Endress+Hauser Analytik Jena multi EA 5000 User manual

Operating Manual
multi EA 5000
C/N/S/X Analyzer

Manufacturer Analytik Jena AG
Konrad-Zuse-Straße 1
07745 Jena / Germany
Telephone: [phone]
Fax: [phone]
E-mail: [email protected]
Technical Service AnalytikJenaAG
Konrad-Zuse-Straße 1
07745 Jena / Germany
Phone: [phone]
Fax: [phone]
Email: [email protected]
General Information http://www.analytik-jena.com
Documentation Number 11-0203-005-23
Edition 02.20
Technical Documentation Analytik Jena AG
© Copyright 2020, Analytik Jena AG
For a proper and safe use of this product follow the instructions.
Keep the operating manual for future reference.

multi EA 5000 Table of contents
3
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 5000 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
4.2.2 Manual Boat Drive (MBD) ............................................................................................................................... 30
5 Installation and commissioning..................................................................................................................................... 31
5.1 Installation conditions...................................................................................................................................... 31
5.2 Installation location requirements................................................................................................................... 31
5.3 Power supply..................................................................................................................................................... 31
5.4 Gas supply ......................................................................................................................................................... 32
5.5 Device layout and space requirements............................................................................................................ 32
5.6 Installing and commissioning the analysis system......................................................................................... 35
6 Operation ........................................................................................................................................................................ 37
6.1 General notes for measuring operations......................................................................................................... 37
6.2 Selecting the measurement method ............................................................................................................... 38
6.3 Switching on the basic module and the modules ........................................................................................... 39
6.4 Switching off the basic module and the modules........................................................................................... 40
6.5 Recommissioning after emergency shutdown (Cl module) ........................................................................... 41
7 Nitrogen analysis with the CLD 5000 ........................................................................................................................... 43
7.1 Function and design ......................................................................................................................................... 43
7.1.1 Function and measuring principle ................................................................................................................... 43
7.1.2 Design................................................................................................................................................................ 43
7.1.3 Connection ........................................................................................................................................................ 44
7.2 Installation ........................................................................................................................................................ 46

Table of contents multi EA 5000
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7.3 Operation .......................................................................................................................................................... 48
8 Chlorine analysis with the Cl module............................................................................................................................. 49
8.1 Function and design ......................................................................................................................................... 49
8.1.1 Function and measuring principle ................................................................................................................... 49
8.1.2 Design................................................................................................................................................................ 49
8.1.3 Connection ........................................................................................................................................................ 57
8.2 Installation ........................................................................................................................................................ 60
8.3 Operation .......................................................................................................................................................... 64
8.3.1 Preparing the measuring cell........................................................................................................................... 64
8.3.2 Operating the analysis system ......................................................................................................................... 66
8.3.3 Notes for measuring operations ...................................................................................................................... 67
9 Sulfur analysis with the UVFD 5000, MPO 5000 ........................................................................................................ 69
9.1 Function and design ......................................................................................................................................... 69
9.1.1 Function and measuring principle ................................................................................................................... 69
9.1.2 Design................................................................................................................................................................ 69
9.1.3 Connection ........................................................................................................................................................ 70
9.2 Installation ........................................................................................................................................................ 71
9.3 Operation .......................................................................................................................................................... 73
10 Sulfur analysis with the Coulometric Sulfur Module .................................................................................................... 74
10.1 Function and design ......................................................................................................................................... 74
10.1.1 Function and measuring principle ................................................................................................................... 74
10.1.2 Design................................................................................................................................................................ 74
10.1.3 Connection ........................................................................................................................................................ 80
10.2 Installation ........................................................................................................................................................ 81
10.3 Operation .......................................................................................................................................................... 83
10.3.1 Preparing the measuring cell........................................................................................................................... 83
10.3.2 Operating the analysis system ......................................................................................................................... 84
11 Carbon analysis with the TC module ............................................................................................................................ 86
11.1 Function and design ......................................................................................................................................... 86
11.1.1 Function and measuring principle ................................................................................................................... 86
11.1.2 Design................................................................................................................................................................ 86
11.1.3 Connection ........................................................................................................................................................ 87
11.2 Installation ........................................................................................................................................................ 88
11.3 Operating the analysis system ......................................................................................................................... 88
12 Carbon analysis with the TOC module .......................................................................................................................... 90
12.1 Function and design ......................................................................................................................................... 90
12.1.1 Function and measuring principle ................................................................................................................... 90
12.1.2 Design................................................................................................................................................................ 90
12.1.3 Connection ........................................................................................................................................................ 95
12.2 Installation ........................................................................................................................................................ 97
12.3 Operation .......................................................................................................................................................... 99
12.3.1 Operating the analysis system ......................................................................................................................... 99
12.3.2 Notes for measuring operations ......................................................................................................................100
13 Troubleshooting.............................................................................................................................................................. 101
13.1 General notes....................................................................................................................................................101
13.2 Remedying software message faults...............................................................................................................101

multi EA 5000 Table of contents
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13.3 Initializing the basic module and the system components ............................................................................107
13.4 Displays in the window Status analyzer .........................................................................................................108
13.4.1 Overview ...........................................................................................................................................................108
13.4.2 Method..............................................................................................................................................................109
13.4.3 Sampling modules ............................................................................................................................................109
13.4.4 Detectors ...........................................................................................................................................................110
13.5 Device faults on the basic module ...................................................................................................................112
13.6 Analytical problems in the basic module.........................................................................................................114
13.7 Device faults on the CLD 5000 .......................................................................................................................115
13.8 Analytical problems during TC determination ................................................................................................116
13.9 Device faults on the chlorine detector.............................................................................................................117
13.10 Analytical problems during AOX, EOX and TX determination .......................................................................118
13.11 Device faults on the UVFD 5000 and MPO 5000 ..........................................................................................119
13.12 Analytical problems during TS determination ................................................................................................119
13.13 Device faults on the coulometric sulfur detector ............................................................................................120
13.14 Analytical problems during coulometric TS determination............................................................................120
13.15 Device faults on the carbon detector...............................................................................................................122
13.16 Analytical problems during TC, EC/OC determination ...................................................................................122
13.17 Device faults on the TOC detector ...................................................................................................................123
13.18 Analytical problems during TC, EC/OC, TOC, NPOC and TIC determination .................................................124
14 Maintenance and care.................................................................................................................................................... 127
14.1 Overview of maintenance work .......................................................................................................................127
14.2 Maintenance of the multi-purpose combustion tube ....................................................................................129
14.2.1 Removing the combustion tube.......................................................................................................................130
14.2.2 Cleaning the combustion tube.........................................................................................................................131
14.2.3 Inserting the quartz wool plug.........................................................................................................................131
14.2.4 Installing the combustion tube ........................................................................................................................132
14.3 Maintenance of the auto-protection valve assembly.....................................................................................134
14.3.1 Installing/removing the auto-protection valve assembly ..............................................................................134
14.3.2 Check and replace the filter..............................................................................................................................135
14.3.3 Replacing the pneumatic seal..........................................................................................................................136
14.4 Replacing the membrane dryer .......................................................................................................................137
14.5 Replacing the hose connections ......................................................................................................................139
14.6 Replacing the septum on the injection port....................................................................................................139
14.7 Replacing the check valves and particle filters................................................................................................140
14.7.1 Replacing the check valves on the gas box .....................................................................................................140
14.7.2 Replacing the particle filters in the gas inlets.................................................................................................141
14.8 Checking the system for leaks..........................................................................................................................142
14.8.1 System tightness for N/S/C methods..............................................................................................................142
14.8.2 System tightness for Cl methods .....................................................................................................................142
14.8.3 System tightness for TOC methods .................................................................................................................144
14.9 Removing and installing the combustion furnace..........................................................................................144
14.10 Maintenance of the CLD 5000 nitrogen detector .........................................................................................146
14.10.1 Replacing the ozone generator........................................................................................................................146
14.10.2 Replacing the absorber.....................................................................................................................................148
14.10.3 Replacing the chemical ozone decomposer ....................................................................................................149

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14.11 Maintenance of the Cl module chlorine detector ..........................................................................................151
14.11.1 Replacing the sulfuric acid and cleaning the sulfuric acid container.............................................................151
14.11.2 Maintenance of the measuring cell.................................................................................................................152
14.11.3 Maintenance and storage of the electrodes ...................................................................................................153
14.12 Maintenance of the UVFD 5000 and MPO 5000 sulfur detector ................................................................156
14.12.1 Replacing the UV lamp .....................................................................................................................................156
14.12.2 Replacing the chemical ozone decomposer ....................................................................................................158
14.13 Maintenance of the coulometric sulfur detector ............................................................................................159
14.13.1 Replacing the absorber.....................................................................................................................................159
14.13.2 Replacing the electrolyte solution ...................................................................................................................161
14.14 Maintenance of the TOC detector ...................................................................................................................162
14.14.1 Replacing the water traps ................................................................................................................................163
14.14.2 Replacing the halogen trap..............................................................................................................................163
14.14.3 Regenerating the TIC reactor...........................................................................................................................165
14.14.4 Cleaning the TIC reactor...................................................................................................................................165
14.14.5 Replacing the pump hose of the condensate pump .......................................................................................167
14.14.6 Cleaning the condensation coil........................................................................................................................168
14.14.7 Replacing the catalyst in the TOC combustion tube.......................................................................................169
15 Transport and storage .................................................................................................................................................... 171
15.1 Transport...........................................................................................................................................................171
15.2 Moving the device in the laboratory................................................................................................................171
15.3 Storage ..............................................................................................................................................................171
15.4 Preparing the basic module for transport and storage ..................................................................................172
15.5 Preparing detection modules...........................................................................................................................172
15.5.1 Notes for the transport of the Cl module .......................................................................................................173
15.5.2 Notes on transport of the Coulometric Sulfur Module ..................................................................................174
15.5.3 Notes on transport of the TOC module ..........................................................................................................174
16 Disposal ........................................................................................................................................................................... 175
17 Specifications .................................................................................................................................................................. 176
17.1 Technical data for the multi EA 5000 ............................................................................................................176
17.2 Technical data of the CLD 5000 .....................................................................................................................180
17.3 Technical data for the Cl module ....................................................................................................................180
17.4 Technical data for the UVFD 5000, MPO 5000 ............................................................................................181
17.5 Technical data for the Coulometric Sulfur Module ........................................................................................182
17.6 Technical data for the TC module ...................................................................................................................182
17.7 Technical data for the TOC module ................................................................................................................183
17.8 Standards and directives ..................................................................................................................................184

multi EA 5000 About this user manual
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1 About this user manual
The multi EA 5000 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 5000
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 operating instructions use the following symbols and signal words to indicate haz-
ards or instructions. 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.

Intended use multi EA 5000
8
2 Intended use
The multi EA 5000 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
multi EA 5000
The analyzer can be used for the following sample types:
¡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 5000:
¡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 5000
analyzer to determine the following parameters as sum parameters.

multi EA 5000 Intended use
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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 5000:
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.

Security multi EA 5000
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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-
bol
Meaning Comment
Warning against dan-
gerous electrical volt-
age
In the device interior on the electronics
cover
Warning against electrical voltage. Be-
fore opening the electronics the device
must be disconnected from the mains.
Warning about hot
surface
In the device interior on the combus-
tion furnace
On the top cover of the combustion
furnace
On the heated gas transfer line from
the Cl module
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-
rosive substances
On the "high sensitive" measuring cell
of the Cl module
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
Exercise caution when handling con-
centrated sulfuric acid
Warning against UV
radiation
In the UVFD 5000, MPO 5000
Switch off the detection module before
performing maintenance on the UV
lamp.

multi EA 5000 Security
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Warning sym-
bol
Meaning Comment
Caution (GHS07) On the absorber and the chemical
ozone decomposer of the CLD 5000
On the chemical ozone decomposer of
the MPO 5000
The cartridges contain hazardous sub-
stances. Do not open the cartridges.
Only replace the entire cartridge.
Mandatory ac-
tion labels
Meaning Comment
Disconnect the power
supply before open-
ing the device cover.
On the rear panel of and/or the side
panels of the basic module and the de-
tector modules
In the device interior on the electronics
cover
Observe the operat-
ing manual
On the rear panel of and/or the side
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 AG 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 AG customer service or specialist personnel trained and
authorized by them is allowed to install and commission the device and its sys-
tem 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.

Security multi EA 5000
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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
Analytik Jena AG. The decontamination report is available from Service when
registering 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 notes:
¡The device must only be operated if all protective equipment (e.g. covers and
doors) are in place, properly installed and fully operational.
¡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 handing quartz glass and glass parts. 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 MMS 5000 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.
Smoking or handling open flames are prohibited in the room in which the device is
operated!

multi EA 5000 Security
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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 or when searching for
a gas leak in the measuring gas connection between the basic module and the
Cl module.
¡Work on the electronics may only be carried out by the customer service of
Analytik Jena AG 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 Concentrated sulfuric
acid
Drying agent in the sul-
furic acid container
Acetic acid Preparing the electrolyte
solution
Concentrated nitric acid
Methanol
Thymol
Coulometric Sulfur Module Acetic acid Preparing the electrolyte
solution
TOC module 40% orthophosphoric
acid
0.2mol/l hydrochloric
acid
Reagent in the TIC reac-
tor
Reagent for NPOC de-
termination
Acetic acid vapors causing strong irritation of the airways can occur in the measuring
cell of the Cl module. Connect the measuring cell with the exhaust hose and connect
the detection module to the laboratory exhaust unit.

Security multi EA 5000
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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 is used: Concentrated sulfuric acid is used as a drying agent in the
detection module. The electrolyte solution in the "high sensitive" measuring 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, ventilation must be
performed manually (→ "Recommissioning after emergency shutdown
(Cl module)" 41).
¡After relieving the overpressure remove the obstruction in the gas path.
3.5 Behavior during emergencies
Observe the following:
¡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!

multi EA 5000 Security
15
¡When closing the argon gas supply, a return of the acid used can occur in the
Cl module. For this reason, the measuring gas lines to this module must be dis-
connected before closing the argon gas supply.
¡When attaching the Cl module: 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 period. After an
emergency shutdown, check that the transfer line and the auto-protection valve
assembly are not contaminated with sulfuric acid (→ "Recommissioning after
emergency shutdown (Cl module)" 41) before recommissioning.
¡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
Coulometric Sulfur Module and the TOC module. Check the measuring gas hoses
for contamination 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 AG 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.

Function and design multi EA 5000
16
4 Function and design
4.1 multi EA 5000 basic module
The multi EA 5000 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 5000 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
multiWin 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
Operation is in vertical or horizontal mode, depending on the installation position of the
furnace. Devices equipped with the optional double furnace enable the device to work in
both vertical and horizontal mode.
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.
For manual sampling, there is a Manual Boat Drive (MBD). The MBD may only be used
to transfer inert solids on quartz glass boats.
Advantages of horizontal operation mode:
¡For gases, LPG, solids, liquid samples independent of viscosity
¡Best for volatile liquids

multi EA 5000 Function and design
17
Sample feed
Liquid/LPG/gaseous
Sample feed
Solid/liquid/LPG/gaseous
Cl analysis - (EOX/TOX/AOX)
C/N/S analysis
C detector N detector S detector
Coulometer
Dryer
Flame sensor Quartz glass boat
Cooled sample port
Figure1 Operating modes of the multi EA 5000
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.

Function and design multi EA 5000
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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)
TOC, NPOC, TIC Condensation through Peltier cooling (in the TOC module)
4.1.2 Design of the basic module
4.1.2.1 Main components
Main components of the basic
module
The multi EA 5000 basic module contains the following main components:
¡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.
The basic module is available in 3 versions with different operation modes (installation
position of the furnace).
Double furnace device ¡Vertical and horizontal operating mode possible
¡Opening with maintenance flaps at the right-hand side panel
Vertical device ¡Furnace in vertical installation position
¡Right side panel closed

multi EA 5000 Function and design
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1
2
3
4
5
6
7
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 device ¡Furnace in horizontal installation position
¡Opening with maintenance flaps at the right-hand side panel
1
2
3
4
Figure3 Basic module in horizontal operation mode
1 Control electronics 2 Combustion furnace
3 Auto-protection valve assembly 4 Gas box

Function and design multi EA 5000
20
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-
tions
The power switch and the interfaces for connecting the system modules and for con-
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.