The mixture of measuring gas and water is added via the lateral outlet of the TIC reactor
via hose 80.
40 % phosphoric acid is placed in the TIC reactor to determine TIC content. The acid and
the sample are added manually via the front connection with septum.
The measuring gas is routed via the top connector in the direction of the water traps
from the TIC condensation vessel.
The condensate or waste solution from TIC determination is pumped out via the lateral
outlet on the glass container. The condensate pump transports the waste to the "waste"
outlet on the rear of the device.
The two following components protect the detector and remove disruptive substances
from the measuring gas.
¡ Water traps
¡ Halogen trap
Two water traps are installed in the TOC module. They remove water from the measur-
ing gas. The water traps are connected to the measuring gas outlet of the TIC reactor.
The water traps prevent condensed water from being transported into the path of the
measuring gas after leaving the TIC condensation unit. The larger water trap (TC pre-
filter) retains aerosols during operation. The smaller water trap retains rising water (dis-
posable retention filter).
The halogen trap removes gaseous halogen compounds from the measuring gas. The
halogen trap is installed in the measuring gas path downstream of the water traps. The
U-tube is filled with special copper wool. The filling of the halogen trap must be replaced
at the latest when half of the copper wool has turned black.

91
Carbon analysis with the TOC module 5100 multi EA 5100

NDIR outlet Measuring gas inlet Waste

(from condensation coil, basic device)

82 81
84

83 80 85

NDIR
NDIR measuring
gas inlet

86

Figure 61Hose diagram of the TOC detector

Straight and angled FAST connectors are used to fasten hose connections.

12.1.3 Connection

The device switch for switching the detection module on and off is located on the top
right of the rear of the device (when viewed from the front). The device fuse and power
connection are located beneath it.

92
multi EA 5100 Carbon analysis with the TOC module 5100

1
2
3

Figure 62Rear of the TOC detector

1 "External (out)" connection socket 2 "C-NDIR" interface cable connection
(25-pin) (9-pin)
3 "External (in)" interface cable con- 4 "Sample in" measuring gas inlet
nection (25-pin)
5 "Sample out" measuring gas outlet 6 "Waste" waste outlet
7 Power switch, fuse holder, power 8 Holder for the NPOC purging hose
connection
Communication with the basic module is performed via a 2 interfaces:
¡ The interface for the 9-pin interface cable is labeled "C-NDIR".
¡ The interface for the 25-pin interface cable is labeled "External (in)".
The "External (out)" interface is not used.
The hose connection are required to be factory-prepared for TOC measurement (in wa-
ter samples) The "Sample in" measuring gas inlet is connected with hose 82.
The purged condensate or waste solution from TIC determination is drained via the
"waste" outlet on the rear of the module. For this, a waste hose is connected to the con-
nector "waste" and inserted into a waste container (included in the scope of delivery).

NPOC The connection for the NPOC purging gas is located on the rear of the basic module and
is labeled with "out ABD". The purge hose is connected to the connector via a FAST con-
nector. The purge hose is fastened to the holder on the rear of the detection module
with the provided connector. From there, a hose with an outer diameter (AD) of 1.6 mm
continues to the holder on the sampler. For manual sample preparation, the hose can be
immersed directly in the sample.

TC, EC/OC The detection module can be used to determine TC and EC/OC.
TC determination can be performed in both the multi-purpose combustion tube (stan-
dard tube) and the special EC/OC combustion tube.

93
Carbon analysis with the TOC module 5100 multi EA 5100

EC/OC determination requires the use of the EC/OC combustion tube.

For the connection to the basic module, hose 82 is removed from the "sample in" mea-
suring gas inlet on the rear of the detection module. The "sample in" measuring gas inlet
is connected to the "Sample OUT N/S/C" outlet on the basic module.

12.2 Installation

NOTICE
Connecting or disconnecting electrical contacts may damage the sensitive electronic
components of the basic module and of the detection module.
¡ Always connect the modules to power when they are switched off.

} Place the detection module to the immediate left of the basic module.
} Connect the supplied power cable to the power cable connection on the rear of the
module and to an earthed socket. Observe the permissible maximum voltage!
} Connect the detection module to the basic module via the two interfaces:
– 9-pin interface cable
"C-NDIR" interface on the rear of the detection module
"C-NDIR" interface on the rear of the basic module
– 25-pin interface cable
"external (in) interface on the rear of the detection module
"External" interface on the rear of the basic module
} Install the halogen trap and the water traps in the detection module as shown in the
illustration. Connect both with hose 81.
} Install the TIC reactor. Connect the TIC reactor to the water traps. Connect the TIC re-
actor to the condensate pump via hose 86.
} Connect the measuring gas hose (hose 80) from the basic module to the lateral out-
let of the TIC reactor.
Hose 80 is connected to the condensation coil outlet in the basic module later.
} Place the waste canister to the left of the detection module.
} Connect the waste hose to the "waste" outlet on the rear of the detection module.
Route the waste hose into the waste canister.
} Leave the "sample out" outlet unconnected or connect it to the measuring gas inlet of
the next detection module.

94
multi EA 5100 Carbon analysis with the TOC module 5100

7
1

2
6

3
4

Figure 63TOC detector, door opened

1 Water traps 2 Measuring gas hose from the basic
module (hose 80)
3 Condensate pump 4 TIC reactor
5 Cooling block (measuring gas dryer) 6 Halogen trap
7 Hose 81

Preparing the basic module } Fill the TOC combustion tube as shown in the illustration.
} Insert the TOC combustion tube into the combustion furnace of the basic module.
Connect the oxygen supply (hose 3). Fasten the combustion tube with the tube
holder.
} Install the condensation coil in the basic module. Connect the condensation coil with
the TOC combustion tube with the spherical joint. Secure the spherical joint connec-
tion with a clamp.
} Connect the condensation coil to the TIC reactor in the detection module with hose
80. Route the hose through the side openings of the modules for this.

95
Carbon analysis with the TOC module 5100 multi EA 5100

1
2
3

Figure 64TOC combustion tube

1 HT mat 2 Quartz glass fragments
3 Quartz wool 4 Catalyst
5 Quartz wool

For NPOC determination } Prepare the detection module and the basic module as previously described.
} Connect the NPOC purge hose (hose 16) to the "out ABD" connection on the basic
module.
} Connect the purge hose with a hose with an outer diameter (AD) of 1.6 mm. Fasten
the hose to the rear on the TOC module.
} Route the hose to the holder on the sampler. Alternatively, use the hose for manual
purging of the acidified samples.

For TC, EC/OC determination The TOC module can be configured for TC determination with the basic module and the
multi-purpose combustion tube or the special combustion tube for EC/OC determina-
tion. For EC/OC determination, the special combustion tube for EC/OC determination
must be used. The measuring gas is routed directly from the combustion tube into the
NDIR detector via the "sample in" outlet.
} Remove hose 82 from the "sample in" measuring gas inlet on the rear of the detec-
tion module.
} Connect the "sample OUT N/S/C" outlet on the basic module with the "sample in"
measuring gas inlet with hose 9.

12.3 Operation

12.3.1 Operating the analysis system

} Switch on the basic module and the detection module.

ü The devices boot up. The status LED on the front of the basic module light up in
green after approx. 30 s.
ü The LED on the front of the detection module flashes during the run-in period.
Depending on the detector, the run-in period can take up to 30 min. After this,
the LED will light up continuously. Starting a measurement is only then possible.
} Open the gas supply and set the required gas pressure.
} Switch on the PC.

96
multi EA 5100 Carbon analysis with the TOC module 5100

} Start the control and analysis software and login with your username and password.
} Initialize the analysis system by clicking on [Initialize analyzer].
ü The initialization and automatic detection of all connected components will be
carried out.
} Ready the samples.
} Activate a pre-existing method via the Method |Method - activate menu item.
} Alternatively: Create a new method in the Method |Method - new menu. Select the
measurement parameter in the method. Release and activate the method.
} Select Start |Start - Analysis in the menu.
} Select an analysis group or create a new one and confirm via [OK].
} Create an analysis sequence.
} Enter the sample ID for all sample in the Name field.
} Release all sequence lines
} Confirm the entries with [OK].
} Click the [Start Measurement] button.
ü The prepared analysis sequence is processed.
For manual sampling, follow the instructions in the software.

12.3.2 Notes for measuring operations

Observe the following instructions for operation of the TOC detector:

¡ Regenerate the TIC reactor before performing TIC determination (→ "Regenerating
the TIC reactor"  161).
¡ Dilute highly acidic and saline samples, e.g., 1:10.
Aerosols can form in the TIC reactor during analysis of these samples. The capacity
of the halogen trap will then be exhausted quickly and may clog.
¡ The water traps protect the NDIR detector from aerosols. In the event of excessive
aerosol formation, the software interrupts the carrier gas supply. Also in the event
of excessive aerosol formation, interrupt the connection between the water traps
and the outlet of the TIC reactor.
¡ To acidify samples: Use hydrochloric acid (HCl) at c = 2 mol/l. Create the acid from
concentrated HCl (p.a.) and TOC water.
¡ For TIC determination: Use 40 % orthophosphoric acid (H3PO4). Create the acid from
concentrated orthophosporic acid (p.a.) and TOC water.
¡ Only store solutions in clean, particle-free glass containers (volumetric flasks, sam-
ple containers).
Carbon dioxide and organic vapor in the air of the laboratory can slightly alter the con-
centration of samples and standard solutions.
¡ Remove the source of any organic vapor from the laboratory.
¡ Create low-concentration solutions (c < 1 mg/l) under a fume hood.
¡ Keep the free space above the liquid small in containers.
¡ Cover the sample containers with foil for sampler operation (differential mode).

97
Troubleshooting multi EA 5100

13 Troubleshooting

13.1 General notes

For fault analysis, log files can be recorded. Log file recording should be activated after
consultation with Analytik Jena GmbH customer service for specific faults.
The save location of the log files can be defined via the Extras |Configuration menu
item in the Configuration |Error analysis window.

CAUTION
¡ If faults cannot be remedied by the customer, the Analytik Jena GmbH service de-
partment must always be informed. This also applies for the repeated occurrence of
individual faults.
¡ Send the correspond files to the service department via email for fault diagnosis
(address on inside of the front cover).

13.2 Remedying software message faults

Communication problems between the hardware and the software can often be reme-
died by a basic initialization of the measuring system (→ "Initializing the basic module
and the system components"  104).

NOTICE
Communication fault due to wrong USB cable
¡ Use the cable supplied by Analytik Jena GmbH.
¡ Extensions are not permitted for the USB connection!

Error Error message/cause Remedy

code
1 No response from firmware!
Basic module not switched on Switch on the basic module
Basic module disconnected from PC Check the connection between the basic module
and the PC
Incorrect port selected Check which port the device is plugged into on the
PC
Select another port (Configuration |Interface
menu item)
Initialize

98
multi EA 5100 Troubleshooting

Error Error message/cause Remedy

code
2 Serial port not available!
3 Serial port not reachable!
communication problems Disconnect the USB connection between the basic
module and the PC and reconnect after approx.
10 s.
Initialize
7 Operating system faults: Unauthorized access
Undefined multiWin end Exit the software and switch off the device
Detach the USB cable and re-connect after ap-
prox. 10 s
Restart the operating system (PC)
Switch on the device
Restart the software
12 Signal echo received, check port selection
Incorrect port selected Check port selection
14 Data transfer interrupted
No data transfer for 10 s Check port selection
17 Incorrect interface protocol ID
Fault after update (the program versions of the Update required
firmware and multiWin do not match)
20 Timeout: InitEnd
Timeout during initialization Initialize
21 Timeout: StatusBusy
Timeout during operation (device not ready to Acknowledge message
measure) Initialize
22 Timeout: End
Timeout when exiting multiWin Acknowledge message
Initialize
23 Timeout: StopEnd
Timeout during measurement cancellation Acknowledge message
Initialize
50 Firmware reset
Internal computer (firmware) restarted Acknowledge message
Initialize
61 Command from PC incomplete
62 Command from PC without STX
64 Command from PC CRC error
65 Command from PC invalid
66 Command from PC invalid MEAS command
Communication error Acknowledge message
Initialize

99
Troubleshooting multi EA 5100

Error Error message/cause Remedy

code
100 C sensor: No connection
101 C sensor: CRC error
Communication interrupted after sensor detection Acknowledge message
during initialization Initialize
104 C sensor: Analog values outside range
The analog values of the detector are outside the Check the quality of the carrier gas
operating range Initialize
Check the analog values in the component test
(System |Component test |NDIR menu item)
110 N sensor: No connection
120 S sensor: No connection
130 Cl sensor: No connection
Communication interrupted after sensor detection Acknowledge message
during initialization Initialize
131 Cl sensor: Incorrect command structure
Communication to the chlorine module inter- Acknowledge message
rupted Switch the chlorine module on/off
Initialize
132 Cl sensor Indicator error
Indicator value out of range after titration start Acknowledge message
(measurement cannot start) Initialize
Run an end point routine
Check the status of the titration cell (System |
Component test |Chlorine menu item)
133 Cl sensor: Incorrect cell
No initialization after cell change Initialize
134 Cl sensor: Incorrect status
Communication error Acknowledge message
Initialize
Check the status of the titration cell ( System |
Component test | Chlorine menu item)
135 Cl sensor: Incorrect version
Transmission fault Acknowledge message
Initialize
Check the status of the titration cell ( System |
Component test | Chlorine menu item)
200 Gas box: No connection
Communication error Acknowledge message
Initialize

100
multi EA 5100 Troubleshooting

Error Error message/cause Remedy

code
201 Gas box: Fault when setting the target flow
Communication to gas box interrupted Acknowledge message
Initialize
202 Gas box: Conversion fault 1
203 Gas box: Conversion fault 2
204 Gas box: Conversion fault 3
205 Gas box: Conversion fault 4
Communication faulty (readout of flows from gas Acknowledge message
box faulty) Initialize
206 Gas pressure error
Overpressure in the analysis system due to WARNING! Extreme caution is required during
blocked gas paths system overpressure! Never switch off a device
subject to overpressure! Otherwise, risk of injury
to operating personnel and damage to the analy-
sis system is present.
Follow the instructions in the section on (→ "Be-
havior during overpressure faults (0206, gas
pressure fault)"  14)
220 Sampler: no connection
Communication interrupted after autosampler de- Acknowledge message
tection during initialization Initialize
222 Boat: Broken
Boat defect during removal from the combustion Remove the broken boat from the system
tube (only if boat sensor is used) Initialize
223 Sampler: Incorrect peak value
No syringe inserted Insert syringe in autosampler
Initialize
Dosed volume in the method greater than in- Adjust dosed volume or insert suitable syringe
serted syringe volume Initialize
A method for dosing liquids is to be activated and Insert sample rack for liquid samples
the gripper and solids track are still inserted Insert syringe
Initialize
224 Sampler: Incorrect gripper
No gripper inserted Insert gripper in autosampler
Initialize
The method for solids is to be enabled and the sy- Insert solids rack
ringe and sample rack for liquid samples are still Insert gripper
inserted
Initialize
226 Sampler: Runtime exceeded
Completion message for the autosampler move- Record log files
ment takes too long (autosampler faulty) Inform customer service department

101
Troubleshooting multi EA 5100

Error Error message/cause Remedy

code
230 ABD: No connection
Communication error after ABD was detected dur- Acknowledge message
ing initialization Initialize
231 ABD: Runtime exceeded
Completion message for the ABD movement Check that the flame sensor is properly applied
takes too long and connected
Record log files
Inform customer service department
232 Flame sensor error
Flame sensor calibration failed Record log files
Inform customer service department
250 LPG: No connection
Communication interrupted after LPG detection Acknowledge message
during initialization Initialize
251 LPG: Runtime exceeded
Communication error Acknowledge message
Completion message at dosing end not received Check argon gas inlet pressure
Initialize
252 LPG: Argon missing during dosing
No argon applied to LPG module Check gas supply
Check gas inlet pressure
253 LPG: Incorrect sample volume
Dosed volume is not a whole multiple of the sam- Adapt dosing volume to sample loop volume
ple loop inserted
260 Sample handling missing
No sampler module detected Connect at least one sampler module
Initialize
270 Auto-injector syringe: No connection
(applies to Autoinjector, Autoinjector AI-EA)
No communication with auto-injector Acknowledge message
Initialize
271 Auto-injector syringe: Runtime exceeded
(applies to Autoinjector, Autoinjector AI-EA)
Communication error Acknowledge message
Completion message at dosing end not received Check auto-injector
Initialize
272 Auto-injector syringe: Incorrect syringe size
Autoinjector: Dosing volume and syringe size dif- Adapt the dosing volume and/or the syringe size
ferent
Autoinjector AI-EA cannot complete this order Initialize

102
multi EA 5100 Troubleshooting

Error Error message/cause Remedy

code
273 Auto-injector syringe: Syringe drawn incorrectly
(Autoinjector only)
Syringe not drawn back all the way Draw syringe back all the way
Insert syringe
274 Autoinjector: No connection
Auto-injector coupling not found Check connection
Acknowledge message
Initialize
No Autoinjector AI-EA was found
Autoinjector AI-EA not connected or faulty Check connection
Acknowledge message
Initialize
275 Autoinjector: No syringe detected
Syringe not drawn Repeat sampling with drawn syringe
Syringe detection faulty Test a different syringe
300 Temperature controller: No connection
Communication error Acknowledge message
Initialize
304 Temperature controller: Communication error
Temperature cannot be set Acknowledge message
Initialize
400 Syringe pump: No connection
Communication error Acknowledge message
Initialize
401 Syringe pump: Initialization
402 Syringe pump: Invalid command
403 Syringe pump: Invalid operand
404 Syringe pump: Invalid command sequence
407 Syringe pump: Device not initialized
Communication error Acknowledge message
Syringe pump faulty Search for cause and remedy fault
Initialize
409 Syringe pump: Pump sluggish
Gas hose clogged or kinked Acknowledge message
Syringe pump faulty search for cause and remedy fault
Initialize
410 Syringe pump: Valve sluggish
Syringe pump faulty Acknowledge message
Valve faulty Search for cause and remedy fault
Initialize

103
Troubleshooting multi EA 5100

Error Error message/cause Remedy

code
411 Syringe pump: Pump step not permitted
415 Syringe pump: Command error
420 Syringe pump: incorrect type
Communication error Acknowledge message
Initialize

13.3 Initializing the basic module and the system components

Initialization of a measuring system establishes communication between the measuring

system and the computer. The multiWin program differentiates between a standard ini-
tialization and a basic initialization.
With standard initialization, only the system components active before the last shut-
down of multiWin are queried and the method last active is loaded.
The basic initialization, on the other hand, is more thorough and tests all connected sys-
tem components activated in the multiWin program in the window. The basic initializa-
tion must always be performed in the following situations:
¡ Connection of new system components
¡ Recognition of system components which were shut down or were not connected
during the last initialization
¡ Fault in the communication between the measuring system and the computer

Performing the basic initializa- Basic initialization is always performed if the Device - edit window was opened and ex-
tion ited via [OK]:
} Select the Device |Device - edit menu item.
} Make any necessary changes and exit the Device - edit window via [OK].
} Click on [Initialize analyzer] in the main window.
ü The system is initialized and the method last used is activated. If the initialization
was successful, the [Start Measurement], [Activate method] and possibly the
[Start calibration] buttons are displayed in the main window.

Standard initialization Click on the [Initialize analyzer] button in the main window. Alternatively, select the Sys-
tem |Initialize menu item.

104
multi EA 5100 Troubleshooting

13.4 Displays in the window Status analyzer

13.4.1 Overview

In the Status analyzer window, information on the device status or information on indi-
vidual modules is displayed.
Status analyzer multi EA 5100 1
TN liquid vertical (1) - liquid 2
Rack : 112 - Syringe : 50 µL 3
C-NDIR
N-CLD-5100 OK
0.15 4

S-UVFD-5100

Cl-POT

MFC 1 300
MFC 2 0
MFC 3 100
5

Furnace temperature 1050 °C 6

Figure 65Status analyzer window

1 Window name and basic module 2 Active method and sample state
3 Sampling modules 4 Detectors with sensor values
5 Gas flow displays 6 Furnace temperature (horizontal
line – horizontal installation, vertical
line – vertical installation)
The displays in the Status analyzer window are color-coded. The colors have the follow-
ing meanings:
Color Description
Black Status of the corresponding component OK, device ready for measure-
ment
Gray Detector is inactive
Green Detector OK, device ready for measurement (OK)
Or
Detector busy, measurement can only be started once the routine is
complete (detector-specific)
Red Component not ready for measurement:
¡ Run-in period not yet complete; wait for run-in time to complete
¡ Error: Troubleshooting, access the corresponding information for
the component via the System |Component test menu item.

105
Troubleshooting multi EA 5100

13.4.2 Method

The following can be displayed in the top line of the Status analyzer window:
Display Description
TN(1) - liquid Example of a method: Name(version) – state
Possible states:
¡ Liquid
¡ Solid
¡ GSS
¡ LPG
¡ AOX, AOX solid
¡ EOX liquid, EOX solid
No method displayed (dis- Device not ready for measurement, no method active:
play empty) Activate method

13.4.3 Sampling modules

Example Rack: 112 - syringe: 50 µl

Meaning Sampling module - rack - syringe size
All sampling modules detected during initialization are displayed and (possibly) de-
scribed in detail. The following displays are possible:
Display Description
GSS (pressureless) Gas dosing module for sampling from bag or in com-
bination with the GSS adapter box from sample cylin-
der
LPG LPG module
GSS/LPG LPG/GSS combination module for sampling under
pressure
Rack: 112 - syringe: 50 µl Autosampler: Specification of rack size and syringe
size
Rack: 35 - gripper Autosampler: Specification of rack and gripper
Auto-injector - syringe: Auto-injector type and syringe size
50 µl
ABD Automatic boat feed
ABD - FS Automatic boat feed and flame sensor

106
multi EA 5100 Troubleshooting

The following status displays are possible:

Device not ready for measurement

Display Description
No sampling module dis- Device not ready for measurement, no sampling mod-
played (display empty) ule identified:
¡ Connect and activate at least one sampling mod-
ule
¡ Basic initialization
Auto-injector - syringe: ? No auto-injector syringe detected
¡ Initialize
¡ Insert auto-injector syringe and register it in mul-
tiWin ("Extras | New auto-injector syringe" menu
item)

13.4.4 Detectors

Example Cl-POT OK 3050

Meaning Detector status Current sensor value
All detector modules detected during initialization are displayed here. The following dis-
plays are possible:
Display Description
C-NDIR C module 5100 or TOC module 5100 with NDIR detector
N-CLD N module 5100 with chemiluminescence detector
S-UVFD S module 5100 basic and S module 5100 MPO with UV
flourescence detector
S-Coul S module 5100 coulometric with microcoulometer
Cl-POT Cl module 5100 with "high sensitive" measuring cell
Cl-AMP smallCell Cl module 5100 with "sensitive" measuring cell
Cl-AMP largeCell Cl module 5100 with "high concentration" measuring cell
The respective status of the detector module is indicated by the color:
Display Description
Black Detector is active, status is queried and displayed (see example
above)
Gray Detector is inactive, status is not displayed
Green Detector OK, device ready for measurement (OK)
Or
Detector busy, measurement can only be started once the routine is
complete (detector-specific)
Red Error, see overview below

107
Troubleshooting multi EA 5100

The following status displays are possible:

Device ready for measurement

Display Description
OK (green, black) Detector is ready for measurement
Device not ready for measurement - general
Display Description
No detector displayed (dis- No detector detected
play empty) ¡ Activate detector
¡ Basic initialization
Communication error (red) Communication interrupted:
¡ Deactivate/activate the device
¡ Basic initialization
No connection (red) Connection interrupted:
¡ Check connection cable
¡ Deactivate/activate the device
¡ Basic initialization
Device not ready for measurement – Cl-POT
Display (red) Description
Inactive No cell detected:
¡ Insert cell
¡ Basic initialization
Drift exceeds range The current indicator drift is greater than the maxi-
mum positive drift set in the method or the max. neg-
ative drift defined in the system.
¡ Wait for the drift to go back into range (this is
normal immediately after cell maintenance or af-
ter commissioning the device)
¡ Check the maximum drift setting in the method
and increase as necessary (e.g., to 100 Counts/
min).
¡ Access further values via the System |Component
test |Chlorine menu item.
¡ If the drift remains outside of range but is com-
pletely stable, the following is also possible: Set-
ting the value "1" for drift shuts off drift monitor-
ing.

End point routine required Indicator value outside the operating range of the
titration cell:
¡ Indicator value greater than 10000: End point
routine starts automatically
¡ Indicator value less than 1000: Start an end point
routine via the System |End point routine menu
item and follow the instructions
Cell temperature exceeds Current cell temperature does not correspond to cell
range temperature configured in the method:
¡ Wait until the desired cell temperature is
achieved
¡ Access the values via the System |Component
test |Chlorine menu item.

108
multi EA 5100 Troubleshooting

¡ Check the cell temperature settings for the

method and adjust as necessary
Device not ready for measurement – Cl-POT
Display (green) Description
End point routine Automatic end point routine running:
¡ Wait for the end point routine to finish
Drift determination Drift determination immediately after titration or end
point routine:
¡ Wait until drift determination is complete (ap-
prox. 1 minute)
Device not ready for measurement - CI-AMP
Display (red) Description
Inactive No cell detected:
¡ Insert cell
¡ Basic initialization
Device not ready for measurement - CI-AMP
Display (green) Description
Stand-by titration Interval titration running:
¡ Measurement start possible
End point routine End point routine running:
¡ Wait for the end point routine to finish
Device not ready for measurement – C-NDIR
Display (red) Description
Analog values warning Analog values outside range:
¡ Access the values via the System |Component
test |NDIR menu item.
Running-in time Detector not yet ready for operation:
¡ Wait for the run-in period after activation to com-
plete (approx. 30 min)
Device not ready for measurement – S-UVFD or N-CLD
Display (red) Description
Preheating phase Detector not yet ready for operation:
¡ Wait for the run-in period after activation to com-
plete (approx. 30 min)
Vacuum/pressure error Pressure in the detector outside the permitted range:
¡ See device faults of the N detector

13.5 Device faults on the basic module

Error Possible cause Remedy

Furnace does not heat Thermocouple connector Connect the connector
not connected (→ "Removing and in-
stalling the combustion
furnace"  141)
Temperature set incor- Check temperature con-
rectly in the software figuration in the method

109
Troubleshooting multi EA 5100

Error Possible cause Remedy

No method loaded Load method
Malfunction in power Switch on the device
supply Check the internal fuses
Check the connection be-
tween the basic module
and the PC
Malfunction in the inter- Inform customer service
nal electronics department
Furnace temperature is Temperature control Inform customer service
outside tolerance limits or faulty department
target temperature is not Electronics error
reached
Process gases (inlet flow) Gas supply not connected Connect the gas supply
not supplied Primary gas pressure too Set the gas inlet pressure
low to 600 kPa (6 bar) at the
delivery point
Gas supply leaking Check gas supply
No method loaded Load method
Gas box faulty Inform customer service
department
Target flow at the outlet Connection between Check connection and en-
to the detector too low hose, angled adapter and sure correct fit at the con-
combustion tube not cor- nection points
rect
Pneumatic seal in the Check Ar supply
coupling not sealing com- Flip the toggle switch for
bustion tube the pneumatic seal down
Septum incorrectly posi- Check position of the sep-
tioned in the injection tum, insert new septum if
port or leaking necessary
Connection of the mem- Check connections (do
brane dryer or transfer not jam thread, tighten
line to the auto-protec- fingertight)
tion valve assembly leak-
ing
Transition between cou- Check the seal of the cou-
pling tube and ABD in pling tube
horizontal mode leaking Check the alignment of
the combustion tube to
the coupling tube
Tighten screw finger-
tight
Gas escaping from pneu- Connector for hose 11 Press hose 11 firmly into
matic seal (audible hiss) loose the quick-release connec-
tor

110
multi EA 5100 Troubleshooting

Error Possible cause Remedy

Pneumatic seal defective Replace pneumatic seal
(→ "Maintenance of the
auto-protection valve as-
sembly"  131)
Auto-protection valve as- Connector not connected Connect the connector
sembly not heating Heating faulty Inform customer service
Temperature control department
faulty
Auto-injector not de- Auto-injector and au- Switch off the autosam-
tected tosampler switched on at pler
the same time

13.6 Analytical problems in the basic module

Error Possible cause Remedy

Burns at the cannula Argon and oxygen con- Connect the process
nections on the combus- gases to the combustion
tion tube mixed up tube properly
Unsuitable settings in the Adjust the method pa-
method: Argon gas flow rameters to the analytical
too low in the inlet (in requirements
particular for methods
with gas autosamplers)
Low results independent Dosing fault Check dosing by auto-in-
of detection jector or autosampler
System leaking Check system tightness
Temperature set too low Check temperature con-
figuration in the method
Wrong or unsuitable cali- Check calibration, recali-
bration brate as necessary
Sample loss due to vapor- Keep liquid samples
ization or spillage closed. If possible, used a
cooled sampler.
Check sampler function
for solids
Post-combustion period Particularly for solids, a
insufficient post-combustion period
of at least 120 s must be
set.
Sooting in the system Clean or replace sooty
components
Carryover Inadequate sampler com- Rinse dosing syringes ad-
ponent rinsing equately prior to sam-
pling

111
Troubleshooting multi EA 5100

Error Possible cause Remedy

Combustion tube not Rinse combustion tube
rinsed adequately adequately with clean
solvent, i.e. blank mea-
surements until values
are constant
Contamination of the in- Replace septum
jector head or the sample Clean sluice
sluice
Scattering measurements Dosing faulty Check dosing
Combustion tube contam- Clean or replace combus-
inated or severely crystal- tion tube
lized

13.7 Device faults on the N module 5100

Error Possible cause Remedy

LED in front panel flash- ¡ Run-in period of de- ¡ Wait for the comple-
ing tection module not tion time for the run-
Ozone generator off yet complete in period of approx
30 min to elapse.
¡ Device in standby ¡ Initialize the device
¡ Gas deactivated ¡ Activate gas flow, see
software manual
¡ Module not con- ¡ Connect module (→
nected to basic mod- "Installation"  94)
ule
¡ No method or ¡ Activate a method
method with no CLD with nitrogen detec-
active tion
¡ Other fault causes ¡ Check the condition
of the module under
System |Component
test
Pressure error ¡ Gas outlet flow im- ¡ Check the "sample
peded out" connection for
unimpeded flow
¡ Absorber clogged ¡ Replace absorber (→
"Replacing the ab-
sorber"  145)
¡ Converter worn out/ ¡ Inform customer ser-
old vice department
¡ Pump faulty ¡ Inform customer ser-
vice department
¡ Device leaking or de- ¡ Inform customer ser-
fective vice department

112
multi EA 5100 Troubleshooting

Error Possible cause Remedy

Exhaust gas temperature ¡ Run-in period of de- ¡ Wait for the comple-
outside range tection module not tion time for the run-
yet complete in period of approx
30 min to elapse.
¡ Thermal ozone de- ¡ Inform customer ser-
composer defective vice department
Heating temperature sen- ¡ Thermal ozone de- ¡ Inform customer ser-
sor defective composer defective vice department
Smell of ozone ¡ Chemical ozone de- ¡ Replace chemical
composer old/inef- ozone decomposer
fective (→ "Replacing the
chemical ozone de-
composer"  146)
¡ Gas hoses on the ¡ Check hoses
ozone generator ¡ Search for leak as
leaky or loose necessary with indi-
cator paper
¡ Device leaking or de- ¡ Inform customer ser-
fective vice department

13.8 Analytical problems during TC determination

Error Possible cause Remedy

Scattering measurements ¡ Oxygen supply to the ¡ Check oxygen con-
module interrupted nection, reconnect as
necessary
¡ Absorber clogged or ¡ Replace absorber,
worn out see (→ "Replacing the
absorber"  145)
¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)
¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing
¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles

113
Troubleshooting multi EA 5100

Error Possible cause Remedy

Very low measurement ¡ Measuring gas con- ¡ Check the measuring
values or no analysis sig- nection incorrect gas connection
nal ¡ Gas outlet flow im- ¡ Check the "sample
peded out" connection for
unimpeded flow
¡ Oxygen supply inter- ¡ Check oxygen con-
rupted nection, reconnect as
necessary
¡ Converter worn out/ ¡ Inform customer ser-
old vice department
¡ Ozone generator ¡ Replace ozone gener-
faulty ator, see (→ "Replac-
ing the ozone gener-
ator"  143)
¡ Device leaking or de- ¡ Inform customer ser-
fective vice department
Results too high ¡ High halogen con- ¡ Dilute samples, if
tents disrupting TN possible
determination
Low results ¡ Incomplete NOx for- ¡ Reduce sample size/
mation due to exces- amount
sive nitrogen content ¡ Dilute sample
¡ Nitrogen compounds ¡ Select an analysis
cannot be completely method with O2+ pa-
converted to NOx due rameter mode
to their structure
(peptides, proteins,
multiple N-N com-
pounds such as azo
dyes, polycondensed
N compounds such as
morpholine)
¡ Metallic cations in ¡ Dilute samples, if
the sample lead to ni- possible
trogen salt formation

13.9 Device faults on the chlorine detector

Error Possible cause Remedy

Drift out of range (dis- Drift > 100 ¡ Replace electrolyte
played in the Status ana- Drift < -15 ¡ Check electrodes for
lyzer window wear, replace as nec-
essary

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multi EA 5100 Troubleshooting

13.10 Analytical problems during AOX, EOX and TX determination

Error Possible cause Remedy

Low results ¡ Incomplete HX for- ¡ Reduce sample size/
mation due too ex- amount
cessive halogen con- ¡ Dilute sample
tents, due to exces-
sive inorganically
bound halogen com-
pounds or due to
metal ions working as
catalysts (X2 forma-
tion).
NOTICE! The analysis
system can become dam-
aged, e.g., by chlorine.
¡ Metallic cations in ¡ Dilute samples, if
the sample lead to possible
halogen salt forma-
tion
¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)
¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing
¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles
Results too high ¡ High sulfur and nitro- ¡ Dilute samples, if
gen content disrupt- possible
ing determination

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Troubleshooting multi EA 5100

13.11 Device faults on the S module 5100 basic and S module 5100 MPO

Error Possible cause Remedy

LED in front panel flash- ¡ Run-in period not yet ¡ Wait for the comple-
ing completed tion time for the run-
in period of approx
30 min to elapse.
LED flashing after run-in ¡ UV lamp defective ¡ Check in System |
time has elapsed Component test if a
defective lamp is dis-
played
¡ Replace lamp as nec-
essary (→ "Replacing
the UV lamp"  152)
¡ If no defect is dis-
played, inform the
customer service de-
partment
Detector sensitivity too ¡ Service life of the UV ¡ Replace lamp
low lamp expired
Smell of ozone ¡ Absorber on rear of ¡ Check connection and
(only for sulfur detectors module worn out or replace absorber as
with MPO option) incorrectly connected necessary
¡ Gas hose on the ab- ¡ Check hoses
sorber leaky or loose ¡ Search for leak as
necessary with indi-
cator paper

13.12 Analytical problems during TS determination

These affect: Detection with the S module 5100 basic and the S module 5100 MPO
Error Possible cause Remedy
Scattering measurements ¡ UV lamp defective ¡ Replace lamp, see (→
"Replacing the UV
lamp"  152)
¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)
¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing

116
multi EA 5100 Troubleshooting

Error Possible cause Remedy

¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles
Low results ¡ Incomplete SO2 for- ¡ Reduce sample size/
mation due to exces- amount
sive sulfur content ¡ Dilute sample
¡ Metallic cations in ¡ Dilute samples, if
the sample lead to possible
sulfur salt formation
Results too high ¡ Excessive halogen ¡ Nitrogen: Use MPO
and nitrogen con- technology
tents disrupt TS de- ¡ Dilute samples, if
termination possible
¡ Incomplete sample ¡ Use a suitable com-
incineration (pyroly- bustion mode or
sis products) sampler, clean device
before continuing
work

13.13 Device faults on the coulometric sulfur detector

Error Possible cause Remedy

Stirring not working ¡ Module not switched ¡ Switch on the module
on
¡ No stirrer rod in the ¡ Insert stirrer rod in
measuring cell the measuring cell
¡ Stirrer rod faulty ¡ Replace stirrer rod
¡ Magnetic stirrer ¡ Inform customer ser-
faulty vice department

13.14 Analytical problems during coulometric TS determination

Error Possible cause Remedy

Scattering measurements ¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)

117
Troubleshooting multi EA 5100

Error Possible cause Remedy

¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing
¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles
False measurement val- ¡ Stirrer function faulty ¡ To remedy, see (→
ues "Device faults on the
coulometric sulfur de-
tector"  117)
¡ Incorrect electrolyte ¡ Create electrolyte,
see (→ "Preparing
the measuring cell"
 80)
¡ Filling level in the ¡ Fill the measuring cell
measuring cell too of to the height of
high or low the port for manual
measurement
¡ Electrolyte used up ¡ Replace electrolyte
¡ Electrodes incorrectly ¡ Check electrode con-
connected or faulty nections or replace
electrodes
Low results ¡ Measurement gas ¡ Check hose connec-
No analysis signal transfer to the mea- tions
suring cell inter-
rupted
¡ Glass or hose compo- ¡ Dry glass/hose com-
nents are wet ponents
Results too high ¡ Excessive nitrogen ¡ Check the NOx and
content and heavy HX absorbers, refill as
metal ions disrupt TS necessary
determination ¡ Replace the elec-
trolyte solution daily
to prevent formation
of disruptive ions

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multi EA 5100 Troubleshooting

13.15 Device faults on the carbon detector

Error Possible cause Remedy

Analog values exceeding ¡ Analog values outside ¡ Check the gas con-
values range (display in of operating range nection to the basic
the Status analyzer win- module
dow) ¡ Check the gas quality
¡ Check the analog val-
ues by performing a
component test: Sys-
tem menuComponent
test
¡ NDIR detector faulty ¡ Inform customer ser-
vice department

13.16 Analytical problems during TC, EC/OC determination

Error Possible cause Remedy

Scattering measurements ¡ Inhomogeneous sam- ¡ Warm up cold sam-
ple matrix or sample ples
matrix containing ¡ Homogenize sample
particles before analysis
¡ NDIR baseline drift ¡ Check settings
¡ Unfavorable integra- ¡ Increase the maxi-
tion criteria: Integra- mum integration
tion canceled to early time
¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)
¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing
¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles
Low results ¡ CO2 concentration ¡ Reduce sample vol-
outside of the operat- ume/amount
ing range of the NDIR ¡ Dilute samples
detector

119
Troubleshooting multi EA 5100

Error Possible cause Remedy

¡ Inlet gas flow set too ¡ Adjust method pa-
low in the method rameters
(EC/OC methods
only)
Results too high ¡ Inlet gas flow set too ¡ Adjust method pa-
low in the method rameters
(EC/OC methods
only)
No analysis signal ¡ NDIR detector faulty ¡ Inform customer ser-
vice department

13.17 Device faults on the TOC detector

Error Possible cause Remedy

Analog values exceeding ¡ Analog values outside ¡ Check the gas con-
values range (display in of operating range nection to the basic
the Status analyzer win- module
dow) ¡ Check the gas quality
¡ Check the analog val-
ues by performing a
component test:
System menuCompo-
nent test
¡ NDIR detector faulty ¡ Inform customer ser-
vice department
Leaking condensate ¡ Leaking hose connec- ¡ Replace the pump
pump tions hose
¡ Pump hose faulty
Sample is not drawn up ¡ Leaking syringe ¡ Check the dosing sy-
without air bubbles ringe
¡ If leaking, replace sy-
ringe
¡ Clogged cannula ¡ Remove the cannula
¡ Wrong cannula used and clean it in an ul-
trasound bath Re-
place cannula as nec-
essary
¡ Dosing syringe con- ¡ Clean the dosing sy-
taminated by grease/ ringe with the follow-
oil ing solutions:
Tenside solution,
30 min acting time
NaOH (0.1 mol/l),
10 min acting time
HCl (0.1 mol/l),
10 min acting time

120
multi EA 5100 Troubleshooting

Error Possible cause Remedy

¡ Rinse the syringe
thoroughly with ul-
trapure water after
each cleaning step
Water traps clogged ¡ Service life expired ¡ Replace the water
(> 6 months) traps
¡ Water trap capacity ¡ Do not analyze any
exhausted due to ex- samples that form
cessive aerosol for- aerosols
mation ¡ Only acidify samples
with hydrochloric acid

13.18 Analytical problems during TC, EC/OC, TOC, NPOC and TIC determination

TC and EC/OC determination in organic liquids, in solids and in gases:

Error Possible cause Remedy
Scattering measurements ¡ Inhomogeneous sam- ¡ Warm up cold sam-
ple matrix or sample ples
matrix containing ¡ Homogenize sample
particles before analysis
¡ NDIR baseline drift ¡ Check settings
¡ Unfavorable integra- ¡ Increase the maxi-
tion criteria: Integra- mum integration
tion canceled to early time
¡ Sample unsuitable for ¡ Use the horizontal
vertical operation operation mode
mode (droplet forma-
tion)
¡ In vertical operation ¡ Check the position of
mode: Quartz wool the quartz wool, ad-
not present or at the just as necessary
wrong position in the
combustion tube
¡ Sample evaporates ¡ Use a cooled sampler.
before dosing
¡ Sample too viscous ¡ Use the horizontal
too be drawn in with- operation mode and
out air pockets dilute the sample, or
dose directly as a
solid.
¡ Inhomogeneous sam- ¡ Homogenize sample
ple or sample con-
taining particles
Low results ¡ CO2 concentration ¡ Reduce sample vol-
outside of the operat- ume/amount
ing range of the NDIR ¡ Dilute samples
detector

121
Troubleshooting multi EA 5100

Error Possible cause Remedy

¡ Inlet gas flow set too ¡ Adjust method pa-
low in the method rameters
(EC/OC methods
only)
Results too high ¡ Inlet gas flow set too ¡ Adjust method pa-
low in the method rameters
(EC/OC methods
only)
No analysis signal ¡ NDIR detector faulty ¡ Inform customer ser-
vice department
TC, TOC, NPOC and TIC determination in water analysis:
Error Possible cause Remedy
Scattering measure- ¡ Filling of combustion ¡ Replace catalyst, see (→
ments tube depleted "Replacing the catalyst in
the TOC combustion
tube"  165)
¡ Dosing faulty ¡ Check dosing
¡ For manual dosing:
Check syringe volume
¡ Cannula damaged or ¡ Replace cannula or re-
clogged move clogging with a
cleaning stylet
¡ Filter samples contain-
ing particles before
analysis
¡ Inhomogeneous sam- ¡ Inhomogeneous water
ples samples with a high or-
ganic content, for exam-
ple oils, must be homog-
enized and may only be
analyzed in horizontal
operation mode (with
ABD)
¡ Faulty, leaky septum ¡ Check septum, replace
as necessary
¡ Only use cannula with ID
0.35 mm for
250/500 µl special sy-
ringes
¡ Sample contamination ¡ Check ambient condi-
with ambient air con- tions and remedy the
tents source of the fault
¡ NDIR baseline drift ¡ Check the gas supply
¡ Unsuitable integration and gas quality
criteria: Integration can- ¡ Adjust the maximum in-
celed too early or exces- tegration time or the
sive duration (baseline start and stop criteria
noise integrated)

122
multi EA 5100 Troubleshooting

Error Possible cause Remedy

Low results ¡ Catalyst depleted ¡ Exchange the catalyst
¡ System is leaking ¡ Check the sluice for leaks
¡ Replace septum
¡ Incorrect injection vol- ¡ For manual sampling:
ume introduce the sample
volume set in the
method
¡ Phosphoric acid in the ¡ Regenerate the TIC reac-
TIC reactor depleted tor, see (→ "Regenerat-
ing the TIC reactor"
 161)
¡ Septum faulty ¡ Replace septum

123
Maintenance and care multi EA 5100

14 Maintenance and care

14.1 Overview of maintenance work

Basic module Maintenance inter- Measure

val
Daily and after Check gas flow
maintenance Check system tightness
Weekly Clean and care of the analyzer
Check all hose connection for proper fit; replace loose connec-
tions
Monthly Check fastening screws for proper fit; tighten loose screw con-
nections
Check combustion tube for damage
Check FAST connectors at the combustion tube for proper fit,
cracks of damage; replace damaged FAST connectors
Quarterly Auto-protection valve assembly: Check filters
Annually Gas box: Check check valve and inlet filter
As necessary Replace combustion tube if it shows cracks, devitrification or
other damage
Replace check valve and inlet filter in the gas box if compo-
nents are clogged/damaged and block the gas flow
Check the correct position of the quartz wool used in vertical
operation mode in the combustion tube (for example after re-
placing the septum or a FAST connector on the combustion
tube)

N module 5100 Maintenance inter- Maintenance task

val
Weekly Clean the module from the outside
Check hoses for cracks, replace as necessary
Check hose connections for tight fit
Annually Replace the chemical ozone decomposer
Replace the ozone generator (recommend during annual rou-
tine maintenance)
Replace the NO converter tube (by customer service depart-
ment, recommended during annual routine maintenance)
As necessary Replace the absorber if the baseline is too high

S module 5100 basic, S module Maintenance inter- Maintenance task

5100 MPO val
Weekly Clean the module from the outside
Check all screw connections for tight fit
Annually Replace the absorber (S module 5100 MPO only)

124
multi EA 5100 Maintenance and care

Maintenance inter- Maintenance task

val
As necessary Replace the UV lamp

Cl module 5100 Maintenance inter- Maintenance task

val
Daily Replace sulfuric acid daily or when empty
Measuring cells "sensitive" and "high concentration":
Change the electrolyte, wipe out measuring cell after each
electrolyte replacement
Measuring cell "high sensitive" :
¡ Refill electrolyte,
Electrolyte replacement only if crystalline deposits form, if
the electrolyte has become opaque or the measurement
sensitivity is reduced
¡ Clean and dry the sulfuric acid container and safety attach-
ment including connectors and gas inlet hose
Weekly Clean the chlorine module
Check all screw connections for tight fit
Measuring cell "high sensitive":
¡ Check the bridge electrolyte fill level of the reference elec-
trode, refill as necessary
¡ Replace bridge electrolyte if the fill level has dropped to
2 cm below the opening or after multiple refills
Clean and dry the sulfuric acid container and safety attachment
including connectors and gas inlet hose (when using the "sen-
sitive" and "high concentration" measuring cells)
Clean measuring cell
Clean the measuring gas hose/gas transfer line including con-
nector with distilled water and dry via blowing out with an in-
ert gas
Monthly Check hoses for cracks and proper fit, replace as necessary
Check the ferrules in the Swagelok connectors (PTFE) for dam-
age, replace as necessary

S module 5100 coulometric Maintenance inter- Maintenance task

val
Daily Replace electrolyte
Weekly Clean the module from the outside
Check all screw connections for tight fit
Check the filling of the NOx and HX absorbers, replace as nec-
essary
Clean measuring cell
Quarterly Check measuring cell for cracks and damage, replace as neces-
sary

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C module 5100 Maintenance inter- Maintenance task

val
Weekly Clean the module from the outside
Check hoses for cracks, replace as necessary
Check hose connections for tight fit

TOC module 5100 Maintenance inter- Maintenance task

val
Daily Check gas flow
Check copper wool in the halogen trap for discoloration
Regenerate the TIC reactor
Weekly Clean the module from the outside
Check hoses for cracks, replace as necessary
Check hose connections for tight fit
Quarterly Check the TOC combustion tube for cracks and damage
Check the TIC reactor for cracks and damage.
Check the condensation coil for cracks and damage
Check the condensate pump for leaks
Check the dosing syringe for leaks
Every six months Replace water traps, earlier if necessary
Annually Replace catalyst in the TOC combustion tube, earlier if in-
structed in the software
Clean the TOC combustion tube
Clean the condensation coil
Replace the pump hose of the condensate pump
Clean the dosing syringe
As necessary Replace the filling of the halogen trap as soon as half of the
copper wool has changed color
Replace the septum on the TOC combustion tube if the system
has any leaks
Replace the septum on the TIC reactor if the system has any
leaks

14.2 Maintenance of the multi-purpose combustion tube

CAUTION
Risk of injury from falling components
The user can be injured if the combustion tube falls down during maintenance.
¡ Exercise extreme caution when performing maintenance on the combustion tube.

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14.2.1 Removing the combustion tube

CAUTION
There is a risk of burns at the combustion furnace and combustion tube!
¡ Only perform removal when cold. Allow the device to cool sufficiently.
¡ Wear the heat-proof gloves included in the delivery when handling hot components.
These gloves are suitable for temperatures of up to 200 °C.

Maintenance of the combustion tube is always performed when the furnace is is the ver-
tical installation position. Remove the combustion tube as follows:
} Exit multiWin.
} Switch off the basic module via the power switch and shut off the gas
supply.
} Remove the upper cover of the basic module.

} Open the device door. Flip the toggle switch for the pneumatic seal up.
ü The auto-protection valve assembly is opened.

} Horizontal operation mode with ABD:

Unscrew the coupling at the connection between the combustion tube
and the ABD. Slide the ABD back slightly. Rotate the furnace to the verti-
cal position.

} Remove hose 3 and hose 4 from the FAST connectors on the combustion
tube.
} Horizontal operating mode:
4 Carefully grip the flame sensor (FS) by the blue ring and pull it off the
FS combustion tube.
The connection to the combustion tube is very fragile!
} Carefully remove the combustion tube from the furnace.
3
} Check the combustion tube for crystallization, cracks and burst spots.
} If the vertical operation mode is in use: Check the condition and position
of the quartz wool plug

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14.2.2 Cleaning the combustion tube

ð Remove the combustion tube from the combustion furnace (→ "Removing the com-
bustion tube"  127).
} Remove the screw cap and septum, if present. Remove the 2 angled FAST connectors
from the combustion tube.
} For nitrogen and sulfur determination in vertical operation mode: Remove the quartz
wool plug from the combustion tube with a long hook.
Wear protective clothing when replacing the quartz wool (labcoat, protective gloves
and glasses) Wear a respiratory mask or work underneath an exhaust vent because
quartz wool dust irritates the respiratory tracts.
} Clean the inside of the combustion tube with a suitable solvent and a cotton swab or
bottle brush. Rinse with distilled water if the solvent is water-soluble. Otherwise,
rinse with ethanol.
} Dry the combustion tube (e.g., by blowing it through with an inert gas).
} Deposits from incomplete incineration, e.g., soot or solid pyrolysis residue, can also
be removed by firing the combustion tube in a muffle furnace at 750–900 °C or with
a suitable burner flame, e.g., propane.
} For nitrogen and sulfur determination in vertical operation mode: Insert a new
quartz wool plug in the combustion tube (→ "Inserting the quartz wool plug"  128).
ü The combustion tube is clean and can be reinserted.

14.2.3 Inserting the quartz wool plug

For nitrogen and sulfur determination in vertical operation mode: Insert a quartz wool
plug in the combustion tube.
Missing quartz wool leads to sooting of the analysis system. Sample with high salt con-
tent form ash and solid oxides during incineration that can build up in the quartz wool.
The quartz wool must then be replaced. The quartz wool plug is not needed for opera-
tion in horizontal mode.

CAUTION
Skin and respiratory system irritation due to quartz wool
Quartz wool tends to form dust. Irritation can occur after breathing in or skin contact
with this dust.
¡ Avoid the formation of dust when working with quartz wool.
¡ Wear protective clothing and gloves.
¡ Work under an extractor or wear a respiratory mask.

NOTICE
Risk of device damage
¡ Only use the pure quartz wool supplied by Analytik Jena GmbH. Contaminated
quartz wool may damage the combustion tube and clog the filter.
¡ Ensure correct positioning of the quartz wool plug. When the plug is not in correct
position the sample does not vaporize evenly.

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multi EA 5100 Maintenance and care

} Remove the combustion tube from the combustion furnace as described.

} Roll a small amount of quartz wool into a loose plug approx. 1.5 to 2 cm
long.

} Insert the quartz wool plug into the inner tube of the combustion tube
with a clean glass rod.
} Push the quartz wool plug into the tube until the positioning mandrel is
at the center of the plug.
The plug must not seal the bottom slot in the inner tube.
The plug should cover the entire cross section of the inner tube.
} After replacing the quartz wool: Clean the analysis system by performing
at least 3 measurements with a pure solvent (e.g., isooctane, toluene, xy-
lene).

14.2.4 Installing the combustion tube

WARNING
Risk of explosion and sooting due to improper connection of the gases to the
combustion tube.
¡ The connections for argon and oxygen on the combustion tube must not be mixed
up!

CAUTION
Risk of burns from hot components and possible damage to the seal of the auto-
protection valve assembly.
¡ Allow the combustion tube to cool before cleaning after incineration.
¡ Allow the combustion furnace to cool before inserting the combustion tube.

NOTICE
Alkaline salts (hand perspiration) cause crystallization in the quartz glass when heating
the combustion furnace. which reduces the service life of the combustion tube.
¡ Wear protective gloves when inserting the combustion tube and do not touch the
tube with bare hands.
¡ Wipe the outside of the combustion tube off with ethanol and a paper towel before
insertion.

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} Place the combustion system in the vertical position.

} For nitrogen and sulfur determination in vertical operation mode: Ensure
that the quartz wool plug has been inserted at the proper place in the
combustion tube.
} Apply FAST connectors to the gas connections of the combustion tube.
NOTICE! For angled FAST connectors: Do not push the combustion tube
connections too far into the limbs of the FAST connectors. The gas flow
may be impeded otherwise.
} Insert the combustion tube into the combustion furnace. The bent gas
connection for hose 3 must be fit into the recesses on the furnace.

} Vertical operating mode:

Screw a screw cap with septum onto the combustion tube.
Press hoses 3 and 4 into the FAST connectors on the combustion tube.
4
3 } Re-insert the cover plate with hole into the top device opening.
Connect the autosampler or auto-injector.

FS

} For horizontal operating mode:

Press hoses 3 and 4 into the FAST connectors on the combustion tube.
Carefully press the flame sensor (FS) onto the combustion tube connec-
4 tion. The connection is very fragile!
FS Move the combustion furnace into the horizontal position.

} Connecting the ABD:

Check the sealing element in the coupling piece of the ABD for correct fit
and insert new a sealing element into the coupling if necessary.
ABD Fasten the ABD with the coupling piece to the combustion tube.
Also see the "ABD user manual".

} Open the gas supply at the pressure reducer.

} Close the pneumatic seal at the auto-protection valve assembly. Flip the
toggle switch down.
ü The combustion tube is now sealed in the auto-protection valve as-
sembly and ready for operation again.

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14.3 Maintenance of the auto-protection valve assembly

CAUTION
Risk of injury from falling components
The user can be injured if the assembly falls down during maintenance.
¡ Exercise extreme caution during maintenance of the auto-protection valve assem-
bly.

14.3.1 Installing/removing the auto-protection valve assembly

CAUTION
Risk of burns from the hot furnace and the gas transfer line.
¡ Switch off the device and allow it to cool before performing maintenance.

Check the condition of the auto-protection valve assembly as follows:

For better clarity, the work steps are displayed with the side panels removed. However,
for the installation and removal of the auto-protection valve assembly it is not necessary
to remove the side panels.
} Exit the multiWin program, switch off the basic module via the power
switch and shut off the gas supply.
} Tilt the combustion furnace into the horizontal position.
} Open the pneumatic seal at the auto-protection valve assembly. Flip the
toggle switch up.
} Remove the combustion tube or pull it out some distance of the combus-
tion furnace.

} Unscrew hose 8 (1) from the connection.

2
} Press the ring on the connector of hose 11 (2) down and pull the hose
1 out of the connection.
3 } Depending on the configuration, detach the connection of the membrane
dryer and the gas transfer line:
– Unscrew the gas transfer line (3).
– Loosen the knurled screw (4) on the membrane dryer connection
4
slightly and pull the connection out toward the bottom.

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Maintenance and care multi EA 5100

} Pull the electrical connection of the auto-protection valve assembly and,

where applicable, the transfer line out of the connection.

} Hold the auto-protection valve assembly with the left hand and pull at
the knob of the clamping mount with the right hand to open the lock. Re-
move the auto-protection valve assembly from the combustion furnace.
} The installation of the auto-protection valve assembly is in reverse order.

14.3.2 Check and replace the filter

} Remove the auto-protection valve assembly.

} Check the filter for carbonization, soiling or cracks through visual inspec-
tion.
– If the filter is OK, reinstall the auto-protection valve assembly.
– If the filter must be replaced, continue to follow the instructions.

} Unscrew the 4 screws attaching the pneumatic seal to the auto-protec-

tion valve assembly.
} Remove the pneumatic seal from the auto-protection valve assembly.

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multi EA 5100 Maintenance and care

} Remove the intermediate ring.

} Remove the worn filter and insert a new filter.

} Reassemble the auto-protection valve assembly again in reverse order.
ü The auto-protection valve assembly is ready for operation again.

14.3.3 Replacing the pneumatic seal

} Remove the auto-protection valve assembly.

} Unscrew the 4 screws attaching the pneumatic seal to the auto-protec-
tion valve assembly.

} Remove the housing with the pneumatic seal from the auto-protection
valve assembly.
} Unscrew the connection bushing for hose 11 from the seal housing.

} Remove the pneumatic seal from the housing.

} Remove the PTFE disks from both sides of the seal.

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Maintenance and care multi EA 5100

} Carefully separate the special seal from the ring.

} Insert a new special seal into the ring.

} Place the PTFE disk (2) in the housing (3).

1 } Place the seal (1) in the housing. The hole in the ring must align with the
hole in the housing.
} Screw in the connection socket for hose 8.
2 3

} Place the second PTFE disk onto the intermediate ring above the filter.

} Place the pneumatic seal onto the auto-protection valve assembly and
attach it with 4 screws.
ü The auto-protection valve assembly is ready for operation again.

14.4 Replacing the membrane dryer

CAUTION
Risk of burns at the hot furnace
¡ Switch off the device and allow it to cool before performing maintenance.

NOTICE
Risk of damage due to pinching or twisting
The sensitive membrane for water vapor exchange in the membrane dryer can be dam-
aged by squeezing or twisting.
¡ Do not pinch the membrane when installing the new membrane dryer.
¡ Do not twist the sensitive connections.

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multi EA 5100 Maintenance and care

For better clarity, some work steps are displayed with the side panels removed. How-
ever, for the installation and removal of the membrane dryer it is not necessary to re-
move the side panels.
} Move the combustion furnace into the horizontal position.
} Detach the connection of the membrane dryer at the auto-protection
valve assembly. Slightly loosen the knurled screw (1) and pull the con-
nection (2) out toward the bottom.

1
2

} Move the combustion furnace into the vertical position.

1 } Remove hose 5 (1) and hose 12 (2).

} Remove hose 13 (see arrow).

} Unscrew the 3 knurled screws and remove the holder.

The membrane dryer is fastened to the furnace with 2 knurled screws on
the top side (see arrows) and 1 knurled screw on the bottom.
} Remove the old membrane heater from the mount.

} Carefully place the new membrane dryer in 2 strap loops, insert and
clamp it in the holder.
} The gas connection at the top end must point to the right and the gas
connection at the bottom end to the left.
NOTICE! The connections must not be pinched or twisted.
} Reinstall the holder with the new membrane dryer in reverse order.
ü The membrane dryer is installed and ready for operation.

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Maintenance and care multi EA 5100

14.5 Replacing the hose connections

Check the hose connections regularly for leaks. Remove and replace faulty hoses and
hose connections. Check the system for leaks after maintenance (→ "Checking the sys-
tem for leaks"  139).
When replacing Fingertight screw connections, observe the following:
¡ Only use straight cut, round and unpinched hose ends for the connection.
¡ Slide the conical nipple with the conical side towards the banjo bolt onto the hose.
¡ The conical nipple and hose end must be flush.

2 3
1

Figure 66Replacing the Fingertight connections

1 Hose 2 Banjo bolt
3 Conical nipple

14.6 Replacing the septum on the injection port

In vertical operation mode, the septum on the injection port of the combustion tube
must be replaced if it is worn out, as this leads to leaks in the system.

Figure 67Replacing the septum on the injection port of the combustion tube
} Open the device door. Flip the toggle switch of the pneumatic seal up to open the
auto-protection valve assembly.
} Remove the cover from the top of the basic module.
} Unscrew the screw cap of the combustion tube.
} Check that the quartz wool plug is still in the proper position in the inner tube of the
combustion tube.

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multi EA 5100 Maintenance and care

} Insert the septum and screw the screw cap back onto the combustion tube.
ü Replacing the septum on the combustion tube is now complete.

14.7 Replacing the check valves and particle filters

14.7.1 Replacing the check valves on the gas box

The check valves must be replaced if the gas flow can no longer be set to the target
value (observe the message in the software) and possible leaks in the system have been
excluded. The check valves are located in the valve block on the gas box on the left side
of the device.
} Switch off the basic module and disconnect the power plug from the
power outlet.
} Switch off the gas supply at the shut-off valve.
} Remove the protective ground conductor on the left side panel. Loosen
the 4 screws on the left side panel and lift off the side panel.

} Pull hoses 3 and 4 out of their connections on the valve block (see ar-
rows).

} Unscrew the screw on the valve block with a 2.5 mm hexagon socket
wrench.

} Remove the top part of the valve block and take the check valves out of
the "main" and "inlet" connections.

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Maintenance and care multi EA 5100

} Replace the sealing rings of the check valves in the upper and lower part
of the valve block.
} Insert new check valves.
} Assemble the valve block and screw on the top part.
} Connect hose 3 to the "main" connection and hose 4 to the "inlet" connec-
tion.
} Connect the protective ground conductor to the side panel and close the
side panel.
} Open the gas supply at the shut-off valve.
} Connect the power cable on the basic module and switch on the module
via the power switch.
ü The basic module is now ready for operation again.

14.7.2 Replacing the particle filters in the gas inlets

The "Ar" and "O2" gas inlets on the rear of the basic module are equipped with particle fil-
ters. The particle filters and check valves must be replaced if the process gases can no
longer be set to their target values (observe the message in the software) and possible
leaks in the system have been excluded.
} Switch off the basic module and disconnect the power plug from the
power outlet.
} Switch off the gas supply at the shut-off valve.
} When using the ABD: Disconnect the ABD from the basic module and
move the sampling module slightly to access the rear of the device.
} Pull the gas hose out of its connection on the rear of the basic module.
To do so, press down the red ring and pull the gas hose out of the con-
nection.
} Unscrew the gas connections with a 13 mm open-ended wrench.

} Unscrew the particle filters inside using a 5 mm hexagon socket wrench.

} Insert and tighten the new particle filter.

} Screw in the gas connections and tighten them with an open-ended
wrench. Connect the gas hoses.
} Reconnect the sampling module, if necessary.
} Switch on the gas supply.
} Connect the power cable to the basic module and switch on the module
via the power switch.
ü The basic module is now ready for operation again.

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multi EA 5100 Maintenance and care

14.8 Checking the system for leaks

} Switch on the basic module and the system components.

} Open the gas supply.
} Start the multiWin program.
} Activate a method.
ü The current gas flows are displayed in the Status analyzer window.
Faulty gas inlet flows are marked in red in the Status analyzer window.

MFC 200 ml/min Oxygen (primary oxygen), hose 3, value cannot

1 be changed in the method

MFC 0 ml/min (idle state) Oxygen for post-combustion phase, hose 4, gas
2 inlet on the combustion tube, value is set in the
method
MFC 100 to 200 ml/min Pyrolysis gas (argon), hose 4, gas inlet on the
3 (example) combustion tube, value is set in the method

14.8.1 System tightness for N/S/C methods

The system tightness for N/S/C methods is monitored automatically. If the system is
leaking, the Gas leak message will appear in the Status analyzer window and the MFC 1
display is marked in red. Starting a measurement is not possible.

14.8.2 System tightness for Cl methods

WARNING
Risk of chemical burns
Concentrated sulfuric acid is used in the detection module as a drying agent. The con-
centrated acid can lead to severe chemical burns.
¡ Wear protective clothing when working with these hazardous substances.
¡ Completely empty the sulfuric acid container prior to the system tightness check.
¡ Observe all notes and specifications in the safety data sheet.

NOTICE
Risk of destruction of the internal MFM due to corrosive gas
¡ To check the system tightness, only use the flow monitoring set included in the
scope of delivery.

The check of the system tightness is not performed automatically, but instead manually
using the hose set (flow monitoring set) included in the scope of delivery.

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Maintenance and care multi EA 5100

3 } Assemble the flow monitoring set in the following order:

– Thread the screw cap, the seal and the sealing cone (1) onto the thin
4 hose (2).
– Connect the hose (2) with the other hose (3).
5
– Attach the water trap and the adapter (4) to the hose (3).
1 – Attach the hose (5) to the adapter.
2

} First, completely empty the sulfuric acid from the sulfuric acid container
of the Cl module 5100 (→ "Replacing the sulfuric acid and cleaning the
sulfuric acid container."  147). Then clean, dry and re-install the con-
tainer and all adjacent components (safety attachment, gas transfer
hose, connector).
} Measuring cell "high sensitive" (image):
– Remove the gas inlet hose from the measuring cell. Remove the elec-
trolyte from the gas inlet hose. Clean and dry the outside and inside
of the tube and the connector.
– Connect the gas inlet hose to hose 5 of the flow monitoring set.
} Measuring cells "sensitive" and "high concentration":
– Disconnect hose 20 from the combined electrode and connect it to
hose 5 of the flow monitoring set.

} Remove the "MFM in" screw connection on the cover of the control elec-
tronics in the basic module and connect the flow monitoring set (hose 2)
(see arrow).
} Read the current gas flow in the Component test |Flow System |Compo-
nent test menu item) window.
The target flow is the sum total of the measured inlet flows (main + inlet
+ argon bypass). For methods using gas samplers, the auxiliary gas flow
of the gas sampler must be added.
} If the displayed flow differs from the target flow by more than ± 15 ml/
min, search for and remedy the possible causes. Contact the customer
service department if this is not successful.
} After the flow measurements, remove the set and reconnect hose 5 to
the MFM inlet to ensure a complete measuring gas path for N/S/C meth-
ods.
} Refill the sulfuric acid container with sulfuric acid.
Alternatively, the system tightness can also be checked at the transfer line. In this case,
it is not necessary to drain the sulfuric acid, but the check does not cover the entire gas
path. As leaks usually occur on the basic module, this check is a simple and quick alter-
native.
} Open the front doors of the basic module and the Cl module 5100.
} Unscrew the heated transfer line from the connector of the sulfuric acid
container.
} Connect the Fingertight connector of the transfer line to the hose of the
flow monitoring set.
} Then proceed as described before.

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multi EA 5100 Maintenance and care

14.8.3 System tightness for TOC methods

System tightness for the gas path from the inlet of the basic module to the outlet of the
TOC module 5100 is not regulated automatically. Use the hose set included in the scope
of delivery and proceed as follows:
ð The basic module and the detection module are switched on and connected.
ð The carrier gas supply is open.
ð The multiWin control and analysis software has been started.
ð A method for TOC determination is active (see software manual).
} Assemble the flow monitoring set (→ "System tightness for Cl methods"  139).
} Connect hose 5 of the flow monitoring set to the "sample out" outlet on the rear of
the detection module.
} Open the doors of the basic module.
} If necessary, disconnect the connection on the "MFM in" connection. The connection
is located on the cover plate of the control electronics on the right in the basic mod-
ule (→ "System tightness for Cl methods"  139).
} Connect the other end of the hose set with the "MFM in" inlet on the basic module.
} Read the current gas flow in the System |Component test menu under Device |Con-
trol flow.
} If the displayed flow differs from the target flow by more than ± 5 ml/min, search for
and remedy the possible causes. Contact the customer service department if this is
not successful.
ü The target flow is displayed in the Status analyzer window:
Target Description
MFC 1 200 ml/min Primary oxygen (hose 3) in the basic module,
value cannot be changed in the method
MFC 2 0 ml/min MFC 2 and MFC 3 are in standby during TOC op-
MFC 3 eration.

14.9 Removing and installing the combustion furnace

WARNING
Risk of electrical shock
¡ Before installing the combustion furnace, switch off the basic device via the power
switch and disconnect the power plug from the power outlet!

CAUTION
Risk of burns at the hot furnace
¡ Switch off the device and allow it to cool before performing maintenance.

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Maintenance and care multi EA 5100

CAUTION
Risk of injury from falling components
The user can be injured if the combustion furnace falls down during installation/re-
moval.
¡ Exercise extreme caution when installing/removing the combustion furnace.

The combustion furnace must be removed for transport.

} Remove the combustion tube (→ "Maintenance of the multi-purpose
combustion tube"  126). Leave the furnace in the vertical position after
this.
} Exit the multiWin program.
} Switch off the basic module via the device switch and disconnect the
power plug from the socket. Switch off the gas supply.
} Remove the top cover and the doors from the module.
} Remove the left side panel: Disconnect the protective ground conductor.
Loosen the screws at the left side panel. Lift the side panel off and store
it safely.

} Remove the hoses from their holders on the combustion furnace (see ar-
row).

} Remove the protective grounding from the base plate of the combustion
furnace.

} Remove the three plug-in connectors from their sockets:

– Flame sensor (1)
2 3 – Electrical connection of the combustion furnace (2). Press the gray
1
lever up slightly when doing this.
– Thermoelement (3) with colored cable

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multi EA 5100 Maintenance and care

} Move the combustion furnace into the horizontal position.

} Remove the auto-protection valve assembly from the combustion fur-
nace (→ "Maintenance of the auto-protection valve assembly"  131).

} Detach hose 14 (see arrow). Press the ring at the plug connector into the
connector and pull off the hose.
} If necessary, remove the connections on the membrane dryer (for S/N/C
methods).
} Carefully lift the combustion furnace of the basic module.
} The installation of the combustion furnace container is performed in the
reverse order.

14.10 Maintenance of the N module 5100 nitrogen detector

14.10.1 Replacing the ozone generator

WARNING
Risk of electric shock
High voltages are present in the interior of the device, which can lead to electric shock if
contacted.
¡ Before opening: Switch off the device via the power switch.
¡ Disconnect the power cable from the socket.

CAUTION
Risk of burns from the thermal ozone decomposer!
¡ Only perform maintenance in the inside of the device when cold/allow the device to
cool sufficiently.

CAUTION
Risk of respiratory problems due to leaking ozone
If the gas hoses are not properly connected to the ozone generator, ozone can leak out
of the detection module.
¡ Ensure proper hose connection.
¡ Check that the gas connections are sealed with indicator paper after maintenance.

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Maintenance and care multi EA 5100

} Switch off the detection module via the power switch.

} Remove the left side panel. Remove the 4 screws to do this. Remove the protective
grounding cable and remove the side panel.
} Remove the communication cable from the ozone generator.
} Remove the 2 hoses from the ozone generator: "O2 in" and "O3 out". The "O2 in" hose
connection is color-coded.
} Remove both angled FAST connectors from the ozone generator.
} Remove the screw the ozone generator is fastened to the base plate with (see ar-
row).
} Carefully push the old ozone generator out of the module and remove it. Insert a new
ozone generator in the detection module. Mount the ozone generator in reverse or-
der. Replace the FAST connectors with new ones when doing so.
After replacement, check the system tightness:
} Connect the detection module to the basic module.
} Switch on both modules and allow them to run in for approx. 30 min.
} Wet a strip of the indicator paper with distilled water and hold it to the ventilator on
the rear of the module for approx. 30 s.
} Also check the gas outlet of the detection modules with the test strip.
} If the strip turns blue, ozone is leaking from the module. If this is the case, switch off
the module, ventilate the room and check the proper connection of the hoses on the
ozone generator.
ü The detection module is ready for operation again.

Figure 68Replacing the ozone generator

1 Oxygen connection (O2 in) 2 Ozone outlet (O3 out)
3 Communication cable (to the PCB)

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multi EA 5100 Maintenance and care

Checking the function of the Check the function of the detection module after maintenance via a control measure-
detection module ment.
} Perform a purge measurement with a solvent, e.g., isooctane.
} Analyze a standard solution (5 mg/l TNb) Compare the curve and area with earlier
measurements.
} For resuming measuring operations: Determine the daily factor to test calibration. If
the daily factor is outside of the tolerance range, the analysis system must be re-cali-
brated.

14.10.2 Replacing the absorber

ð Replace the absorber if the analysis baseline has been permanently raised. Replace
the entire absorber (replacement part).
} Remove the screw connection from the absorber. Do not pull the hose out of the de-
vice!
} Pull the absorber out of the holding clamps.
} Press the new absorber into the holding clamps. Reconnect the hose.
ü The detection module is ready for measurement again.

Figure 69Absorber
1 Hose 6 connection 2 Holding clamp
3 Absorber

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Maintenance and care multi EA 5100

14.10.3 Replacing the chemical ozone decomposer

WARNING
Risk of electric shock
High voltages are present in the interior of the device, which can lead to electric shock if
contacted.
¡ Before opening: Switch off the device via the power switch.
¡ Disconnect the power cable from the socket.

CAUTION
Risk of burns from the thermal ozone decomposer!
¡ Only perform maintenance in the inside of the device when cold/allow the device to
cool sufficiently.

ð Replace the entire chemical ozone decomposer annually. Optionally, have the de-
composer replaced by the customer service department.
} Switch off the detection module via the power switch.
} Remove the left side panel. Remove the 4 screws to do this. Remove the protective
grounding cable and remove the side panel.
} Disconnect the following hose connections:
Disconnect hose 25 from the T piece.
Unscrew hose 24 from the bottom of the ozone decomposers.
} Remove the ozone decomposer with its filter and hose 25 from the holding clamps.
Recommendation: Remove it from the top clamp first.
} Install the new filter in the reverse order.
ü The detection module is ready for measurement.

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multi EA 5100 Maintenance and care

Figure 70Replacing the chemical ozone decomposer

1 Ozone decomposer 2 Hose 24
3 Filter with hose 25

14.11 Maintenance of the Cl module 5100 chlorine detector

14.11.1 Replacing the sulfuric acid and cleaning the sulfuric acid container.

WARNING
Risk of chemical burns
Concentrated sulfuric acid can cause severe chemical burns!
¡ Before replacing the sulfuric acid: Switch off the gas supply via the software. Risk of
splashing if the gas supply is running.
¡ Wear protective clothing when working on the sulfuric acid container.
¡ Observe all instructions and specifications in the safety data sheet.

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

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Maintenance and care multi EA 5100

The sulfuric acid absorbs the water that is produced during the combustion process. If
the acid content falls below 85 % the sulfuric acid can no longer sufficiently dry the reac-
tion gas. Chlorine values that are too low are then measured.

7 1

5 2

4
4 3

Figure 71Connection of the heated gas transfer lines to the sulfuric acid container
1 Safety attachment 2 Sulfuric acid container
3 Hose for measuring gas infeed 4 Connector
5 Banjo bolt 6 Heated gas transfer line
7 Measuring gas transfer to the mea-
suring cell with PTFE connector
ð Replace the sulfuric acid daily. High sample throughput may require more frequent
replacement.
} Exit the multiWin software and switch off the analysis system. Switch of the detec-
tion module via the switch on the rear of the device.
} Allow the heated gas transfer line to cool or wear heat-proof gloves when replacing
the sulfuric acid.
CAUTION! Risk of burns at the ends of the heated gas transfer line! The ends can
achieve temperatures of up to 100 °C during operation.
} Remove the banjo bolt from the connector, separating the heated gas transfer line
from the sulfuric acid container.
} Disconnect the PTFE connection and remove hose 20 from the safety attachment.
} Carefully pull the sulfuric acid container with its remaining components out of the
holding clamps toward the top and remove it from the module.
A large beaker is suitable for safe transport and storage (e.g., 500 ml).
} For the "high sensitive" measuring cell: Remove the gas inlet tube from the detection
module with PTFE screw joint and hose 20.
} Remove the safety attachment from the sulfuric acid container.
NOTICE! The bases of the PTFE screw joints remain on the safety attachment, the
hose and the gas inlet tube.

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multi EA 5100 Maintenance and care

} Unscrew the connectors for the heated gas transfer line from the sulfuric acid con-
tainer. Remove the thin hose from the container.
CAUTION! Sulfuric acid residue can still be present on the hose.
} Empty the sulfuric acid via the top opening. Dispose of the sulfuric acid.
} Rinse the sulfuric acid container and the safety attachment multiple times with ultra-
pure water and then rinse with ethanol or methanol:
} Rinse hose 20 including the PTFE screw joint with ultrapure water and then with
ethanol or methanol.
} Dry the cleaned components, e.g., by blowing it through with an inert gas.
} Place the sulfuric acid container down somewhere safe and fill it with 20 ml of con-
centrated sulfuric acid.
} Install the filled sulfuric acid container in the detection module in reverse order (→
"Installation"  59).
NOTICE! Ensure the proper fit of the conical nipples when connecting the gas trans-
fer line and the PTFE connectors.
ü The detection module is ready for operation again.

14.11.2 Maintenance of the measuring cell

WARNING
Risk of chemical burns
The electrolyte solution contains high concentrations of acetic acid.
¡ Wear protective clothing when replacing the electrolyte solution.
¡ Observe all instructions and specifications in the safety data sheet.

ð For the "sensitive" and "high concentration" measuring cells: Replace the electrolyte
solution daily.
ð For the "high sensitive" measuring cell: Refill the electrolyte solution daily.
Only replace the electrolyte solution in the event of analytical problem and if crys-
talline deposits form.
} For replacement of the electrolyte: Empty the measuring cell. Dispose of the elec-
trolyte solution.
} Rinse the empty measuring cell and the magnetic stirrer first with ultrapure water,
then with ethanol.
} Carefully wipe the measuring cell and the magnetic stirrer with tissue to remove any
possible silver chloride residue.
} Fill the measuring cell with fresh electrolyte solution:
"high sensitive" measuring cell: 65 ml
"sensitive" measuring cell: 15 to 20 ml
"high concentration" measuring cell: 120 ml
ü The measuring cell is ready for operation again.
Also observe the following:
¡ If the detection module is put out of operation for multiple days, clean the measur-
ing cell and store it in a dry place.
¡ Check the casing of the magnetic stirring rod for cracks regularly. If metal ions from
the stirring rod come into contact with the electrolyte solution, they can disrupt the
analysis.

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Maintenance and care multi EA 5100

¡ Due to risk of short-circuits: Prevent fluids from entering the stirring/cooling block
and the plug-in contacts.

14.11.3 Maintenance and storage of the electrodes

Combined electrode

NOTICE
Risk of possible destruction of the electrode due to cleaning, abrasive or polish-
ing agents.
The combined electrode consists of ceramic materials which is mechanically sensitive es-
pecially near the fused electrodes.
¡ Only rinse the combined electrode with ethanol and ultrapure water to clean it.

When handled incorrectly, the electrical connection of the combined electrode can
break.
¡ Carefully remove the electrode from the lid of the measuring cell.
¡ Grip the electrode from above and pull it straight out of the lid.
¡ Do not pull on or jerk the side connection sleeve for the electrical connections. The
connections in the sleeve will break otherwise (not visible from outside)!

Figure 72Correct handling of the combined electrode

Drying of electrolyte on the combined electrode can cause an irreversible reduction of its
sensitivity or damage the electrode. Therefore, make sure that the electrolyte never
dries on the combined electrode.
¡ For brief operational interruptions (one full day): Store the combined electrode in
fresh electrolyte solution.
¡ When put out of operation for multiple days: Carefully rinse the combined electrode
with ethanol and subsequently rinse it with ultrapure water. Also rinse the inner
opening for the gas inlet while doing so. Wipe the combined electrode with cellulose
and store it in dry condition.
¡ For intensive cleaning: Fill the measuring cell with ethanol. Insert the combined
electrode in the measuring cell and allow the solution to stir for several hours in the
detection module. Do not connect the measuring cell or the electrode to their elec-
trical connections for this.
¡ Before an end point routine: Store a new combined electrode or one that has been
stored in a dry place in fresh electrolyte solution for at least one hour.

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multi EA 5100 Maintenance and care

¡ Do not touch the measuring cell and the electrode during operation (during a mea-
surement or an end point routine). The measurement result will be falsified other-
wise.
¡ The generator anode is located at the bottom of the measuring cell in the form of
the stable silver plate (silver circle). The silver electrode wears out with increasing
use. If necessary, the entire measuring cell must be replaced.

Sensor electrode

NOTICE
Risk of damage to the sensor electrode
The sensor pin and the gold contact of the sensor electrodes are sensitive to touch.
¡ Apply scratch protection to the sensor pin for storage.
¡ Rinse the sensor pin with ultrapure water before use or to clean it. Do not touch it
again after this. Do not dry the pin or wipe it dry!
¡ Before use or to clean it, wipe the gold contact with a cloth and some ethanol. Do
not touch it again after this.

Storing the sensor electrode:

¡ The sensor electrode can be stored in the measuring cell for several days if it is suffi-
ciently filled with electrolyte solution.
¡ Clean the sensor electrode with ultrapure water before longer storage. Apply scratch
protection to the sensor pin. Store the electrode in a dry place.

Reference electrode

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.
¡ Check the condition and filling level of the bridge electrolyte weekly. The bridge
electrolyte must be clear and free of deposits or other particles.
¡ If necessary: Refill or replace the electrolyte solution.
Storing the reference electrode:
¡ The reference electrode can be stored in the measuring cell for several days if it is
sufficiently filled with electrolyte solution.
¡ For storage of less than 1 month: Close the refill opening. Apply the empty protec-
tive cap to the electrode.
¡ For storage longer than 1 month: Empty the bridge electrolyte completely via the re-
fill opening with a syringe or disposable pipette. Close the refill opening. Apply the
empty protective cap to the electrode.
Putting the reference electrode back into operation after longer storage:
¡ Rinse the inside of the electrode with approx. 2 ml electrolyte solution.
¡ Fill the electrode with electrolyte solution up to the refill opening.
¡ Fill the measuring cell with electrolyte solution. Insert the electrode in the measur-
ing cell and allow the solution to stir for several hours in the detection module. Do
not connect the electrode to its electrical connection for this.

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Maintenance and care multi EA 5100

Platinum electrode The platinum electrode is maintenance-free. The salt bridge of the platinum electrode
has a diaphragm. The electrolyte solution must not be allowed to crystallize inside the
diaphragm, otherwise it can clog. Remove the salt bridge and rinse with sufficient dis-
tilled water for longer storage intervals.

The silver electrode in the "high Wipe the silver surface with cellulose after use. Otherwise, the electrode is mainte-
sensitive" measuring cell nance-free. The silver electrode can show discoloration from longer use.

14.12 Maintenance of the S module 5100 basic and S module 5100 MPO sulfur
detector

14.12.1 Replacing the UV lamp

WARNING
Risk of electric shock
High voltages are present in the interior of the device, which can lead to electric shock if
contacted.
¡ Before opening: Switch off the device via the power switch.
¡ Disconnect the power cable from the socket.

WARNING
Risk due to UV radiation
The UV lamp emits UV radiation that can damage eyes and skin.
¡ Before opening the detection module: Switch off the device via the power switch.

CAUTION
Risk of burns
The UV is hot directly after operation.
¡ Allow the lamp to cool before maintenance.

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

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multi EA 5100 Maintenance and care

NOTICE
Contamination reduces the effectiveness of the UV lamp.
¡ Do not touch the glass of the new lamp. In particular, protect the radiation emission
point made of quartz glass.
¡ If the glass is touched, wipe it with a lint-free cloth and pure alcohol.

The following states indicate a defective UV lamp:

¡ The run-in period of the detection module takes is not complete after 30 min. The
LED on the front flashes continuously.
¡ The measurement sensitivity is too low or the detection limit can no longer be
reached.
¡ Check the state of the UV lamp in the System |Component test menu in the detec-
tion module tab. If a defect is indicated or the lamp is worn out, replace the lamp.
} Switch off the detection module via the power switch.
} Remove the left side panel. Remove the 4 screws to do this. Remove the
protective grounding cable and remove the side panel.
ü The UV lamp is located to the left in the module (see arrow).

} Unscrew both fastening screws with a Phillips screwdriver.

} Pull the connection plug on top out of the socket.

} Carefully remove the lamp from its holder.

} Insert a new lamp in the holder.
NOTICE! Only touch the new lamp by its base or its cable. Do not touch
the glass. Do not scratch the lamp.

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Maintenance and care multi EA 5100

} Place the lamp in the proper position when inserting: The pin on the
holder must fit into the groove of the lamp body.
} Fasten the new lamp with the 2 screws.
} Plug the connection plug back into the socket all the way.
} Fasten the side panel again.
ü The detection module is ready for operation again.

14.12.2 Replacing the chemical ozone decomposer

Only for the S module 5100 MPO

ð Replace the entire chemical ozone decomposer at least once annually.
ð Always replace the ozone decomposer when the smell of ozone is noticeable.
} Undo the hose from the chemical ozone decomposer. Do not pull the hose out of the
device!
} Pull the ozone decomposer out of the holding clamps.
} Press the new ozone decomposer into the holding clamps. Reattach the hose.
ü The detection module is ready for measurement again.

Figure 73Replacing the chemical ozone decomposer

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multi EA 5100 Maintenance and care

14.13 Maintenance of the coulometric sulfur detector

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

14.13.1 Replacing the absorber

CAUTION
Skin and respiratory system irritation due to quartz wool
Quartz wool tends to form dust. Irritation can occur after breathing in or skin contact
with this dust.
¡ Avoid the formation of dust when working with quartz wool.
¡ Wear protective clothing and gloves.
¡ Work under an extractor or wear a respiratory mask.

ð Check the absorber once per week. Replace the filling if necessary.
ð Replace the filling of the NOx absorber if the color has turned from light green to
yellow or light brown.
ð Replace the filling of the HX absorber if the color has turned from metallic silver to
dark gray.
} Remove the hose connection of the absorber tube.
} Remove the absorber tube from the clamps.
} Disconnect the FAST connector from the tube on one side. Remove the quartz wool
plug.
} Remove the use filling from the tube.
} Fill fresh absorber material (silver wool for the HX absorber, ammonium iron(II) sul-
fate for the NOx absorber) into the tube. Reinsert the quartz wool plug. Connect the
FAST connector.
} Carefully place the absorber tube back in the clamps.
} Connect the hoses to the absorber tube.
ü The detection module is ready for operation again.

155
Maintenance and care multi EA 5100

2 1

Figure 74NOx absorber and HX absorber

1 NOx absorber 2 HX absorber

156
multi EA 5100 Maintenance and care

14.13.2 Replacing the electrolyte solution

8 1

2
6

5 4

Figure 75Coulometric sulfur detector with measuring cell (without door)

1 Indicator electrodes connection 2 Indicator electrode (black)
3 Gas inlet 4 Measuring cell
5 Port for manual dosing 6 Anode (yellow)
7 Cathode (red) 8 Generator electrodes connection
ð Replace the electrolyte solution daily and when it is used up.
} Switch of the magnetic stirrer via the rotary switch.
} Switch off the detection module via the power switch.
} Disconnect the two electrode cables on the "generation" and "indication" connections.
} Disconnect hose 72 from the HX absorber.
} Remove the measuring cell from the detection module.
} Remove the electrodes and the gas inlet tube from the measuring cell. Empty the re-
maining electrolyte solution from the generator electrodes. Set the components
down.
} Remove the electrolyte solution from the measuring cell.
} Rinse the stirring rod with ultrapure water. Rinse out the measuring cell.

157
Maintenance and care multi EA 5100

} Fill the measuring cell with approx. 100 ml of fresh electrolyte solution (approx up to
the manual dosing port). For creation of the electrolyte solution, see (→ "Preparing
the measuring cell"  80).
} Carefully place the stirring rod back in the measuring cell.
} Reinsert the electrodes in the measuring cell. Connect the electrodes to the "Genera-
tion" and "Indication" connections.
} Place the measuring cell in the holder on the magnetic stirrer.
} Insert the gas inlet tube into the measuring cell. Connect the gas inlet tube with the
HX absorber via hose 72.
} Activate the magnetic stirrer (set to stage 3 approx.).
NOTICE! The magnetic stirring rod can damage the electrodes if the rotation fre-
quency is set too high. Operate the rotary switch with care.
} Wait for approx. 5 min for the new electrolyte to collect in the salt bridge of the gen-
erator electrodes and for the measuring cell to establish equilibrium. Before starting
any measurement, the end point routine must be performed.
ü The detection module is ready for operation again.

14.14 Maintenance of the TOC detector

NOTICE
Risk of gas leaks
System tightness for the gas path from the inlet of the basic module to the outlet of the
detection module is not regulated automatically.
¡ Always check the system tightness after performing maintenance on the detection
module (→ "System tightness for TOC methods"  141).

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multi EA 5100 Maintenance and care

14.14.1 Replacing the water traps

81
1

2
3
4

Figure 76Replace the water traps

1 FAST connector (angled) 2 Screw connection
3 Disposable retention filter (water 4 Clamp
trap)
5 Aerosol trap (large water trap) 6 Hose connector (to the cooling
block)
ð Replace the water traps at least every 6 months.
} Remove the hose connections from the water traps. Remove the water traps from
the clamps.
} Assembly the new water traps:
The "INLET" marking on the large water trap (aerosol trap) must be facing down-
ward.
The red labeling on the small water trap must face upward.
} Insert the new water traps into the clamps. The large water trap has to be positioned
at the bottom.
} Connect the hose connections to the water traps.
NOTICE! For angled FAST connectors: Do not push the connections too far into the
limbs of the FAST connectors. The gas flow may be impeded otherwise.
} Check the system for leaks.
ü The detection module is ready for operation again.

14.14.2 Replacing the halogen trap

CAUTION
Skin and respiratory system irritation due to quartz wool
Quartz wool tends to form dust. Irritation can occur after breathing in or skin contact
with this dust.
¡ Avoid the formation of dust when working with quartz wool.
¡ Wear protective clothing and gloves.
¡ Work under an extractor or wear a respiratory mask.

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Maintenance and care multi EA 5100

NOTICE
Risk of device damage due to aggressive combustion products
When the copper wool is used up, aggressive combustion products can damage the opti-
cal and electronic components of the detection module.
¡ Replace the complete filling of the halogen trap as soon as half of the copper wool
has turned black.

82 81

Figure 77Replacing the halogen trap

1 FAST connector 2 Copper wool
3 Brass wool 4 Clamp
ð Replace the contents of the halogen trap when half of the copper wool is discolored.
} Remove the FAST connectors from the halogen trap and remove the U-tube from the
clamps.
} Remove the quartz wool plugs.
} Pull out the depleted copper wool or brass wool from the U-tube with a tweezers or a
small hook.
} Inspect the U-tube for cracks.
NOTICE! Use only completely intact U-tubes.
} If necessary, rinse the U-tube with ultrapure water and let it dry.
} Fill the U-tube with new copper and brass wool. Replace the entire contents.
Make sure that the copper and brass wool is not compacted too much, but also en-
sure that there are no larger hollow spaces.

160
multi EA 5100 Maintenance and care

} Cover the copper and brass wool with quartz wool.

} Carefully press the filled U-tube into the clamps.
} Connect the fast connector with hose 81 to the gas inlet limb with copper wool and
hose 82 to the gas outlet limb with brass wool.
} Check the system for leaks.
ü The detection module is ready for operation again.

14.14.3 Regenerating the TIC reactor

WARNING
Risk of chemical burns
The TIC reactor is regenerated and cleaned with 40 % phosphoric acid. Phosphoric acid
can irritate eyes, skin and mucous membranes.
¡ Wear protective clothing when handling the concentrated acid.
¡ Observe all notes and specifications in the safety data sheet.

NOTICE
Risk of leaks
A cannula that is too large will damage the septum on the septum port.
¡ Only use cannula with an outer diameter of 0.63 mm for the septum port.

ð For TIC determination or TIC determination in differential mode: The TIC reactor
must be regenerated daily. How often this must be done is dependent on the TIC
content of the samples. For high TIC content, regenerate the TIC reactor more than
once daily.
ð Regeneration of the TIC reactor is also required after longer times of inactivity.
ð If only the TC or NPOC mode is used, regeneration of the TIC reactor is not required.
} Select the System |Component test menu.
} Select Regeneration TIC reactor from the list field in the Device tab.
} Click the Regeneration TIC reactor button.
} After prompt via software: Add 40 % phosphoric acid to the TIC reactor via the sep-
tum port with the supplied 5 ml syringe.
ü The TIC reactor is drained off and purged.

14.14.4 Cleaning the TIC reactor

WARNING
Risk of chemical burns
The TIC reactor is regenerated and cleaned with 40 % phosphoric acid. Phosphoric acid
can irritate eyes, skin and mucous membranes.
¡ Wear protective clothing when handling the concentrated acid.
¡ Observe all notes and specifications in the safety data sheet.

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Maintenance and care multi EA 5100

ð Check the TIC reactor for deposits and cracks quarterly. Cleaning is only required if
TIC samples are no longer properly purged.
} Undo the connection between the TIC reactor and the water traps.
} Remove the 2 knurled screws on the cover of the cooling block. Remove the cover.
} Remove the FAST connector with hose 80 from the side outlet of the TIC reactor.
} Remove the waste hose (hose 86) to the condensate pump from the connection on
the bottom of the TIC reactor.
} Remove the TIC reactor from the detection module and check it for deposits and
cracks.
} Rinse the TIC reactor with ultrapure water.
} Reinstall the TIC reactor in the detection module is reverse order.
} Check the system for leaks.
ü The detection module is ready for operation again.

7
1

2
6

3
4

Figure 78TOC detector, door opened

1 Water traps 2 Measuring gas hose from the basic
module (hose 80)
3 Condensate pump 4 TIC reactor
5 Cooling block (measuring gas dryer) 6 Halogen trap
7 Hose 81

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multi EA 5100 Maintenance and care

14.14.5 Replacing the pump hose of the condensate pump

WARNING
Risk of chemical burns
Residue of 40 % phosphoric acid can still be found in the pump hose. Phosphoric acid
can irritate eyes, skin and mucous membranes.
¡ Wear protective clothing when handling the concentrated acid.
¡ Observe all notes and specifications in the safety data sheet.

ð Check the condensate pump for leaks every 3 months. If any liquid is escaping from
the pump hose, replace the pump hose.
ð When the pump body and the roller carrier are heavily damaged, they must be re-
placed. Inform customer service for this.
} Press the bracket on the condensate pump to the left.
} Remove hoses 85 and 86 from the pump's connections.
} Remove the guide piece with the pump hose from the pump body.
} Check the pump hose and the connections on excessive wear and cracks.
} Wipe the pump body and roller carrier with ultrapure water.
} Check the pump body and roller carrier for wear.
} Push the intact or new pump hose back into the guide piece.
During installation, the hose clamps must be turned downwards.
} Push the hose guide into the groove on the guide piece.
} Position the guide piece with the hose around the pump body again. Press the guide
piece down with one hand to do this. Move the bracket to the right until it engages
with the other hand.
} Press hoses 85 and 86 back onto the metal connections of the pump hose.
} Check the system for leaks.
ü The detection module is ready for operation again.

Figure 79Installing the pump hose in the guide piece

1 Guide piece 2 Groove
3 Hose clamp 4 Metal connection

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Maintenance and care multi EA 5100

14.14.6 Cleaning the condensation coil

CAUTION
Risk of burns at the hot furnace
¡ Switch off the device and allow it to cool before performing maintenance.

ð Clean the condensation coil annually.

} Switch off the basic modules via the power switch and allow the device to cool.
} Switch off the gas supply and disconnect the power plug from the power outlet.
} Open the doors of the basic module.
} Release the fork clamp connecting the outlet of the TOC combustion tube with the
condensation coil.
} Remove the fork clamp and disconnect the spherical joint connector
} Remove the FAST connector on the bottom end of the condensation coil.
} Carefully remove the condensation coil from the clamps on the combustion furnace.
} Inspect the condensation coil for deposits and cracks.
} Rinse the condensation coil with ultrapure water and dry it well.
} Reinstall the condensation coil in reverse order.
} Check the system for leaks.
ü The analysis system is ready for operation again.

Figure 80Components in the basic module

1 TOC combustion tube injection port 2 Spherical joint (fasten with forked
clamp)
3 Condensation coil

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multi EA 5100 Maintenance and care

14.14.7 Replacing the catalyst in the TOC combustion tube

CAUTION
Risk of burns at the hot furnace
¡ Switch off the device and allow it to cool before performing maintenance.

CAUTION
Skin and respiratory system irritation due to quartz wool
Quartz wool tends to form dust. Irritation can occur after breathing in or skin contact
with this dust.
¡ Avoid the formation of dust when working with quartz wool.
¡ Wear protective clothing and gloves.
¡ Work under an extractor or wear a respiratory mask.

ð If the catalyst loses effectiveness, the combustion tube must be refilled. A check has
to be performed after the maintenance interval has elapsed (max. 1500 injections).
A software message will indicate when the maintenance interval has elapsed.
ð The service life of the catalyst depends largely on the samples. On average, approx.
1500 injections can be performed, more are sometimes possible. The service life can
be lower with especially loaded samples, especially high salt content.
} Switch off the basic modules via the power switch and allow the device to cool.
} Switch off the gas supply and disconnect the power plug from the power outlet.
} Open the doors of the basic module and remove the top cover.
} Remove the FAST connector with hose 3 from the combustion tube.
} Unscrew the knurled head screw at the fork clamp and remove the fork clamp con-
necting the outlet of the combustion tube to the condensation coil.
} Disconnect the spherical joint. The condensation coil remains in the basic module.
} Remove the tube holder for holding the combustion tube.
} Carefully pull the combustion tube out of the combustion furnace toward the top.
} Remove the screw cap with septum from the combustion tube.
} Remove the used catalyst filling.
} Check the combustion tube for heavy crystallization, cracks and burst spots. Only re-
use intact combustion tubes.
} Rinse the combustion tube with ultrapure water and allow it to dry.
ü The TOC combustion tube is clean.

Filling the TOC combustion

tube

NOTICE
Risk of devitrification of the quartz glass due to sweat
Alkaline salts in sweat from hands leads to devitrification of quartz glass when heated.
Devitrification reduces the service life of the combustion tube.
¡ Only touch the cleaned combustion tube when wearing gloves.

165
Maintenance and care multi EA 5100

} Insert approx. 500 mg of quartz glass wool in the combustion tube. Carefully press
the glass wool down to a height of approx. 1 cm with a glass rod. Do not press it
down too tightly.
} Carefully pour 16 g of platinum catalyst onto the quartz wool (fill height approx
4 cm).
} Cover the catalyst completely with approx 250 mg of quartz glass wool. Carefully
tamp down the quartz wool.
} Fill approx. 10 g of ground quartz glass into the combustion tube (fill height approx.
2 cm).
} Cover the ground quartz glass with a piece of high temperature fiber mat (HT mat)
(layer height approx 1 cm).
} Close the filled TOC combustion tube with septum and screw cap and reinstall it in
the furnace in reverse order.
} Check the analysis system for leaks.
ü The analysis system is ready for operation again.

1
2
3

Figure 81TOC combustion tube

1 HT mat 2 Quartz glass fragments
3 Quartz wool 4 Catalyst
5 Quartz wool

NOTICE
The catalyst may emit gas during first heating, this can be seen as mist formation in the
TIC reactor.
¡ Allow the catalyst to normalize during first heating for approx. 30 min until mist no
longer forms. Disconnect the gas path between the TIC reactor and the water traps
for this.

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multi EA 5100 Transport and storage

15 Transport and storage

15.1 Transport

When transporting the device, observe the safety instructions in the "Safety instructions"
section.
Avoid the following during transport:
¡ Impact and vibration
Risk of damage due to shock, impact or vibration!
¡ Large temperature fluctuations
Risk of condensation!

15.2 Moving the device in the laboratory

CAUTION
Risk of injury during transport
Dropping the device poses a risk of injury and damage to the device.
¡ Proceed carefully when moving and transporting the device. Two persons are re-
quired to lift and carry the device.
¡ Grip the device firmly at the bottom with both hands and lift it simultaneously.

Observe the following when moving the device within the laboratory:
¡ Insufficiently secured components pose a risk of injury!
Before moving the device, remove all loose parts and disconnect all connections
from the device.
¡ For safety reasons, two persons are required to transport the device, one person on
each side of the device.
¡ As the device does not have carrying handles, grip the device firmly with both hands
at the lower end. Lift the device simultaneously.
¡ Observe the guide values and adhere to the legally mandated limits for lifting and
carrying loads without auxiliary means.
¡ Observe the installation conditions at the new location.

15.3 Storage

NOTICE
Risk of device damage due to environmental conditions
Environmental influences and condensation can destroy individual components of the
device.
¡ Only store the device in air-conditioned rooms.
¡ Ensure that the atmosphere is free of dust and corrosive vapors.

167
Transport and storage multi EA 5100

If the device is not installed immediately after delivery or not required for longer periods,
it should be stored in its original packaging. A suitable desiccant should be added to the
equipment to prevent damage from moisture.
The requirements for the climatic conditions of the storage location can be found in the
specifications.

15.4 Preparing the basic module for transport and storage

Prepare the basic module for transport as follows:

} Switch off the basic modules via the power switch and allow the device to cool.
} Switch off the gas supply and disconnect the power plug from the power outlet.
} Disconnect all connection on the rear of the module.
} Remove the combustion tube (→ "Maintenance of the multi-purpose combustion
tube"  126).
} Remove the auto-protection valve assembly (→ "Maintenance of the auto-protection
valve assembly"  131).
} Remove the membrane dryer with holder from the combustion furnace (→ "Replac-
ing the membrane dryer"  134).
} Remove the combustion furnace (→ "Removing and installing the combustion fur-
nace"  141)
} Pack open hose ends in protective bags and secure them with adhesive tape.
} Close the doors of the basic module.
} Position the top cover and secure it with adhesive tape.
} Secure the maintenance flaps on the right device side with adhesive tape.
} Carefully pack the combustion furnace and additional accessories in the original
packaging. Especially the glass components must be packed safely against breakage.

15.5 Preparing detection modules

CAUTION
Risk of injury
A risk of injury due to broken glass is present when handling glass parts.
¡ Handle glass parts with extreme caution.

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multi EA 5100 Transport and storage

WARNING
Risk of chemical burns due to acid and electrolyte solution return
Concentrated sulfuric acid is used in the Cl module 5100, phosphoric acid in the TOC
module 5100 and a slightly acidic electrolyte solution in the S module 5100 coulomet-
ric.
A vacuum can be created in the analysis system when the combustion furnace is cooling.
This vacuum can lead to acid being drawn all the way into the auto-protection valve as-
sembly via connection hoses and lines.
¡ For the Cl module 5100: Only switch off the basic module and the gas supply when
the analysis system has cooled. The argon safety bypass on the auto-protection
valve assembly prevents a vacuum from being created during cooling for the chlo-
rine analysis branch. Alternatively: Remove the hose connection between the basic
module and the detection module before cooling.
¡ For the TOC module 5100 and the S module 5100 coulometric: Before shutting
down the basic module via the software, disconnection the hose connection to the
detection module.

} Switch off the detection module via the power switch. Disconnect the power plug
from the power socket.
} Shut off the gas supply.
} Disconnect all connections on the rear of the detection module.
} Seal the open gas connections with the ends of a short, fitting piece of hose to pre-
vent contamination during transport.
} Remove loose components such as the absorber from the rear of the detection mod-
ule and package them individually.
} If the detection module can be opened via the front door, remove all moving compo-
nents and package them individually. Observe the notes for individual detection
modules for this.
} Carefully package the detection module and the accessories (cables, glass compo-
nents, hoses, clamps) in the original packaging.
} Add a desiccant to the package to prevent moisture damage.

15.5.1 Notes for the transport of the Cl module 5100

WARNING
Risk of chemical burns
The concentrated sulfuric acid used as a drying agent and the acetic acid electrolyte so-
lution can cause severe chemical burns.
¡ Wear protective clothing when working on the sulfuric acid container and the mea-
suring cell.
¡ Observe all instructions and specifications in the safety data sheets.

} Disconnect the electrodes (and the measuring cell) from the electrical connections on
the inside of the rear panel of the detection module.
} Disconnect the measuring gas hose from the gas inlet tube/from the combined elec-
trode. Ensure that the seals of the PTFE screw connection are not lost during trans-
port.

169
Transport and storage multi EA 5100

} Disconnect the measuring cell from the exhaust hose and remove the measuring cell.
Empty the measuring cell.
} Disconnect the gas transfer line from the sulfuric acid container.
} Remove the sulfuric acid container from the detection module. Empty and rinse the
container (→ "Replacing the sulfuric acid and cleaning the sulfuric acid container."
 147).
} Put all electrodes into their original packaging. Observe the instructions on mainte-
nance and care of the electrodes (→ "Maintenance and storage of the electrodes"
 150).
} Clean the measuring cell with distilled water and ethanol. Carefully wipe out/off the
measuring cell and the magnetic stirring rod with tissue.
} Fasten the exhaust hose in the detection module, e.g., with adhesive strips.

15.5.2 Notes on transport of the S module 5100 coulometric

} Disconnect the electrode cables from the "Generation" and "Indication" connections.
} Disconnect the hose connections to the HX and NOx absorbers and remove both ab-
sorbers from the module.
} Remove the measuring cell from the module.
} Remove the electrodes and the gas inlet tube from the measuring cell.
} Empty the measuring cell, remove the magnetic stirring rod and rinse both with ul-
trapure water.
} Package the glass components and the electrodes in their original packaging.

15.5.3 Notes on transport of the TOC module 5100

WARNING
Risk of chemical burns
The TIC reactor can contain 40 % phosphoric acid residue. Phosphoric acid can irritate
eyes, skin and mucous membranes.
¡ Wear protective clothing when emptying and cleaning the TIC reactor.
¡ Observe all notes and specifications in the safety data sheet.

} Remove the halogen trap and the water traps from the detection module.
} Remove the TIC reactor from the detection module and rinse it out.
} In the basic module: Remove the condensation coil and the TOC combustion tube af-
ter the furnace has cooled.
CAUTION! Risk of burns around the hot furnace!
} Package all components and connection hoses in their original packaging.

170
multi EA 5100 Disposal

16 Disposal
When the respective service life has expired, the multi EA 5100 basic module, the detec-
tors and sampling modules must be disposed of as electronic waste in accordance with
the applicable regulations.
Waste water containing acids and sample material is generated during device operation.
Dispose of the neutralized waste in accordance with the legal requirements.

Cl module 5100 electrodes The metals used for the electrodes (platinum, silver) must not be allowed to contami-
nate the sewage systems, the surface or ground water or the soil. Dispose of the elec-
trodes in accordance with applicable regulations on hazardous waste.

The chemical ozone decom- The chemical ozone decomposer contains metal oxides. The absorber is filled with active
poser on the absorber of the carbon and soda lime. The used cartridges must be disposed of in accordance with local
N module 5100 or S module regulations.
5100 MPO

TOC module 5100 The TOC combustion tube contains a platinum catalyst. Dispose of the used catalyst in
consumables accordance with local regulations. Analytik Jena GmbH will accept the special catalyst
back for disposal. Please contact the customer service department (see inside front
cover).
The halogen trap contains copper. Contact the responsible institution (authority or
waste disposal company). There you will receive the information regarding recycling or
disposal.

171
Specifications multi EA 5100

17 Specifications

17.1 Technical data for the multi EA 5100

General characteristics Name on the basic module multi EA 5100

Dimensions (W x H x D) 510 x 470 x 550 mm
Mass 25 kg

Procedural data Digestion principle ¡ Catalyst-free high-temperature in-

cineration
2-phase process for C/N/S/Cl, EOX,
EC/OC
1-phase process for AOX
¡ Catalyst-assisted incineration (with
the TOC module 5100)
¡ Wet chemical digestion (in the TIC
reactor of the TOC module 5100)
Digestion temperature 700 to 1100 °C
Measuring meth- Vertical and hori- TS, TN, TX, TC, EOX
ods zontal
Horizontal: AOX, EC/OC
Vertical: TOC, TIC, NPOC

Sampling (vertical) TS, TN, TX, TC Direct injection of liquids into the multi-purpose combus-
tion tube via injection port with septum
Direct injection of gases with a special, long injection nee-
dle into the multi-purpose combustion tube via injection
port with septum
EOX Direct injection of an extract into the multi-purpose com-
bustion tube via injection port with septum
TC, NPOC Direct injection of aqueous samples into the TOC combus-
tion tube via injection port with septum
TIC Direct injection of aqueous samples into the TIC reactor
via injection port with septum

Sampling (horizontal) TS, TN, TX, TC Injection of liquids via injection port with septum (ABD) in
quartz glass boats or direct transfer of solid samples in
quartz glass boats into the multi-purpose combustion tube
Direct injection of liquids via injection port with septum
into the multi-purpose combustion tube
Injection of gaseous samples with a special, flexible injec-
tion cannula via injection port with septum (ABD) into the
multi-purpose combustion tube
AOX Transfer of the loaded active carbon with a quartz con-
tainer (column method, max. 18 x 6 mm columns) in the
quartz glass boat into the multi-purpose combustion tube

172
multi EA 5100 Specifications

Transfer of the loaded, filtered active carbon without a

quartz container (vibration method, with polycarbonate
filters) in the quartz boat with holding-down clamp into
the multi-purpose combustion tube
EOX Injection of an extract via injection port with septum
(ABD) into quartz glass boats and transfer into the multi
purpose combustion tube
EC/OC Transfer of the quartz-fiber filters or partial filters con-
taining deposits in the quartz glass boat with holding-
down clamp into the multi-purpose combustion tube

Sample volume TS, TN, TX, TC, Liquids 1 to 100 µl (horizontally with ABD)
TOC 1 to 500 µl (vertically with MMS or TOC
module 5100 and direct manual dosing)
Solids 0.001 to 110 mg
Non-pressurized 1 to 100 ml
gases
Pressurized gases 1 to 20 ml (with GSS/LPG combi mod-
ule)
1 to 100 ml (with GSS module and GSS
adapterbox)
LPG 1 to 50 µl
EOX (extract) 10 to 100 µl
TOC (aqueous samples) 10 to 500 µl

Dosing speed (vertical) TS, TN, TX, TC Liquids 0.2 to 2 µl/s

Recommended: 0.5 µl/s
Non-pressurized 1 to 40 ml/min
gases Recommended: 20 ml/min
Pressurized gases Fixed (with GSS/LPG combi module)
1 to 40 ml/min
Recommended: 20 ml/min (with GSS
module and GSS adapterbox)
LPG Solid
EOX 0.2 to 2 µl/s
Recommended: 0.5 µl/s
TC, NPOC 100 to 700 µl/s
Recommended: 350 µl/s
or manually adjusted
TIC Manually adjusted

173
Specifications multi EA 5100

Dosing speed (horizontal) Liquids, EOX 1 to 10 µl/s

Recommended: 3 µl/s (with ABD +
MMS or manual dosing)
ABD transfer speed to furnace controlled
automatically via flame sensor or soft-
ware settings
0.2 to 2 µl/s
Recommended: 0.5 µl/s (with Autoin-
jector)
Solids Fixed/transfer speed to furnace con-
trolled automatically via flame sensor or
software settings.
Non-pressurized gases 1 to 40 ml/min
Recommended: 20 ml/min
Pressurized gases Fixed (with GSS/LPG combi module)
1 to 40 ml/min
Recommended: 20 ml/min (with GSS
module and GSS adapterbox)
LPG Solid
AOX Fixed/transfer speed to furnace con-
trolled via software settings for the ABD

Measuring gas dryer TS, TN, TC, EC/OC Membrane dryer

TX, AOX, EOX Concentrated sulfuric acid
TOC, NPOC, TIC Condensation through Peltier cooling

Detection modules Total nitrogen TN N module 5100 Chemiluminescence

Total sulfur TS S module 5100 basic and UV fluorescence
S module 5100 MPO
S module 5100 coulo- Coulometric titration
metric
AOX, EOX, TX, TCl, TOX, Cl module 5100 Micro-coulometric end
TIX point titration
(argentometry)
Total carbon TC, EC/OC C module 5100 NDIR (non-dispersive
infrared absorption
spectrometry)
Total carbon TC, TIC, TOC module 5100 NDIR (non-dispersive
TOC, infrared absorption
NPOC, EC/OC spectrometry)

Sampling modules Liquids Multi Matrix Sampler Auto scaling

MMS
Autoinjector Semi-automatic
Solids ABD + MMS Auto scaling
Automatic Boat Drive Semi-automatic
ABD

174
multi EA 5100 Specifications

Non-pressurized gases GSS module

Pressurized gases GSS/LPG combi module, GSS module + GSS adapterbox
LPG LPG module 2.0, GSS/LPG combi module

Process control Control and analysis software multiWin

Software function scope (extract) Control of the analysis system, data log-
ging and analysis, recalculation, data ex-
port/import, maintenance wizard, on-
line help, real-time chart, service mod-
ule, report generator, automatic leak
check, self-check system

Gas supply Oxygen Purity ≥ 4.5

Inlet pressure 600 kPa (6 bar)
Consumption Combustion 200 ml/min
Post-combustion 200 to 400 ml/min
Membrane dryer Approx. 500 ml/min
drying flow
Argon Purity ≥ 4.6
Inlet pressure 600 kPa (6 bar)
Consumption Combustion 100 to 200 ml/min
Post-combustion 0 ml/min
Pneumatic seal Argon must be present
switch
Argon protective Approx. 20 ml/min
gas bypass (only
for the Cl module
5100)

Electrical variables Voltage 110 to 240 V +10/-5 %

Frequency 50/60 Hz
Overvoltage category II
Fuses T 10 AH
Number of device fuses 2
Typical average power consumption 1000 VA
PC interface 1 USB 2.0
Only use original fuses from Analytik Jena!

Environmental conditions Temperature during operation +21 to 35 °C

Humidity during operation 90 % at 30 °C
Air pressure 0.7 to 1.06 bar
Temperature and humidity during stor- +15 to 55 °C at 10 to 30 % humidity
age (use desiccant)
Maximum elevation 2000 m

175
Specifications multi EA 5100

Computer specifications Graphics resolution 1280x1024

(1024x768 possible with restrictions)
CD/DVD drive Required for software installation
Interface 1 USB 2.0
Operating system Windows 8.1, Windows 10 (32, 64 bit )
Other Activation of DoNetFrameWork 3.5

17.2 Technical data of the N module 5100

Procedural data Analytical parameters Total nitrogen TN

Detection principle Chemiluminescence
Measuring range (N in sample) 0.01 to 10000 mg/l N
Measuring range (N absolute) 0 to 100 µg N

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 4.0 A H
Number of device fuses 2
Typical average power consumption 200 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

Gas supply Oxygen 4.5 80 ml/min

400 to 600 kPa (4 to 6 bar)

General characteristics Dimensions (W x H x D) 300 x 500 x 550 mm

Mass 13 kg

17.3 Technical data for the Cl module 5100

Procedural data Analytical parameters AOX, EOX, TX, TCl, TOX, TIX
Detection principle Micro-coulometric end point titration
(argentometry)
Sample feed ¡ In carrier gas stream (from basic
module)
¡ Direct injection of aqueous samples
and HCl for test purposes
(into the measuring cell)
Temperature control for measuring cell Integrated cooling

176
multi EA 5100 Specifications

Stirring mechanism of the measuring Integrated magnetic stirrer

cell (with fixed speed)
Operating range of the wide-range 3
coulometer
measuring cells ¡ "high sensitive"
¡ "sensitive"
¡ "high concentration"

The "high sensitive" measuring Measurement mode Potentiometry

cell
Measuring range (Cl absolute) 0.01 to 10 µg
Generator current 100 µA
Electrolyte volume 65 ml

The "sensitive" measuring cell Measurement mode Bi-amperometry

Measuring range (Cl absolute) 1 to 100 µg
Generator current 1 mA
Electrolyte volume 15 to 20 ml

The "high concentration" mea- Measurement mode Bi-amperometry

suring cell
Measuring range (Cl absolute) 10 to 1000 µg
Generator current 10 mA
Electrolyte volume 120 ml

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 2.0 A H
Number of device fuses 2
Typical average power consumption 50 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

General characteristics Dimensions (W x H x D) 300 x 470 x 530 mm

Mass 12 kg

17.4 Technical data for the S module 5100 (basic, MPO)

Procedural data Analytical parameters Total sulfur TS

Detection principle UV fluorescence
Measuring range (S in sample) 0.01 to 10000 mg/l S
Measuring range (S absolute) 0 to 100 µg S

177
Specifications multi EA 5100

MPO option TS determination in the presence of

elevated nitrogen concentrations (only
available with the S module 5100 MPO)

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 4.0 A H
Number of device fuses 2
Typical average power consumption 200 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

General characteristics Dimensions (W x H x D) 300 x 470 x 550 mm

Mass 13 kg

17.5 Technical data for the S module 5100 coulometric

Procedural data Analytical parameters Total sulfur TS

Detection principle Coulometric titration
Measuring range (S in sample) 0 to 40000 mg/l S
Measuring range (S absolute) 0 to 200 µg S

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 1.0 A H
Number of device fuses 2
Typical average power consumption 20 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

General characteristics Dimensions (W x H x D) 300 x 470 x 530 mm

Mass 11 kg

17.6 Technical data for the C module 5100

Procedural data Analytical parameters Total carbon TC, EC/OC

Detection principle NDIR (non-dispersive infrared absorp-
tion
spectrometry)

178
multi EA 5100 Specifications

Measuring range (C in sample) 0.1 to 10000 mg/l C

Measuring range (C absolute) 0 to 500 mg C

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 4.0 A H
Number of device fuses 2
Typical average power consumption 50 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

General characteristics Dimensions (W x H x D) 300 x 470 x 530 mm

Mass 12 kg

17.7 Technical data for the TOC module 5100

Procedural data Analytical parameters Total carbon TC, TIC, TOC, NPOC, EC/OC
Sample feed for TIC analysis Direct injection in the TIC reactor
Detection principle NDIR (non-dispersive infrared absorp-
tion
spectrometry)
Measuring range (C in aqueous samples) 0.2 to 10000 mg/l C
Measuring range (C in organic samples) 0.1 to 10000 mg/l C
Measuring range (C absolute) 0 to 500 mg C

Electrical variables Power supply 110 to 240 V +10/-5 %

Overvoltage category II
Frequency 50/60 Hz
Module fuse protection T 4.0 A H
Number of device fuses 2
Typical average power consumption 50 VA
Interface to the basic module RS 232
Only use original fuses from Analytik Jena!

General characteristics Dimensions (W x H x D) 300 x 470 x 530 mm

Mass 12 kg

179
Specifications multi EA 5100

17.8 Standards and directives

Protection class and protection The device is protection class I. The housing is protection type IP 20.
type

Device safety The device complies with the following safety standards
¡ EN 61010-1
¡ EN 61010-2-081
¡ EN 61010-2-010

EMC compatibility The device has been checked for transient emissions and noise immunity.
It meets the requirements for transient emissions according to
¡ EN 61326-1 (EN 55011 group 1, class B)
The device meets the requirements for noise immunity according to
¡ EN 61326-1 (requirements for use in a basic environment)

Environmental compatibility The device has been tested for environmental compatibility and meets the requirements
according to
¡ ISO 9022-2
¡ ISO 9022-3

EU directives The device meets the requirements of the directive 2011/65/EU.

The device is designed and tested in accordance with standards meeting the require-
ments of EU directives 2014/35/EU and 2014/30/EU. The device leaves the factory in a
sound condition with regard to technical safety. To maintain this condition and to en-
sure safe operation, the user must strictly observe the safety and operating instructions
contained in this operating manual. For accessories delivered with the device and sys-
tem components from other manufacturers, the information provided in their respective
operating manuals has priority.

Guidelines for China The device contains substances subject to regulation (according to the directive GB/T
26572-2011). Analytik Jena guarantees that, if the device is used as intended, these
substances will not leak within the next 25 years and therefore will not pose a threat to
the environment or health within this time period.

180
multi EA 5100 Table of figures

Table of figures
Figure 1 Operating modes of the multi EA 5100 ............................................................................................................ 17
Figure 2 Front view in vertical operation mode ................................................................................................................ 19
Figure 3 Basic module in horizontal operation mode....................................................................................................... 19
Figure 4 Basic module with a sampling module and a detection module....................................................................... 20
Figure 5 Interfaces on the rear of the device .................................................................................................................... 21
Figure 6 Power connection, power switch......................................................................................................................... 21
Figure 7 Interfaces for detector modules and sampling modules.................................................................................... 22
Figure 8 Connection for the sensors and the combustion furnace in the device ............................................................ 22
Figure 9 Connections for the auto-protection valve assembly and transfer line ............................................................ 23
Figure 10 Hose diagram for horizontal operation .............................................................................................................. 24
Figure 11 Hose diagram for vertical operation ................................................................................................................... 25
Figure 12 Gas connections at the rear of the device........................................................................................................... 26
Figure 13 Gas connections on the gas box .......................................................................................................................... 27
Figure 14 Connections on the combustion tube ................................................................................................................. 27
Figure 15 Combustion furnace in the vertical and horizontal operating mode ................................................................ 28
Figure 16 Multi-purpose combustion tube.......................................................................................................................... 28
Figure 17 Membrane dryer................................................................................................................................................... 29
Figure 18 Space required for the basic device and modules (vertical operation) ............................................................. 32
Figure 19 Space required for the basic device and modules (horizontal operation) ........................................................ 33
Figure 20 Media connections of the rear of the device ...................................................................................................... 35
Figure 21 Basic module with detection module and sampling module............................................................................. 43
Figure 22 Rear of the nitrogen detector .............................................................................................................................. 44
Figure 23 Absorber ............................................................................................................................................................... 45
Figure 24 Connecting detection modules to the basic module .......................................................................................... 46
Figure 25 Design of the chlorine detector (without measuring cell) ................................................................................. 49
Figure 26 Measuring cell "sensitive" with lid........................................................................................................................ 50
Figure 27 Equipped measuring cell...................................................................................................................................... 50
Figure 28 Combined electrode ............................................................................................................................................. 51
Figure 29 Measuring cell "high concentration" with lid....................................................................................................... 51
Figure 30 Measuring cell "high sensitive" with lid ............................................................................................................... 52
Figure 31 Lid of the "high sensitive" measuring cell equipped with all electrodes ............................................................ 53
Figure 32 Reference electrode and sensor electrode.......................................................................................................... 54
Figure 33 Exhaust connection.............................................................................................................................................. 54
Figure 34 Platinum electrode with salt bridge .................................................................................................................... 55
Figure 35 Silver electrode ..................................................................................................................................................... 55
Figure 36 Rear of the chlorine detector............................................................................................................................... 56
Figure 37 Measuring cell connections ................................................................................................................................. 57
Figure 38 Connection of the heated gas transfer lines to the sulfuric acid container ...................................................... 57
Figure 39 Gas infeed tube with PTFE connector................................................................................................................. 58
Figure 40 Gas infeed to the "sensitive" measuring cell ....................................................................................................... 58

181
Table of figures multi EA 5100

Figure 41 Connection of the heated gas transfer lines to the sulfuric acid container ...................................................... 60
Figure 42 Connection of the gas transfer line in the basic module ................................................................................... 61
Figure 43 Basic module with detection module and sampling module............................................................................. 67
Figure 44 Rear of the sulfur detector................................................................................................................................... 68
Figure 45 Chemical ozone decomposer ............................................................................................................................... 69
Figure 46 Coulometric sulfur detector with measuring cell (without door) ...................................................................... 72
Figure 47 Coulometric sulfur detectors without measuring cell......................................................................................... 73
Figure 48 Coulometric measuring cell ................................................................................................................................. 74
Figure 49 Generator and indicator electrodes, gas inlet tube ............................................................................................ 75
Figure 50 NOx absorber and HX absorber........................................................................................................................... 76
Figure 51 Hose diagram ....................................................................................................................................................... 76
Figure 52 Rear of the coulometric sulfur detector .............................................................................................................. 77
Figure 53 Coulometric sulfur detector with measuring cell (without door) ...................................................................... 79
Figure 54 Basic module with detection module and sampling module............................................................................. 83
Figure 55 Rear of the carbon detector................................................................................................................................. 84
Figure 56 TOC detector, door opened.................................................................................................................................. 88
Figure 57 Components in the basic module ........................................................................................................................ 89
Figure 58 TOC combustion tube (unfilled) .......................................................................................................................... 89
Figure 59 Tube holder for the TOC combustion tube ......................................................................................................... 90
Figure 60 Condensation coil ................................................................................................................................................. 91
Figure 61 Hose diagram of the TOC detector...................................................................................................................... 92
Figure 62 Rear of the TOC detector ..................................................................................................................................... 93
Figure 63 TOC detector, door opened.................................................................................................................................. 95
Figure 64 TOC combustion tube........................................................................................................................................... 96
Figure 65 Status analyzer window ......................................................................................................................................105
Figure 66 Replacing the Fingertight connections ...............................................................................................................136
Figure 67 Replacing the septum on the injection port of the combustion tube ...............................................................136
Figure 68 Replacing the ozone generator ...........................................................................................................................144
Figure 69 Absorber ...............................................................................................................................................................145
Figure 70 Replacing the chemical ozone decomposer........................................................................................................147
Figure 71 Connection of the heated gas transfer lines to the sulfuric acid container ......................................................148
Figure 72 Correct handling of the combined electrode ......................................................................................................150
Figure 73 Replacing the chemical ozone decomposer........................................................................................................154
Figure 74 NOx absorber and HX absorber...........................................................................................................................156
Figure 75 Coulometric sulfur detector with measuring cell (without door) ......................................................................157
Figure 76 Replace the water traps .......................................................................................................................................159
Figure 77 Replacing the halogen trap .................................................................................................................................160
Figure 78 TOC detector, door opened..................................................................................................................................162
Figure 79 Installing the pump hose in the guide piece.......................................................................................................163
Figure 80 Components in the basic module ........................................................................................................................164
Figure 81 TOC combustion tube...........................................................................................................................................166

182