Endress+Hauser Analytik Jena multi EA 5100 User manual

Operating Manual
multi EA 5100
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 11-0203-002-23
Edition 01.20
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 5100 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 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

Table of contents multi EA 5100
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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

multi EA 5100 Table of contents
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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

Table of contents multi EA 5100
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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

multi EA 5100 About this user manual
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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 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 5100
8
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
multi EA 5100
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 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.

multi EA 5100 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 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.

Security multi EA 5100
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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 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-
rosive substances
On the "high sensitive" measuring cell
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
radiation
In the S module 5100 (basic, MPO)
Switch off the detection module before
performing maintenance on the UV
lamp.