LiquiTOCi Manual Operation

Ident-Nr. 35.
00-5006
High Temperature TOC/TNb Analyzer
liquiTOC
Operating Instructions
starting with serial-no.35 04 3041

Issue September 2004
Elementar Analysensysteme GmbH, Donaustraße 7, D-63452 Hanau-Germany

Tel. +49/6181-9100-0, Fax: +49/6181-9100-10, e-mail: info@elementar.de
Contents page I
Contents
1. Scope of delivery 1-1
2. Specifications and technical data 2-1

2.1 Specification 2-1
2.2 Technical data 2-2
3. Safety instructions 3-1
4. Installation and start-up 4-1

4.1 Preparation for operation 4-1
4.1.1 Working environment 4-1
4.1.2 Necessary gases and chemicals 4-3
4.2 Instrument installation 4-3
4.2.1 Front of the unit 4-3
4.2.2 Right side with removed sidewall 4-5
4.2.3 Left side with removed sidewall 4-6
4.2.4 Back panel 4-7
4.2.5 Tubing diagram, functional diagram 4-9
4.3 Filling of the quartz and glass parts 4-10
4.3.1 Reactor 4-10
4.3.2 HCl absorption tube 4-10
4.3.3 Drying tube 4-11
4.3.4 Storage container for hydrochloric acid 4-11
4.3.5 Storage container for deionized water 4-11
4.4 Start-up 4-12
4.4.1 Concentration ranges 4-15
5. Performance of a measuring series 5-1

5.1 Operational test 5-1
5.2 Routine analysis 5-2
6. Despription of the analysis modes 6-1

6.1 TC Mode 6-1
6.2 TIC/NPOC Mode 6-2
6.3 POC/TIC/NPOC Mode 6-3
6.4 TNb measurement 6-4
6.5 Measurement of the TNb
03/2003 Operating instructions liquiTOC

Copyright by E l e m e n t a r Analysensysteme GmbH
Page II Contents
7. liquiTOC software description 7-1

7.1 General 7-1
7.2 Installation 7-1
7.3 Starting the program 7-1
7.4 The operation elements 7-2
7.4.1 Caption bar 7-2
7.4.2 Menu bar 7-3
7.4.3 Tool bar 7-3
7.4.4 Status bar 7-4
7.4.5 Status field 7-4
7.4.6 Sample field 7-4
7.4.7 Combi window 7-4
7.5 Editing sample data 7-5
7.5.1 Sample input 7-5
7.5.2 Further input possibilities 7-6
7.5.3 Menu hierarchy 7-6
7.6 Processing of the liquiTOC data with MS-Excel 7-16
8. Calibration 8-1
8.1 General 8-1
8.2 Stock solution 8-1
8.3 Single point calibration 8-2
8.4 Multiple point calibration 8-2
8.4.1 Multiple point calibration from one standard solution 8-2
8.4.2 Mulitple point calibration from mulitple standard solutions 8-2
8.5 TNb 8-3
8.6 Performing the calibratoin 8-3
8.7 Calibration in the measuring range < 0,5 mg/l 8-4
9. Maintenance / Replacement of consumables 9-1

9.1 Replacement of the reactor 9-1
9.1.1 Flushing of the reactor with saline samples 9-2
9.2 Replacement of the drying tube 9-2
9.3 Replacement of the HCl absorption tube 9-2
9.4 Filling up the water and acid stock 9-3
9.5 Leak test/leak search 9-3
9.6 Blockings 9-3
10. Appendix A-1

10.1 Index of illustrations A-1
Note to PC problems A-2
Installation requirements A-3
Operating instructions liquiTOC 01/2004

Scope of delivery page 1-1
1. Scope of Delivery:
Basic unit :
♦ liquiTOC
carbon/nitrogen analyzer for the determination of C or C and TNb in aqueous samples,
including instrument software in German or English, basic equipment.
Basic equipment sufficient for installation and training .
order no. 35.10-0000 (C version)
order no. 35.20-0000 (C/TNb version)
♦ control- and evaluation unit ♦ control and evaluation unit

with German Windows® with English Windows®
operation system operation system
order no. 50 008 369 order no. 50 008 368
(for 230 V, 50/60 Hz, other voltages (for 230 V, 50/60 Hz, other voltages
upon request) upon request)
♦ printer with printer cable

order no. 50 031 857
(for 230 V, 50/60 Hz, other voltages upon request)
Necessary Accessories :
♦ O2 pressure reducing valve for synthetic air or oxygen

two-stage, 2nd stage 0 - 3 bar with shut-off valve
for gas purity 99.995 % or better
order no. 04 278 800

Page 1-2 Scope of delivery
Optional accessories :
♦ Automatic sample feeder

− for liquids and particles containing samples
− micro processor controlled
− 36 sample vials with max. 30 ml volume each (variable)
up to 6 sample injections per position
− before and during dosing of particles containing solutions up to 27 samples can be
homogenized by means of a magnetic stirrer for 27 samples
− function for automatic purging of TIC
incl. interface cable, sample vials, magnetic stirrers and tin foil
order no. 34.00-0115
♦ Sample magazine 53 for automatic sample feeder

for 53 samples with max. 17 ml volume each (variable), up to 4 sample injections per
position.
Before and during the dosing of particulates containing solutions up to 41 samples can
be automatically homogenized by a magnetic stirrer.
order no. 05 001 305
♦ Solids module
for instrument modification for the determination of TC in solids, suspensions and
sludges.
Recommended work range: max. 500 mg sample weight or max. 100 mg C abs.
order no. 35.00-0001
♦ Set of small parts

O-rings, screwings, sealings for the performance of minor maintenance work
order no. 35.00-0069
For further ordering information for spares or consumables, see appendix and the newest
catalog for consumables.

Specification and technical data page 2-1
2. Specifications and technical data
2.1 Specifications
Operating modes TC, TIC, TOC, NPOC, POC as well as combinations
thereof, also TNb simultaneously, depending on
instrument version
according to DIN 38409 H3, ISO 8245, EPA 415.1

US standard method 5310 A
European standard EN 1484
working range 0-10,000 mg/l C,

selectable or automatic adjustment
0-5,000 mg/l N (EC detector)
liquiTOCtrace: 0-200 mg/l C

0-200 mg/l N
calibration linear
or selectable 1 or multipoint calibration, fully
automatic and/or acc. to customer's specification
precision / TOC/NPOC/TC/TIC
standard deviation* ≤ 2 % at ≥ 10 mg/l C
≤ 5 % at ≥ 0.2 mg/l C
(*depends on injection volume; TNb (EC detector)
values based on 2ml)
≤ 5 % at > 5 mg/l N
≤ 4 % at > 20 mg/l N
sample volume 0.05 to 4 ml, depending on concentration range
particle size up to approx. 200 µm
duration of analysis 6 to 22 minutes,

depending on mode of operation, parameters to be
determined, sample volume and content
sample digestion dynamic combustion at 850°C,

catalytic postcombustion at max. 800°C,
acetous digestion of the TIC with hydrochloric acid,
0.8%
data storage respectively storage on hard disc or discette,

data output transfer to LIMS possible,
Data output on monitor and printer

Page 2-2 Specification and technical data
2.2 Technical data
detector 1 cuvette multi-channel IR-detector

1 channel for NO-detection
control and evaluation unit PC with Windowsoperating system
printer (optional)
software Windows program; German or English,
menu operated, status display during analysis, real
time graphic; LIMS-capable, GLP-suitable data
reduction and documentation.
interfaces RS 232 /V24, low safety voltage
according to DIN IEC 380/VDE 0806/08.81
dimensions approx. 400 x 550 x 480 mm (W x D x H) for the
basic instrument additional 200 mm distance from
rear and side walls
weight approx. 50 kg
voltage 120-230 Volt AC ± 10 %, 50/60 Hz
connected load approx. 1.9 kVA
protection class I, grounding terminal
type of protection IP 20, installation in dry rooms only
carrier gas synthetic air
(carbon hydrogens ≤ 0.1 ppm, CO2 ≤ 1 ppm)
1.0 bar, usage approx. 500 ml/min.
ambient temperature permissible max.: + 35°C
min.: + 15°C

Safety Instructions page 3-1
3. Safety Instructions
Please adhere to the safety instructions and only operate

the unit in accordance with manufacturer's instructions.
The warnings on the individual instruments and in the
appropriate chapter of these instructions are also valid.
General instructions
• The analyzer liquiTOC is suitable only for the carbon/nitrogen analysis in aqueous
samples, which have a controllable combustibility under conditions depending on the
mode of operation. Analyzing aggressive chemicals, acids, solvents, explosives or
materials that can form explosive gases is explicitly forbidden. It can lead to damages
of the instrument and to injuries of the operating personnel. For the above mentioned or
other difficult applications, we recommend to use the counseling possibilities of our
application laboratory, in order to work out safe operating procedures and to use certain
parameters or special equipment.
♦Operation, maintenance and repairs should only be carried out by trained personnel.
For a smooth and efficient operation of the liquiTOC, please read the following operating
instructions thoroughly. Please keep the operating instructions for future questions. We
reserve the right of deviations in illustrations and technical data described in the operating
instructions due to further developments. The data shown in the software illustrations are
only examples and can deviate from the actual parameters to be set. Please take the
parameters valid for your instrument from the supplied installation CD.
Installation / Start-up
• Operation of the liquiTOC and peripheral equipment should only be carried out by
persons who have been authorized by E l e m e n t a r Analysensysteme GmbH.
Upon request, technically experienced instrument users may put the instrument into
operation themselves. The instructions of the manufacturer – especially the safety
instructions – shall be adhered to at all times. No liability by the manufacturer for damages
caused by improper handling.
• Opening the transport packing by unauthorized personnel can lead to loss of
warranty rights! If the supplied instruments show damages, please contact the freight
forwarder and the manufacturer.
• For the operation of the liquiTOC analyzer it is mandatory to use the furnished power
supply cable only!

• The installation room must be well ventilated!

The exhaust gas pipe (connection IR and if necessary CLD) must lead into the open
air or into a fume hood because it is possible that during operation toxic gases (e.g. SO2,
NO, NO2, CL2, etc.) emerge from the instrument. During constant operation the respective
gas concentration can exceed the permissible maximum workplace concentration.
• The end of the gas pipes must lead to a sheltered (wind-free) place in the open air to avoid
fluctuations of the base line which would lead to detector instabilities.
• Liquid residues can be very acetous and must be neutralized before leading them into the
sewerage system. If the analyzed samples contain compounds which are hazardous to the
water, the liquid residues will have to be disposed of according to the respective
regulations.
Reagents
• When handling chemicals, observe the safety instructions of the chemical manufacturer
(see labels on bottles and safety data sheets)!
• When handling hydrochloric acid, Sicapent® (Phosphorpentoxide) or magnesium
perchlorate, it is absolutely necessary to wear safety goggles and protective gloves.
!!!Danger of Causticization !!!
• When handling cold quartz and glass parts wear the supplied leather gloves to avoid
danger of injuries in case of broken glass.
Maintenance/Exchange of tubes
• The efficiency of the liquiTOC can only be guaranteed when original consumables as
well as original spare parts which can be obtained only through Elementar
Analysensysteme GmbH or their authorized dealers, are used. The use of different
consumables or chemicals of an unsuitable standard can lead to injuries as well as to
instrument damages. It can also falsify the results of the analysis. Unsuitable spares
lead to instrument damages and loss of warranty.
• All the operation dependent maintenance and exchange times mentioned in the Operating
instructions depend very strongly on the respective test matrix. They are, therefore, only
examples and do not guarantee life times for consumables or wear and tear parts!
• The walls of the liquiTOC should only be opened by authorized personnel for
maintenance and servicing purposes.
• Before opening the rear wall of the liquiTOC, disconnect all peripheral equipment and
the liquiTOC itself by turning the main switch off and pulling the mains plug. Danger
of electricution - 230 Volt !!!
Attention: the furnaces must be cold otherwise components will become overheated. The
walls must be properly in place before starting a new analysis. (Check grounding
connection.)
Safety Instructions page 3-3
• The liquiTOC and the gas pipe system must be checked periodically for leaks.
• For safety reasons, the hydrochloric acid must be removed from the storage container
before checking for leaks.
• Never subject the IR-detector to overpressure. It could damage the detector.
• Replacing the reactor can only be carried out when the tube is cold. For this purpose
set furnaces to nominal temperature 0°C and let the tubes cool down to room temperature
(max. 100°C).
When working at hot furnaces or tubes there is danger of burning!!
Therefore, always wear the supplied protective gloves (order No. 05 000 094), because it is
possible that some components (e.g. heated tube line) are still hot. We are not liable for
accidents that are due to disregarding these warnings.
• Before replacing the reactor turn off the gas supply into the instrument.
• After changing the reactor wait until the furnaces as well as the new reactor has warmed
up (ca. 10 to 15 minutes) before starting the next analysis. In addition, it is necessary to
adhere to the conditioning rules for the tubes (chapter 9)
• Before installation into the furnace all finger prints must be cleaned off the quartz
parts (for instance with acetone) to avoid crystallization areas which lead to premature
aging of the quartz.
• If the supply voltage has been interrupted for more than 15 minutes, the liquiTOC must
be checked for leaks. If necessary, replace all o-rings inside the furnace chamber since they
may have been brittle because of the interrupted ventilation.

Installation and start-up page 4-1
4. Installation and start-up

Installation and operation of the liquiTOC and
peripheral equipment should only be carried out by
persons who have been authorized by
E l e m e n t a r Analysensysteme GmbH.
Opening the transport packing by unauthorized
personnel can lead to loss of warranty rights! If
the supplied instruments show damages, please
contact the freight forwarder and the manufacturer
immediately.
4.1 Preparations for operation

These prerequisites are absolutely adhered to for a smooth operation of the liquiTOC.
4.1.1 Working environment

The installation site for the liquiTOC and the respective peripheral equipment as
autosampler and PC should be protected from draught and direct sources of heat. An
air conditioned room is recommended as some parts of the analyzer give off heat.
In addition, appropriate steps are to be taken to avoid electrostatic charges. Electrical
discharges on the unit can lead to malfunctions.
At the installation site the surrounding CO2 concentration should be stable and low
(< 800 ppm CO2).
placement area type of protection: IP 20

only in dry, well ventilated rooms; installation of the
liquiTOC only on an acid and heat resistant surface
space requirement entire surface area

(incl. PC, autosampler approx. 120 x 55 x 35 cm
and reagent vessels) distance from the walls at least 20 cm at all sides,
otherwise the fans of the unit will not function properly.
Optional modules require additional space.

Page 4-2 Installation and start-up
Ambient temperature constant temperature

permissible min.: + 15°C
max.:+ 30°C
power supply 120-230 Volt AC ± 10 %, 50/60 Hz
connected load: 1.9 kVA
power supply and frequency must match the information
on the legend plate of the instrument
connections 6 sockets
protection class I, connection for grounded conductor
wire
required fuse protection: 16 A/delay-action fuse
gas connections gas connections must be available in the immediate
vicinity of the instrument. Pressure reducing valves are
required for connection. Pressure reducing valves O2 for
synthetic air with two steps (2nd step 0-3 bar) with shut-
off valve (for order instructions see chapter 1).
exhaust pipe atmospheric into the open air or a fume hood because of
toxic gases (see safety instructions).
waste pipe atmospheric; a totally undisturbed discharge into a non
metallic outlet must be guaranteed (see safety
instructions).
The installation room must be well ventilated! The

exhaust gas pipe (connection IR and maybe CLD)
must lead into the open air or into a fume hood
because during operation some sample components
may release toxic gases (e.g. SO2 , NO, NO2, Cl2 etc.)
with the carrier gas. It is possible that during constant
operation the gas content of the air exceeds the
permissible maximum workplace concentration .
The end of the gas pipes must lead to a sheltered (wind-
free) place in the open air since pressure fluctuations,
for instance through wind, lead to detector instabilities.

4.1.2 Necessary gases and chemicals
When handling chemicals observe the safety

instructions of the chemical manufacturer (see labels on
bottles and safety data sheets)!
When handling hydrochloric acid, it is necessary to
wear safety goggles and suitable protective clothing!
!!!Danger of caustic burns!!!
carrier gas synthetic air (carbon hydrogen ≤ 0.1 ppm, CO2 ≤ 1 ppm)
prepressure 1.0 bar
use: approx. 500 ml/min
reagents • deionized water (C-content < 1 mg/l)

(see chapter 4.3.5)
• 0.8 % hydrochloric acid p.a. (see chapter 4.3.4)
chemicals for filling the reactor and/or absorption
tubes are included in the basic set of consumables.
calibration standards Potassium hydrogen phtalate (KHP),

sodium carbonate Na2CO3,
ammonium sulfate (NH4)2 SO4) and
potassium nitrate (KNO3)
These substances must have at least p.a. quality (see
chapter 8).
4.2 Instrument installation
The walls of the liquiTOC should only be opened by

authorized personnel for maintenance and servicing
purposes.
The design of the basic unit of the liquiTOC is as follows:
4.2.1 Front of the unit

Behind the front door there is the furnace (bottom combustion, top post combustion)
with the inserted reactor. The reactor is connected with the gas supply injection valve
(bottom) and the condenser tube inlet (top) by means of a ground-in ball-and-socket
joint.
On the top at the right side there is also a fan.

5
2
6
7
8
illustration 4.1: front view (behind door)
legend to
illustration
4.1 1 reactor
2 furnace, post combustion zone
3 furnace, combustion zone
4 reactor connection, bottom
(gas and sample supply)
5 reactor connection, top, to the cooler
6 fan
7 electrical connections of the furnace
8 thermoelement connections

4.2.2 Right side with removed sidewall

On the right side there are the outlet slots for the fan, another fan and the electrical
connection boxes as well as the membrane dryer.
1
8
5
3 4
illustration 4.2: connections at the right side
legend to
illustration
4.2 1 cooling vent for reactor
2 membrane drying
3 mains switch
4 power supply plug
5 connection sampler
6 connection PC
7 connection CLD
8 connection TIC

4.2.3 Left side with removed sidewall

The connections for the gas and reagents supply and the waste are freely accessible on
the bottom on the left side. The pre-installed sample suction connection is on top of
the right side in the casing frame. All other components are accessible, if the left side
panel is removed.
1 4
10
11
3 8
7
5 6
illustration 4.3: connections at the left side

legend to
illustration
4.3 1 flow controller
2 water trap
3 connection panel for supply gas, water, acid, etc.
4 water condenser
5 filter (before the water drainage valve)
6 syringe 10 ml
7 drying tube
8 buffer volume
9 HCl absorption tubes
10 sample suction connection
11 leak test hose

1 2 3
4 5 6 7 8
illustration 4.4: connection panel
legend to
ill. 4.4
1 connection water supply
2 connection acid supply
3 gas outlet IR and membrane drying λ 450 ml/min
4 connection carrier gas approx. 1 bar
5 gasing water supply
6 gasing acid supply
7 gasing sample
8 waste
4.2.4 Back panel

Behind the back panel you will find the fuse boxes.
Before opening the back panel cut off the power supply
for peripheral instruments and the analyzer by turning
off the mains switch and pulling the power plug!

mains
connection
IR
automatic circuit breaker
F1: 2 A
F2: 2 A
F3. 10 A
F4: 10 A
F5: 50 A
F6: 50 A
illustration 4.5: electronic connections on the back panel

4.2.5 Tubing diagram, functional diagram
illustration 4.6: tubing diagram liquiTOC
4.3 Filling of the quartz and glass parts
4.3.1 Reactor
catalyst
illustration 4.7: reactor
The reactor shall be filled as follows:

The reactor will be filled with catalyst in the upper half through the gas outlet opening.
The filling height is 70 mm. For filling the reactor the furnished funnel with hose
connection which is been pulled over the ground-in ball-and-socket joint, will be used.
Make sure that the ground-in ball-and-socket joint. does not get in contact with sharp
edged obstacles. Minor splinters may already cause leaks.
4.3.2 HCl Absorption tube
Cu chips
silver wool
illustration 4.8: HCl absorption tube

The right absorption tube (absorption tube 1) will be filled with one half Ag-wool
(approx. 3 g) and one half Cu chips. The ends will be closed with filter material. Make
sure that the tube with the Cu chips is installed toward the top.
The left adsorption tube will be completely filled with 6 g Ag-wool. The filter material
is not needed.
4.3.3 Drying tube
The U-shaped drying tube will be

filled with magnesium perchlorate.
The ends will be closed with

filter material.
illustration 4.9: drying tube
4.3.4 Storage container for hydrochloric acid

The storage container (glass bottle) will be filled with 0.8% HCl.
25 ml of commercially available TOC-free HCL, concentration approx. 32% will be
diluted with deionized water to 1000 ml.
Hydrochloric acid is caustic, make sure to wear

protective clothing!
Start filling the hydrochloric acid into the storage

container after the leak test has been performed.
4.3.5 Storage container for deionized water

The storage container (glass bottle) will be filled with deionized water.
(TOC < 0.5 mg/l).
The precision of the TOC measurements depends especially on the low measuring
range from the quality of the used pure water. In general, the low measuring range
limit has to be at least the triple of the blank value.

4.4 Start-up
Start-up of the liquiTOC and peripheral equipment

should only be carried out by persons who have been
authorized by E l e m e n t a r Analysensysteme
GmbH.
For start-up please follow these instructions successively:

Please also note the shut-down condition of the unit.
a) Set instrument up (for instructions regarding placement area see chapter 4.1.1) and
connect peripheral instruments.
autosampler
CLD
liquiTOC ¡ ¬
PC printer
illustration 4.10: connections of the liquiTOC with the peripheral instruments
As shown in illustration .4.10, the TOC analyzer consists of a basic instrument

liquiTOC and several peripheral instruments. The PC is absolutely necessary as
control and evaluation unit while CLD, printer or sample feeders are optional. The
peripheral instruments are connected to the appropriate socket at the back panel of the
liquiTOC with the supplied cables (see illustration 4.2 and inscription on the
instrument). The sample feeder must be placed in such a way that the sample suction
syringe is not below the water level of the water vessel. Otherwise, water could drop
out of the suction syringe if the valve position is unfavorable.
b) Connect gas supply and install flushing gas and exhaust gas outlets. Reagent hoses and
drain pipes must also be connected.
The installation room must be well ventilated! The exhaust

gas pipe (connection IR and maybe CLD ) must lead into
the open air or into a fume hood because during operation
some sample components may release toxic gases (e.g. SO2 ,
NO, NO2, Cl2 etc.) with the carrier gas. It is possible that
during constant operation the gas content of the air exceeds
the permissible maximum workplace concentration .
The end of the gas pipes must lead to a sheltered (wind-free)
place in the open air since pressure fluctuations, for instance
through wind, lead to detector instabilities.

Illustration 4.4 shows the connections on the left side panel of the liquiTOC. The acid
or water vessel is connected to the gasing acid supply and/or gasing water supply
(HCl or H2O) with a thin hose and to the connection water and/or acid supply (HCl
or H2O) with a thicker hose. The gasing sample for sample vessels is usually closed
with a blind stopper. The carrier gas is connected to the first inlet (O2/N2). Outlet for
gas (IR) must lead into open air (see safety instructions above). Outlet for liquids for
waste must lead into a non-metal container (for disposal see safety instructions below).
Note: It is important that the supplied hoses are used for exhaust and waste. The
prescribed dimensions and the material of the hoses are necessary for
failure free operation (for order information see catalog for consumables).
Liquid residues can be very acetous and must be

neutralized before leading them into the sewerage
system. If the analyzed samples contain compounds
which are hazardous to the water, the liquid residues
will have to be disposed of according to the respective
regulations.
Note: for first start-up remember to remove the cable ties from the hoses.
c) Fill quartz and glass parts (reactor) and install (see chapter 4.3). Fill water and acid
container with water first.
d) Loosen valve out of the transportation clamp below the reactor and connect it with ground
in clamps to the reactor
e) Turn PC and printer on and wait for booting procedure to be ended. If necessary - install
software (see chapter 7) and remain in Windows-Desktop.
f) Turn on autosampler - if available - and wait for reference run to be ended.
g) Turn on the main switch of the liquiTOC (see illustration 4.2).

Wait until the syringe has moved down and found its end position.
h) Load the liquiTOC software by clicking on the liquiTOC icon.

The software is menu controlled, so that the user sees most of the operational steps
displayed on the screen. Moreover, most of the standard operation parameters have been
set in the factory (see chapter 4.4.5) which the user does not need to change.
i) Turn gas supply on and set prepressure. Then check gas flow at the flow meter displays of
the software and - if necessary - re-adjust using an external flow meter.

These are the suggested standard instrument settings
gas pressure
Set the prepressure to approx. 1.0 – 1.2 bar at the bottle pressure
reducing valve. The pressure display at the PC should show
0.95 – 1.0 bar.
flow rate
outlet IR 200 ml/min
This flow rate has been factory set. The value will be displayed at
the "flow MFC" bar as well as at the "FM" bar. If the instrument
is duly leak proof, both displays will be almost identical.
MFC shows the outcoming gas flow and FM shows the incoming
gas flow.
The display "FM" may vary during an analysis, especially during
the combustion.
A flow check must always to be carried out in standby.
outlet
sample flushing / 30-40 ml/min each (factory set)
reagents flushing
outlet approx. 250 ml/min. (factory set)

gas drying
j) The selection of the operation mode is realized in System/Mode.(see illustration 4.11).

The mode selected starting installation of the system is the default mode. When the
mode has to be changed a dialog appears which lists the necessary hardware and the
required parameter settings.
Example: For the solid mode, the solid module has to be installed and combustion
temperature has to be changed.
illustration 4.11: menu System/Mode

k) Perform leaktest. Close the flexible hose with the connected clamps on the left
instrument side (with side wall taken off). If the flowmeter display shows a drop to 0
within 30 seconds, the leak test has been passed.
l) Fill hydrochloric acid into the acid vessel (see chapter 4.3.4).
m) Start heaters and check parameter setting at the PC (see chapter 5.3.5). The catalyst
furnace should have reached its operating temperature after 15 minutes. The catalyst
has to be flushed for approx. 10 minutes with the carrier gas turned on.
n) Select in the menu System/Feeding the type of feeding; select maybe autosampler type
and amount of multiple determinations.
o) Measure blank values of water (see chapter 5.1). If the blind value peak area is
somewhere around 7.00 area units, it is possible to already measure test standards of
100mg C/l. For measurements below 5 ppm a stable blind value (< 2,00 area units)
are necessary.
Note: The liquid system will also be flushed air-free during the first measurements.
4.4.1 Concentration ranges

The measuring range of the liquiTOC is mainly determined by two influence
parameters: the injection volume and the IR channel where the peak is measured.
These parameters are under Options/Settings/Concentration range.
The following parameters are allocated to a defined concentration range:
¾ Injection and/or sample volume
¾ Evaporation temperature of the liquid sample: a temperature of 250°-300°C is

recommended.
¾ Waiting time during sample evaporation.

This time depends on the sample volume and is approx. 60-120 sec.
Upon delivery of the instrument, the following concentration ranges are predefined:
injection interim 1. temperature approx.

volume [sec] stage [°C] concentration
[ml] range
20 ppm 1 120 250 0.5-50
100 ppm 0.5 120 250 1-100

The column sensitive refers to the peak recognition parameters. If this function is
activated, more rigid criteria will be determined for the peak beginning and the peak
end (stability of baseline, admissible difference of the peak end to the baseline, etc.).
In general, an activation of this function will lead to a better precision in the lower
concentration range (< 0.5 mg/l) but results in a longer measuring time.
Note for all instruments with detector identification IR-type: JU-C/xxxxxxx:

This detector has no automatic measuring range switch. Therefore, the IR channel
where the signal shall be detected has to be selected additionally. Channel 1 is the
sensitive channel (up to approx. 40 mg/l at 2 ml injection volume), channel 2 is the
non sensitive detector. The detector identification may be read out via the menu
„?/About liquiTOC.
Basicallly it is recommended to measure the CO2 peaks in channel 1 and not in

channel 2 and to adjust the injection volume accordingly. The highly precise dosing
technique of the liquiTOC allows a dosing volume of 4 ml-20 µl without losing the
measuring precision of small dosing volumes.
If it may be necessary to extend the measuring range upwards or downwards, every
customer has the option to determine his own concentration range. When increasing
the injection volume also a longer interim of the 1st temperature stage is required in
order to evaporize the entire sample volume safely. When determining the interim as
well as the temperature special attention shall be paid that during an analysis there will
not be a complete breakdown of the gasflow (FM). In this case has interim has to be
prolonged and/or the temperature has to be adjusted.
According to our experiences a temperature of 250° C is a good compromise between

careful and effective evaporation. This value should be chosen normally.

Performance of a measuring series page 5-1
5. Performance of a measuring series
It has to be dinstinguished between
1) general operational test during initial operation and/or after installation of a new reactor
and
2) the routine analysis.
5.1 Operational test

First of all, blanks will be measured with deionized water (TOC < 0.5 mg/l), since the
complete system has to be flushed TOC-free.
As operation mode we recommend the TIC-NPOC-process.
The procedure is as follows:
¾ Turn on instrument acc. to chapter 4, select TIC-NPOC under System / Mode.
¾ Open carrier gas and flush for 10 minutes.
¾ Fill 5 sample vials of the autosampler with deionized water and put them on the
autosampler. If no autosampler is available, the sample hose is lead directly into the
corresponding glass vial.
Note:
There are special positions on the autosampler for control standards or blanks. These
special positions can be defined in the column "hole pos." by entering e1, e2 or e3.
¾ Determine the number of determinations per sample under System / Feeding (1, 2 or 3),
e.g. 3.
¾ Open the following input diaglogs via double click in the sample field (Text-View) :
1. Input dialog "Name"

e.g. enter name "blank" for the number of requested blank samples
example: 5 sample vials à 3 determinations = 15 x.
2. Input diaglo "Conc.range"

The name has to be defined under Options / Settings / Conc.range.
Example: "UP-water"
¾ After closing the input dialogs the measuring series can be started.

¾ For permanent operation click symbol .
¾ For single analysis click symbol .
¾ Now the number of selected blank determination will be procesed. The TIC and NPOC
blank should be down to peak areas of < 3.0 within 15 blank measurements. In case that
after 15 measurements there is no stable blank value, the blank measurements have to be
continued.
¾ With a stable blank value test standards can then be measured, e.g. 20 mg TIC/
20 mg NPOC or 50 mg TIC / 50 mg NPOC per liter etc., in order to check the stability of
the measuring results.
The procedure is as follows:
1. e.g. fill 3 sample vials of the autosampler with test standard 20 mg TIC/l + 20 mg
NPOC/l.
2. Enter the name 20+20 in the input dialog "Name" for the number of requested
measurements, e.g. 3 sample vials à 3 determinations = 9x.
3. Enter the name "20 ppm" in the input dialog "Conc.range". By clicking "OK" the
concentration range will automatically be copied for all entered sample names.
¾ After closing the input dialogs the measuring series can be started.
¾ For permanent operation click symbol .
¾ For single analysis click symbol .
¾ Now the number of the selected blanks will be processed. For statistical evaluation you
will find the statistics function under Math / Statistics.
If the statistical evaluation has a satisfying precision the routine analysis can be started.
5.2 Routine analysis

Prerequisite: instrument is turned on, function checked acc. to 5.1.
¾ Select TIC-NPOC mode , select 3-fold determination.
¾ Fill sample vial no. 1 of the autosampler with a test standard referring to the application
for conditioning (example 20+20).
¾ Fill sample vial no. 2 of the autosampler with deionized water for blank determination.

Performance of a measuring series page 5-3
¾ Fill sample vial no. 3 of the autosampler with a standard referring to the application
(example 20+20) for checking the calibration.
¾ Enter the following measuring series in the PC:
no. position of the hole name conc. range

1 1 Run-in 20+20 20 ppm
2 1 Run-in 20+20 20 ppm
3 1 Run-in 20+20 20 ppm
4 2 blank 20 ppm
5 2 blank 20 ppm
6 2 blank 20 ppm
7 3 Caltest 20+20 20 ppm
etc.
Notice: name and concentration range will be entered manually and/or copied,
the number and the position of the hole will be generated automatically.
¾ From sample vial no. 4 on, the real samples can be put in the autosampler, by entering the
relevant concentration range.
¾ Prior to the start, check the following points (PC display, instrument in standby):
♦ Maintenance intervals o.k.?

♦ Gas on?
♦ Pressure and flow rate display o.k.?
Pressure approx. 0.95 bar
Flow rate MFC and FM 200 ml/min. each.
♦ Drying tube still enough capacity?
Ö last third not yet used up
♦ Syringe and sample loop air-free?
♦ IR signal small and stable?
♦ Furnace to nominal temperature?
Catalyst 800°C, reactor approx. < 90°C
♦ Water and acid stock o.k.?
¾ For permanent operation click symbol , now all samples entered in the PC will
be processed. In case the blank value and the result of the calibration test have changed by
more than 10% relative, a recalibration can be performed after completion of the
measuring series in menu Math. The results of the real samples can then be recalculated
with the new calibration with function Math / Recalculate.

Description of the analysis modes page 6-1
6. Description of the analysis modes

The requested analysis mode can be selected under System / Mode.
The actual processes will be displayed on the PC in the status field under "Process", e.g.
"Standby" or "Peak processing" etc.
6.1 TC Mode
¾ Start of analysis with or .

¾ Auto Zero Adjust and baseline determination of the IR detector for the TC peak.
¾ Carrier gas will be turned off.
¾ Dosing of approx. 300 µl HCl into the reactor (syringe runs, valves switch).
¾ Dosing of sample in the reactor (sampler runs, syringe runs, valves switch).
¾ Carrier gas will be turned on.
¾ The temperature of the dynamic heater for the sample combustion increases up to max.
850°C.
At the same time the integrator module waits for the TC measuring peak to start.
¾ TC peak integration.
¾ After completion of the combustion the dynamic heater will be turned off, the cooling fan
works.
¾ Integration end
¾ Water drain
¾ Process end, a new start can be done.
illustration 6.1: peak graphics TC determination

Page 6-2 Description of the analysis modes
6.2 NPOC Mode

(available starting with serial no. 3503001)

¾ Auto Zero Adjust and baseline determination of the IR detector for the NPOC peak.
¾ Dosing of the sample in the reactor (sampler runs, syringe runs, valves switch).
¾ The integrator module waits for the NPOC peak to start.
¾ NPOC peak integration.
¾ Integration end
¾ After end of integration the dynamic heater will be turned off, the cooling fan does not
run.
¾ Water drain
General notes to the NPOC mode:

The samples have to be acidified externally. Otherwise the alkaline and earth alkaline oxides
resulting from the combustion may destroy the reactor in a very short period of time. If there
is also TIC, it has to be carefully purged after the acidification in order to avoid higher NPOC
results.
Make sure that the front door is always closed during the operation in NPOC mode since
overheating problems in the front area may occur.
illustration 6.2: peak graphics TIC/NPOC determination

6.3 TIC/NPOC Mode

¾ Auto Zero Adjust and baseline determination of the IR detector for the TIC peak.
At the same time the integrator module waits for the TIC measuring peak to start.
¾ TIC peak integration.
¾ After TIC integration end the baseline determination of the IR for the NPOC peak
follows.
880°C.
At the same time the integrator module waits for the NPOC measuring peak to start.
works.
¾ Integration end
¾ Water drain
illustration 6.3: peak graphics TIC/NPOC determination

Page 6-4 Description of the analysis modes
6.4 POC/TIC/NPOC Mode

¾ Auto Zero Adjust and baseline determination of the IR detector for the POC peak.
At the same time the integrator module waits for the POC measuring peak to start.
¾ POC integration
¾ After POC integration end the baseline determination of the IR for the TIC peak follows.
At the same time the integrator module waits for the TIC measuring peak to start.
¾ TIC peak integration.
¾ After TIC integration end the baseline determination of the IR for the NPOC follows.
880°C.
At the same time the integrator module waits for the NPOC measuring peak to start.
works.
¾ Integration end
¾ Water drain
illustration 6.4: peak graphics POC/TIC/NPOC determination

General Notes on POC/TIC/NPOC Mode
¾ The samples have to be made alcalic, pH λ 11-12. Otherwise, it might be

possible that due to acid residues of previous samples the TIC will be purged
together with the POC.
Alcality should be at 0.01 n. E.g. 0.56 g KOH will be added to 100 ml of
sample, if the sample is neutral. If the samples have been acidified before, the
amount of KOH has to be increased accordingly.
¾ Depending on the chemical compound and on the affinity toward water, the
POC peak is very sharp and quick (e. g. halogenized hydrocarbons) or it is
broad, flat and slow (e. g. acetone, alcohols). The integration time of the POC
peak is therefore limited in time.
6.5 Measurement of the TNb

The measurement of the TNb can be added to all analysis modes. The procedures do not
change, only the electrochemical cell will be activated via the protective valves.
Prerequisite is that the instrument is equipped with an adequate detector.

liquiTOC Software Description page 7-1
7. liquiTOC Software Description
7.1 General
The following software description is only an abbrevated version. A complete description for
the individual menus can be found in the implemented help file of the software.
The liquiTOC software is a software to control the liquiTOC analyzer. It can be run under
the Windows platform. The Windows operating systems 95, 98, NT (from version 4.0 on) and
2000 will be supported. The communication of the Windows PC will be done via a serial
interface (RS232). Basically, the liquiTOC software allows the following actions:
• enter and/or modify sample data

• control of an analysis process
• recording and filing analysis results
• protocol of measuring results
• calibration of the system
• statistical processing of the measuring results
• leak and system test possibilities
7.2 Installation
For the installation of the liquiTOC software insert the furnished CD into the CD-ROM drive
The CD will start automatically. If the CD does not run automatically a start with
CDMNENUPRO.EXE will be possible. Choose the language. Choose Software Installation
in order to start the setup program.
For the first installation choose 1. New Installation

For the update of an existing installation choose 2. Update Installation.
7.3 Starting the program

After the program has been started, a dialog box appears in which the user has to register by
means of a password. Level 1 is the administrator level. If a registration takes places via this
level, all operating functions are disabled. There is only one menu ("Admission") where the
admission authorization for each user can be determined. Level 2 is the super user level. This
level allows the operation of the software with all rights, e.g. change of the analysis mode,
change of the parameter settings, etc. Level 3 is the user level. The user has only limited
operation rights, basically entering of samples and the performance of analysis. Each user is
assigned to the a certain level. The program identifies the indivdual user via a certain
password. The administrator is authorized to give out the passwords. It is also his
responsability that each password is unique. By doing so a clear identification of the
registered user via a password is possible. To make a first access easy, the following
passwords are pre-defined for the different levels: for level 1 (administrator) it is password
"1", for level 2 (super user) it is "2" and for level 3 (user) it is "3".

Page 7-2 liquiTOC Software Description
Subsequently, the program tries to create the communication connection with the analyzer. If
it was sucessful, the status field appears with a light green background, otherwise the
background will be light red.
7.4 The operation elements

After start of program and registration the program starts, similar to illustration 7.1.
caption bar
menu bar tool bar
status field
sample
field
combi
window
status bar
illustration 7.1: View main frame
The operating elements and their effects will be described in the following.
7.4.1 Caption bar

The name of the program and the name of the document (or file) of the current process
appears in the caption bar. For a new document the document name is “untitled“. At
the right end of the caption bar there are three buttons "Minimize",
"Maximize/Restore" and "Close". By clicking the symbol on the left end of the caption
bar the system menu with individual items like "Restore", "Move", "Size",
"Mimimize", "Maximize" and "Close" opens.

7.4.2 Menu bar

The main menus are listed in the menu bar. Branching into a sub menu can be done by
clicking the equivalent menu name with the mouse, pull over to the requested sub
menu and clicking it. As an alternative, the menu navigation can also be activated via
the keyboard. The relevant menu can be reached by entering the underligned letter of
the corresponding menu name.
7.4.3 Tool bar

The tool bar allows a quick access to important and/or often used menus without going
through the entire menu hierarchy. The buttons have the following meaning:
see description "File / New"

see description "File / Open"
see description "File / Save"
see description "Edit / Cut"
see description "Edit / Copy"
see description "Edit / Paste"
see description "Edit / Insert Line"
see description "Edit / Group"
see description "Edit / Include/Exclude"
see description "File / Print"
see description "View / Toggle"
see description "View / Zoom"
see description "View / Previous"
see description "View / Next"
see description "View previous sample"
see description "View next sample"
see description "System / Wakeup"
see description "? / About..."
context sensitive help
see description "System / Run"
see description "System / Single"

7.4.4 Status bar

A short description of the currently selected menu and the name of the registered user
appears.
7.4.5 Status field

The status displays the currently actual instrument status. If an analyzer is connected
the background of this window appears in light green and an update of the values will
be done in approx. seconds intervals. If no analyzer is connected or if there is no
communication, the background appears in light red. Furthermore, the corresponding
instrument parameters which are relevant for the communication appear in grey. If the
mouse pointer is moved over this window, it will get the shape of a hand when it is
over the maintenance bar. By clicking with the left button the maintenance dialog can
be invoked directly.
The status field can be activated by clicking with the mouse to any place within its
window. If the window is activated, the window title appears in dark blue.
7.4.6 Sample field

The sample data are displayed in the sample field. The individual data can be
showed/hidden and the display sequence can be changed. The current sample, i.e. the
sample which is currently analyzed, is highlighted with a light green bar. The
consecutive number which represents the stop mark is displayed in red. At this point
the continuous operation is terminated. If the mouse pointer is moved over this
window at some places it will get the shape of a hand. This signalizes that this place
can be edited (see description "Editing sample data").
The sample field can be activated by clicking with the mouse to any place within its
7.4.7 Combi window

The combi window shows either the graphic analysis run of a sample, the statistical
results or a performed calibration as a graphic – depending on the activation. It can be
switched between the individual displays by means of the menu "View / Toggle".
The combi window can be activated by clicking with the mouse to any place within its
The three windows "status field", "sample field" and "combi window" can be changed
among each other in their size. The mouse pointer shall be moved either onto the
vertical line between sample field and combi window or onto the horizontal line
between status field and sample field and/or combi window until it gets the shape of a
double arrow. Then press the left mouse button and pull the line (while mouse button
is held down) in the requested direction. The window sizes set at the latest will be
saved. This means that during a new start of the program there will be the same
division of windows like when leaving it.

7.5 Editing sample data

In order to measure samples and/or analyze them, their basic data have to be entered in
the sample storage. Normally this would be the name of the sample and the
concentration range in which the sample should be measured.
7.5.1 Sample input

The input of sample data can be done in different ways:
¾ Input via mouse:

Simply position the mouse pointer over the sample data type to be edited and
double click. The input dialog box opens and the required data type can be
modified. By pressing the "OK" key the input will be accepted and the next sample
will be activated. If a different data type shall be edited, one has to simply go to
the corresponding place with the mouse and double click again.
¾ Input via menu:

the menu "Edit / Edit" has to be invoked. A dialog box appears where it has to be
stated which sample and which data type shall be edited. After entering this
information the dialog box closes and the input dialog box appears where the data
type – selected before - of the corresponding sample can be edited. After the data
input the corresponding value appears in the sample field in the corresponding
place – subsequently the input dialog selects automatically the next sample and
allows another input. Therefore it is possible to edit consecutively sample by
sample the once selected data type. If another data type shall be edited, the still
open dialog box shall be closed with the "Esc" key and the menu "Edit / Edit" shall
be invoked again to select the required data type.
For editing sample data further functions are available which simplify the input – apart
from the "normal input". These are:
¾ Automatic increase of the number of sample names:

if a sample name ends with a number (e.g. "name001"), this number will
automatically be increased by a certain value and suggested for the next sample
(e.g. "name002"). However, there are certain restrictions: if the number is
exhausted in terms of digits (e.g. "name999"), there will be no increase but the
name remains unchanged and will be suggested for the next sample. If the number
is not at the end of the name (e.g. "name001xyz"), there will be no increase in
number.
¾ Automatic decrease of the number in the sample name:

the same applies as for the item before, however the number as part of the name
will be decreased. When reaching the value "zero", there will be no further
decrease.

¾ Copying the name for multiple determinations:

if activated and if e.g. a double determination has been set, the sample name will
be allocated twice after each sample name input. This applies for the samples
which have the same hole position.
¾ Increase / decrease interval:

the automatic increase and/or decrease of the number as being part of the name is
not limited to the value 1 but can be done for an amount to be freely selected
(1...99). This means that the amount has to fit in the area to be displayed in terms
of number of digits, otherwise there will be no change in number.
¾ Fill up conc. range names up to stop tag:

the selected concentration range will be copied for all samples.
The before mentioned types of input can be set via the menu "Options / settings /
input".
7.5.2 Further input possibilities

Further input possibilities are given by the methods typical for Windows like "Copy",
"Cut" and "Paste". E.g. a recurring sequence of samples names can be obtained by
using the function "Edit / Copy". If e.g. the name sequence "nameAA", "nameBB" and
"nameCC" shall be repeated in the sample row, it can be proceeded as follows: first,
the three names will be entered. Then they will be highlighted as a block. This will be
done by clicking the first name (single click) so that is is highlighted in color, then the
last name will be clicked by pressing the "Shift" key at the same time. Now the area of
the sample which has been clicked first up to the last is highlighted in color. This area
will now be copied into the clipboard by the function "Edit / Copy". Subsequently, it
shall be clicked with the mouse to the position below the block end (single click – this
position is highlighted) and "Edit / Paste" shall be selected. The block from the
clipboard will thus be inserted into the selected position. This function can be repeated
as often as requested, until the sample row has been filled.
7.5.3 Menu hierachy

The individual menus are described in the following:
File / New
Creates a new document. If necessary, the user will be asked to save the data which
are currently in the sample storage.
File / Open
Opens an existing document. A diaglog field appears where the document to be
opened can be selected. If necessary, the user will be asked to save the data which are
currently in the sample storage.

File / Save
Saves the content of the sample storage under the actual document name. If no
document name has been defined so far ("Untitled"), a dialog box appears "Save as"
where the document name has to be selected and/or defined.
File / Save As
Saves the content of the sample storage under the actual document name. A dialog box
appears "Save as" where the document name has to be selected and/or defined.
File / Load Graphics

Loads a graphic of a sample (only possible during standby) and shows it in the graphic
display of the combi window.
File / Report Configuration

Allows the setting of how the analysis printout shall look like. A dialog box appears
where the headline can be entered. Furthermore, it will be determined whether also the
calibration coefficients and the instrument parameters shall be printed out together
with the sample data.
File / Print
Prints the document. Which printout will be processed depends on which window is
currently activated. If the sample field is activated the sample data will be printed out.
The sequence of the data types is identical to those on the screen. If the combi window
is activated and the grahpics view is selected, the graphic analysis process will be
printed out. The settings for the screen (zooming factor, activated graphics, etc.) apply
for the printout as well. If the statistics view is selected, the data of the statistics
storage will be printed. If the calibration view is selected, the individual calibration
lines will be printed. If the status window is activated, this function cannot be invoked.
File / Print Preview

Displays on the screen how the printout will look like.
File / Printer Setup

Allows the setup of the printer. The layout of the appearing setting dialog depends on
the used printer type and/or driver.
File / 1...4
The names of the four recently used documents will be displayed here (if available).
By clicking one of these document names the corresponding document can be quickly
opened.
File / Exit
Leaves the liquiTOC program. Can only be invoked if the system is in standby.
Edit / Cut
Deletes the highlighted data type and puts it to the clipboard. Can only be invoked if
something was highlighted and the text view is activated.
Edit / Copy
Copies the highlighted data type and puts it to the clipboard. Can only be invoked if
Edit / Paste
Pastes the content of the clipboard to the highlighted position. Can only be invoked if
Edit / Insert Line

Inserts an "empty" sample line at the highlighted position. Can only be invoked if the
text view is activated and a complete line was copied to the clipboard.
Edit / Group
Combines the highlighted samples to a statistical group and loads them into the
statistics storage. Can only be invoked if at least two samples were highlighted and the
text view is activated.
Edit / Include/Exclude
With statistics view in the combi window activated
Includes and/or excludes a sample highlighted in the statistics field from the statistical
computation. Can only be invoked if a sample was highlighted in the statistics field
and at least three samples that are not excluded are within one group. A sample in the
statistics field can be highlighted by clicking with the mouse. Calling up the function
on an already excluded sample includes the sample again.
In general, only those samples should be excluded from the statistics which were not
analyzed properly (e.g. not enough sample in the vial).
With calibration view activated
Includes and/or excludes a sample selected from the calibration computation. Can only
be invoked if a sample was selected in the calibration field. A sample in the calibration
field can be selected by clicking with the mouse. Calling up the function on an already
excluded sample includes the sample again.
Edit / Sort Group

Sorts groups included in the statistics storage in rising sequence starting each with the
number of the first sample. Can only be invoked if the statistics storage is not empty
and statistics field is activated.
Edit / Delete Group

Deletes the group highlighted in the statistics field. Can only be invoked if a group is
highlighted in the statistics field and the statistics field is activated. A group can be
highlighted by clicking with the mouse to one of the result lines (mean value, standard
deviation rel. or abs., Delta).
Edit / Clear Statistics

Deletes the entire content of the statistics storage. Can only be invoked if the statistics
storage is not empty.
Edit / Edit
Allows the opening of an input dialog without using the mouse.
View / Toggle
Changes between statistics, graphics and calibration view. Can only be invoked if the
combi window is activated.
View / Next
With graphics view in the combi window activated
Displays the graphic analysis run of the next sample – if existing. Can only be invoked
if the graphics view in the combi window is activated.
Changes to next calibration data.
View / Previous
With graphics view in the combi window activated
Displays the graphic analysis run of the previous sample – if existing. Can only be
invoked of the graphics view in the combi window is activated.
Changes to previous calibration data.
View / Zoom
Allows the selection of the zooming factor in steps 1, 2, 5, 10, 20, 50 and 100. Can
only be invoked if either the graphics or the calibration view in the combi window is
activated.
View / Next sample

Moves the crosshair to the next sample. Only accessible, if the calibration view in the
combi window is activated.
View / Previous sample

Moves the crosshair to the previous sample. Only accessible, if the calibration view in
the combi window is activated.
View / Configuration
Allows the configuration of the corresponding view. Depending on the activated view
different dialog boxes appear where the individual settings can be performed. These
are:
¾ Sample field: the individual date types can either be hidden completely
(column number = 0) or determined in the sequence of the display
(column number = 1: the furthest to the left).
¾ Graphics view in the combi window: from eight graphs up to four can be selected
which shall appear in the graphics field. For each graph the display area can be set
(Y-axis). For all graphs the time frame will be defined (X-axis in seconds).
Furthermore it can be selected on which grid line the zero line should be.
Consequently, it is possible to follow the direction of an IR channel if it is
negative.
¾ Statistics field in the combi window: the individual concentration can be hidden
(identification number = 0) and their sequence can be set (identification number =
1: is the furthest to the left). Whereas the mean value of the individual
concentration always appears, the other result lines can be shown/hidden as
requested.
¾ Calibration view in the combi window: there is no configuration possible.
¾ Status field: there is no configuration possible.
View / Tool Bar

This command shows/hides the tool bar.
View / Status Bar

This command shows/hides the status bar.
Wizard / Calibration
This menu starts a wizard which supports the user in performing a calibration for an
analysis series. After completion, the program enters the corresponding sample data in
the sample storage. By invoking the wizard again a further calibration series – e.g. for
a different concentration range – can be amended to the previously produced one. The
user has to prepare the corresponding samples (autosampler) after the wizard has
entered the sample data and then has to invoke the start function. After completion of
the analysis run a calibration of the system can be performed by means of the menu
"Math. / Calibration".
Wizard / System Suitability Test

This menu starts a wizard which supports the user in perfoming a System Suitability
test for an analysis series. After completion, the program enters the corresponding
sample data in the sample storage. The user has to prepare the corresponding samples
(autosampler) after the wizard has entered the sample data and than has to invoke the
start function.
After completion of the analysis run the test can be started by means of the menu
"Math. / System Suitability Test". Can only be invoked if the document is empty.
Assistant / Validation
Not yet implemented.
System / Run
Starts the continuous analysis. During a continuous analysis samples will be processed
until either the stop mark or the sample where the system should go into sleep mode is
reached. This depends on the settings in menu "Options / Settings / Sleep/Wakeup"
(see relevant menu item). Can only be invoked if an analyzer is conneted and if the
corresponding samples for a concentration range were entered.

System / Single
Starts a single analysis, i.e. after the analysis of one sample the system goes back to
standby. If this function is invoked during a continuous analysis the continuous
analysis will be stopped, i.e. the system goes back to standby after the analysis of the
currently processed sample is completed. Can only be invoked if an analyzer is
connected and if the corresponding samples for a concentration range were entered.
System / Wakeup
If the system is in sleep mode, this command wakes up the system again (see also
Options / Settings / Sleep/Wakeup).
System / Stop Tag

Allows the manual setting of a stop tag. The stop mark is the position where the
program stops its continuous analysis. Usually the stop tag is automatically
administered during the input of sample data, i.e. it is shifted accordingly. With this
menu it is possible to have an impact on this automatic procedure and therefore to end
the continuous analysis earlier than usual, e.g. for control purposes.
System / Current Sample

Allows the manual definition of the current sample. Current sample means the sample
which is currently being processed (analysis run) or which is going to be processed
next (standby). Also here an automatic procedure applies: at the begin of a continuous
analysis the current sample is the one with the consecutive number 1. With the
proceeding of the analysis run also the number of the current sample will be increased.
In case of malfunctions (power failure, etc.) or if a measurement shall be advanced, it
may sometimes be necessary to have an impact on the automatic procedure.
System / Feeding
With this menu it will be defined how the feeding shall be performed: either without
or with autosampler. For the feeding mode "without" it is presumed that the suction
needle is tightly in a sample vial and/or in a sample bypass. For the feeding mode
"autosampler" the number of plate positions has to be specified in order to ensure that
the sampling will be performed from the correct sample vials. The option "Needle
plunged" can be selected if the sample material e.g. has to be stripped out. It can also
be set if a single, double or triple determination shall be run.
Depending on this setting the computation of the correct sampling position will be
done automatically for each sample.
Sytem / Mode
Allows the selection of the analysis mode. Can only be invoked if the document is
empty.
Options / Maintenance / Intervals

This menu allows the specification of up to ten maintenance events. For each event a
text, a limiting value and the actual count of the meter can be defined. The program
compares the count of the meter with the limiting value and produces a bar in
corresponding length for each event. The color of the bar reflects when the next
maintenance is due.

The bar with the largest length and its percentage is displayed in the status field. After
each analysis the count of the meter will be increased by 1. If a mainenance event is
due, a blinking warning triangle appears in the status field, combined with the
corresponding event text. If the warning triangle appears without event text, it occurs
during an analysis run. If there are multiple maintenance events due, only one event
appears in the status field. It will be the first event in the sequence.
Options / Maintenance / EC-cell

The EC cell has a limited lifetime of approx. 2 years due to its principle. When the EC
cell will be replaced, this measure has to be considered in the menu.
Options / Maintenance / Change Part

The selection of this menu results in a shut-off of the carrier gas and the furnaces.
When working in temperature sensitive areas (reactor/catalyst) the maintenance work
shall only be started if the furnace temperature has dropped to < 50°C.
Options / Maintenance / Flush

Activates the flush of the sample carrying tubings with UP water.
Options / Maintenance / Ventilate

The loop will be flushed three times with UP water to ventilate the system.
Options / Diagnosis / System test

Opens a dialog box where different aggregates can be tested for their functionality.
This dialog presents a schematic display of the components in the instrument. By
moving the mouse pointer to the required aggregate and by clicking it, its function can
be tested.
The following tests are possible:
Valves: switching of the valve
Syringe: opens a dialog box where the manual procedure of the syringe is made
possible
Furnaces: opens a dialog box which allows the manual heating up of the
furnaces
Autosampler: opens a dialog box which allows the performance of different
functions of the autosampler, e.g. selection of positions, moving of the
needle, etc.
MFC: opens a dialog box which allows the manual setting of the flow rate
Options / Diagnosis / Error buffer

Opens a dialog box where all detected errors are listed in chronological order. The
relevant event is displayed as a code (for space saving reasons). By doubleclicking of
the corresponding event code another dialog box will be opened where the event code
is displayed in decoded form.
Options / Settings / Input

Serves for the definition of how the program should react during the input (see
description "Edit of sample data").

Options / Settings / Keywords

Serves for the definition of various keywords. The program is able to classify certain
samples due to their names and to treat them accordingly. These keywords can be
specified in the appearing dialog box.
Options / Settings / Number Format

Country specific decimal notation can be set. Since the liquiTOC program works with
the point as decimal notation it may be necessary for some Windows versions to
change the format from point to comma.
Options / Settings / Acoustic Signals

It is possible to fade in and out acoustic signals to certain events with this menu.
Acoustic signals may be issued when
¾ a maintenance event is due
¾ an error occurs
¾ start of analysis.
Options / Settings / LIMS

Serves for determing how a data transfer to a superior LIM system shall be performed.
The following settings are possible:
¾ Data to be sent: determination which sample data shall be transferred

¾ Typ of data transfer: none, serial port, via network – connected with the settings of
the serial interface and the path name for filing the data in a network.
¾ Passwords for the identification of the instrument while sending data.
The before mentioned settings will be made in a dialog box which opens.
Options / Settings / Concentration range

Serves for the definition of a certain concentration range. The following criteria define
a concentration range:
¾ Injection volume in [ml]

¾ Waiting temperature in [°C], prior to heatup of the reactor to its operating
temperature
¾ Waiting time in [sec], how long the waiting temperature shall be maintained.
¾ Sensitive, activation of this button recommended if concentrations < 2 mg/l shall
be measured.
Up to 8 different concentration ranges can be defined. They will be identified by the

program during the analysis run via their names.
Options / Settings / Sleep/Wakeup

This menu determines how the system shall respond to the end of an analysis run
and/or to a certain sample. The following options can be set:
¾ Sleep deactivated: when reaching the last sample (stop tag) the system goes to
standby mode. The reactor temperature and gas flow remain the same.

¾ Sleep at end of samples: when reaching the last sample (stop mark) the system
goes to the sleep mode, i.e. the furnace temperature will be lowered to the set
value (as selected and set in option and/or input field "Reduce temperature to" and
the gas will be switched off (as selected in option "Cut off carrier gas").
¾ Sleep at sample no.: when reaching the corresponding sample the system goes into
the sleep mode (see previous description).
By clicking the button "Sleep Now" the system can be put immediately into the sleep
mode.
If the system is at sleep, there are the following possibilities for a wakeup:
¾ Wakeup at time/date: waking-up will be performed at a determined date and a

determined time – both can be set under "Time" and/or "Date". Is the date in the
past, it has to be waken up manually.
¾ Daily Wakeup at time: waking-up will be performed at a certain time and daily –
except for those week days which are clicked in the day bar below.
By clicking the button "Wakeup Now" the system can be manually waken up.
During the wakeup prodecure the reactor is heated up first, then the gas will be turned
on again. A certain time will pass until the instrument can be put into operation again.
The behavior after the wakeup depends on how the instrument "fell asleep": are there
still samples in the sample storage up to the stop mark which have not been analyzed,
the continuous analysis will be automatically performed up to the stop mark after the
instrument is ready for operation. However, there will be no other sleep procedure!
If there are no further to be processed samples up to the stop mark, the system waits
for an analysis start after it is ready for operation.
Math. / Coefficients
This menu allows the manual input of calibration coefficients. The coefficients can
only be entered and/or altered with an empty document.
Math. / Calibrate
If there are calibration samples in the sample storage the calibration field in the combi
window will be activated and for each existing concentration range as well as for each
element type (e.g. TIC, NPOC, etc.) the course of the calibration line as well as the
position of the samples will be displayed in a graphic one after the other. The user can
do a visual outlier elimination by clicking the suspected sample and subsequently
invoking the function "Edit / Include/Exclude". By invoking the function "View /
Next" the next calibration curve can be seen. After the last calibration graphic has
been displayed a further invocation of "View / Next" will cause the display of the
calibration coefficients dialog. By leaving the dialog with OK, the last calculated
calibration coeffients will taken over and are available for the next measurement.

Math. / System Suitability Test

The menu performs a system suitability test. Prerequisite is that equivalent samples
were analyzed and their measuring results are available. The program puts the
measuring results of the samples easy and hard to digest into proportion and displays
in a dialog box whether the system suitability test was sucessful or not. Upon request
the results can be printed.
Math. / Statitistics / By Names

Beside the function that the statistical computation will be automatically performed
when the selection of the group is done manually, a grouping can also be performed
automatically. However, it has to be ensured that the samples (and only those) which
shall be summarized in a group have the same name. With careful selection of the
name the grouping can be done only by invoking this menu which is much simpler.
Math. / Statistics / By Muliple Determination

Beside the function that the statistical computation will be automatically performed
when the selection of the group is done manually, a grouping can also be performed
automatically. The samples which were taken from the same vial will be automatically
summarized to one group.
Math. / Blank Value / Calculate

If there are blank samples in the sample storage the program calculates the
corresponding blank rates and presents them in a dialog box that will be opened. By
leaving the dialog with OK the last calculated blank rates will be taken over.
Math. / Blank Value / Enter

Opens a dialog box which allows the manual input of blank rates.
Math. / Recalculate
This menu performs a complete recalculation of the sample data.
? / HelpTopics
Not yet implemented
? / About liquiTOC
Shows a dialog box where the program version and the version number of the analyzer
and the autosampler (if connected) are displayed.

7.6 Processing of the liquiTOC data with MS-Excel
The liquiTOC data files are filed in ASCII format and are therefore legible by any
common spreadsheet program. The following describes the procedure of loading the
liquiTOC data under MS-Excel.
1. Start MS-Excel.
2. Load the liquiTOC data file that you want to have processed. Invoke the
command „File/Open”. First select “All data types”(*.*) under “files of type”
in the appearing file open dialog. Now select in the field „Look in“ the folder
in which the data file to be loaded is and select it in the listing below. By
clicking „OK“ the file open dialog closes and a text wizard opens. Confirm the
displayed steps with “next” and the last step with „Finish“. The liquiTOC data
will now be displayed in an Excel worksheet.
Now you can further process the data as required.
Please make sure to save the data under a different name (e.g. with the
extension „xls“) since otherwise the original file will not be legible from the
liquiTOC program anymore!

Calibration page 8-1
8. Calibration
8.1 General
The calibration creates the relation between the detector signal (in relative units) and the
carbon and/or nitrogen contents in the sample. This relation is linear within the given
measuring ranges. The plot as measuring signal (in relative units) against the absolute content
C and/or N. Compared with the plot against the concentration it has the advantage that the
calibration can be used for different injection volumes.
The liquiTOC analyzer knows different calibration ranges to which different concentrations
for TIC and TOC are allocated. For each sample type an individual calibration can be stored,
as described in chapter 7.
If a peak has been recognized, the area of the peak will be saved if the peak maximum lies
below the saturation concentration of the detector. Otherwise, the peak will not be taken
under consideration for the calibration.
TIC and TOC can either be calibrated by means of a mixed standard or by means of a single
standard. For time reasons the calibration by means of mixed standard is recommended. It
does not have an influence on the analytical results.
For stability of the calibration one can say that due to the mass flow controller the carbon can
be run over a very long period of time without a new calibration. Even an exchange of the
reactor does not necessarily mean a new calibration. A calibration should be stable for at least
one month. For TNb a new calibration is necessary more often, i.e. at least once a week or if
necessary, every working day.
8.2 Stock solution

It is recommended to prepare a higher concentrated parent solution (500 mg/l TIC + 500 mg/l
TOC) and to dilute this parent solution accordingly. As a TOC standard potassium phthalate
(KHP) shall be used, as TIC standard sodium carbonate (Na2CO3). We strongly advise against
using sodium hydrogen carbonate as a TIC standard as part of a mixed standard since
hydrocarbons may be decomposed in the mix due to the slightly acid character of KHP.
The parent solution is stable over approx. 4 weeks, stronger dilutions over 1-2 days. The
composition of the above described solutions, related to 1 liter, is as follows:
4412.1 mg sodium cabonate

1062.7 mg KHP

Page 8-2 Calibration
8.3 Single point calibration

The single point calibration is the fastest way to calibrate the liquiTOC analyzer. The
following shall be considered:
• The ordinate section will be automatically set to 0. For low conentrations this may lead to
strong falsifications in measuring results. Therefore, it is recommended to perform a blank
value determination for the methods drinking water, ultra pure water and sea water when
using a single point calibration.
• An outlier identification for a single point calibration is only be possible with a triple
determination. Therefore, a single point calibration shall not be performed with a double
or a single determination.
• A verfication of the linearity of a calibration function is not possible with a single or

double calibration. Therefore, the user shall stick to the given concentration ranges for
single point calibration.
8.4 Multiple point calibration
8.4.1 Multiple point calibration from one standard solution

The user is able to perform the calibration from one standard solution. The system
automatically selects the different injection volumes over one order of magnitude (from
0.1-2 ml). This is possible because the sample volume has no influence on the signal size due
to the use of a massflow controller. It only depends on the content of C and/or N.
8.4.2 Multiple point calibration from multiple standard solutions

This is the most flexible but also the most costly possibility of a calibration. Any
number of calibration points in any concentration steps can be selected via the
calibration assistant. However, it may be possible to extend the concentration range
over the admissible range. It is not at all sufficient to mind the linearity of the
calibration straight line. The requirements for variant homogeneity according to DIN
ISO 8466-2 have to be fulfilled. The liquiTOC analyzer is linear within the measuring
ranges stated in the following table and within these concentrations the differences
among the variants are purely accidental.
The following table contains concentrations of typical samples.

Calibration page 8-3
method concentration concentration

TIC- standard TOC standard
drinking water 1-30 0.2-5
waste water 10-200 10-200
surface water 0.5-10 0.5-10
sewage plant supply 5-30 5-30
ultra pure water 0,2-4 0.2-4
sea water 5-30 0.2-4
elution water 10-200 10-200
8.5 TNb
Basically TNb can be calibrated similar to TIC or NPOC. Since the TNb analysis can be
influenced more easily by outside influences than the TOC analysis which has to do with the
different thermodynamic stability of the measuring species (here CO2, there NO), some
specialties have to be considered.
The NO yield depends on the chemical bond of the nitrogen. Nitrate for instance has a
recovery rate of approx. 100% whereas ammonium of about 90%. When knowing the
approximate sample composition, this should be considered when selecting the calibration
standard. For unknown samples a mixed calibration of 50% ammonium-N and 50% nitrate-N
is recommended. Such a standard for 500 mg/l TNb has the have following composition:
955 mg/l NH4Cl

1518 mg/l NaNO3
It is possible to calibrate TNb and TIC/TOC from one and the same stock solution. In this
case, the above quantities of NH4Cl and NaNO3 shall be added to the TIC/TOC stock
solutions as described in chapter 8.1. The advantage of this procedure is an immense time
saving. But it shall be considered that due to high TOC contents (> 200 mg/l) the N recovery
may be impaired.
8.6 Performing the calibration

The computation of the calibration coefficients is done as described in chapter 7. First, the
blank value rates will be computed, then a graph with the calibration line with the calibration
coefficient is displayed in the calibration view. a represents the offset and b the slope of the
line. Out of this coefficient the concentrations will be calculated:
a + b Ik
c:
lV

Page 8-4 Calibration
IV represents the injection volume in l and Ik represents the peak ares corrected by the blank
value of the flushing volume. Furthermore, you will receive the information on the correlation
coefficient r. The value of r should be > 0.9900. If r < 0.990 a closer look should be given for
outliers.
Outliers can be highlighted with a left click of the mouse and eliminated from the calibration
under menu "Exclude".
In general one should be careful with the elimination of outliers. Calibration points should
only be eliminated in case of very clear outliers.
8.7 Calibration in the measuring range < 0,5 mg/l

If measurements shall be done in the trace and ultra trace range, special attention shall be paid
to the calibration. In general, working with at least a 5 point calibration and a triple
determination per calibration point is recommended. Furthermore, it has been proven to be
advantegous to lay the calibration line through the coordinate origin. For this purpose set
manually the coefficent „a“ = 0 after completion of the calibration evaluation.

Maintenance / Replacement of consumables page 9-1
9. Maintenance / Replacement of consumables

In the menu Options / Maintenance / Intervals up to ten different maintenance events can be
specified. For each maintenance a text, a limiting value and the actual count of the meter can
be defined.
There is also a bar display in the main window which reflects the maintenance status. Prior to
large sample series the maintenance status should be checked.
The following maintenance events are factory given:
¾ 1000 ml water stock, approx. 150 analysis

¾ 1000 ml acid stock, approx. 700 analysis
¾ reactor with filling, approx. 1500 analysis
¾ drying tube, approx. 500 analysis
¾ HCl absorption tube 1, approx. 300 analysis
¾ HCl absorption tube 2, approx. 1000 analysis
The replacement of the consumables will be done under Options / Maintenance / Replace
part. The carrier gas and the furnace heatings will be switched off. After the overpressure has
been decreased in the instrument the corresponding ground-in clamps or screwings can be
opened.
It is absolutely necessary to wear protective

equipment (goggles, gloves) since acid liquid residues
may squirt.
When replacing the reactor make sure that it is cooled
down to < 100°C. Wear the furnished thermo gloves.
!!! Danger of burnings !!!
9.1 Replacement of the reactor

The new reactor will be filled with catalyst according to chapter 4.3.1. The reactor is located
behind the front door. For a replacement the ground-in clamps will be opened on bottom and
top. The cooled down reactor can now be pulled out of the instrument (remove cover plate of
casing). The new reactor will be inserted into the furnace in reversed order, the ground-in
clamps will be closed on bottom and top.
After leaving the function Replace Part the carrier gas will be turned on, the furnaces will be
heated up. A new reactor should now be heated out with streaming carrier gas for approx. 30
minutes. Subsequently, some blank value measurements should be carried out (see chapter
5.1).

Page 9-2 Maintenance / Replacement of consumables
After the replacement of the reactor also the pressure and flow display at the PC should be
checked after approx. 10 minutes whether they correspond to the nominal values (see chapter
4.4.1, point h).
If the display FM is far bigger than 200 and the display MFC is far smaller than 200 or even
zero, a leak has been created during assembly of the ground-in clamps. It has to be removed
by orderly assembly.
9.1.1 Flushing of the reactor when analyzing saline samples

If mainly saline samples with e.g. 35 g/l NaCl are analyzed, the absorption capacity of
the reactor for the salt is limited to approx. 50 – 100 samples.
The water soluble salt will be dissolved by flushing the reactor incl. filling with
deionized water and will then be removed from the reactor.
The flushing of the reactor has to be done outside the furnace. Therefore, the reactor
has to be removed for flushing.
In order to avoid longer intermissions in the sample measurements it is recommended

to work alternately with two reactors:
one reactor is in the liquiTOC

one reactor is being flushed.
9.2 Replacement of the drying tube

The drying tube will be filled according to chapter 4.3.3.
The drying tube is located behind the left sidewall (see chapter 4.2.3). The consumption of the
drying tube will be shown by a change in color: from light blue to pink.
For replacing the drying tube the two large screw caps at the inlet and outlet of the drying
tube have to be loosened. The drying tube will be held at the lower leg and carefully pulled
out of the holding clamps.
The installation of the new drying tube will be done in reversed order.
9.3 Replacement of the HCl aborption tubes

The new HCl absorption tube will be filled according to chapter 4.3.2.
The HCl absorption tubes are located behind the left sidewall (see chapter 4.2.3).
The consumption of the absorption tubes will be shown by a change in appearance: from
silver shine to black and to violet.
For replacing the absorption tube the two screw caps at the inlet and outlet have to be
loosened. The used up absorption tube can now be pulled out of the holding clamps.
The installation of the absorption tube will be done in reversed order.
9.4 Filling up the water and acid stock

The filling of the water and acid stock will be done according to chapter 4.3.4 und 4.3.5.
Maintenance / Replacement of consumables page 9-3
9.5 Leak test/leak search

A leak is displayed by an significantly higher flow (>5 ml/min) by the flow meter in standby
mode compared to the flow of the mass flow controller. If the leak test to be performed
detects a leak, the latter shall be located.
The upper outlet of the reactor shall be closed with a device (included in the leakage set). If
the flow display of the flow meter goes back to 0, the leak is located behind the reactor. If the
flow meter shows an residual flow, the supply line to the reactor shall be closed with a blind
plug. If no gas flow can be seen, the reactor is leak (hair crack or splintering at the ground-in
ball-and-socket joint). Otherwise, check the connections to the buffer container first, then the
gas outlet of the flow meter. If all these connections remain without findings, the flow meter
is probably defective.
If the leak is located behind the reactor, first all connections of the desending cooling tube
with the spiral cooler shall be checked. Both outlet connections of the spiral cooler (to hoses
no. 40 and 50) shall be sealed. If the flow meter shows a flow, the screw connection of the
descending spiral cooler shall be fastened and if necessary the o-ring shall be replaced.
If the flow meter does not show any flow, first the waste hose no. 50 shall be reconnected
with the spiral cooler. If there is a flow in the flow meter again, the leak is located in the drain
area of the condensed water. Valve V9 or the blind screw connection located in the valve is
probably defective.
If there is no flow after connection of hose no. 50, hose no. 40 shall be reconnected with the
spiral cooler. Subsequently, the membrane gas drying (in the right side of the instrument)
shall be driven around by means of the double groun-in ball and socket joint (leakage set). If
the instrument is tight afterwards, the membrane gas drying shall be replaced. If there is still a
leak, the connections of the silver wool tubes and the U-tube filled with drying agent shall be
checked.
9.6 Blockings
Blockings mostly occur in the area of the reactor and the sample feeding. They will be
indicated by a heavily fluctuating flow in the flow meter during evaporation of the sample.
Blockings can also be detected by loosening the upper ground-in clamp at the reactor. The gas
flow through the flow meter shall be >400 ml/min. If the flow is lower
(<350 ml/min) a blocking can be assumed. In this case the lower ground-in clamp of the
reactor should be loosened first. If afterwards the flow is >400 ml/min, the reactor shall be
cleaned (see operating instructions) or, if necessary, replaced.

Page 9-4 Maintenance / Replacement of consumables
Otherwise the supply line to the reactor shall be checked and if necessary cleaned – or for
later instruments the valve at the lower end of the reactor. If a supply line is blocked, the
blockings usually can be found at the ends of the hose line. In this case, remove the fitting and
cut the hose lines approx. 2 mm from the end with a sharp knife (or with a scalpel, if
available).
Subsequently, a new fitting shall be mounted and the hose line can be reinstalled.

Appendix page A-1
10. Index of illustrations
Illustration 4:1: Front view 4-4

Illustration 4:2: Connections at the right side 4-5
Illustration 4:3: Connections at the left side 4-6
Illustration 4.4: Connection panel 4-7
Illustration 4:5: Electronic connections on the back panel 4-8
Illustration 4:6: Tubing diagram, functional diagram 4-9
Illustration 4.7: Reactor 4-10
Illustration 4.8: HCl absorption tube 4-10
Illustration 4.9: Drying tube 4-11
Illustration 4.10: Connections of the liquiTOC with the peripheral instruments 4-12
Illustration 4.11: Menu System/Mode 4-14
Illustration 6.1: Peak graphics TC determination 6-1

Illustration 6.2: Peak graphics TIC/NPOC determination 6-2
Illustration 6.3: Peak graphics POC/TIC/NPOC determination 6-3
Illustration 7.1: View main frame 7-1

page A-2 Appendix
Solving PC problems
Occasionally, there are problems with the PCs which probably are in connection with the
Elementar instrument software. Possible problems may be occasional system crashes or a
freeze of the instrument software. The cause can be explained by the connection of the
settings in the operation system for the power management of the PC. The settings shall be
checked in the power management under Control Panel-> Power Option Properties and/or
Power Schemes. The options for "Turn off monitor", "Turn off hard disks", "System standby"
and "System hibernates" shall be set to "Never". If possible, also the power management in
the BIOS of the PC shall be deactivated.
If the PC is connected to a network a further measure can be the deactivation of the

network. If possible, deactivate the network adapter under Systemsteuerung->
Gerätemanager or remove the network cable and restart the PC without network.
Under Windows NT4.0, Windows 2000 Professional and Windows XP Professional

the instrument software has to be started under equivalent user rights in order to be
able to change files in the instrument software directory (e.g. c:\variomax) and in the
system directory (e.g. c:\windows).
General Note
For future generations of the Elementar instrument software the operation systems
Windows 2000 Professional or Windows XP Professional will be a prerequisite.
Windows 9x/ME and Windows NT will not be supported anymore. This has to be
taken under consideration when purchasing new PC hardware.

Appendix page A-3
Installation requirements
Dear User,
we thank you for your order and the confidence expressed to our representative and
Elementar by this decision.
You have made you choice for a TOC-TIC analyzer of highest analytical performance and
reliability. In order to secure a fast and smooth installation of the instrument in your
laboratory, we kindly ask you to take the following hints into consideration:
Installation location
• The analyzer can be installed under normal laboratory conditions, i.e. no fume hoods or air
condition (ambient temperature between +15°C max. +30°C) are necessary.
• However, like for all analytical equipment direct sun beams, draft or other inconvenient
conditions for precision instruments should be avoided.
• For the installation of the unit (without PC, printer and balance) a stable laboratory table with
heat resistant surface is sufficient.
• Minimum dimensions: length 1.50 m * depth 0.80 m with autosampler length approx.
1,70m
• Weight liquiTOC approx. 50 kg.
Gas supply
For the operation of the analyzer the following gases are required which should be kept ready
by you on the spot for installation:
• Synthetic air (hydrocarbon <0.1 ppm and CO2 <1ppm),
1.5 bar, consumption approx. 500 ml/min
Unless delivered from us, the availability of two-step high precision pressure reducers (Air
Liquide or similar) is necessary. Pressure reducers of inferior quality will influence negatively
the analysis results!
! Pay attention to the bottle pressure !
Instrument control
If PC and balance were not delivered from Elementar, we reserve the right to perform the
installation with own instruments. Possible modifications to our analyzer have to be done by
the customer.
We would like to emphasize that the PC is the central control system of the analyzer. The
operating ability of the analyzer depends on a failure-free operation of the PC. Due to
experiences in the past with the use of control PC in mixed operation as office workplace
impairments due to software instabilities may occur.

page A-4 Appendix
Therefore, we recommend to only use programs on this PC for operation and data evaluation
of this analyzer.
Control PC
In case the PC was not delivered by us, the following minimum requirements have to be met:
For operation without modem:
• PC with Pentium III Processor 500 MHZ (or equivalent) or faster

• Operating system
• Windows 2000 Professional (SP3 or later), with 128 Mbyte RAM
or
• Windows XP Professional (SP1 or later), with 256 Mbyte RAM
• At least 100 MB fee momory on hard disc
• 1 free serial port RS 232
• CD-ROM or DVD-ROM drive
For operation with modem:
• 2 free serial ports RS 232

• CAUTION: The mouse must not occupy any of these ports.
• 1 analog telephone socket TAE-6N in 6 m periphery from the PC.
• This connection is necessary to guarantee the remote control maintenance of the instrument
via an analog modem.
• 1 analog modem with at least 56 kBaud transfer rate.
• Remote control maintenance software Symantec PC-Anywhere 10.5 or later.
Installation requirements for the instrument software:

To install the instrument software correctly, administrator rights for the PC have to be made
available.
Requirements for the correct operation of the instrument software:

The instrument software has to be operated under a user account that is provided with writing rights in
the instrument software directory (e.g. c:\liquitoc) and in the system directory (e.g. c:\windows).
The PC where the instrument software will be installed should be checked for settings in the control
panel under Control PanelÖPower Option Properties and/or Power Schemes. Setting should be made
as follows: "Turn off monitor", "Turn off hard disks", "System stand by" and "System hibernates"
should always be set to "Never". If possible, also deactivate the power management in the BIOS of the
PC.
As screen saver use only the Windows standard screen saver.

Appendix page A-5
Generally, it is not recommended to overload the PC where the instrument software is installed with
other software programs. This may lead to instable operation of the instrument software.
Balance
! Only required for operate with solids module !
Requirements for the balance: readability of 0.1 mg,

weighing range 5,1 g
tara 5,0 g
If the balance was not furnished by us, we reserve the right to enter the weights manually.
Possible adjustments to our analyzer have to be made by the customer.
General remarks
The instrument will be installed by a factory trained service engineer and the analytical
performance will be demonstrated by max. 10 standard calibration samples.
In case of specific handling and application questions, you are kindly invited to contact our
representative for assistance. The elaboration of specific operation procedures can be ordered
there against separate charge.
The instrument is calibrated over a standard measuring range from works`side which is stable
for a long time. If specific applications are not within this range, the user can perform an
extended calibration by himself.
Our agent and Elementar will of course assist you at all arising questions.
Please do not hesitate to contact us under:
Service: +49/6181/91 00-16
Application Lab: +49/6181/91 00-47
Sales Department: +49/6181/91 00-12

Page 4 of 3
Safety data sheet Art.-Nr./Part-No.: 05 001 059
1. Company Identification
of the company/undertaking
Identification of the product
Product name: Magnesium perchlorate (blue indicating), 6 ~ 14 mesch

MSDS Code: 9179E
Manufacturer’s name: KISHIDA CHEMICAL. LTD. (Sanda factory)

Adress: 14-10, Technopark, Sanda-shi,
HYOGO 669-1339, JAPAN
Phone number: Telephone: (0795) 68-1531
Facsimile: (0795) 68-1586
2. Component/information on ingredients
Chemical Name: Magnesium perchlorate

Synonyms: Perchloric acid, magnesium salt; Anhydrone; Dehydrite
CAS.-Nr.: 10034-81-8
Molecular Formular:Mg(ClO4)2
Formular Weight: 223.21
3. Hazards identification
Emergency Overview:
Irritating to eyes, respiratory systems and skin.
Contact with combustible material may cause fire.
Moisture sensitive.
Potential Health Effects:

Eyes: Causes eye irritation
Skin: Causes skin irritation
Inhalation: Causes respiratory tract irritation
Ingestion: May cause irritation of the digestive tract. May cause nausea and vomiting.
4. First aid measures
Eyes: Flush eyes with plenty of water for at least 15 minutes, and have a medical consultation
immediately.
Skin: Remove contaminated clothes and shoes, and rinse skin with plenty of water immediately. Use a
soap to help assure removal. If irritation persists, have a medical consultation immediately.
Inhalation: Move victim to flesh air. If breathing is difficult, give oxygen. If breathing has stopped,
administer artifical respiration. Have a medical consultation immediately.
Ingestion: Wash out mouth with water to a conscious person. never give anything by mouth to an
unconscious person. Have a medical consultation immediately..
5. Fire-fighting measures
Flash Point: No information available.

Autoignition Point: No information available.
Explosion Limits: No information available.
Extinguishing Media: Do not use water directly on fire. Use water spray to cool fire.exposed
containers. In case of fire use water spray, dry chemical, carbon dioxide, or
chemial foam.
Fire and explosion Hazards: May accelerate combustion.
Contact with other material may cause fire.
May emit toxic fumes (e.g.Hydrogen chloride) under fire condition.
Fire Fighting Instruction: Wear self-contained breathing apparatus and prtoective clothing to prevent
contact with eyes and skin.
Page 1 of 4
Safety data sheet
Product name: Magnesium perchlorate
6. Accidental release measures
Wear self-contained breathing apparatus and protective clothing to prevent contact with eyes and skin.
Sweep up and place the spill into a chemical waste container. Avoid raising dust. Ventilate the area and wash
the spill site after material pickup is complete.
7. Handling and storage
Handling: Avoid breathing dust, vapor, mist or gas. Avoid contact with eyes, skin and clothing.
Wear suitable personal protection. Refer to Section 8.
Storage: Do not store near combustible materials. Store in a cool and dry space. Keep a container tightly
closed.
8. Exposure controls/personal protection
Exposure Control: Use exhaust ventilation to keep airborne concentration below exposure limits.
Mechanical exhaust required.
Personal Protection: Safety glasses (goggles), Chemical resistant gloves, Full-body protective clothing,
MSHA/NIOSH approved respirator.
Exposure Guidelines: No information available.
9. Physical and chemical properties
Appearance: Blue flakes.

Decomposing point: > 250° C
Specific gravity/Density: ca. 26 g /cm³
Solubility: Easily soluble in water
Soluble in alcohol. Insoluble in ether.
10. Stability and reactivity
Chemical Stability: Stable under normal temperatures and pressures. Reacts violently with water with
evolution of heat.
Condition to Avoid: Incompatible materials, combustible materials, exposure to moist air or water.
Incompatibilities: Strong reducing agents, strong acids, ammonia, combustible materials (e.g., organic
solvents, finely powdered metals, hydrazine, phosphorus.
Hazardous Decomposition Products: Hydrogen chloride, oxides of magnesium.

Hazardous Polymerization: Will not occur.
11. Toxicological Information
Acute Effect: No information available

Chronic Effect: Prolonged or repeated skin contact may cause dermatitis.
RTECS no. SC8925000 (Perclorid acid, magnesium salt).
Irritation data: no information available
Acute toxicity data: Intraperitoneal (Mouse) LD50 1500 mg/kg
Carcinogenicity: Not listed as a carcinogen by ACGIH, IARC, NIOSH, NTP, OSHA, or CA Prop 65.
12. Ecological information
No information available.
Page 2 of 4
Safety data sheet
Product name: Magnesium perchlorate
13 Disposal considerations
Observe all federal, state and local environmental laws and regulations.
14. Transport information
IMO IATA
Shipping Name: Magnesium perchlorate Magnesium perchlorate
Hazard Class: Class 5.1 Class 5.1
UN Number: UN 1475 UN 1475
Packing Group: Group II Group II
15. Regulatory information
European Information:
EINECS No. 233-108-3
Hazard Symbol: O (Oxidiing), Xi (Irritating)
Risk Phrases: R8 Contact with combustible material may cause fire.
R14 Reacts violently with water.
R36/37/38 Irritating to eyes, respiratory system and skin.
Safety Phrases: S17 Keep away from combustible material.

S26 In case of contact with eyes, rinse immediately with plenty of water and seek
medical advice.
S27 Take off immediately all contaminated clothing
S36/37/39 Wear suitable protective clothing, gloves and eye/face protection.
US Federal Information
CAS No. 10034-81-8 is listed on the TSCA Inventory.
16. Other information
The above information is believed to be correct to best of our knowledge but does not purport to be all
inclusive and shall be used only as a guide. KISHIDA CHEMICAL shall not be held liable for any damage
resulting from handling or from contact with the above product.
Date of issue: 17.09.02 Supersedes edition of : 25.10.1999
The information contained herein is based on the present state of our knowledge. It
characterizes the product with regard to the appropriate safety precautions. It does not
represent a guarantee of the properties of the product.
Page 3 of 4
Safety data sheet Art.-Nr./Part-No.: 22 131 365
1. Identification of the substance/preparation and name

Identification of the product
Catalogue No.: 22 131 365

Product name: Silver wool, 50 g
Manufacturer/supplier identification
Manufacture:r WC Heraeus GmbH

Heraeusstr. 12-14
63450 Hanau
Supplier: Elementar Analysensysteme GmbH, Donaustr. 7, D-63452 Hanau,

Tel.: 06181-9100-0, Fax.: 06181-9100-10
e-mail: info@elementar.de
2. Composition/information on ingredients
CAS-No.: 7440-22-4
M: 107.87 g/mol EC-No.: 231-131-3
Molecular formula: Ag
Hill
No hazardous product as specified in Directive 67/548 EEC.
After inhalation (particles, dust): fresh air.

After skin contact: wash off with plenty of water.
After eye contact(particles, dust): rinse out with plenty of water with the eyelid held wide open,
summon eye specialist if necessary..
After swallowing: make victim drink water, avoid vomiting, summon doctor.
Suitable extinguishing media:

In adaption to materials stored in the immediate neighbourhood.
Special risks:
Non-combustible.
Person-related precautionary measures:

Avoid generation of dusts; do not inhale dusts.
Procedures for cleaning/absorption:
Take up dry mechanically. Forward for recycling.
Handling:
No further requirements
Storage:
Tightly closed. Dry. Storage temperature: no restrictions
Page 1 of 4
Safety data sheet
Product name: Silver wool
Personal control parameter:
German regulations:
MAK Germany (max. workplace conc.)
Name: Silver
Value 0.1 mg/m³ inhalable dust
Peak limit III resorptive substance, 10 x TLV
Embryotoxic cat. IIc classification not still possible in A-D categories
Personal protective equipment:

Protective clothing should be selected specifically for the working place, depending on concentration and
quantity of the hazardous substances handled. The resistance of the protective clothing to chemicals should
be ascertained with the resptective supplier.
Respiratory protection: required when dusts are generated

Eye protection: required
Hand protection: use recommended
Industrial hygiene
Wash hands after working with substance.
Change contaminated clothing. Wash hands after working with substance.
Form: solid
Colour: silver grey
Odour: odourless
pH-value: not available
Melting temperature: 960.5 °C

Boiling temperature: 2212 °C
Ignition temperature: not available

Flash point: not available
Explosion limits lower not available

upper not available
Density (15 °C) 10.49 g/cm3

Bulk density ~145 kg/m³
Solubility in
water (20 °C) insoluble
Page 2 of 4
Safety Data Sheet
Conditions to be avoided
no information available
Substances to be avoided
Acetylidene, azides, alcohols/nitric acid, ethylene oxide, peroxi compounds, hydrogen peroxide
organic substances, ammonium compounds, halogen-halogen compounds, fluorine, oxalic acid, ozone,
performic acid, zinc.
Hazardous decomposition products:

11. Toxicological Information
Acute toxicity
Quantitative data on the toxicity of this product are not available.
Subacute to chronic toxicity

Checks into the substance have so far not disclosed any investigations conerning
possible teratogenic effects.
Further toxicological information.

Hazardous properties cannot be excluded, but are relatively improbable due to the
compound’s poor water solubility.
Further data
The product should be handled with the care ususal when dealing with chemicals.
Ecotoxic effects:
Quantitative data on the ecological effect of this product are not available.
Further ecological data:

No ecological problems are to be expected when the product is handled and used with due care and
attention.
Product:
There are no uniform EC regulations for the disposal of chemicals or residues. Chemical residues
generally count as special waste. The disposal of the latter is regulated in the EC member countries
through corresponding laws and regulations. We recommend that you contact either the authorities
in charge or approved waste disposal companies which will advise you on how to dispose of special waste.
Packaging:
Disposal in compliance with official regulations. Handle contaminated packaging in the same way
as the substance itself. If not officially specified differently, non-contaminated packaging may be
treated like household waste or recycled.
Page 3 of 4
Safety data sheet
Not subject to transport regulations.
Labelling according to EC Directives

Symbol: -
R-Phrases: -
S-Phrases: -
Reason for alteration

Change in the chapter on first aid measures.
General update.
Regional representation:
This information is given on the authorised Safety Data Sheet for your contry.
Page 4 of 4
Safety data sheet Art.-No.: 03 679 908
1. Identification of the substance/preparation and

Identifacation of the product Supplier:

Elementar Analysensysteme GmbH,
Product name: Quartz wool, 10 g Donaustr.7, D-63452 Hanau
Tel.: 06181-9100-0, Fax: 06181-9100-10
Manufacturer/supplier identification e-mail: info@elementar.de
Company: Westdeutsche Quarzschmelze GmbH&CoKG, Borsigstr. 1-7, D-21502 Geesthacht
2. Composition/information on ingredients
Molecular formula: SiO2, 99,99 %
Special care for eyes and respiration
after inhalation: /
after contact with skin: wash with water
after contact with eyes: wash with water
after swallowing: /
Suitable extinguishing media:
Special risks: /
Other instructions: Non-combustible
Special personal protection:

Caution when stamping, pushing and pressing. The smallest, sharp parts of the quartz glass wool (in the
µm range) may cause cuts and skin injuries
Procedure for cleaning/taking up

Take up dry/disposal/final cleaning
Handling:
No further requirements
Storage:
Store tightly closed.
Page 1 of 3
Safety Data Sheet
Product Name: Quartz wool
Personal protective equipment
Respiratory protection: required when dust raises

Eye protection: required
Hand protection: required
Industrial hygiene:
Special care for eyes and respiration
Form: solid
colour: white-transparent
Odour: odourless
pH-value: not available
Melting temperature : 1730 °C

Boiling temperature : /
Ignition temperature : /
Flash poit : /
Explosion limits lower /

upper /
Density (20 °C) 0,001 g/cm3

Bulk density /
Solubility in
Water (20 °C) /
Conditions to be avoid
Substances to be avoided
with acetylidene, azides alcohols/nitric acid, ethylene oxide, peroxi compounds, organic substances.
Hazardous decomposition products

Page 2 of 3
Safety Data Sheet
Product Name: Quartz wool
11. Toxicological information
acute toxicity
Quantitative data regarding toxicity of this product are not available.
Ecotoxical effect:
no spezific information
Other ecological informations:

No ecological problems are to be exected.
Product: household waste
Not subject to transport regulations
Labelling according to EC Directives

Symbol: Xn
Name: Injurious to health
R-phrases: /
S-phrases: /
none
Page 3 of 3

LiquiTOCi Manual Operation

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Ident-Nr. 35.

High Temperature TOC/TNb Analyzer

starting with serial-no.35 04 3041

Elementar Analysensysteme GmbH, Donaustraße 7, D-63452 Hanau-Germany

1. Scope of delivery 1-1

2. Specifications and technical data 2-1

3. Safety instructions 3-1

4. Installation and start-up 4-1

5. Performance of a measuring series 5-1

6. Despription of the analysis modes 6-1

03/2003 Operating instructions liquiTOC

7. liquiTOC software description 7-1

9. Maintenance / Replacement of consumables 9-1

10. Appendix A-1

Operating instructions liquiTOC 01/2004

♦ control- and evaluation unit ♦ control and evaluation unit

♦ printer with printer cable

♦ O2 pressure reducing valve for synthetic air or oxygen

03/2003 Operating instructions liquiTOC

♦ Automatic sample feeder

order no. 34.00-0115

♦ Sample magazine 53 for automatic sample feeder

order no. 05 001 305

order no. 35.00-0001

♦ Set of small parts

order no. 35.00-0069

Operating instructions liquiTOC 03/2003

2. Specifications and technical data

according to DIN 38409 H3, ISO 8245, EPA 415.1

working range 0-10,000 mg/l C,

liquiTOCtrace: 0-200 mg/l C

sample volume 0.05 to 4 ml, depending on concentration range

particle size up to approx. 200 µm

duration of analysis 6 to 22 minutes,

sample digestion dynamic combustion at 850°C,

data storage respectively storage on hard disc or discette,

01/2004 Operating instructions liquiTOC

2.2 Technical data

detector 1 cuvette multi-channel IR-detector

Operating instructions liquiTOC 03/2003

Please adhere to the safety instructions and only operate

03/2003 Operating instructions liquiTOC

• The installation room must be well ventilated!

03/2003 Operating instructions liquiTOC

4. Installation and start-up

4.1 Preparations for operation

4.1.1 Working environment

placement area type of protection: IP 20

space requirement entire surface area

09/2004 Operating instructions liquiTOC

Ambient temperature constant temperature

The installation room must be well ventilated! The

Operating instructions liquiTOC 09/2004

4.1.2 Necessary gases and chemicals

When handling chemicals observe the safety

reagents • deionized water (C-content < 1 mg/l)

calibration standards Potassium hydrogen phtalate (KHP),

4.2 Instrument installation

The walls of the liquiTOC should only be opened by

The design of the basic unit of the liquiTOC is as follows:

4.2.1 Front of the unit

09/2004 Operating instructions liquiTOC

illustration 4.1: front view (behind door)

Operating instructions liquiTOC 09/2004