Endress+Hauser analytikjena TOC module User manual

Operating Manual
TOC module

Analytik Jena AG
Konrad-Zuse-Str.1
07745 Jena Germany
Phone + 49 3641 / 77 70
Fax + 49 3641 / 77 92 79
Email [e-mail]
Analytik Jena AG
Konrad-Zuse-Str. 1
07745 Jena Germany
Phone + 49 3641 / 77-7407 (Hotline)
Email [e-mail]
http://www.analytik-jena.com
Microsoft and Windows are registered trademarks of Microsoft Corp.
The identification with ® or TM is omitted in this manual.
11-889.684
January 2010
Analytik Jena AG
© Copyright 2010, Analytik Jena AG
Manufacturer
Service
General information
Copyrights and
Trademarks
Documentation number
Edition
Implementation of the
Technical Documentation

Table of Contents
TOC module Edition 01/2010 i
Table of Contents
1Basic information................................................................... 1
1.1 User manual notes.................................................................................1
1.2 Application.............................................................................................2
1.3 Proper use.............................................................................................2
1.4 Warranty and liability..............................................................................2
1.5 Scope of delivery ...................................................................................3
2Technical data........................................................................ 4
3Safety instructions................................................................. 5
3.1 General notes........................................................................................5
3.2 Safety instructions for the TOC module..................................................5
3.2.1 Summary of safety instructions..............................................................5
3.2.2 Safety instructions - operation................................................................6
3.2.3 Safety instructions - protection against explosion and fire......................6
3.2.4 Safety instructions - electrical equipment...............................................6
3.2.5 Handling of auxiliary and operating materials.........................................7
3.2.6 Behavior during emergencies.................................................................8
4Technical description ............................................................ 9
4.1 System design .......................................................................................9
4.1.1 Overview................................................................................................9
4.1.2 Combustion tube..................................................................................10
4.1.3 Sample preparation..............................................................................11
4.1.3.1 Sample preparation in the TOC combustion tube.................................12
4.1.3.2 Sample preparation in the TIC reactor .................................................12
4.1.4 Components for measuring gas drying and cleaning............................12
4.1.4.1 Condensation coil in the basic module.................................................12
4.1.4.2 TIC condensation unit in the TOC module............................................12
4.1.4.3 Water traps..........................................................................................13
4.1.4.4 Halogen trap........................................................................................13
4.1.5 Pneumatic/hose system.......................................................................13
4.1.5.1 Hose diagram ......................................................................................13
4.1.5.2 Connection method..............................................................................14
4.1.5.3 Condensate pump................................................................................15

Table of Contents
ii Edition 01/2010 TOC module
4.1.6 Detector...............................................................................................15
4.1.7 Indicator and control elements, connectors..........................................15
4.1.7.1 LED displays........................................................................................15
4.1.7.2 Equipment switch, interfaces................................................................15
4.1.7.3 Gas connectors....................................................................................18
4.1.7.4 Connector for waste.............................................................................18
4.2 Function...............................................................................................19
4.3 Measuring method...............................................................................19
4.3.1 TC analysis..........................................................................................19
4.3.2 TOC analysis .......................................................................................20
4.3.3 TIC analysis.........................................................................................20
4.3.4 NPOC analysis.....................................................................................20
4.4 Catalysts..............................................................................................20
5Transport and storage......................................................... 21
5.1 Transport .............................................................................................21
5.1.1 Preparation of the TOC module for transport .......................................21
5.1.2 Transport notes....................................................................................21
5.1.3 Moving the TOC module in the laboratory............................................22
5.2 Storage................................................................................................22
5.3 Recommissioning after transport or storage.........................................23
5.3.1 Assembling the components................................................................23
5.3.2 Connecting the TOC module................................................................24
6First commissioning............................................................ 25
6.1 Site requirements.................................................................................25
6.1.1 Installation conditions...........................................................................25
6.1.2 Space ..................................................................................................25
6.1.3 Energy supply......................................................................................26
6.1.4 Gas supply...........................................................................................26
6.1.5 Unpacking and positioning the TOC module........................................26
7Operation.............................................................................. 27
7.1 Basic information .................................................................................27
7.2 General information for the analysis work ............................................27
7.2.1 Standard commissioning......................................................................28
7.3 Performing measurements...................................................................29
8Fault removal........................................................................ 30

Table of Contents
TOC module Edition 01/2010 iii
8.1 General information .............................................................................30
8.2 Equipment faults and analytical problems............................................30
9Maintenance and care.......................................................... 33
9.1 Service intervals...................................................................................33
9.2 Replacing the water traps ....................................................................34
9.3 Replacing the halogen trap ..................................................................35
9.4 Exchanging the catalyst.......................................................................36
9.4.1 Lifetime of the catalyst .........................................................................36
9.4.2 Removing the combustion tube............................................................36
9.4.3 Filling the combustion tube ..................................................................37
9.4.4 Inserting the combustion tube..............................................................38
9.5 Regenerating the TIC reactor...............................................................39
9.6 Cleaning the TC condensation vessel..................................................40
9.7 Removing and installing the condensation coil.....................................41
9.7.1 Removing and cleaning the condensation coil .....................................41
9.7.2 Inserting the condensation coil.............................................................41
9.8 Removing and replacing the pump hose..............................................42
9.9 Replacing hose connections ................................................................42
9.10 Checking the system for tightness........................................................43
9.11 Exchanging the septums......................................................................44
9.12 Spare part list.......................................................................................45
9.13 Notes on ordering ................................................................................46
10 Waste disposal..................................................................... 47
10.1 Waste water.........................................................................................47
10.2 Halogen trap........................................................................................47
10.3 Catalyst................................................................................................47
10.4 TOC module ........................................................................................47

Index of Figures
iv Edition 01/2010 TOC module
Index of Figures
Fig. 1 Front view, TOC module –Door open....................................................9
Fig. 2 View of the basic module, left door open..............................................10
Fig. 3 TOC combustion tube..........................................................................11
Fig. 4 Tube holder for TOC combustion tube .................................................11
Fig. 5 Condensation coil with spherical joint and FAST connector .................12
Fig. 6 Hose diagram TOC module..................................................................14
Fig. 7 Equipment backplate............................................................................17
Fig. 8 TOC combustion tube, filled.................................................................38

Basic information
TOC MODULE Edition 01/2010 1
1Basic information
1.1 User manual notes
The TOC module is a system module of the modular analyzers multi EA®5000 or
multi X®2500. It can only be used in combination with one of the two basic modules.
The control of the modules and the analysis of the measurements is performed with the
software multiWin®.
This user manual is therefore only valid in conjunction with the following documents:
-User manual multi EA®5000 or user manual multi X®2500
-Software manual of the control and analysis software multiWin®
IMPORTANT
Carefully read the above-mentioned documents before connecting the TOC module
to the basic module and using it. Observe in particular the notes in the chapter
"Safety notes" of the user manuals.
The following user manual informs about the design and function of the TOC module
and provides the necessary know-how for the safe handling of the device and its
components to personnel familiar with analysis. The user manual further includes notes
on the maintenance and service of the device and potential causes and remedies of
any faults.
Conventions
Instructions for action which occur in chronological order are numbered and
combined into action units and furnished with the corresponding results.
Lists which are not in chronological order are shown as itemized lists, sub-listings as
bullet points.
Safety notes are indicated by pictographs and signal words. The type and source of
the danger are stated together with notes on preventing the danger. The meaning of
the pictographs and signal words used is explained in the chapter "Safety notes" of the
user manual multi EA®5000 or multi X®2500 (basic module).
The elements of the control and analysis software are indicated as follows:
Buttons and menus are shown in bold and by square brackets (e.g. button
[OK], menu [Method])
Menu and selection sequences are divided by arrows (e.g. menu [Method]
[Edit method])
Window names are shown in italics (e.g. Configuration window)
Field, frame and tab names are shown in bold (e.g. Devices tab,Automatic
initialization frame)

Basic information
2 Edition 01/2010 TOC MODULE
1.2 Application
The expansion of the multi EA®5000 or the multi X®2500 with the TOC module
enables the determination of the carbon content in aqueous samples by digestion with
the aid of thermocatalytic high-temperature oxidation in the presence of special
catalysts according to national and international standards.
1.3 Proper use
The device must only be used for the methods described in this user manual to
determine the carbon content in aqueous samples. Any other use is not as intended!
Only the operator is liable for any damages that result from this.
The operational safety of the TOC module is only ensured during proper use according
to the information in this user manual. The intended use also requires that you observe
the notes in the user manual of the multi EA®5000 or multi X®2500.
1.4 Warranty and liability
The warranty duration and liability comply with the legal requirements and the
provisions in the general terms and conditions of Analytik Jena AG.
Deviations from the intended use described in this user manual result in limitations of
warranty and liability during a damage event. Damage to wearing parts is not included
in the warranty.
Warranty and liability claims are excluded for personal injury and property damage due
to one or several of the following causes:
use of the TOC module other than intended
improper commissioning, operation and service of the TOC module
modifications of the device without prior consultation with Analytik Jena AG
unauthorized intervention in the device
operation of the device with faulty safety equipment or improperly fitted safety
and protection equipment
inadequate monitoring of the device components subject to wear
use of other than original spare parts, wearing parts or consumables
improper repairs
faults due to the non-observance of this user manual

Basic information
TOC MODULE Edition 01/2010 3
1.5 Scope of delivery
IMPORTANT
The scope of delivery is listed in the table below for information purposes.
Completeness is not guaranteed. Modifications are reserved.
When checking the delivered components always refer to the current packing list
included in the scope of delivery.
Name
TOC module, pre-assembled
Mains cable
Connection cable basic device -TOC module, 9 pin
Connection cable basic device –TOC module, 25 pin
TOC combustion tube
Gas connection hose (6x4 mm), 3m
Syringe, 500 µl, calibrated
Replaceable canulas (OD 0.63 mm), set of 3
Syringe 5 ml for phosphoric acid with canula
NPOC hose
Condensation vessel with manual TIC port
Condensation unit with:
Condensation coil
Connection hose to
condensation vessel
FAST connector, straight
TC prefilter
Disposable retention filter
Halogenide trap, filled
Waste canister
Outlet tube, 1m
Consumables:
Pt catalyst
Quartz glass fragments
Quartz glass wool
HT mat
Septums Ø 12.5 mm –manual TIC port
Septum Ø 17 mm –injection port combustion tube
Filling rod for combustion tube
User manual
Packing list

Technical data
4 Edition 01/2010 TOC MODULE
2Technical data
General characteristics
Designation/type
TOC module
Basic device dimensions (W x H x D)
approx. (300 x 470 x 530) mm
Weight
approx. 10 kg
Procedural data
Digestion principle
Thermocatalytic oxidation
Digestion temperature
700 °C (Pt/Al2O3)
up to 900 °C, depending on the catalyst
Detection
NDIR (Non-dispersive infra red absorption)
0 –20 % CO2 in analyte gas
Measuring method
TC, TIC, TOC, NPOC
Sample Feed
Direct injection via injection port with
septum into the combustion tube in the
basic module
Direct injection into the TIC condensation
vessel –TIC manual
Sample volume
(50 –500) µl
Gas supply from the basic device
Oxygen (minimum 4.5)
Preliminary pressure 4 –6 bar
Gas consumption
200 mlmin
Dosing rate
According to the method settings or manual
Measuring gas drying
Condensation and freeze desalination
Electrical variables
Power supply
(110 –240) V AC, 50/60 Hz
Protection
T 4.0 A H (2x)
Typical average power consumption
50 VA
Interface to the basic module
RS 232
Interference suppression
(electromagnetic compatibility)
In accordance with the EC directive
2004/108/EC
Environmental conditions
Temperature during storage
(15 –55) °C
Temperature during operation
(20 –35) °C
Humidity during operation
Max. 90 % at +30 °C
Humidity during storage
(10 –30) % (use desiccant)
Air pressure
(0.7 –1.06) bar

Safety instructions
TOC MODULE Edition 01/2010 5
3Safety instructions
3.1 General notes
IMPORTANT
This user manual is only valid in conjunction with the following documents:
–User manual multi EA®5000 or multi X®2500 (basic module)
–Software manual of the control and analysis software multiWin®
Observe in particular the notes in the chapter "Safety notes" of the user manual
multi EA®5000 or multi X®2500 (basic module). The notes included there apply
analog also to the TOC module without any limitations. Special danger emanating
from the TOC module is referred to in the following chapters.
For your own safety and to ensure error-free and safe operation of the TOC module,
please read this chapter carefully before commissioning.
Observe all safety notes listed in this user manual and observe all messages and
displayed by the control and analysis software on the monitor.
3.2 Safety instructions for the TOC module
3.2.1 Summary of safety instructions
The TOC module was manufactured according to the currently valid technology
regulations and the approved safety related regulations.
When constructing the TOC module the relevant safety and health requirements of the
applicable laws, standards and regulations were applied. The safety of the module is
confirmed by the CE mark and the declaration of conformity.
Information regarding safety corresponds to the currently valid regulations of the
European Union. In other countries the applicable laws and country specific regulations
have to be complied with.
Besides the safety instructions in this user manual and the local safety regulations that
apply to the operation of the TOC module the general applicable regulations regarding
accident prevention, occupational health and safety and environmental protection have
to be observed and complied with.
Unauthorized modifications or changes, especially such that affect the safety of the
staff and the environment, are generally not allowed.

Safety instructions
6 Edition 01/2010 TOC MODULE
3.2.2 Safety instructions - operation
The operator of the analyzer with TOC module is obligated to assure that the condition
of the devices including the safety equipment is correct before startup. This especially
applies after each modification and extension or all repair work.
The following has to be observed:
Free access to the power switch on the back of the enclosure has to be ensured
during operation.
The ventilation equipment on the TOC module has to be in good working
condition. Covered vents or ventilation slits may cause the device to break down
or may cause damage to it.
The oven works at temperatures of at least 700 °C. Hot parts (oven, TOC
combustion tube, condensation coil) may not be touched during or directly after
the operation of the analyzer.
Keep all combustible material away from the module.
3.2.3 Safety instructions - protection against explosion and
fire
The TOC module may not be operated in an explosive environment. Smoking or
handling open flames in the operating room of the module is forbidden!
The operating staff has to be aware of the location of the fire-fighting equipment in the
operating room of the module.
3.2.4 Safety instructions - electrical equipment
Work on the electrical components of the TOC module is only to be performed by a
qualified electrical technician according to the electro-technical regulations.
The TOC module always has to be connected or disconnected from the basis module
in a deactivated condition.
The TOC module has to be switched off on the power switch (on the back of the
enclosure) and the power supply has to be disconnected from the mains if there is any
interference on the electric components.

Safety instructions
TOC MODULE Edition 01/2010 7
3.2.5 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 dangerous substances local safety codes and guidelines must be
observed.
The following general notes do not replace the specific local regulations or the
regulations in the EG safety data sheets of the manufacturers for the auxiliary and
operating materials.
The following has to be observed:
The relevant regulations and the notes in the EG safety data sheets of the
manufacturers have to be observed and complied with regards to storage,
handing, use and disposal for all auxiliary and operation materials used during
operation or maintenance of the TOC module.
Auxiliary and operation materials may never be placed in containers or vessels
for food. The approved containers for the relevant material are to be used and
these have to be labeled accordingly.
The notes on the labels have to be observed!
Protective goggles and rubber gloves have to be worn when handing reagents.
The notes on the labels have to be observed.
The regulations and notes on the safety data sheets for the handling of
orthophosphoric acid (H3PO4) or hydrochloric acid (HCl) have to be observed!
The catalyst (platinum catalyst multi N/C) should be handled with the usual
caution when handling chemicals.
Biological samples have to be handled according to local guidelines regarding
the handling of infectious material.
Caution when handing quartz glass and glass parts. Risk of broken glass and
therefore risk of injury!
Avoid dust formation and inhalation of dust when handing the quartz glass wool
during filling of the combustion tube.
Auxiliary and operating materials as well as their containers may not be
disposed in domestic waste or enter the sewage system or the soil. The
applicable regulations for disposal of these materials must be meticulously
observed.
Ensure good room ventilation in working rooms.

Safety instructions
8 Edition 01/2010 TOC MODULE
3.2.6 Behavior during emergencies
The TOC module has to be switched off on the power switch (on the back of the
enclosure) and the power supply has to be disconnected from the mains if there are
any dangerous situations or accidents.
Because a rapid response can save lives during an emergency, the following has to be
ensured:
The operating staff has to be aware where safety equipment, accident and
danger alarms as well as first aid and rescue equipment are located and be
familiar with their handling.
The operator is responsible for the respective training of the operating staff.
All equipment for first aid (first-aid kit, eyewash bottles, stretcher, etc.) as well as
equipment for firefighting (fire extinguishers) has to be within reach and easy to
access. All equipment has to be in a faultless condition and should be checked
regularly.

Technical description
TOC MODULE Edition 01/2010 9
4Technical description
4.1 System design
4.1.1 Overview
The TOC module is a detection module for the modular analyzers
multi EA®5000 or multi X®2500.
All components of the TOC module which have to be operated or serviced by the
operator are accessible via the door on the front side of the module and via the front
doors or the covers on the basic module.
The TOC module consists of the following main components:
TOC combustion tube (in the basic module)
Components for measuring gas drying and cleaning
Pneumatic system/hose connections
Detector
Indicator/control elements, connectors
Accessories
Arrangement of the components in the TOC module
Fig. 1 Front view, TOC module –Door open
1 TIC reactor
2 Halogen trap
3 Water traps
4 Condensate pump
5 Hose no. 80
6 Hose no. 81

Technical description
10 Edition 01/2010 TOC MODULE
Arrangement of the components in the basic module
Fig. 2 View of the basic module, left door open
1 Injection port combustion tube
2 Condensation coil
3 Spherical joint, fixated with a fork type clamp
4.1.2 Combustion tube
The combustion tube (reactor) consists of quartz glass (refer to Fig. 3). It is filled with
catalyst and auxiliary material (refer to Fig. 8). If the effectiveness of the catalyst
decreases, the combustion tube has to be filled again (refer to chapter 9.4.3).
Screw the screw cap with the septum on the top opening of the combustion tube.
Connect the condensation coil with the aid of a fork type clamp to the spherical joint on
the lateral outlet.
Connect the oxygen gas supply (hose No. 3 of the basic model) to the lateral outlet
directly below the screw cap with a FAST connector (refer to the user manual
multi EA®5000 or multi X®2500).
The TOC combustion tube is fixated in the oven with the tube holder (refer to Fig. 4).

Technical description
TOC MODULE Edition 01/2010 11
Fig. 3 TOC combustion tube
1 Screw cap with septum (injection port)
2 Connector oxygen gas supply,
hose No. 3 of the basic module
3 Connector condensation coil
Fig. 4 Tube holder for TOC combustion tube
4.1.3 Sample preparation
Sample feed is performed directly with microliter syringes. A calibrated syringe is used
for manual dosing. Special microliter syringes (special geometry, with gas connector for
analysis in NPOC mode) are used for the automatic sample feed with the autosampler.
They are not calibrated and therefore not suitable for analysis in manual operation.
The injection volume ranges between 50 - 500 μl. Optimum measurement results are
reached when 50 to 100 % of the volume of the used microliter syringe is used.

Technical description
12 Edition 01/2010 TOC MODULE
4.1.3.1 Sample preparation in the TOC combustion tube
The injection of the aqueous samples into the combustion system is performed via the
injection port of the TOC combustion tube (refer to 1 in Fig. 3). This can be done
manually or with the Multi Matrix autosampler (TC or NPOC).
The septums which are normally used are temperature resistant and have a high
puncture tolerance.
4.1.3.2 Sample preparation in the TIC reactor
An aliquot of the sample is directly dosed into the TIC reactor with a calibrated
microliter syringe (only manual dosing) to determine the inorganic carbon materials
(TIC).
4.1.4 Components for measuring gas drying and cleaning
4.1.4.1 Condensation coil in the basic module
Connect a glass condensation coil via the spherical joint to the combustion tube in the
basic module (refer to Fig. 2). Connect hose No. 80 to the FAST connector on the other
end of the condensation coil (refer to Fig. 5).
The analyte gas is cooled down quickly in the condensation coil and the water vapor
condenses. The analyte gas water mixture is guided to the TIC reactor in the TOC
module via the hose line No. 80.
Fig. 5 Condensation coil with spherical joint and FAST connector
1 Spherical joint
2 FAST connector (angled adapter)
4.1.4.2 TIC condensation unit in the TOC module
The TIC condensation unit combines the TIC reactor, the gas-liquid separator, and the
measuring gas drying (refer to Fig. 1).
The analyte gas/water mixture is fed via the top lateral connector of the TIC reactor
with hose No. 80.

Technical description
TOC MODULE Edition 01/2010 13
For the TIC determination, 40 % phosphoric acid is placed into the TIC reactor. The
dosing of the acid as well as the sample is performed via the front lateral connector
with the septum port (refer to chapter 9.5 for the regeneration of the TIC reactor).
The analyte gas is guided via the top connector in the direction of the water traps from
the TIC condensation vessel. The condensate or the waste agent of the TIC
determination is sucked out by a pump via the lower lateral outlet on the glass
container. The condensate pump guides the waste to the outlet "waste" on the back of
the device.
4.1.4.3 Water traps
The TOC module contains two water traps for the greatest possible removal of
disturbing components in the analyte gas and also to protect the detector. They are
connected with the analyte gas outlet of the TIC reactor.
The water traps prevent that condensed water enters the analyte gas line after exiting
the TIC condensation vessel. The larger water trap (TC prefilter) retains aerosol during
operation, the smaller water trap (disposable retention filter) retains rising water.
4.1.4.4 Halogen trap
The TOC module contains a halogen trap (U-tube) after the TIC reactor and the water
traps for the greatest possible removal of disturbing components in the analyte gas and
also to protect the detector (refer to Fig. 1).
The U-tube is filled with special copper wool. The filling of the halogen trap has to be
renewed at the latest once half of the copper wool is discolored black (refer to chapter
9.3).
4.1.5 Pneumatic/hose system
4.1.5.1 Hose diagram
The connection between the individual components is made with labeled hoses. The
encircled numbers and letters in the hose diagram correspond to the labels on the
hoses in the device.

Technical description
14 Edition 01/2010 TOC MODULE
Fig. 6 Hose diagram TOC module
4.1.5.2 Connection method
So called FAST connectors (as angled adapter and straight adapter) are used in the
TOC module for the connection of the hose connections. They guarantee simple
handling and operation without gas leakage.
IMPORTANT for angled adapters:
Make that the hose ends are not pushed
over the leg length so that an
unobstructed gas flow is ensured (refer to
the graphic on the right).
FAST connector (angled adapter)