743 Rancimat: Manual

743 Rancimat
Manual
8.743.8003EN / 2019-09-25
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com
743 Rancimat
Manual
8.743.8003EN / 2019-09-25
Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.

This documentation has been prepared with great care. However, errors
can never be entirely ruled out. Please send comments regarding possible
errors to the address above.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.2 Rancimat method ................................................................. 2
1.3 About the documentation ................................................... 3
1.3.1 Symbols and conventions ........................................................ 3
1.4 Safety instructions ................................................................ 4
1.4.1 General notes on safety ........................................................... 4
1.4.2 Electrical safety ........................................................................ 5
1.4.3 Flammable solvents and chemicals ........................................... 6
1.4.4 Recycling and disposal ............................................................. 6
2 Overview of the instrument 7

3 Installation 10
3.1 Setting up the instrument .................................................. 10
3.1.1 Packaging .............................................................................. 10
3.1.2 Checks .................................................................................. 10
3.1.3 Location ................................................................................ 10
3.2 Mounting accessories ......................................................... 10
3.2.1 Mounting accessories for the internal air supply ..................... 10
3.2.2 Mounting accessories for the external air supply .................... 13
3.2.3 Equipping the reaction and measuring vessels ........................ 13
3.2.4 Inserting vessels / Establishing tubing connections ................. 16
3.2.5 Mounting the exhaust collection tube (optional accessories) .. 17
3.3 Mains connection ............................................................... 17
3.3.1 Checking the mains voltage ................................................... 18
3.3.2 Replacing fuses ...................................................................... 18
3.3.3 Connecting the instrument to the power grid ........................ 19
3.3.4 Switching the instrument on/off ............................................ 19
3.4 Connecting a PC ................................................................. 20
3.4.1 Connecting the 743 Rancimat and the PC .............................. 20
3.4.2 Installing the software ........................................................... 20
3.4.3 Carrying out basic settings ..................................................... 22
4 Operation 25
4.1 Fundamentals of operation ............................................... 25
4.1.1 Starting and exiting the program ........................................... 25
4.1.2 Terms .................................................................................... 26
4.1.3 Control window .................................................................... 26
4.1.4 Results window ..................................................................... 28
4.1.5 File types ............................................................................... 31
4.1.6 Context-sensitive menus ........................................................ 32
743 Rancimat ￭￭￭￭￭￭￭￭ III

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4.1.7 Mouse functions .................................................................... 32

4.1.8 Help ...................................................................................... 33
4.2 Instrument and Program Settings ..................................... 34
4.2.1 Establishing the instrument communication ........................... 34
4.2.2 Managing access rights ......................................................... 35
4.2.3 Timer ..................................................................................... 38
4.2.4 Gas flow control .................................................................... 40
4.2.5 Recording the temperature .................................................... 41
4.2.6 Optimizing program and database ......................................... 42
4.3 Program information .......................................................... 43
4.3.1 Instrument information .......................................................... 43
4.3.2 Status overview ..................................................................... 45
4.3.3 Displaying, filtering and deleting event overview .................... 46
4.4 Calibration functions .......................................................... 49
4.4.1 Determining cell constants ..................................................... 49
4.4.2 Determining Delta T ............................................................... 51
4.5 Methods .............................................................................. 56
4.5.1 Managing methods ............................................................... 56
4.5.2 Parameter description ............................................................ 61
4.6 Determinations ................................................................... 76
4.6.1 Preparing samples ................................................................. 77
4.6.2 Preparing the instrument and the accessories ......................... 80
4.6.3 Preparing the determination .................................................. 82
4.6.4 Starting the determination ..................................................... 84
4.6.5 Cleaning the instrument and accessories ................................ 84
4.6.6 Adjusting the method parameters during the determination .. 85
4.6.7 Stopping the determination manually .................................... 86
4.6.8 Status of the live curve ........................................................... 87
4.7 Results ................................................................................. 88
4.7.1 Determination overview ......................................................... 88
4.7.2 Determination and method data .......................................... 104
4.7.3 Graph and reevaluation ....................................................... 113
4.7.4 Extrapolation ....................................................................... 118
4.7.5 Recalculating a determination .............................................. 122
4.7.6 Printing and exporting data ................................................. 129
4.7.7 Program settings .................................................................. 136
4.7.8 Arranging windows ............................................................. 142
4.8 GLP functions .................................................................... 143
4.8.1 General information on GLP and validation .......................... 143
4.8.2 GLP monitoring ................................................................... 143
4.8.3 GLP status ........................................................................... 145
4.8.4 Carrying out GLP tests ......................................................... 146
4.8.5 GLP results ........................................................................... 156
IV ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
5 Handling and maintenance 160

5.1 General information ......................................................... 160
5.1.1 Care .................................................................................... 160
5.1.2 Maintenance by Metrohm Service ........................................ 160
5.2 Replacing the dust filter .................................................. 161
5.3 Regenerating or replacing the molecular sieve ............. 161
5.4 Self test when switching on ............................................ 162
6 Troubleshooting 163
6.1 Problems ........................................................................... 163
7 Technical specifications 169

7.1 General data ..................................................................... 169
7.2 Temperature regulation and measurement .................... 169
7.3 Conductivity measurement .............................................. 170
7.4 Gas flow regulation .......................................................... 170
7.5 GLP test set ....................................................................... 171
7.6 RS-232 interface ............................................................... 171
7.7 Mains connection ............................................................. 171
7.8 Ambient temperature ....................................................... 172
7.9 Housing ............................................................................. 172
8 Accessories 173
Index 174
743 Rancimat ￭￭￭￭￭￭￭￭ V

Table of figures ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Table of figures
Figure 1 Measuring arrangement (schematic representation) ........................... 3
Figure 2 Front 743 Rancimat ........................................................................... 7
Figure 3 Rear 743 Rancimat ............................................................................ 8
Figure 4 Mounting accessories for the air supply (rear of the instrument) ...... 11
Figure 5 Equipping the reaction and measuring vessels ................................. 14
Figure 6 Equipping the reaction vessel for determining Delta T ...................... 52
Figure 7 Accessories for GLP test Temperature ............................................ 146
VI ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
1 Introduction
1.1 Instrument description

The 743 Rancimat is a PC-controlled measuring device for determining the
oxidation stability of samples containing oil and fat.
It is equipped with two heating blocks each with 4 measuring positions
(channels). Every block can be heated individually, i.e. 4 samples can each
be measured at 2 different temperatures or 8 samples at the same tem-
perature. The measurements at the individual measuring positions can be
started individually for this.
Operation of the 743 Rancimat is realized completely via a PC connected
to the RS-232 interface using the control and evaluation program 743
Rancimat. Up to 4 instruments can be connected to each PC, hence
allowing a maximum of 32 samples to be analyzed. The evaluation algo-
rithm of the PC program determines the break point of the Rancimat curve
fully automatically and hence the induction time. Besides the induction
time, the so-called stability time, i.e. the time duration until attaining a
defined conductivity change, can also be determined. In the case of con-
ductivity changes (stages) which do not have anything to do with the
autoxidation, the evaluation can be interrupted for definite time intervals.
The results determined can be processed further by computer. In particu-
lar, the induction times can be converted to the default temperatures of
the corresponding standards.
Each Rancimat curve can also be evaluated manually. A PC-supported
tangential method is available for this, in which you can position the tan-
gents anywhere on your curves. This makes evaluations possible in
extreme cases as well.
The results of the determinations are saved in a database together with
all methods and determination data. Determinations can be searched for,
sorted, filtered, exported and printed in the program part for the results
display. Besides the graphic display of single and multiple curves, recalcula-
tion with altered parameters and extrapolation of the results to a definite
temperature is also possible.
GLP (Good Laboratory Practice) and instrument validation are becoming
increasingly important. The 743 Rancimat enables GLP tests for tempera-
ture, conductivity and gas flow measurement. You determine whether and
which tests have to be carried out. You can also specify the time interval
between the tests as well as the requirements regarding accuracy. If the
GLP function has been selected, each result report will receive a comment
743 Rancimat ￭￭￭￭￭￭￭￭ 1

1.2 Rancimat method ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
stating whether the GLP tests have been fulfilled. Metrohm offers a GLP
test set to carry out these tests .
1.2 Rancimat method

The decay of vegetable and animal fats, which can be perceived in the ini-
tial stage through a deterioration of odor and taste (rancidity), is to a great
extent the result of chemical alterations caused by the effect of atmos-
pheric oxygen. These oxidation processes progressing slowly at ambient
temperatures are referred to as autoxidation. They start with radical
reactions on unsaturated fatty acids and undergo a process involving mul-
tiple stages resulting in diverse decomposition products, in particular per-
oxides as primary oxidation products and alcohols, aldehydes and carbox-
ylic acids as secondary oxidation products.
With the Rancimat method, the sample is exposed to an air flow at a
constant temperature between 50…220 °C (see figure 1, page 3).
Highly volatile, secondary oxidation products (for the most part formic
acid) are transferred into the measuring vessel with the air flow, where
they are absorbed in the measuring solution (distilled water). Here the
conductivity is continuously registered. The organic acids can thus be
detected by increasing the conductivity. The time until occurrence of these
secondary reaction products is referred to as the induction time or induc-
tion period, which is a good indicator for the oxidation stability.
The Rancimat method has been developed as an automated variant to the
extremely complex AOM (active oxygen method) for determining the
induction time of fats and oils. This method has become established
over the course of time and has been incorporated in various national and
international standards, e.g. AOCS Cd 12b-92 and ISO 6886.
2 ￭￭￭￭￭￭￭￭ 743 Rancimat

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Measuring
vessel
Conductivity
measuring cell
Measuring
solution
Reaction vessel
Sample
Heating block
Figure 1 Measuring arrangement (schematic representation)
1.3 About the documentation
CAUTION
Please read through this documentation carefully before putting the

instrument into operation. The documentation contains information
and warnings which have to be followed by the user in order to ensure
safe operation of the instrument.
1.3.1 Symbols and conventions

The following symbols and styles are used in this documentation:
Cross-reference to figure legend

The first number refers to the figure number, the sec-
ond to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
743 Rancimat ￭￭￭￭￭￭￭￭ 3

1.4 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
[Next] Button or key

Warning
This symbol draws attention to a possible life hazard
or risk of injury.
Warning
This symbol draws attention to a possible hazard due
to electrical current.
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.
Note
This symbol marks additional information and tips.
1.4 Safety instructions

1.4.1 General notes on safety
WARNING
Operate this instrument only according to the information contained in

this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
Hot reaction vessels
WARNING
The reaction vessels can become very hot.

Avoid any contact with the hot reaction vessels. Place these in the ves-
sel holders provided for cooling down.
4 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
Flammable substances
WARNING
The heating block of the 743 Rancimat can be heated to 229.9 °C.
Flammable substances may ignite at such temperatures.
Adjust the oven's maximum heating temperature to the sample that is
to be analyzed.
Defective glass vessels
WARNING
Caution with defective glass vessels.

An overflow of flammable samples into the heating block can be dan-
gerous.
Check the glass vessels before each use.
1.4.2 Electrical safety

The electrical safety when working with the instrument is ensured as part
of the regulations IEC 1010-1 (protection class 1, degree of protection
IP20).
WARNING
Only personnel qualified by Metrohm are authorized to carry out service

work on electronic components.
WARNING
Never open the housing of the instrument. The instrument could be

damaged by this. There is also a risk of serious injury if live components
are touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
743 Rancimat ￭￭￭￭￭￭￭￭ 5

1.4 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Mains voltage
WARNING
An incorrect supply voltage can damage the instrument.

Only operate this instrument with a supply voltage specified for it (see
rear panel of the instrument).
Protection against electrostatic charges
WARNING
Electronic components are sensitive to electrostatic charges and can be

destroyed by discharges.
Do not fail to pull the power cord out of the power socket before you
set up or disconnect electrical plug connections at the rear of the
instrument.
1.4.3 Flammable solvents and chemicals
WARNING
All relevant safety measures are to be observed when working with

flammable solvents and chemicals.
￭ Set up the instrument in a well-ventilated location (e.g. fume cup-
board).
￭ Keep all sources of flame far from the workplace.
￭ Clean up spilled liquids and solids immediately.
￭ Follow the safety instructions of the chemical manufacturer.
1.4.4 Recycling and disposal

This product is covered by European Directive 2012/19/EU, WEEE – Waste
Electrical and Electronic Equipment.
The correct disposal of your old instrument will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old instrument can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.
6 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument
2 Overview of the instrument

6
1
7
2 8
3 9
4 10
5
11
743 Rancimat
Figure 2 Front 743 Rancimat
1 Pilot lamp 2 Gas flow display

Lights up when the instrument is switched Flashes when the gas flow is switched on.
on. Lights up when the gas flow has been
reached.
3 Temperature display 4 Error display (red)

Flashes when the heating is switched on. Lights up or flashes when a fault has occur-
Lights up when the temperature has been red in the instrument (see Troubleshooting
reached. Chapter).
5 Instrument number display 6 FEP tubing 250 mm (6.1805.080)

Indicates the number of the instrument. For supplying air into the reaction vessel.
Lights up if the instrument is registered.
Flashes (all LEDs) if the connection to the PC
is interrupted.
7 Measuring vessel cover (6.0913.130) 8 Measuring vessel (6.1428.100)

Contains an integrated conductivity measur-
ing cell.
743 Rancimat ￭￭￭￭￭￭￭￭ 7

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
9 Silicone tubing (6.1816.010) 10 Reaction vessel cover (6.2753.107)

For connecting the reaction vessel to the
measuring vessel.
11 Reaction vessel (6.1429.040)
1
2
Molecular sieve flask
Made by Metrohm Herisau Switzerland Filter
Type:
Nr.: f:
U: S:
From To
flask flask
Air out
Fuse
100-115V: 4A(TH) RS 232 Pt 100
220-240V: 2A(TH)
Air/N 2in
WARNING - Fire Hazard -
For continued protection replace only
with the same type and rating of fuse
4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Figure 3 Rear 743 Rancimat
1 Collection tube holder 2 Electrode connector

For fastening the optional exhaust collection For connecting the conductivity measuring
tube (6.2757.000). cell integrated in the measuring vessel cover
(2-7).
3 Air supply connection 4 Mains switch

For connecting the FEP tubing 250 mm For turning the instrument on and off.
(2-6). I = ON / 0 = OFF.
5 Mains connection socket 6 Fuse holder

For important information on the mains con- Replacing fuses, see Chapter 3.3.2.
nection, see Chapter 3.3.
7 Type plate 8 RS-232 connector

Contains specifications concerning mains For connecting the PC.
voltage and serial number.
8 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument
9 Pt100 connector 10 Drying flask cover (6.1602.145)

For connecting an external temperature sen- Cover for the drying flask.
sor.
11 Drying flask (6.1608.050) 12 Flask holder

For fastening the drying flask.
13 FEP tubing 250 mm (6.1805.080) 14 FEP tubing 250 mm (6.1805.080)

For supplying the air from the internal pump For supplying the air from the drying flask to
to the drying flask. the reaction vessel (2-11).
15 "From Flask" connection 16 "Air/N2 in" connection
17 FEP tubing 130 mm (6.1805.010) 18 "Air out" connection

For connecting the Air out connection to
the Air/N2 in connection during normal
operation with the internal air pump.
19 "To Flask" connection 20 Dust filter (6.2724.010)
743 Rancimat ￭￭￭￭￭￭￭￭ 9

3.1 Setting up the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
3 Installation
3.1 Setting up the instrument

3.1.1 Packaging
The instrument is supplied in protective packaging together with the sepa-
rately packed accessories. Keep this packaging, as only this ensures safe
transportation of the instrument.
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory suitable for operation
and free of vibrations, if possible protected from corrosive atmospheres
and contamination by chemicals.
The instrument should be protected against excessive temperature fluctua-
tions and direct sunlight.
NOTICE
In order to improve accessibility for the measuring positions, the instru-

ment can be placed on the optionally available 6.2059.000 turning ring.
3.2 Mounting accessories

3.2.1 Mounting accessories for the internal air supply
The gas in the Rancimat is normally supplied using the internal air
pump, which sucks in laboratory air. For air supply and air purification,
the following accessories must be mounted on the rear of the Rancimat:
10 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
Molecular sieve flask

8
Filter
1
From To 9
flask flask
2
Air out
10
3
11
Air/N2 in
12
4 5 6 7
Figure 4 Mounting accessories for the air supply (rear of the instru-
ment)
1 Drying flask cover (6.1602.145) 2 Drying flask (6.1608.050)

Cover for the drying flask.
3 Flask holder 4 Filter tube (6.1821.040)

For fastening the drying flask.
5 FEP tubing 250 mm (6.1805.080) 6 FEP tubing 250 mm (6.1805.080)

For supplying the air from the internal pump For supplying the air from the drying flask to
to the drying flask. the reaction vessel (2-11).
7 "From Flask" connection 8 Dust filter (6.2724.010)
9 "To Flask" connection 10 "Air out" connection
11 FEP tubing 130 mm (6.1805.010) 12 "Air/N2 in" connection
Mount the accessories for the air supply as follows:
1 Mount dust filter

￭ Insert the dust filter (4-8) on the connection marked with Filter
on the rear of the Rancimat.
￭ If the laboratory air is heavily contaminated, a tubing for supply-
ing fresh air can be connected to the dust filter.
743 Rancimat ￭￭￭￭￭￭￭￭ 11

3.2 Mounting accessories ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
NOTICE
The dust filter serves for filtering the air sucked through the air
pump and must be replaced at periodic intervals (see chapter 5.2,
page 161).
2 Mount drying flask
CAUTION
Do not fill the hot molecular sieve directly into the drying flask
after regeneration, as otherwise the plastic filter on the filter tube
will melt.
Wait until the molecular sieve has cooled down before filling.
￭ Fill the molecular sieve into the drying flask (4-2).

￭ Screw the filter tube (4-4) on the lower side of the drying flask
cover (4-1) into the opening marked (above) with a dot.
￭ Screw the drying flask cover with mounted filter tube onto the
drying flask and insert in the flask holder (4-3) on the rear of the
Rancimat.
￭ Screw the one end of the FEP tubing 250 mm (4-6) onto that
opening on the drying flask cover at the bottom of which the fil-
ter tube is located.
￭ Screw the other end of the FEP tubing onto the From flask con-
nection (4-7) on the rear of the Rancimat.
￭ Screw the one end of the second FEP tubing 250 mm (4-5) onto
the second opening on the drying flask cover.
￭ Screw the other end of the second FEP tubing onto the To flask
connection (4-9).
NOTICE
The molecular sieve serves for adsorbing interfering oxidizing gases

as well as water from the sucked in air. You can regenerate it in
the drying oven at +140…+180 °C for 24 to 48 h (see chapter
5.3, page 161).
3 Mount the FEP tubing for the supply air

￭ Screw the one end of the FEP tubing 130 mm (4-11) onto the Air
out connection (4-10).
12 ￭￭￭￭￭￭￭￭ 743 Rancimat

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￭ Screw the other end of the FEP tubing onto the Air/N2 in con-
nection (4-12).
3.2.2 Mounting accessories for the external air supply

If the laboratory air is heavily contaminated, an external gas supply with
synthetic air can be provided. For this, the corresponding accessories must
be mounted on the rear of the Rancimat.
Mount the accessories for the external air supply as follows:
1 Mount the FEP tubing

￭ Screw the one end of the FEP tubing 130 mm (4-11) onto the
Air/N2 in connection (4-12) on the rear of the Rancimat.
￭ Screw the tubing adapter M6 / olive (6.1808.020) onto the other
end of the FEP tubing.
2 Connect the gas supply

￭ Mount the gas supply from the bomb with synthetic air onto the
tubing adapter M6 / olive (6.1808.020).
NOTICE
With an external gas supply, the gas flow cannot be regulated in the PC
program. The gas flow must be set manually using the reducing valve
and the gas flow display (see chapter 4.2.4, page 40).
3.2.3 Equipping the reaction and measuring vessels

The following figure shows in detail, how the accessories parts for mea-
suring the oxidation stability have to be mounted and connected to one
another.
743 Rancimat ￭￭￭￭￭￭￭￭ 13

2
11
12
13
3
14
4
5 15
6
16
7
8 17
18
9
19
10
20
Figure 5 Equipping the reaction and measuring vessels
1 FEP tubing 250 mm (6.1805.080) 2 Silicone tubing (6.1816.010)

For supplying air into the reaction vessel. For connecting the reaction vessel to the
measuring vessel.
3 Thread adapter M8 / M6 (6.1808.090) 4 Tubing connector

For connecting the silicone tubing.
5 Air tube (6.2418.100) 6 O-ring (6.1454.040)
7 Connection 8 Reaction vessel cover (6.2753.107)

For connecting the thread adapter M8 / M6.
9 Foam barrier (6.1451.010) 10 Reaction vessel (6.1429.040)
11 Tubing adapter M8 / olive (6.1808.050) 12 Opening "Out"

For connecting the silicone tubing to the For removing the air from the measuring
opening In (5-13). vessel.
13 Opening "In" 14 Labeling field

For supplying the air to the measuring ves- For entering the cell constant.
sel.
14 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
15 Connector plug 16 Measuring vessel cover (6.0913.130)

Contains integrated conductivity measuring
cell.
17 PTFE tube (6.1819.080) 18 Electrode

For supplying the air to the measuring solu-
tion.
19 Protection ring 20 Measuring vessel (6.1428.100)
Proceed as follows to mount the measuring and reaction vessel:
1 Mount the measuring vessel cover

￭ Insert the PTFE tube (5-17) from above into the opening In (5-13)
of the measuring vessel cover.
￭ Screw the tubing adapter M8 / olive (5-11) into the opening In of
the measuring vessel cover.
￭ Place the measuring vessel cover (5-16) on the measuring vessel
(5-20).
2 Mount the reaction vessel cover

￭ Insert the air tube (5-5) from below into the connection (5-7) of
the reaction vessel cover.
￭ Place the O-ring (5-6) over the upper end of the air tube.
￭ Screw the thread adapter M8 / M6 (5-3) gently into the connec-
tion (5-7) and, at the same time, press the air tube against the
thread adapter M8 / M6.
￭ Now fix the air tube onto the reaction vessel cover by firmly pull-
ing the thread adapter M8 / M6.
￭ If determinations are carried out with highly foaming samples,
clamp the foam barrier (5-9) onto the air tube.
￭ Place the reaction vessel cover on the reaction vessel.
WARNING
The foam barrier can melt if it projects too deeply into the heating
block.
Ensure that the foam barrier is at least 7 cm above the base of the
reaction vessel.
743 Rancimat ￭￭￭￭￭￭￭￭ 15

3.2.4 Inserting vessels / Establishing tubing connections

After you have assembled the reaction and measuring vessels, insert them
in the Rancimat and establish the tubing connections as follows:
1 Insert the measuring vessel

￭ Fill the measuring vessel (5-20) with distilled water.
￭ Place the measuring vessel cover on the measuring vessel.
￭ Insert the measuring vessel into the openings provided on the
Rancimat. At the same time, carefully insert the connector plugs
(5-15) into the electrode connector (3-2).
￭ Connect the white silicon tubing (5-2) to the tubing adapter
M8 / olive (5-11) of the measuring vessel cover.
2 Mount the tubings for the air supply

￭ Screw the FEP tubings 250 mm onto the air supply connections
(3-3) of the Rancimat.
3 Insert the reaction vessel

￭ Fill the reaction vessel (5-10) with the sample.
￭ After reaching the required temperature, insert the reaction vessel
with the mounted reaction vessel cover in the openings provided
on the Rancimat.
4 Establish the tubing connections

￭ Connect the white silicone tubing (5-2), which is fastened on the
measuring vessel cover, to the tubing connector (5-4) of the reac-
tion vessel cover.
￭ Screw the FEP tubing 250 mm (5-1), which is fastened on the
tubing adapter M8 / olive (5-11) of the Rancimat, onto the thread
adapter M8 / M6 (5-3) of the reaction vessel cover.
NOTICE
Instead of the measuring vessel 6.1428.100 made from polycarbonate,

the optionally available measuring vessel 6.1428.020 made from clear
glass can be used. In contrast to the polycarbonate vessel, the measur-
ing vessel 6.1428.020 can also be cleaned with acetone.
16 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
3.2.5 Mounting the exhaust collection tube (optional accessories)

The optionally available exhaust collection tube 6.2757.000 can be moun-
ted on the 743 Rancimat for targeted removal of the exhaust air. In addi-
tion to the exhaust collection tube, 8 silicone tubings 6.1816.010
(220 mm) also have to be ordered.
Proceed as follows to mount the collection tube:
1 Mount the exhaust collection tube

￭ Insert the exhaust collection tube with both nozzles into the col-
lection tube holders (3-1) on the Rancimat in such a way that the
connection to the exhaust air removal is located to the rear.
2 Connect the measuring vessels

￭ Screw the tubing adapter M8 / olive (5-11) into the opening Out
(5-12) of the measuring vessel cover.
￭ Connect the one end of the silicone tubing (5-2) to the tubing
adapter M8 / olive.
￭ Insert the other end of the silicone tubing into the corresponding
opening on the collection tube.
￭ Seal the unused openings on the collection tube with the
enclosed plugs E.400.0010.
3 Connect the exhaust collection tube

￭ Connect a suitable tubing to the connection of the exhaust collec-
tion tube and connect this to an active suction device (e.g. water
jet pump).
3.3 Mains connection
WARNING
There is a risk of fire if the instrument is operated with an incorrect

mains fuse!
Follow the regulations below for the mains connection.
743 Rancimat ￭￭￭￭￭￭￭￭ 17

3.3 Mains connection ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
3.3.1 Checking the mains voltage

Before switching the 743 Rancimat on for the first time, check whether
the mains voltage indicated on the type plate (3-7) corresponds to the
mains voltage present. If this is not the case, please contact Metrohm Ser-
vice.
3.3.2 Replacing fuses

Two fuses 4 A (slow-acting) for 115 V or 2 A (slow-acting) for 230 V are
installed in the fuse holder (3-6) of the 743 Rancimat as standard.
WARNING
Ensure that the instrument is never put into operation with fuses of
another type, otherwise there is a risk of fire!
Proceed as follows to replace defective fuses:
1 Pull out the mains cable

￭ Pull the mains cable out of the mains connection socket of the
Rancimat.
2 Remove the fuse holder

￭ Use a screwdriver to loosen and completely pull out the fuse
holder (3-6) above the mains connection socket.
3 Replace fuses
￭ Carefully take the defective fuses out of the fuse holder and
replace them with two new fuses suitable for the set mains volt-
age of the type TH (slow-acting, with high switching capacity):
– 115 V 4 A (TH) Metrohm No.: U.600.0022
– 230 V 2 A (TH) Metrohm No. U.600.0107
4 Insert the fuse holder

￭ Push the fuse holder back into the instrument until it latches into
place.
18 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
3.3.3 Connecting the instrument to the power grid
WARNING
Electric shock from electrical potential

Risk of injury by touching live components or through moisture on live
parts.
￭ Never open the housing of the instrument while the power cord is
still connected.
￭ Protect live parts (e.g. power supply unit, power cord, connection
sockets) against moisture.
￭ Unplug the power plug immediately if you suspect that moisture has
gotten inside the instrument.
￭ Only personnel who have been issued Metrohm qualifications may
perform service and repair work on electrical and electronic parts.
Connecting the power cord
Accessories Power cord with the following specifications:

￭ Length: max. 2 m
￭ Number of cores: 3, with protective conductor
￭ Instrument plug: IEC 60320 type C13
￭ Conductor cross-section 3x min. 0.75 mm2 / 18 AWG
￭ Power plug:
– according to customer requirement (6.2122.XX0)
– min. 10 A
NOTICE
Do not use a not permitted power cord!
1 Plugging in the power cord

￭ Plug the power cord into the instrument's power socket.
￭ Connect the power cord to the power grid.
3.3.4 Switching the instrument on/off

The Rancimat is switched on and off using the mains switch. When
switching the instrument on, the pilot lamp ON lights up on the front of
the instrument auf.
743 Rancimat ￭￭￭￭￭￭￭￭ 19

3.4 Connecting a PC ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
3.4 Connecting a PC
3.4.1 Connecting the 743 Rancimat and the PC
CAUTION
Always switch the Rancimat and PC off before you connect the two
devices with the RS-232 cable 6.2134.100.
The PC program 743 Rancimat allows control of max. 4 instruments. The

following options are available for connecting the instruments to serial PC
interfaces:
￭ Connection to integrated COM interfaces of the PC
￭ Connection to an additional integrated interface expansion card
Connect the RS-232 interface of the Rancimat to the required serial COM
port on the PC using the RS-232 cable 6.2134.100 (9-pin/9-pin). For 25-
pin COM ports, the optional RS-232 cable 6.2125.110 (not in the scope of
delivery) or a commercially available adapter must be used.
3.4.2 Installing the software

3.4.2.1 System requirements
Operating system Windows 2000, Windows XP Professional, Win-
dows Vista
RAM 256 MB (Windows 2000 / Windows XP)
1 GB (Windows Vista)
Processor Pentium III or higher
Memory approx. 20 MB for program files
RS-232 interface one free RS-232 interface (COM)
The windows user must have administrator rights in order to be able to
install 743 Rancimat.
20 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
3.4.2.2 Installing the program

Proceed as follows to install 743 Rancimat:
1 Start the installation program

￭ Place the installation CD in the CD drive. The installation program
is started automatically.
If this option is deactivated on your computer, double click the file
Setup.exe.
Windows Vista: Select the option "Approve".
￭ Click on 743.
2 Select the dialog language

￭ Select the dialog language of the program.
￭ Click on the [OK] button.
￭ Click on the [Next >] button.
3 Accept the license agreement

￭ Read through the license agreement and accept it with [Yes].
4 Define a target folder for the program

￭ If required, choose another folder than the default target folder
for the program files. For that, click on the [Browse...] button.
￭ Confirm the target folder with [Next >].
5 Define the components of the program

￭ Click on the [Next >] button.
6 Define a target folder for the program icon

￭ Choose or enter the program folder of the Start menu in which
the program icon is to be inserted and confirm with [Next >].
The program will be installed.
7 Complete the installation

￭ Click on the [Finish] button after the successfully completed
installation.
The installation program will be exited.
743 Rancimat ￭￭￭￭￭￭￭￭ 21

3.4 Connecting a PC ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
3.4.2.3 Windows Vista
CAUTION
If you run the software 743 Rancimat on a computer with Windows

Vista, you need a special update in order to be able to display the help.
Due to licensing reasons you have to download this file from a Micro-
soft web page. On the installation CD the link "Download Win-
Help.url" to the corresponding Microsoft web page can be found in
the folder "Vista Update for HLP help". Download the necessary
installation file and save it.
Proceed as follows to install the update:
1 ￭ Exit 743 Rancimat if you have started the software after the instal-
lation.
￭ Start the installation file by double-clicking and follow the instruc-
tions of the installation program.
3.4.3 Carrying out basic settings
Setting the Administrator password
When starting the program for the first time, the Administrator password
must be set. Proceed as follows:
1 Switch on the instruments

￭ Check whether the Rancimat is correctly connected to the PC (see
chapter 3.4.1, page 20).
￭ Switch on the Rancimat using the mains switch.
￭ Switch on the PC.
2 Start program
￭ In the Windows Start menu under Pro-
grams ▶ Metrohm ▶ Rancimat, click on the menu item Ranci-
mat.
The login window for the Administrator opens:
22 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation
3 Set Administrator password

￭ Do not enter a password, instead click on [OK].
￭ Confirm the displayed message with [OK].
The following dialog window appears:
￭ Leave the Old password field empty.

￭ Enter a new password for the Administrator in the New pass-
word field.
￭ Reenter the password in the Confirm new password field and
confirm with [OK].
The dialog window Login opens again:
4 Log in as Administrator
￭ Enter the Administrator password set before in the Password
field and confirm with [OK].
￭ Confirm the message "There are no units configured yet!"
with [OK].
743 Rancimat ￭￭￭￭￭￭￭￭ 23

3.4 Connecting a PC ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Establishing the device communication
1 Follow the instructions in Section 4.2.1.
24 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
4 Operation
This section describes the most important points for operation of the 743
Rancimat.
You can find more detailed information in the Online help of the software,
which you can use to rapidly and easily call up the required information
everywhere, via [F1].
4.1 Fundamentals of operation

4.1.1 Starting and exiting the program
Proceed as follows to start and exit the program:
NOTICE
If you are starting the program for the first time, you first have to set an
Administrator password (see chapter 3.4.3, page 22).
1 Start program
mat.
2 Log in
￭ Select the required User.
￭ Enter the Password and confirm with [OK].
3 Close program
￭ Click on the menu item File ▶ Exit or the symbol in the upper
right corner of the dialog window.
743 Rancimat ￭￭￭￭￭￭￭￭ 25

4.1 Fundamentals of operation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
For opening and closing the Results window, see page 29.
4.1.2 Terms
Control window The main window 743 Rancimat Control is
called the control window. It contains all the
functions for monitoring and controlling the
Rancimats connected to the PC.
Method A method comprises all parameters for carrying
out and evaluating a determination.
Determination Determination refers to the automatic determi-
nation of the induction time and/or stability time
for a sample. In order to carry out a determina-
tion, a method suitable for the samples must be
selected.
Results The results of a determination are automatically
saved in the database Repos.mrd and can be
viewed in the Results window.
Reevaluation Reevaluation refers to the subsequent revision of
a determination, in particular the manual specifi-
cation of the induction time using tangents.
Recalculation The recalculation can be used to subsequently
recalculate results, formulas and standards.
Extrapolation Extrapolation can be used to convert the results
measured at various temperatures to a required
target temperature. In addition, the factor for
converting the induction time to the standard
time can be determined.
4.1.3 Control window

The dialog window 743 Rancimat Control serves for controlling the
devices, managing methods, displaying the live curves and accessing vari-
ous program functions. The dialog window opens automatically when the
program is started.
Structure
The elements of the Control window are the menu bar, the toolbar, the
control panel and the status bar.
26 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
An image of the Rancimat is shown in the Control panel, which can be

used for starting, displaying and stopping determinations.
The following information is shown in the status bar:
￭ a short description of the menu item highlighted in the menu bar
￭ the registered user
￭ the instrument status
Menus
The Control window contains the following main menus:
File Create new methods, open existing methods,
manage methods, open Results window, print,
new login, close program.
View Activate/Deactivate toolbar and status bar, dis-
play instrument information, change live param-
eters, display status overview, display event log-
ging, select instrument.
Tools Manage cell constants, perform GLP tests, set
timer, set gas flow control, start all channels,
determine Delta T, record temperature, perform
service diagnosis.
743 Rancimat ￭￭￭￭￭￭￭￭ 27

Options Carry out general settings, set instrument config-

uration, manage access rights.
Help Call up program-specific Online help.
Symbols
New method Create a new method (see chapter 4.5.1, page 56).
Open method Open an existing method (see chapter 4.5.1, page 56).
Method Manager Open, rename and delete methods (see chapter 4.5.1, page 56).
Print Print results (see chapter 4.7.6, page 129).
Results Open Results window (see "Opening and closing the Results window", page
29).
Live parameters Display live parameters which can be changed for a current determination (see
Status overview Display status overview for the instruments connected (see chapter 4.3.2, page
45).
Instrument informa-
tion Instrument information (see chapter 4.3.1, page 43).
GLP status Display GLP status (see chapter 4.8.3, page 145).
Instrument 1…4 Select instrument 1…4.
Start all channels

Block A Start all channels of Block A (see chapter 4.6.4, page 84).
Start all channels

Block B Start all channels of Block B (see chapter 4.6.4, page 84).
Help topics Call up the Online help.
4.1.4 Results window

The dialog window 743 Rancimat Results serves for displaying, output-
ting and recalculating results of the determinations recorded with the 743
Rancimat. The determination data is saved in database files *.mrd and can
be displayed in this dialog window in the form of overview tables and
curves. The Results window can also run if the Control window is closed.
28 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Opening and closing the Results window
Proceed as follows to open and close the Results window:
1 Open Results window

￭ In the dialog window 743 Rancimat Control, click on the menu
item File ▶ Results... or the symbol .
When opening the Results window, the database Repos.mrd is
automatically loaded, in which all recorded determinations are saved
by default.
2 Close Results window

￭ In the dialog window 743 Rancimat Results, click on the menu
item File ▶ Back or the symbol .
Structure
The elements of the Results window are the menu bar, the toolbar, the
subwindows (determination overview, live, single and multiple graphs)
and the status bar.
743 Rancimat ￭￭￭￭￭￭￭￭ 29

In the Results window subwindows with a determination overview, single,

multiple or live graphs can be opened.
Menus
The Results window contains the following main menus:
File Open database, print, close dialog window.
Edit Copy, select, delete content of the filter.
View View selection: determination overview, determi-
nation and method data, GLP.
Determination Search, sort, filter, display graphs, perform
extrapolation, perform recalculation, export
determinations, delete determinations.
Format Format determination overview.
Options Carry out general program settings.
Window Arrange subwindows.
Help Display program-specific Online help.
Symbols
The toolbar of the Results window contains the following symbols:
Print Print results, curves and overview lists (see chapter 4.7.6, page 129).
Copy Copy data to clipboard.
Select fields for

determination over-
view Format determination overview (see chapter 4.7.1, page 88).
Display determina-
tion overview Display determination overview (see chapter 4.7.1, page 88).
Display all methods

and determination Display all methods and determination data of the selected determination (see
data chapter 4.7.2, page 104).
Search Search in the database (see chapter 4.7.1, page 88).
Ascending Sort column in ascending order (see chapter 4.7.1, page 88).
Descending Sort column in descending order (see chapter 4.7.1, page 88).
Selection-based filter Filter by selection (see chapter 4.7.1, page 88).
30 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Special filter Define filter (see chapter 4.7.1, page 88).
Apply filter Apply filter (see chapter 4.7.1, page 88).
Remove filter Remove filter (see chapter 4.7.1, page 88).
Delete filter Delete content of the filter (see chapter 4.7.1, page 88).
Filter selection Only display selected determinations (see chapter 4.7.1, page 88).
Selection not in filter Hide selected determinations (see chapter 4.7.1, page 88).
Single graph Display single graph (see chapter 4.7.3, page 113).
Multiple graph Display multiple graph (see chapter 4.7.3, page 113).
Live graph with

reevaluation Reevaluate live graph (see chapter 4.7.3, page 113).
Export to Word Export Determination overview to Word (see chapter 4.7.6, page 129).
Export to Excel Export Determination overview to Excel (see chapter 4.7.6, page 129).
Export measured val-

ues Export measured values to a TXT file (see chapter 4.7.6, page 129).
Export determination
Export determination and method data to a TXT file (see chapter 4.7.6, page
and method data
129).
Tile vertically Arrange subwindows on top of each other (see chapter 4.7.8, page 142).
Tile horizontally Arrange subwindows beside each other (see chapter 4.7.8, page 142).
Return to main pro-

gram Close Results window and return to main program.
4.1.5 File types

The following file types are generated by the program 743 Rancimat:
*.mrd Database file
This file contains the measured data and results
of the determinations. The file repos.mrd is
automatically saved in the directory Database.
When exporting databases, the memory location
can be freely selected.
743 Rancimat ￭￭￭￭￭￭￭￭ 31

*.mel Event file

This file contains a protocol of all events which
have occurred with the connected Rancimats.
The file *.mel is automatically saved in the Log
directory.
*.txt Text file
Measured values, determination and method
data as well as the data of the temperature log
can be saved in ASCII format as a TXT file. The
memory location can be freely selected, except
for the temperature log. This file is saved in the
Log directory.
4.1.6 Context-sensitive menus

Many menu functions of the Program window can also be selected by
clicking with the right mouse button on the required dialog window or
element. The menu options opened depend on the active dialog window
or element selected.
4.1.7 Mouse functions

The standard functions for program control such as selecting menu items
and fields can be executed using the mouse.
It also serves for magnifying a curve sector (Zooming).
Zooming
Proceed as follows:
1 Drag zoom square

￭ Place the cursor on the upper left corner of the sector to be mag-
nified.
￭ Keeping the left mouse button pressed down, pull the cursor to
the lower right corner of the sector.
The cursor assumes the form of a magnifying glass.
2 Release mouse button

￭ Release the mouse button in order to magnify the selected area to
the full size of the window.
32 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
3 Switch zoom off again

￭ Right click in the graphs window.
The context-sensitive menu for graphs appears.
￭ Click on the menu item Zoom Off.
4.1.8 Help
You can call up help for the current topic anywhere with the symbol ,
the menu item Help ▶ Help topics or the key [F1].
Green text can be clicked on. This takes you to another help
topic.
Violet text marks menu items, parameters or buttons in the
program.
Blue text marks titles and important information.
743 Rancimat ￭￭￭￭￭￭￭￭ 33

4.2 Instrument and Program Settings ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4.2 Instrument and Program Settings

4.2.1 Establishing the instrument communication
Up to four instruments can be controlled with the program 743 Ranci-
mat. Configure the communication between your PC and the 743 Ranci-
mat as follows:
1 Select number of instruments connected

￭ In the Control window, click on the menu item
Options ▶ Communication....
￭ Enter the number of connected instruments and confirm with

[OK].
2 Select interface
￭ Under COM port, select the serial interface of the PC to which
the instrument is connected.
34 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
￭ If a softswitch is used, activate the option Softswitch in use and

select the serial interface of the softswitch to which the instru-
ment is connected under Softswitch port.
￭ Confirm the entry with [OK].
3 Restart program
￭ Close the program with the menu item File ▶ Exit.
mat.
￭ Enter the Administrator password and confirm with [OK].
The program is opened. The message Instr.#: Ready now appears
in the status bar for all connected instruments.
4.2.2 Managing access rights

The 743 Rancimat program offers extensive password protection, allow-
ing each menu item to be provided with individual access rights.
The dialog Users and groups manager, used to manage the access
rights, is only accessible to the Administrator. The Administrator himself is
not listed as a user, but has all access rights.
First of all, the access rights are given to different Groups. Then, individ-
ual Users can be assigned to a specific group.
NOTICE
User lists are best created and passwords are best entered immediately
after the first program start.
The setup for the users and their access rights is carried out in the follow-
ing order:
1. Add a new group
2. Adjust rights for this group
3. Create users in this group
743 Rancimat ￭￭￭￭￭￭￭￭ 35

After having entered the access rights, the Login window for selecting the
user and entering the password appears each time the program is started.
All methods, determinations and reports are marked with the user name.
It is possible to change the user at any time with the menu item
File ▶ New login....
Adding a new group
In order to add a new group, proceed as follows:
1 Open Users and groups manager

Options ▶ User permissions....
2 Create new group

￭ Right click on an existing group to select the menu item Add
group....
￭ Under Enter new group name enter the name for the group
and confirm with [OK].
Adjusting access rights for the group
Proceed as follows to set the access rights:

2 Open Properties dialog

￭ Right click on the relevant group whose access rights are to be
adjusted to select the menu item Properties....
36 ￭￭￭￭￭￭￭￭ 743 Rancimat

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3 Activate/Deactivate the rights

￭ Click on the symbol to open the menu tree for the access
rights..
￭ Activate or deactivate the required options by clicking on the sym-
bol .
￭ Confirm the changes with [OK].
Adding a new user
Proceed as follows to add a new user:

2 Create new user

￭ Right click on an existing group to select the menu item Add
user....
￭ Under Enter new user name enter the name for the user and
confirm with [OK].
743 Rancimat ￭￭￭￭￭￭￭￭ 37

Deleting a user
Proceed as follows to delete an existing user:

2 Delete user
￭ Right click on the user to be deleted to activate the menu item
Delete user.
￭ Confirm the message Do you really want to delete user "user
name"? with [Yes].
Deleting a group
Proceed as follows to delete an existing group:

2 Delete group
￭ Right click on the group to be deleted in order to select the menu
item Delete group.
￭ Confirm the message Do you really want to delete group
"group name"? with [Yes].
4.2.3 Timer
The function Timer can be used to start the two heating blocks A and B,
independently of one another, automatically and at a time specified by
you. The Rancimat has to be switched on and the software must be run-
ning.
Two different examples will explain how to program the timer.
38 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Starting heating block A once automatically
Proceed as follows to automatically start the heating of block A at a spe-

cific time:
1 Open dialog window

￭ In the Control window, click on the menu item Tools ▶ Timer
function....
2 Set automatic start time

￭ Under Start heating select the option Once.
￭ Under Start at... enter the required time and date.
￭ Confirm the entries with [OK].
Starting heating block B daily automatically at the same

time
Proceed as follows to automatically start the heating of block B on a spe-

cific day of the week, at a specific time:

￭ In the Control window, click on the menu item Tools ▶ Timer
function....
743 Rancimat ￭￭￭￭￭￭￭￭ 39

2 Set automatic start time

￭ Under Start heating select the option Daily.
￭ Click on the button [Which days...].
￭ Select the required day(s) and confirm with [OK].

￭ Under Start at... enter the required time and confirm with [OK].
4.2.4 Gas flow control

The gas flow produced by the internal pump through the reaction ves-
sels to the measuring vessels can be switched on and off manually and
displayed in a separate window.
Switching the gas flow on and off
Proceed as follows:
1 Switch on
￭ Click on the menu item Tools ▶ Gas flow control ▶ Gas flow
on.
2 Switch off
off.
40 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Displaying the gas flow
Proceed as follows:

￭ Click on the menu item Tools ▶ Gas flow control ▶ Display
gas flow....
NOTICE
This option is only available if no determination is running.
4.2.5 Recording the temperature

The temperature can be recorded at any time for each individual heating
block.
The program writes the recorded measured values into a text file contain-
ing the following values:
t(s) Time in seconds.
Block [°C] Temperature measured in the heating block.
Ext. Sensor [°C] Temperature measured with the external temper-
ature sensor.
The text file is saved under the name U#X-YYMMDD-hhmmss.txt in the
folder Log, # denoting the instrument number (1...4), X denoting the
block (A or B) and YYMMDD-hhmmss denoting the date and time when
the data logging started.
743 Rancimat ￭￭￭￭￭￭￭￭ 41

Switching the temperature log on and off
Proceed as follows:
1 Switch on the recording for block A or B

￭ Click on the menu item Tools ▶ Temp. logging ▶ Block A on.
or
￭ Click on the menu item Tools ▶ Temp. logging ▶ Block B on.
2 Switch off the recording for block A or B

￭ Click on the menu item Tools ▶ Temp. logging ▶ Block A off.
or
￭ Click on the menu item Tools ▶ Temp. logging ▶ Block B off.
4.2.6 Optimizing program and database

The data which the program Rancimat requires for displaying the Results
window is saved in the file Nachaus.prg. With the standard installation,
this file is located at C:\Program Files\Metrohm\Rancimat\Template. As
soon as the file is greater than 10 MB, you should optimize and com-
press the program, so that this file no longer has any superfluous data and
the program runs faster again.
The file size of the database Repos.mrd can make access to existing
determinations considerably slower. If you regularly work with the pro-
gram and carry out a large amount of determinations, you should opti-
mize the standard database Repos.mrd once a month.
Optimizing the program
Proceed as follows to optimize the program:
1 Quit program
￭ Close the program Rancimat (see chapter 4.1.1, page 25).
2 Optimize program
￭ In the windows Start menu, click on the menu item Pro-
grams ▶ Metrohm ▶ Rancimat ▶ Optimize ▶ Program.
42 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Optimizing the database
Proceed as follows to optimize the standard database:
1 Export database
￭ Export determinations not currently required from the database
Repos.mrd into a newly created database (see "Exporting deter-
minations to another database", page 134).
￭ Close the Results window and the program Rancimat (see chap-
ter 4.1.1, page 25).
2 Optimize database
￭ In the Windows Start menu, click on the menu item Pro-
grams ▶ Metrohm ▶ Rancimat ▶ Optimize ▶ Database.
4.3 Program information

4.3.1 Instrument information
Displaying and printing the instrument information
Proceed as follows to display and print the instrument information of the

currently selected Rancimat:

￭ In the Control window, click on the menu item View ▶ Unit
information….
743 Rancimat ￭￭￭￭￭￭￭￭ 43

4.3 Program information ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2 Print instrument information

￭ Click on the button [Print report…].
The status report is printed on the printer which is defined on your
PC as the default printer.
Meaning of the individual parameters
Serial number
Serial number of the selected instrument.
Program number
Number of the EEPROM program of the selected instrument.
Last maintenance
Date of the last maintenance with signature of the service technician who
has carried out the service work.
Last calibration
Date of the last instrument adjustment with signature and code of the
responsible body.
Unit operating hours

Number of hours during which the instrument was switched on.
Pump operating hours

Number of hours during which the internal pump was in operation.
44 ￭￭￭￭￭￭￭￭ 743 Rancimat

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NOTICE
The block Service diagnosis is password-protected and only accessi-

ble for trained service personnel.
4.3.2 Status overview
Displaying the status overview
Proceed as follows to display and adjust the status overview:

￭ In the Control window, click on the menu item View ▶ Status
overview.
2 Adjust and save column width

￭ You can adjust the column width to the required size by dragging
the right field border with the mouse.
Options ▶ Save settings now.
Meaning of the columns in the status overview
Unit
Instrument number (1…4).
Block
Instrument block (A or B).
Channel
Channel (1…4).
Method
Name of the method loaded.
743 Rancimat ￭￭￭￭￭￭￭￭ 45

Sample ID1
Sample identification 1.
Status
Status of the channel.
ready: No active measurement. The channel is ready for starting a deter-
mination.
running: Instrument is measuring.
finished: Determination finished. The channel is ready for starting a new
determination.
error: Communication error between instrument and PC.
Stab. time
Stability time determined.
Induc. time
Induction time determined.
Set temp.
Setpoint temperature (defined in the method).
Current temp.
Current block temperature.
4.3.3 Displaying, filtering and deleting event overview
Opening and saving the event log file
Proceed as follows to display and save all events of the Rancimats con-
nected to the PC:
1 Open current log file

￭ In the Control window, click on the menu item View ▶ Event
log overview.
46 ￭￭￭￭￭￭￭￭ 743 Rancimat

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NOTICE
You can find the meaning of the symbols and columns in the event
overview at "Meaning of the symbols and columns in the event
overview", page 48.
2 Update view
￭ Click on the symbol or the menu item View ▶ Refresh to
view the current status of the log file.
3 Save log file

￭ Click on the symbol or the menu item File ▶ Save as….
￭ In the dialog window Save file as enter a file name and confirm
with [OK].
4 Open saved log file

￭ Click on the symbol or the menu item File ▶ Open….
￭ In the dialog window Open, select the required file and confirm
with [OK].
Filtering entries in the event overview
Proceed as follows to filter the entries in the event file:
1 Filter the entries

￭ Click on the required filter criterion (e.g.: date = "30.08.2006").
743 Rancimat ￭￭￭￭￭￭￭￭ 47

￭ Click on the symbol or the menu item Filter ▶ Selection

based filter.
Only entries with the date "30.08.2006" are displayed in the dialog
window.
2 Remove the filter again

￭ Click on the symbol or the menu item Filter ▶ Remove filter.
All entries are once again displayed in the dialog window.
Deleting entries from the event overview
Proceed as follows to delete certain entries from the event file:

Options ▶ Event log….
2 Delete entries
￭ Enter the maximum age in days, which the entries are allowed to
have in the list. All older entries are deleted.
￭ Confirm the entry with [OK].
Meaning of the symbols and columns in the event overview
Type
- Information on correctly executed events.
- Indication of a special event.
- Error message for error event.
Date
Date of the event. The format depends on the settings defined in Win-
dows in Control Panel ▶ Country settings ▶ Date.
48 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Time
Time of the event. The format depends on the settings defined in Win-
dows in Control Panel ▶ Country settings ▶ Time.
User
Name of the user logged in at the time of the event.
Unit
Instrument number (1…4).
Event
Description of the event.
4.4 Calibration functions

4.4.1 Determining cell constants
Only the change in conductivity is measured an evaluated during the
Rancimat measurement. As a result, the cell constants of the conductivity
measuring cells used in the Rancimat, which are normally in the range
from 1.00...1.20, only have to be entered exactly if the absolute con-
ductivity measured value is to be displayed correctly.
The value also has to be entered before carrying out the GLP test "Con-
ductivity". The cell constants can thereby be entered manually or deter-
mined automatically using a defined standard solution .
Entering cell constants manually
Proceed as follows if you wish to enter the cell constants manually:

￭ Click on the menu item Tools ▶ Cell constants ▶ Manual....
743 Rancimat ￭￭￭￭￭￭￭￭ 49

4.4 Calibration functions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2 Enter cell constants

￭ Enter the cell constants of the conductivity measuring cells for the
required channels and confirm with [OK].
Determining cell constants automatically
Proceed as follows if you wish to enter the cell constants automatically:

￭ Click on the menu item Tools ▶ Cell constants ▶ Automatic....
2 Select channels and define conductivity

￭ Activate the check boxes of those channels, for which the cell
constant is to be determined.
50 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
￭ Enter the conductivity of the standard used.

c(KCl) = 1 mmol/L can be used as a standard solution. This is
derived from the optionally available conductivity standard
6.2301.060 (KCl 0.1 mol/L) through dilution with distilled water. The
conductivity of this diluted solution is:
Temperature Conductivity
18 °C 127 µS/cm
19 °C 130 µS/cm
20 °C 133 µS/cm
21 °C 136 µS/cm
22 °C 138 µS/cm
23 °C 141 µS/cm
24 °C 144 µS/cm
25 °C 147 µS/cm
Alternatively, the conductivity standard 6.2324.000 (undiluted) can

be used.
3 Start determination and check the values

￭ Click on [Start] to start the determination of the cell constant.
After the determination is finished, the dialog window Enter/Check
cell constants appears again.
If you wish to accept the displayed values, click [OK].
If you wish to maintain the old values, click [Cancel].
4.4.2 Determining Delta T

The temperature correction Delta T indicates the deviation of the cur-
rent temperature of the sample from the temperature in the heating block
and belongs to the method as a parameter (see chapter 4.5.2, page 61).
It can automatically be determined with the calibrated, external tempera-
ture sensor (part of the optionally available GLP test set, ).
743 Rancimat ￭￭￭￭￭￭￭￭ 51

2
3
4
5
6
10
Figure 6 Equipping the reaction vessel for determining Delta T
1 FEP tubing 250 mm (6.1805.080) 2 Pt100 temperature sensor

For supplying air into the reaction vessel.
3 Thread adapter M8 / M6 (6.1808.090) 4 Opening for temperature sensor

For inserting the temperature sensor.
5 Air tube 6 O-ring (6.1454.040)
7 Connector 8 Reaction vessel cover (6.2753.107)

For connecting the thread adapter M8 / M6.
9 Spacer (6.2042.040) 10 Reaction vessel (6.1429.040)
52 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Preparing Delta T determination
Figure 6 shows in detail how the accessories for determining Delta T are
mounted. Proceed as follows:
1 Prepare reaction vessel cover

￭ Mount the air tube on the reaction vessel cover (see "Mount the
reaction vessel cover", page 15).
￭ Clamp the first spacer at a distance of approx. 12 cm from the
lower end onto the air tube.
￭ Clamp the second spacer at a distance of approx. 5 cm from the
lower end onto the air tube.
￭ Insert the temperature sensor from above into the temperature
sensor opening of the reaction vessel cover and fasten it in the
corresponding openings of the spacers.
2 Prepare reaction vessel

￭ Fill the reaction vessel with 5 g silicone oil (e.g. FLUKA 85409).
￭ Place the reaction vessel cover with the temperature sensor on
the reaction vessel.
￭ Push the temperature sensor fully downwards (the sensor must be
on the vessel base).
3 Insert and connect reaction vessel

￭ Insert the reaction vessel with the mounted reaction vessel cover
in channel 2 or 3 of the required heating block.
￭ Screw the one end of the FEP tubing 250 mm onto the thread
adapter M8 / M6 of the reaction vessel cover.
￭ Screw the other end of the FEP tubing onto the corresponding
connector (3-3) of the Rancimat.
4 Set method parameters
NOTICE
Create a unique method for both blocks, so that you can sepa-
rately enter the temperature correction for both blocks.
￭ In the Control window, select the required method for the

heating block for which the temperature correction Delta T is to
be determined (see "Select method", page 82).
743 Rancimat ￭￭￭￭￭￭￭￭ 53

￭ Click on the symbol .

The dialog window with the method parameters is opened.
￭ Under Temperature enter the required setpoint temperature for
the sample and set Delta T to 0 °C.
￭ Set the gas flow to the required value and finalize with [Save].
5 Start gas flow and heating

on.
￭ Click on the button [Heat to xx °C].
Executing a Delta T determination
After you have prepared everything for determining Delta T (see "Prepar-
ing Delta T determination", page 53), you can now execute the determi-
nation of Delta T as follows:
1 Enter sensor calibration data

￭ Click on the menu item Tools ▶ Determine Delta T ▶ Block A
or Block B.
￭ Enter a Sensor name.

￭ Enter the calibration data (temperature and resistance) for Points
1 to 3 and confirm with [OK].
54 ￭￭￭￭￭￭￭￭ 743 Rancimat

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NOTICE
You can find the calibration data (T1 to T3) for Metrohm sensors
on the certificate enclosed with the sensor or on the label fastened
on the sensor cable.
2 Wait for measurement

￭ Wait until the message Measured temperature is now stable!
appears in the message box.
The following three values are displayed below the message box:
Block temperature Temperature which has been measured in the
heating block with the internal temperature
sensor.
Temperature of ext. sensor Temperature which has been measured in the

reaction vessel with the external temperature
sensor.
Delta T Temperature correction which is determined

from the difference between the block temper-
ature and the temperature of the ext. sensor.
743 Rancimat ￭￭￭￭￭￭￭￭ 55

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
NOTICE
If the temperature which is defined in the method, has not yet

been reached, the heating is started automatically. At the same
time the message Waiting until temperature is reached...
As soon as the temperature defined in the method has been
reached, the message Measuring temperature. Please wait...
3 Accept measured values

￭ Click on the [Accept] button in order to accept the determined
temperature correction Delta T in the method.
This is followed by the message that Delta T is now set to the corre-
sponding method. It is automatically saved with the changed value
of Delta T.
4.5 Methods
4.5.1 Managing methods
Creating a new method
Proceed as follows to create a new method:
1 Open empty method

￭ In the Control window, click on the symbol or the menu
item File ▶ New method.
56 ￭￭￭￭￭￭￭￭ 743 Rancimat

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2 Adjust parameters
￭ Adjust the required parameters.
￭ Click on the tab Evaluation and also adjust the parameters.
￭ Repeat for all remaining tabs.
NOTICE
You can find a detailed description of all tabs and their parameters
at 4.5.2 Parameter description.
3 Save method
￭ Click on the [Save as...] button.
The dialog window Save method as... opens.
￭ Enter the method name and confirm with [Save].
743 Rancimat ￭￭￭￭￭￭￭￭ 57

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Opening a selected method and adjusting parameters
Proceed as follows to open the method which is selected in the Control

window and adjust its parameters:
1 Open method
￭ In the Control window, click on the symbol in the required

Block A or B.
The dialog window "Method name" appears.
2 Adjust parameters and save changes

￭ Adjust the parameters (see chapter 4.5.2, page 61).
￭ Confirm the changes with [Save].
Opening an existing method and adjusting parameters
Proceed as follows to open an existing method and adjust its parameters:
1 Open existing method

item File ▶ Open method....
The dialog window Open method appears.
￭ Click on the required method and confirm the selection with
[Open].
2 Adjust parameters and save changes

￭ Adjust the parameters (see chapter 4.5.2, page 61).
￭ Confirm the changes with [Save].
Renaming an existing method
Proceed as follows to rename an existing method:
58 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
NOTICE
A method which is still selected in one of the blocks A or B, cannot be

renamed. Select another method first in order to rename the required
method.
1 Open Method manager

item File ▶ Method manager....
2 Select and rename method

￭ Click on the required method and then the button [Rename].
The method name is highlighted in blue.
￭ Enter the new method name and click with the mouse on the free
white area below the method name in order to accept the
change.
￭ Click on the [Close] button.
Saving a method under a new name
Proceed as follows to save an existing method under a new name:
1 Open method
[Open].
743 Rancimat ￭￭￭￭￭￭￭￭ 59

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2 Save it with a new name

￭ If necessary, adjust the parameters (see chapter 4.5.2, page 61).
￭ Click on the [Save as...] button.
The dialog window Save method as... appears.
￭ Enter the method name and confirm with [Save].
Deleting an existing method
Proceed as follows to delete an existing method:
NOTICE
A method which is still selected in one of the blocks A or B, cannot be

deleted. Select another method first in order to delete the required
method.
1 Open Method manager

item File ▶ Method manager....
2 Select and delete method

￭ Click on the required method and then the button [Delete].
The safety prompt "Do you really want to delete method
"method name"?" appears.
￭ Confirm the safety prompt with [Yes].
60 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Operation
Printing parameters of a method
Proceed as follows to print the parameters of an existing method:
1 Open method
[Open].
2 Print parameters
￭ Click on the [Print...] button.
The dialog window Print Setup opens. All the printers installed
on your PC appear under Name.
￭ Select the required printer and confirm with [OK].
4.5.2 Parameter description

A method contains several parameters which are distributed on various
tabs. This section explains all the parameters, arranged according to tab.
4.5.2.1 "Parameters" tab

The most important parameters (temperature, gas flow, Delta T) for carry-
ing out the measurement are set using this tab. The settings affect the
progression of the measurement curve recorded.
743 Rancimat ￭￭￭￭￭￭￭￭ 61

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Temperature
Setpoint temperature of the sample.
Input range 50 - 220 °C
Delta T
Temperature correction: indication of how much the block temperature
has to be increased so that the sample reaches the setpoint temperature.
This value is determined through measurement of the deviation by the
current temperature of the sample from the heating block temperature
using a calibrated, external temperature sensor (see chapter 4.4.2, page
51).
NOTICE
If no temperature sensor is available for determining Delta T, you can

enter the approximate values listed in the table below, which have been
determined with 5 g silicone oil and a gas flow of 20 L/h (air).
Input range -9.9 - 9.9 °C
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Table 1 Approximate values for determining Delta T

Setpoint temperature Delta T
80 °C +1.1 °C
90 °C +1.3 °C
100 °C +1.4 °C
110 °C +1.5 °C
120 °C +1.6 °C
130 °C +1.7 °C
140 °C +1.8 °C
150 °C +1.9 °C
160 °C +2.0 °C
Gas flow
Gas flow through the sample. The gas flow can only be set for both
blocks jointly. The value of the method loaded for block A is always deci-
sive.
Input range 7 - 25 L/h
Use internal pump

on | off (Default value: on)
Switch on/off gas supply with internal pump. If the internal pump is
switched off, an external gas supply must be connected to the Air/N2 in
connection (see chapter 3.2.2, page 13).
Start options
Start delay
Waiting time until starting the measurement.
Input range 0 - 1000 min
Start mode
Mode for starting and stopping the channels.
Selection per channel | per 2 channels | per block
per channel
All channels can be started and stopped individually.
per 2 channels
2 channels each can be started and stopped jointly. The [Start] button
in the control window changes automatically for this.
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4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
per block
The 4 channels of a block can be started and stopped jointly.
Stop criteria
Time
on | off (Default value: off)
Time until the automatic stop of the determination.
Input range 0.1 - 9999 h
Conductivity
Conductivity limit value. If this value is reached, the determination is
ended automatically.
Input range 1 - 400 µS/cm
Endpoint(s)
Automatic stop of the determination, as soon as every active channel has
reached all endpoints (induction time and stability time).
Table 2 Overview of stop criteria

Time Conductivity Endpoint(s) Analysis stops...
not automatically.
✔ after the time entered, independently of reach-
ing the induction/stability time (endpoint).
✔ after reaching the conductivity entered, inde-
pendently of reaching the induction/stability
time (endpoint).
✔ after reaching the induction and stability time
(endpoint) defined on the Evaluation tab. If
the induction and stability time are evaluated,
both endpoints have to be found.
✔ ✔ after reaching the first criterion (time or con-
ductivity), independently of reaching the induc-
tion/stability time (endpoint).
✔ ✔ after reaching the first criterion (time or end-
point). If the time entered has been reached,
there is no further measuring until the induc-
tion/stability time (endpoint) has been reached.
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Time Conductivity Endpoint(s) Analysis stops...

✔ ✔ after reaching the first criterion (conductivity or
endpoint). If the conductivity entered has been
reached, there is no further measuring until the
induction/stability time (endpoint) has been
reached.
✔ ✔ ✔ after reaching the first criterion. If the time or
conductivity entered has been reached, there is
no further measuring until the induction/stabil-
ity time (endpoint) has been reached.
Actions at end of determinations...
Shut off heater

Automatic deactivation of the heating at the end of the determination.
Shut off gas flow

Automatic deactivation of the gas flow at the end of the determination.
CAUTION
If the gas flow is automatically switched off, the reaction vessels must
be removed from the instrument within 30 to 60 min after the end of
the determination. If the vessels are not removed, a vacuum could
develop over the course of time, which would thus result in back suc-
tion of the measuring solution into the hot reaction vessel.
4.5.2.2 "Evaluation" tab

These settings serve for automatic evaluation of the curve. After finishing
the measurement, curves can also be reevaluated in the database (see
743 Rancimat ￭￭￭￭￭￭￭￭ 65

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Evaluate induction time

Determination of the induction time (see "Induction time", page 67).
Evaluate stability time

Determination of the stability time (see "Stability time", page 68).
NOTICE
If you select this evaluation mode, you always need to calibrate the
conductivity measuring cell beforehand.
Delta Kappa
Conductivity change for the determination of the stability time.
Options for induction time
Evaluation delay
Waiting time until starting the curve evaluation.
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Input range 0 - 100 h
Evaluation suppression
Start
Time from the start of the determination to the start of the evaluation
suppression.
End
Time from the start of the determination to the end of the evaluation sup-
pression.
Evaluation sensitivity
This value defines the minimum value which the maximum of the curve of
the second derivative has to reach in order to be accepted as a result. The
result, i.e. the induction time, is the time until the first accepted maximum.
The default value "1" will lead to the correct result for most applications.
Smaller values will cause the acceptance of smaller maximums of the sec-
ond derivative. Higher values require a higher maximum.
Input range 0.1 - 9999
Induction time
The induction time is the time to the break point of the curve conduc-
tivity vs. time recorded with the Rancimat. The induction time is a parame-
ter for the oxidation stability of the sample examined and corresponds to
a large extent to the results from the complex AOM method.
For automatic determination of the induction time, the second derivative
of the measured curve is used, which exhibits a maximum at the break
point and which can be displayed in the window Live graph. To enable
detection of a break point, certain criteria must be fulfilled with regard to
the height and width of the peak in the second derivative. The break point
can also be determined manually as the intersection point of the two tan-
gents at the extended straight branches of the curve (see "Setting tan-
gents manually", page 117).
743 Rancimat ￭￭￭￭￭￭￭￭ 67

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Conductivity 2nd derivative
Beginning End
Induction time
Time
With certain samples, it may occur that the conductivity rises in steps, to a
small degree, long before the actual induction time (e.g. through side
reactions or with volatile compounds). To prevent this rise being evaluated
as an endpoint, the user can delay the evaluation or suppress it for a cer-
tain range.
Stability time
The stability time is the time which is necessary in order to attain a speci-
fied conductivity change Delta Kappa.
Conductivity
Conductivity
Change
Stability time
Time
The entry of an evaluation delay or evaluation suppression does not have

any effect on this evaluation mode. In all cases the time from the start
point of the measurement is calculated.
4.5.2.3 "Curves" tab

The scaling of the x and y axis can be defined here. The settings have an
effect on the expression of the curves, but not on the measurement and
evaluation. After completing the determination, the scaling for single and
live graphs can be changed again in the determination overview.
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Time axis (x)

Selection Auto scaling | Manual scaling
Auto scaling
Automatic definition of the start and end value of the time axis.
Manual scaling
Manual definition of the end value of the time axis.
End value
End value of the time axis with manual scaling.
Input range 0.5 - 100 h
Conductivity axis (y)

Selection Auto scaling | Manual scaling
Auto scaling
Automatic definition of the start and end value of the conductivity axis.
Manual scaling
Manual definition of the end value of the conductivity axis.
End value
End value of the conductivity axis with manual scaling.
743 Rancimat ￭￭￭￭￭￭￭￭ 69

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4.5.2.4 "Formulas" tab

You can enter values for further automatic calculations with the induction
and stability time on this tab. The settings here do not have any effect on
the measuring sequence or the evaluation. After finishing the measure-
ment, a post-calculation or recalculation is possible at any time in the
determination overview (see chapter 4.7.5, page 122).
Formula 1 for induction time:

If this option is activated, the automatically determined induction time will
be calculated with the entered values. The result will be saved under the
name entered in the field "R1".
Formula 2 for stability time:

If this option is activated, the automatically determined stability time will
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Formula 3 for stability time:

If this option is activated, the automatically determined stability time will
4.5.2.5 "Standards" tab

This function can be used to automatically calculate the induction time for
a temperature deviating from the measuring temperature, the so-called
standard time. The settings here do not have any effect on the measuring
sequence or the evaluation. After finishing the measurement, a post-cal-
culation or recalculation is possible at any time in the determination over-
view (see chapter 4.7.5, page 122).
Calculate standard time

Activation/Deactivation of the calculation of the standard time according
to the following formula:
Standard time = Factor(Temperature - Target temperature)/10 x induction time
Formula according to...

Selection AOCS Cd12b-92 | AOM | free
743 Rancimat ￭￭￭￭￭￭￭￭ 71

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
AOCS Cd12b-92
Formula calculation according to standard AOCS Cd12b-92 with Tar-
get temperature = 110 °C.
AOM
Formula calculation according to standard AOM with Target temper-
ature = 97.8 °C.
free
Formula calculation with freely selectable Target temperature.
Formula parameters
Factor
Parameter for the calculation of the standard time, which indicates the
factor by which the time changes per 10 °C. This value can be determined
through the extrapolation (see chapter 4.7.4, page 118) of results, which
have been recorded at different temperatures.
Input range 0.001 - 100
Target temperature
Target temperature for the calculation of the standard time.
Input range 20 - 300 °C
4.5.2.6 "Documentation" tab

This tab contains parameters for the automatic report output.
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Include in report...
Header
Output of the header with company settings (see ""Company settings"
tab", page 138), date of the printout, sample identifications, instrument
information, determination date, user, cell constant and serial number.
Method parameters
Output of the method parameters.
Curve(s)
Output of the curves.
Method description
Output of the method description entered on the tab Description.
Results
Output of the selected results.
Selection Induction time | Stability time | Standard time |
Formula 1 | Formula 2 | Formula 3
Automatic report output
Send to printer immediately

Automatic printout of the report defined under Include in report... after
finishing the determination.
Send to file
Automatic output of determination and method data after finishing the
determination as TXT file for further processing in other programs. The
content of this report is independent of the report elements defined at
Include in report....
Browse…
Selection of the directory for saving this file.
743 Rancimat ￭￭￭￭￭￭￭￭ 73

4.5 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Example of an automatically printed report
Unit 1 Serial number 01109 Printing date 09.09.2006 09:34:03

Block A Cell constant 1 Determination date 23.06.2006 13:25:52
Channel 1 User Administrator
ID 1 ID 2
Peanut oil DBG2307
Induction time 3.26 h
3.26
30
25
20
15
µS/cm
10
0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
h
Method name Oil 120°C

Creator Administrator Creation date 23.06.2006 08:27:20
Temperature 120 °C Stop time 0.00 h

Delta T 1.60 °C Stop at conductivity 0 µS/cm
Gas flow 20 L/h Stop at endpoint
Start delay 0 min Delta Kappa 0 µS/cm
Start mode per channel Evaluation delay 0.00 h
per 2 channels Evaluation delay start 0.00 h
per block Evaluation delay end 0.00 h
Send to file
GLP test passed.
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4.5.2.7 "Description" tab

You can enter a comment on the method in this tab.
743 Rancimat ￭￭￭￭￭￭￭￭ 75

4.6 Determinations ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4.6 Determinations
Standard sequence Optional steps Further information
Prepare samples Section 4.6.1
Section .4.6.2
Prepare instrument and accessories
Section 4.6.3
Select method
Modify method parameters Section 4.5.2
Start heating Section 4.6.3
Enter sample identifiers Section 4.6.3
no
Temperature
reached?
yes
Insert and connect reaction vessels Section 4.6.3
Start determination Section 4.6.4
no Modify live parameters Section 4.6.6

Stop crit.
reached? Section 4.6.7
Stop determination manually
yes
Determination finished
Automatic report output Section 4.5.2.6
Result display Section 4.7
Section 4.6.5
Clean vessels and accessories
76 ￭￭￭￭￭￭￭￭ 743 Rancimat

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4.6.1 Preparing samples

This section contains information on how to prepare the following sam-
ples:
￭ Pure, clear oils (see page 77)
￭ Non-liquid, pure fats (see page 77)
￭ Samples containing oil and fat (see page 78)
￭ Emulsion fats (see page 80)
NOTICE
Use new reaction vessels and air tubes for each measurement.
Blow the reaction vessel out with nitrogen before use.
Preparing pure, clear oil
Prepare the oil, which is completely pure and clear, as follows:
1 Weigh in the sample

￭ Weigh in 3 g sample material directly in the reaction vessel.
2 Check the filling level

￭ Check whether the quantity of the sample material rises to such
an extent in the reaction vessel that the air tube immerses suffi-
ciently deeply. If this is not the case, add more sample material.
Preparing non-liquid, pure fats
Prepare non-liquid, pure fat as follows:

either
￭ Completely liquefy the fat in a water bath or in a drying oven at
a temperature exceeding its melting point by 10 °C.
￭ Then transfer 3 g sample material using preheated pipettes to
the reaction vessel.
or
￭ Weigh in the fat as solid. For this, weigh in 3 g sample mate-
rial directly in the reaction vessel and insert this briefly in the
heated block of the 743 Rancimat, so that the fat melts.
743 Rancimat ￭￭￭￭￭￭￭￭ 77

4.6 Determinations ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2 Check the filling level

￭ Check whether the quantity of the melted sample material rises to
such an extent in the reaction vessel that the air tube immerses
sufficiently deeply. If this is not the case, add more sample mate-
rial.
Preparing samples containing oils and fats
Oils and fats made from products containing oil and fat must be extracted
as follows with petroleum ether (low boiling point) protected from light:
1 Crush the samples

￭ Finely and homogeneously grind oilseed fruit, cocoa beans as well
as other solids in coarse form in a knife mill or another suitable
crushing apparatus (if possible, metal-free).
NOTICE
Oil/Fat extraction through pressing off has not proven effective in

practice.
2 Extraction
￭ Prepare an Erlenmeyer flask 300 mL with normal grinding.
￭ Weigh in between 50 and 100 g (depending on oil/fat content) of
the sample in powder form (e.g. milk powder, cocoa powder,
hazel nut powder) or the finely ground material.
￭ Cover the sample material with a layer of approx. 1 cm of petro-
leum ether (low boiling point).
￭ Extract the oil or fat while continuously stirring for around 12 h
and keeping it protected from light.
NOTICE
In order to carry out at least one double determination on the 743

Rancimat, you have to extract approx. 10 g pure oil or fat, allow-
ing for a certain transfer loss (for more than two determinations
accordingly more is necessary).
￭ Prepare a clean round-bottom flask 250 mL with standard ground

joint and a folded filter.
￭ Filter off, if possible protected from light. Rewash the residue with
a little petroleum ether.
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NOTICE
If the folded filter becomes blocked (e.g. due to the consistency of

the sample material), a Soxhlet apparatus should be used for solid/
liquid separation. You can use up to 40 g of sample material here
per approach.
3 Distillation and filtration

￭ Distill the petroleum ether from the clear, perhaps slightly yellow
extract.
NOTICE
It is safest and easiest if you do this in a rotation evaporator; in a

slight vacuum and at a temperature of +30...35 °C the petroleum
ether can gently and efficiently be removed, protected from direct
light (cover the water bath e.g. with aluminum foil).
￭ Dry the oil/fat sample obtained after completing the distillation:

during around 30 min at a pressure of p < 1330 Pa (13.3 mbar).
￭ Filter the oil/fat sample now present together with Na2SO4
water-free over a folded filter. If necessary, work in the drying
oven at a temperature exceeding the melting point of this fat by
10 °C.
4 Further sample preparation

￭ Treat the isolated oil/fat samples afterwards just as pure oils and
fats.
NOTICE
If the isolated oil/fat samples are not immediately measured out,

you have to store the samples in a cool place and protected
from light; for storing the samples, they should be covered over
in their vessels with a nitrogen layer. This type of storage does not
provide complete protection against unintended and uncontrolled
changes in the oxidation stability, but represents a usable preserva-
tion in many cases.
You can find further information on the treatment of oil and fat samples in
Rancidity in Foods, Allen J.C., Hamilton R.J., Applied Science Publishers,
London and New York, 1983.
743 Rancimat ￭￭￭￭￭￭￭￭ 79

4.6 Determinations ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Preparing emulsion fats
You can use water-soluble fats as pure substances and prepare them as
follows:

￭ Weigh in the sample.
NOTICE
As the water evaporates right at the beginning of the analysis and

is carried away by the air blown through, you have to use corre-
spondingly more sample material.
2 Mount foam barrier

￭ Mount the foam barrier (see figure 5, page 14), as the samples
can significantly foam.
NOTICE
If the water-soluble fat samples are not immediately measured

out, you need to store the samples in a cool place and protec-
ted from light; for storing the samples, they should be covered
over in their vessels with a nitrogen layer. This type of storage does
not provide complete protection against unintended and uncon-
trolled changes in the oxidation stability, but represents a usable
preservation in many cases.
Alternatively you can melt out the emulsion fats (e.g. butter, margarine) at
a temperature, exceeding the melting point of these fats by 10 °C (i.e. at
approx. +50 °C), centrifuge them and pipette off the resultant oil phase.
4.6.2 Preparing the instrument and the accessories

The cleanliness of instrument and accessories is an indispensable prerequi-
site for reliable, reproducible and correct analysis results. Even the
slightest contamination could catalytically accelerate the oxidative decom-
position and lead to completely incorrect results. Therefore always observe
the instructions for use of measuring and reaction vessels in this section.
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Check and prepare the instruments and vessels as follows (see also figure
5, page 14):
1 Check openings for reaction vessels

￭ Check whether the openings are clean and empty. Blow the dust
out of the openings with nitrogen.
If the instrument is not used, always seal the openings with the
sealing plugs.
2 Fill the measuring vessels
NOTICE
Only use measuring vessels and accessories which are abso-

lutely clean and in a perfect condition.
￭ Fill the cleaned measuring vessels with 60 mL distilled water

each.
For analysis times > 24 h approx. 7 mL more distilled water must
be added per day to compensate for the evaporation loss, so that
the electrodes remain safely immersed.
3 Insert the measuring vessels

￭ Place the clean measuring vessel covers equipped with a PTFE
tube on the measuring vessels.
￭ Insert the measuring vessels with the measuring vessel covers into
the openings provided for this on the 743 Rancimat and, at the
same time, carefully guide the connection plugs (5-15) of the
cover carefully into the electrode connectors (3-2).
NOTICE
Use new reaction vessels and air tubes for each measure-
ment. Blow the reaction vessels out with nitrogen before use so
that any particles adhering are removed.
￭ Weigh in 3 g of the prepared samples in each of the reaction

vessels (see chapter 4.6.1, page 77).
743 Rancimat ￭￭￭￭￭￭￭￭ 81

4.6 Determinations ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
5 Mount the accessories

￭ Take the upper edge of the reaction vessel in your hand (e.g. in
the gap between your thumb and index finger) and turn the glass
round once.
This serves for covering the degreased glasses with a light fat
film so that the vessel covers can be removed more easily after
the determination.
￭ Insert an air tube (5-5) in the connector (5-7) of the reaction ves-
sel cover, fix it with the O-ring (5-6) and fasten it by screwing in
the thread adapter M8 / M6 (5-3).
￭ Place the reaction vessel cover on the reaction vessel. Turn the
cover in such a way that the air tube is as close as possible to the
vessel wall.
￭ Connect the white silicone tubing to the tubing connector (5-4)
of the reaction vessel cover.
￭ Place the prepared reaction vessel in the vessel holder.
4.6.3 Preparing the determination
1 Select method
￭ Under Unit x Block A, click on the symbol in order to select
the method for Block A.
￭ If required, also select a method for Block B.
NOTICE
Different methods with different temperatures can be selected for

Block A and Block B. For the gas flow, on the other hand, the
value which is defined in the method loaded for Block A applies
for both blocks.
See also "Opening a selected method and adjusting parameters",
page 58.
2 Start heating
￭ Under Unit x Block A, click on the button [Heat to xx °C].
￭ If required, also switch on the heating for Block B.
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The color of the button frame changes to red and the temperature
display (2-3) on the instrument flashes. The current temperature is
displayed directly next to the button.
Heating up duration for 120 °C: approx. 45 min.
Heating up duration for 200 °C: approx. 60 min.
NOTICE
If you wish to turn off the heating, click on the button [Heat to
xx °C] again.
3 Enter sample identification

￭ Enter the sample identifications ID1 & ID2 for all sample posi-
tions used.
The entry for ID1 can be selected from the automatically created list
of already entered identifications. This list can be deleted again in the
Control window with the menu item Options ▶ Clear sample
ID1 history.
4 Insert and connect reaction vessels
NOTICE
The temperature defined in the method must be reached, before

you insert the reaction vessels, i.e. the frame of the button [Heat
to xx °C] must be green.
￭ Seal the channels not used with the sealing plugs or empty reac-
tion vessels for protection against impurities.
￭ Insert the prepared reaction vessels into the openings of the heat-
ing block.
￭ Connect the white silicone tubings which are fastened to the
reaction vessel cover to the tubing adapter M8 / olive (5-11) of
the measuring vessel covers.
￭ Screw the FEP tubings 250 mm (5-1) to the thread adapters (5-3)
of the reaction vessel covers and the air supply connections (3-3)
of the Rancimat.
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4.6.4 Starting the determination

Before you can carry out the determination, the channels you intend to
use must be ready(see chapter 4.6.8, page 87).
1 Start determination
￭ Start of an individual determination: Click on the button
[Start] of the corresponding channel.
￭ Start of all channels of Block A: Click on the button .
￭ Start of all channels of Block B: Click on the button .
After the determination has been started, the live curve is dis-
played for every channel:
As soon as a stop criterion defined in the method (see table 2, page

64) has been reached, the determination is ended:
The determination is automatically saved in the database

Repos.mrd. The channel is ready for starting a new determination.
2 Clean vessels and accessories
NOTICE
Always clean the vessels and accessories directly after each

determination (see chapter 4.6.5, page 84).
4.6.5 Cleaning the instrument and accessories

1 Clean the measuring vessels and accessories
￭ Clean used measuring vessels after pouring off the measuring
solution with ethanol or 2-propanol (do not use acetone!). Pre-
clean with washing-up liquid in the case of severe contamination.
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￭ Rinse the product thoroughly with distilled water.

￭ Clean the measuring vessel covers (5-16), the PTFE tubes
(5-17) and the electrodes (5-18) with acetone or 2-propanol
and rinse with distilled water. Pre-clean with washing-up liquid in
the case of severe contamination.
Remove the protective ring (5-19) to be able to clean the elec-
trodes.
2 Clean the reaction vessels and accessories

￭ Dispose of used reaction vessels and air tubes and use new
reaction vessels and air tubes for the next measurement.
￭ Clean the reaction vessel covers with acetone or 2-propanol
and rinse with distilled water. Pre-clean with washing-up liquid in
the case of severe contamination.
￭ Then heat the reaction vessel covers in the drying oven for 2
hours at 80 °C.
NOTICE
Replace the reaction vessel covers if they are not tightly on the
reaction vessel anymore or the material is obdurate.
3 Clean the tubings

￭ Clean the silicone tubings (5-2) with acetone or 2-propanol and
rinse with distilled water. Pre-clean with washing-up liquid in the
case of severe contamination.
￭ Then heat the silicone tubings in the drying oven for 2 hours at
80 °C.
4.6.6 Adjusting the method parameters during the determination
1 Open the dialog window Live parameters

item View ▶ Live parameters....
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2 Adjust the parameters

￭ Adjust all required parameters (see chapter 4.5.2.1, page 61).
￭ Confirm the changes with [OK].
4.6.7 Stopping the determination manually

Determinations are normally automatically stopped after reaching the stop
criteria defined in the method. Current determinations can also be stop-
ped manually.
1 Stop determination
￭ In the Control window, click on the button [Stop].
The message Do you want to save this determination? appears.
2 Save measured data and results

￭ Confirm the message with [Yes] to save all data of the determina-
tion.
￭ or confirm the message with [No] to reject all data.
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4.6.8 Status of the live curve

Before a determination:
No active measurement. No active measurement.

The channel is ready for starting a Communication error between
determination. instrument and PC.
During a determination:
Determination started. Current measurement.

The first measured value is mea- Measured value and time are dis-
sured. played above the live curve.
After a determination:
Determination finished.
The channel is ready for starting a
new determination.
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4.7 Results
4.7.1 Determination overview
The determination overview displays selected information on all determi-
nations which are saved in the opened database, in tabular form. You can
adjust this overview, i.e. you can for example hide fields, adjust the col-
umn width or change the font type.
You can also filter and sort the content of the determination overview
according to specific criteria.
You will find step-by-step instructions on various actions, which you can
execute in the determination overview, below. You can also execute many
actions in addition to the described methods via the context menu.
Further below in this section you will find a detailed description of all
parameters of the dialog windows of the determination overview (see
"Parameter description", page 96).
Displaying the determination overview
Proceed as follows to open a determination overview:

item File ▶ Results....
The Results window is opened with the standard database
Repos.mrd.
If you wish to open another database, carry out step 2.
2 Open database
￭ In the Results window, click on the menu item File ▶ Open
database....
The dialog window Open database appears.
￭ Click on the required database and confirm the selection with
[OK].
Formatting the determination overview
Proceed as follows to format the determination overview.
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A detailed description of the parameters can be found at "Parameter

description", page 96.
1 Select fields
￭ Click on the symbol or the menu item Format ▶ Select
fields.
Only those fields are shown in the determination overview which

are listed in the right column under Display.
￭ In the column Selection, click on a field which is to be displayed
in the determination overview.
￭ Click on the [>] button.
￭ In the column Display, click on a field which is not to be dis-
played in the determination overview.
￭ Click on the [<] button.
2 Adjust the column width

￭ Click in any cell of the column whose width is to be adjusted.
￭ Click on the menu item Format ▶ Adjust width.
￭ Under Column width, enter the number of characters of a col-

umn and confirm with [OK].
or
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￭ Position the cursor in the title line of the table between two col-
umns.
The cursor assumes the following form:
￭ Drag the column width to the required size keeping the left
mouse button pressed down.
3 Adjust the cell format

￭ Click on the menu item Format ▶ Fields....
￭ Carry out the required settings and confirm with [OK].
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4 Change the font

￭ Click on the menu item Format ▶ Fonts....
￭ Carry out the required settings and confirm with [OK].
Selecting determinations
Proceed as follows to select one or more lines of the determination over-

view:
1 Select a line
￭ Place the mouse button on the left edge of the line to be
selected.
￭ Click on the line.
2 Select several lines

￭ Place the mouse button on the left edge of the line to be
selected.
￭ Keep the mouse button pressed down and move over the left
edge of all lines to be selected.
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3 Select all lines

￭ Click on the menu item Edit ▶ Select all records.
or
￭ Click on the upper left in the title line.
Searching for determinations
Proceed as follows to search for specific determinations.

A detailed description of the parameters can be found at "Find What",
page 101.
1 Open search field

￭ Click on the symbol or the menu item Determina-
tion ▶ Find...
The dialog window Find in field: 'Field name' appears.
2 Enter search criteria

￭ Enter the search term and the other search criteria.
￭ Click on the button [Find first] in order to search through the
determination overview.
Sorting determinations
Proceed as follows to sort the columns of the determination overview:
1 Sort column ascending

￭ Click in the title line of the column to be sorted.
The entire column is highlighted in black.
tion ▶ Sort ▶ Ascending.
2 Sort column descending

￭ Click in the title line of the column to be sorted.
The entire column is highlighted in black.
tion ▶ Sort ▶ Descending.
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3 Remove sorting again

￭ Click on the symbol or the menu item Determination ▶ Fil-
ter ▶ Remove filter/sorting.
Displaying or hiding selected determinations
Proceed as follows to display or hide previously selected determinations

only:
1 Select determinations
￭ See "Selecting determinations", page 91.
2 Display selected determinations only

ter ▶ Filter selection.

4 Hide selected determinations

ter ▶ Selection not in filter.
Filtering determinations with the "Selection based filter"
Proceed as follows to filter the entries of the determination overview

according to a specific selection (cell or cell content):
1 Filter the entries

￭ Click in that cell which contains the required filter criterion (e.g.
Determination date = "12.2005").
ter ▶ Selection based filter.
Only the entries with the Determination date "12.2005" are dis-
played in the dialog window.
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Filtering determinations with the special filter
With a special filter you can define complex conditions for filtering and
sorting data sets. In the following section, you will see a simple example
of a special filter. You will find a detailed description of all parameters
under "BestimmungsübersichtFilter", page 103.

ter ▶ Special filter/sorting....
2 Select the fields which are to be filtered

￭ In the dialog window Anzeigeübersicht, double-click on the
field Determination date.
￭ In the dialog window Anzeigeübersicht, double-click on the
field Temperature.
NOTICE
In the dialog window Anzeigeübersicht, only those field are

available for selection which are displayed in the determination
overview (see "Formatting the determination overview", page 88).
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The two fields are displayed in the lower part of the window under
Field:
3 Specify the filter criteria

￭ In the column determination date in field Criteria enter the
value 05.04.2000* (incl. asterisk as wildcard).
￭ In the column Temperature and the field Criteria enter the
value > 110.
NOTICE
You will find a detailed description of the possible filter criteria

under "Criteria", page 103.
4 Apply and remove the filter

ter ▶ Apply filter/sorting.
In the window Determination data, all determination data is
now displayed that was carried out on April 5, 2000 at a tempera-
ture of over 110 °C. In addition, the dialog window Determina-
tion data uses the word FILTER to indicate that the displayed
data is filtered.
The special filter has been removed again.
Deleting determinations
NOTICE
Only the Administrator can delete determinations.
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Proceed as follows to delete specific entries from the determination over-

view:
1 Select the determination

2 Delete the entry

￭ Click on the menu item Determination ▶ Delete.
The safety prompt Do you really want to delete the selected
determinations? appears.
￭ Confirm the security query with [Yes].
Printing and exporting the determination overview
See Chapter 4.7.6, Page 129.
Parameter description
Selection
Selection of all fields, which can still be selected for the determination
overview. The following fields of the determination overview are
available:
Send to file
Directory in which the determination file (TXT file) has been saved.
Evaluation sensitivity used for the determation of the induction time.
User
Name of the user who was logged in when recording the determination.
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Determination date
Date and time at which the determination was started.
Block
Letter of the block used for the determination.
Delta Kappa
Formula 1 for induction time

Result of the calculation with formula 1.
Formula 2 for stability time


Gas flow
Gas flow through sample.
Unit
Number of the instrument used for the determination.
ID 1
ID 2
Induction time automatic

Automatically determined induction time.
Induction time manual

Induction time manually determined with the reevaluation.
Channel
Number of the channel used for the determination.
Method name
Name of the method with which the determination has been carried out.
Standard time
Automatically calculated standard time.
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Serial number
Serial number of the instrument used to record the determination.
Stability time
Automatically or, with the reevaluation, manually determined stability
time.
Temperature
Temperature as defined in the method.
Cell constant
Cell constant of the conductivity measuring cell used to record the deter-
mination.
Display
Fields which have been selected for the determination overview.
Selection Fields of the determination overview
Move all fields in Selection to Display.
Move selected field in Selection to Display. The field is inserted at the

end of the list.
Move selected field in Selection to Display. The field is inserted above

the field selected in Display.
Move selected field in Display to Selection.
Move all fields in Display to Selection.
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Column width
Width of the column in characters.
Entry 'Number of characters'
Standard width
Reset the column width to standard width (18.5 characters).
[Best Fit]
Adjust the column width to the longest field content (including title).
Gridlines Shown
Horizontal
Display horizontal grid lines.
Vertical
Display vertical grid lines.
Cell Effect
Selection Flat | Raised | Sunken
Flat
Flat view of the cells.
Raised
Raised view of the cells.
Sunken
Sunken view of the cells.
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Gridline Color
Color of the horizontal and vertical grid lines.
Selection Color
Background color
Color of the cell background.
Selection Color
Preview
Display of the selected format for the cells.
Font
Selection of the font type from the fonts installed on the PC.
Selection Font type
Effects
Underline
Choice of underlining for characters.
Color
Color for the selected font type.
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Selection Color
Font style
Choice of font style for the selected font type.
Selection Standard | Italic | Bold | Bold italic
Sample
Display of the selected font type.
Size
Font size in points for the selected font type.
Selection Font size
Find What
Required search term.
Entry 'Search term'
The following characters can be used as wildcards:
*: any character sequence (e.g. *ab, *ab*, ab*)
?: single character (e.g. a?a, ??a, ab?)
#: single numeral (e.g. ##20, ab###, #23##)
Search
Search mode
Selection All | Down | Up
All
Search in the entire table.
Down
Search downwards as far as the table end.
Up
Search upwards as far as the table start.
Match
Search area where the entered text is to be searched for.
Selection Whole field | Start of field | Any part of field
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Whole field
The search is only successful if the entire field matches the search term.
Start of field
The search is successful if the start of the field content matches the
search term.
Any part of field
The search is successful if the field content partly matches the search
term.
Match case
If this option is activated, the search is only successful if the uppercase and
lowercase of the search term and field content match.
Search Fields As Formatted

If this option is activated, the unit is also matched in the search for the
entire field content in fields with units (e.g. °C, h). If only the numerical
value is to be searched for, this option must be deactivated.
Search Only Current Field

If this option is activated, the search is restricted to the selected field. The
field name is displayed in the window title. This option is not available if
one or more entire lines are selected.
[Find first]
Start search at the start of the determination overview.
[Find next]
Continue with the search at the cursor location in the determination over-
view.
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Field
Selection of a field (column) from the determination overview.
Selection Field from the determination overview
Sort
Sorting for the selected field.
Selection Ascending | Descending | (not sorted)
Criteria
Criteria for filtering data sets.
or
Further criteria for filtering data sets.
In the lines Criteria and or and in all following lines, data sets can be fil-
tered using expressions. An expression is a combination of operators,
functions and field names for determining a condition for filtering data
sets. In the following only the most important elements and rules are
described and a few selected examples are given. For more extensive
information please refer to the documentation on Microsoft Access.
Operators, functions, Mathematical +, –, =, *, /
field names operators
Comparison opera- <, >, <>, <=, >=, Between…, And…
tors
Logical operators AND, OR, NOT
Wildcards * (any character string), ? (single character), #
(single numeral)
Current date Date()
Current time Now() (date and time)
Other fields ["Field name"]
Links with various If conditions are specified in various fields, these conditions can also be
fields linked with AND and OR. The following applies:
Criteria in the same line apply as AND conditions, i.e. only those data sets
are displayed which satisfy all conditions.
Criteria in various lines apply as OR conditions, i.e. all data sets which fulfill
one condition are displayed.
Examples > 10 Values greater than 10.

*oil* All data with "oil" as part of the name.
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*2007* All data of the year 2007.

Between Date() All data of the previous week.
And (Date() - 7)
4.7.2 Determination and method data

For each determination you can view all the determination data (name,
determination date etc.) and method data (name, parameters etc.) and
print or export these.
Displaying determination and method data
Proceed as follows to display all determination and method data for a

selected determination:
1 Display determination overview

￭ See "Displaying the determination overview", page 88.

￭ Select the desired determination (see "Selecting determinations",
page 91).
￭ In the Results window, click on the symbol or the menu item
View ▶ Determination and method data.
The dialog window Determination and method data appears.
Printing and exporting determination and method data
See Chapter 4.7.6, Page 129.
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ID 1
ID 2
Determination date
Date and time at which the determination was started.
User
Name of the user logged in when recording the determination.
Serial number
Serial number of the instrument used to record the determination.
Cell constant
Cell constant of the conductivity measuring cell used to record the deter-
mination.
GLP test
GLP status at the time of recording the determination. The following dis-
plays are possible:
GLP test switched off: The GLP monitoring was not activated for either
temperature or conductivity or gas flow.
GLP test due: The next GLP test was due.
GLP test not passed: The last GLP test carried out was not passed.
GLP test passed: The last GLP test carried out was passed.
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Display of the instrument, block and channel on which the determination

was carried out.
Induction time automatic

Automatically determined induction time.
Induction time manual

Induction time manually determined with the reevaluation.
Stability time
Automatically or, with the reevaluation, manually determined stability
time.
Delta Kappa



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Standard time
Automatically calculated standard time.
Method name
Name of the method.
Creation date
Date when the method was last saved.
Creator
Name of the logged in user who last saved the method.
Method description
Description of the method.
Temperature
Setpoint temperature of the sample.
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Delta T
Temperature correction: indication of how much the block temperature
has been increased so that the sample reaches the setpoint temperature.
Gas flow
Gas flow through sample.
Use internal pump

Gas supply with internal pump switched on/off.
Start options
Start delay
Waiting time until starting the measurement.
Start mode
Mode for starting the channels:
per channel: all channels were started individually.
per 2 channels: 2 channels each have been started jointly.
per block: the 4 channels of a block were started jointly.
Stop criteria
Time
Time until the automatic stop of the determination.
Conductivity
Conductivity limit value. The determination was automatically ended upon
reaching this value.
Endpoint
Automatic stop of the determination, as soon as every endpoint (induction
and stability time) has been reached.
Actions at end of determinations...
Shut off heater

The heating was automatically deactivated at the end of the determina-
tion.
Shut off gas flow

The gas flow was automatically deactivated at the end of the determina-
tion.
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Evaluate induction time

The induction time has been automatically determined (see "Induction
time", page 67).
Evaluate stability time

The stability time has been automatically determined (see "Stability time",
page 68).
Delta Kappa
Options for induction time
Evaluation delay
Start
suppression.
End
pression.
Evaluation sensitivity used for the determation of the induction time.
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The automatically determined induction time was calculated with these
values and saved under the name shown in the field "R1".

The automatically determined stability time was calculated with these val-
ues and saved under the name shown in the field "R2".

The automatically determined stability time was calculated with these val-
ues and saved under the name shown in the field "R3".
Calculation of standard time

Indicates whether the standard time has been calculated or not.

AOCS Cd12b-92: Formula calculation according to standard AOCS
Cd12b-92 with Target temperature = 110 °C.
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AOM: Formula calculation according to standard AOM with Target tem-

perature = 97.8 °C.
free: Formula calculation with freely selectable Target temperature.
Formula parameters
Factor
Parameter for the calculation of the standard time. It indicates by which
factor the time changes per 10 °C.
Target temperature
Time axis (x)
Autoscaling
Automatic definition of the start and end value of the time axis.
Manual scaling
Manual definition of the end value of the time axis.
End value
End value of the time axis with manual scaling.
Conductivity axis (y)
Autoscaling
Automatic definition of the start and end value of the conductivity axis.
Manual scaling
Manual definition of the end value of the conductivity axis.
End value
End value of the conductivity axis with manual scaling.
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Report elements
Header
Output of the header.
Curve
Method description
Output of the method description entered on the tab Description.
Results
Output of the results selected below.
Method parameters
Results
Output of the selected results: Induction time, Stability time, Stan-
dard time, Formula 1...3.
Automatic report output
Send to printer immediately

Automatic printout of the report after finishing the determination.
Send to file
Automatic output of determination and method data after finishing the
determination as a TXT file.
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Directory
Directory in which the report has been saved.
Description
The following warning messages are possible for incorrectly executed
determinations:
Temperature not reached: setpoint temperature at start of the determi-
nation not reached.
Missing measuring points (start time): measuring points are missing
from the given time (in s) onwards.
Missing measuring points (end time): measuring points are present
again from the given time (in s) onwards.
Manual Stop: the determination was stopped manually with [Stop].
Stop after communication error: Automatic stop of the determination
because of interrupted connection between the Rancimat and the PC.
Value
Value for warning (e.g. temperature, time).
4.7.3 Graph and reevaluation

You can either open a graph of an individual determination (single
graph) or have graphs of several determinations displayed above one
another (multiple graph). In addition, you can open the so-called live
graph of a determination, in the dialog window of which you can man-
ually perform reevaluations of measuring curves.
You have the following options for reevaluation of graphs:
￭ Setting the induction time manually
￭ Setting the stability time manually
￭ Setting tangents manually
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Single graph, multiple graph or live graph
Proceed as follows to open a single graph or several graphs:

2 Open single graph

￭ Select the determination for which the graph is to be displayed
(see "Selecting determinations", page 91).
tion ▶ Graphics ▶ Single graph.
The dialog window with the single graph appears (ID 1 / ID 2).
If present, the determined induction time (red, vertical line and
numerical value) and stability time (black, vertical line and numeri-
cal value) are displayed in the graphics window next to the mea-
surement curve (green). A maximum of 16 single graph windows
can be opened.
NOTICE
In contrast to the windows Multiple graph and Live graph, the

window with the single graph is not automatically updated upon
selecting another determination in the determination overview
3 Open multiple graph

￭ Select the determinations for which the graphs are to be dis-
played (see "Selecting determinations", page 91).
tion ▶ Graphics ▶ Multiple graph.
The dialog window Multiple graph appears.
The individual measurement curves are displayed in color, the legends
for the color (sample identifications ID 1 and ID 2) are located in the
header of the graph. If present, the determined induction time (▼)
and stability time (▲) are displayed as well.
4 Open live graph

￭ Select the determination for which a reevaluation of the measure-
ment curve is to be performed (see "Selecting determinations",
page 91).
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tion ▶ Graphics ▶ Live graph with reevaluation.
The dialog window Live graph appears.
If present, the determined induction time (red, vertical line and
numerical value) and stability time (black, vertical line and numeri-
cal value) are displayed in the graphics window next to the mea-
surement curve (green).
With the button [Evaluation] you can display the second derivative
of the measuring curve as well as the used evaluation sensitivity.
Zooming graphs, switching on/off offset and autoscaling
Proceed as follows to adjust the graph display:
1 Zoom graph
￭ See "Zooming", page 32.
2 Switch on/off offset for multiple curves

￭ Right click in the dialog window of a multiple graph.
￭ Click on the menu item Offset.
The offset for the displayed measurement curve is switched on or
switched off.
In the case of an activated offset, the curves are arranged with an
offset above one another. Instead of the usual lettering of the con-
ductivity axis, the difference of the entire axis is in this case displayed
in µS/cm.
3 Switch on/off autoscaling for single and live graphs

￭ Right click in the dialog window of a single graph or live graph.
￭ Click on the menu item Autoscaling.
The autoscaling for the displayed measurement curves is now acti-
vated or the manually performed scaling (see chapter 4.5.2.3, page
68) is canceled.
If this option is activated, the start and end values of the axes are
automatically specified in such a way that all measured values are
visible.
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Copying graphs and pasting them into other programs
Proceed as follows to copy a graph to the clipboard and then paste it into
another program:
1 Copy graph
￭ Right click in the dialog window of a graph.
￭ Click on the menu item Copy.
2 Paste graph
￭ Open program (e.g. Word, Excel, any graphics program, etc.)
￭ Paste the graph using the key combination [Ctrl] + [V].
Printing graphs
See "Printing graphs", page 131.
Setting the induction time manually
Proceed as follows to subsequently and manually set the induction time:

￭ Right click in the dialog window of a live graph and click on the
entry Reevaluation in the context-sensitive menu.
The dialog window Reevaluation appears.
2 Set induction time

￭ Place the cursor on the red line.
￭ With the [Ctrl] key and left mouse button pressed down,
drag the line to the required location.
The value of the manually set induction time is displayed both in the
dialog window Live graph at the top right beside the red line and
also in the dialog window Reevaluation under Manual.
3 Save changes
￭ In the dialog window Live graph click on the button [Save].
The new induction time is accepted in the determination overview.
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Setting the stability time manually
In order to set the stability time manually, you need to adjust the conduc-
tivity change Delta Kappa. After this, the stability time is recalculated
automatically. Proceed as follows:

2 Adjust Delta Kappa

￭ Under Delta Kappa enter the required value and confirm with
the symbol .
The value of the calculated stability time is displayed both in the dia-
log window Live graph at the top right beside the gray line and also
in the dialog window Reevaluation under Stability time.
3 Save changes
The new stability time is accepted in the determination overview.
Setting tangents manually
For determining the induction time, you can manually set the tangents.
The induction time is then defined as the intersection of the tangents.
Set the tangents as follows:

2 Set first tangent

￭ Keep the [Ctrl] key and left mouse button pressed down to
set the first tangent.
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3 Set second tangent

￭ Keep the [Shift] key and left mouse button pressed down to
set the second tangent.
4 Adjust the position of the tangents

￭ Position the cursor on a black square on the tangent.
The cursor assumes the form of a cross hair.
￭ Keep the [Ctrl] key and the left mouse button pressed down
to move the point to the required position.
After you have adjusted the position of both tangents, you can read
the value of the new induction time both in the dialog window Live
graph at the top right beside the red line and also in the dialog win-
dow Reevaluation under Manual.
5 Save changes
The new induction time is accepted in the determination overview.
Deleting manually set tangents
Proceed as follows to delete the previously set tangents:
1 Delete tangents
Resetting all reevaluations
1 Reset induction and stability time to the original value

￭ Click on the [Reset] button.
4.7.4 Extrapolation
Extrapolation can be used to extrapolate the results measured at various
temperatures to the required target temperature. In addition, the factor
for converting the induction time to the standard time can be deter-
mined.
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Extrapolation of several results
Proceed as follows to carry out an extrapolation of several results:

￭ Open the Results window and the database (see "Displaying the
determination overview", page 88).
￭ Select the required determinations (see "Selecting determina-
tions", page 91).
￭ Click on the menu item Determination ▶ Extrapolation.
The dialog window Extrapolation with the extrapolation values
which the program has calculated from the selected results (determi-
nations) appears.
2 Select result and target temperature

￭ Click on the [Settings] button.
￭ Select the result which is to be used for extrapolation (Induction

time, Stability time, etc.).
￭ Enter the Target temperature.
NOTICE
The time determined for a particular sample by extrapolation to

low target temperatures (e.g. 25 °C) is a purely theoretical value.
The interrelation between this time and e.g. the perishability of the
sample must be determined experimentally.
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3 Update the display

￭ Click on the [Update] button.
The graph and all results are updated.
NOTICE
For extrapolation of the induction times, the manually changed

values of the selected determinations (if present) are used, other-
wise the automatically determined values are used.
Setting the correlation limit
NOTICE
The correlation limit for the correlation coefficient r2 can only be set
by an Administrator.

￭ In the Results window, click on the menu item
Options ▶ Administrator ▶ Extrapolation parameter.
2 Adjust limit
￭ Under correlation limit (r2) enter a value between 0 and 1 and
confirm with [OK].
Copying a graph and pasting it into other programs
See "Copying graphs and pasting them into other programs", page 116.
Printing extrapolation results
See "Printing extrapolation results", page 133.
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In the graphic temperature vs. time the linear regression is used to rep-
resent the calculated straight line T = ln(t)/B – ln(A)/B. The measured val-
ues of the selected determination are shown in black, the regression line
in green and the time calculated for the target temperature in red.
Results
Formula
Exponential formula for calculating the time extrapolated from the mea-
sured values for the target temperature.
A
Calculated coefficient A of the exponential formula.
B
Calculated coefficient B of the exponential formula.
r2
Calculated correlation coefficient. If this value is below the limit value (see
"Setting the correlation limit", page 120) specified by the administrator a
warning appears when opening the extrapolation window.
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Time
Result of the extrapolation for the target temperature in hours and years.
Target temperature
Target temperature for the extrapolation.
Number of determinations
Number of determinations used for the extrapolation.
Standard factor
Value determined from the regression straight line which indicates the fac-
tor by which the time changes per 10 °C. This value can be entered in the
formula for the determination of the standard time as a factor (see "Cal-
culation of standard time", page 110).
[Settings]
Open the dialog window Program settings. The extrapolation parame-
ters are to be entered in the tab Extrapolation (see ""Extrapolation"
tab", page 140).
[Update]
Update graphics and result display. This function has to be carried out if
the selection of determinations in the determination overview or the set-
tings for the extrapolation have been changed.
[Detail]
Display only the area with the results of the determinations in the graph.
4.7.5 Recalculating a determination

For a determination, you can recalculate the Induction time, the Stabil-
ity time, the Formulas and the Standard time.
Recalculating the induction time
Proceed as follows to recalculate the induction time:

￭ Select the determination which is to be recalculated (see "Select-
ing determinations", page 91).
￭ Click on the menu item Determination ▶ Recalculation.
The dialog window Recalculation appears.
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￭ Activate the options Recalculate induction time and Calcula-
tion active.
￭ Under Evaluation delay and Evaluation suppression
start/end, enter the required values.
￭ Under Evaluation sensitivity, enter the required value.
The software suggests a value with which the highest maximum
of the second derivative is accepted as the induction time. If there
is no suggestion then the highest maximum has already been
accepted.
The default value "1" will lead to the correct result for most appli-
cations. Smaller values will cause the acceptance of smaller maxi-
mums of the second derivative. Higher values require a higher
maximum.
NOTICE
A detailed description of the parameters can be found at "Recalcu-

late induction time", page 125.
Recalculating the stability time
Proceed as follows to recalculate the stability time:


￭ Activate the options Recalculate stability time and Calcula-
tion active.
￭ Under Delta Kappa enter the required value and confirm with
[OK].
NOTICE

late stability time", page 126.
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Recalculating formulas
Proceed as follows to recalculate the results of the formulas:

￭ Click on the tab Formulas.

￭ Activate the options Recalculate formula 1 for induction
time and Calculation active.
or
Activate the options Recalculate formula 2 for stability time
and Calculation active.
or
Activate the options Recalculate formula 3 for stability time
and Calculation active.
￭ Re-enter the parameters for the formula and confirm with [OK].
NOTICE

late formula 1 for induction time", page 127.
Recalculating the standard time
Proceed as follows to recalculate the standard time:

￭ Click on the tab Standards.

￭ Activate the options Recalculate standard time and Calcula-
tion active.
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￭ Under Formula according to... and Formula parameters,

enter the required values and confirm with [OK].
NOTICE

late standard time", page 128.
Recalculate induction time

Activate/Deactivate recalculation of the induction time. If the recalculation
is deactivated, the original result is kept.
Calculation active
If this option is activated, the parameters can be re-entered for the calcu-
lation of the induction time.
If this option is deactivated, the original result is deleted.
Evaluation delay
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Evaluation suppression start

suppression.
Evaluation suppression end

pression.
This value defines the minimum value which the maximum of the curve of
the second derivative has to reach in order to be accepted as a result. The
result, i.e. the induction time, is the time until the first accepted maximum.
The default value "1" will lead to the correct result for most applications.
Smaller values will cause the acceptance of smaller maximums of the sec-
ond derivative. Higher values require a higher maximum.
The software suggests a value with which the highest maximum of the
second derivative is accepted as the induction time. If there is no sugges-
tion then the highest maximum has already been accepted.
Recalculate stability time

Activate/Deactivate recalculation of the stability time. If the recalculation is
deactivated, the original result is kept.
Calculation active
If this option is activated, Delta Kappa can be re-entered for the calcu-
lation of the stability time.
Delta Kappa
Conductivity change for the determination of the stability time in µS/cm.
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Recalculate formula 1 for induction time

Activate/Deactivate the recalculation of the result calculated with formula
1. If the recalculation is deactivated, the original result is kept.
Calculation active
If this option is activated, the parameters for formula 1 can be re-
entered.
Recalculate formula 2 for stability time

Calculation active
entered.
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Recalculate formula 3 for stability time

Calculation active
entered.
Recalculate standard time

Activate/Deactivate the recalculation of the standard time from the
induction time. If the recalculation is deactivated, the original result is
kept.
Calculation active
If this option is activated, the parameters for the calculation of the stan-
dard time can be re-entered.

Selection AOCS Cd12b-92 | AOM | free
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AOCS Cd12b-92
Formula calculation according to standard AOCS Cd12b-92 with Tar-
get temperature = 110 °C.
AOM
Formula calculation according to standard AOM with Target temper-
ature = 97.8 °C.
free
Formula calculation with freely selectable Target temperature.
Formula parameters
Factor
Parameter for the calculation of the standard time, which indicates the
factor by which the time changes per 10 °C.
Target temperature
4.7.6 Printing and exporting data
Printing results from the Control window
Proceed as follows to print results of the completed determinations shown

in the Control window:

item File ▶ Print....
2 Print results
￭ If required, adjust the column width (see "Formatting the deter-
mination overview", page 88).
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￭ Select the required determinations and click on [Print].

The results are printed according to the settings which have been
defined in the method on the tab Documentation.
Printing determination overview
You can print a determination overview either in the form of a table or a

list. Proceed as follows:

2 Select type of output (table or list)

￭ Click on the symbol or the menu item File ▶ Print....
The dialog window Printing of... appears.
￭ Click on the option Overview table and/or Overview list.
NOTICE
In the overview table, only those columns are printed which are
within the maximum print width (15 cm).
3 Print determination overview

￭ Click on the [Print] button.
The dialog window Print appears.
￭ Select the required printer and click on [Print].
The determination overview will be printed.
Printing determination and method data
Proceed as follows to print the determination and method data of one or

several determinations:

2 Select determination
￭ Select the determination of which the data is to be printed (see
"Selecting determinations", page 91).
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3 Select data
￭ Select the option All determination and method data and
confirm with [Print].
4 Print data
The determination and method data will be printed.
Printing graphs
Proceed as follows to print a single graph, multiple graph or live graph:
1 Open graph
￭ See "Single graph, multiple graph or live graph", page 114.
2 Print graph
The graph will be printed.
Printing the report defined in the method
Proceed as follows to print the report of one or several determinations,

which has been defined in the method (see chapter 4.5.2.6, page 72):

￭ Select the determination of which the report is to be printed (see
3 Select data
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￭ Select the option Determination according to method and

confirm with [Print].
4 Print report
The report will be printed.
Printing the report defined under "Settings"
Proceed as follows to print the report of one or several determinations,

which has been defined under Settings:

￭ Select the determination of which the report is to be printed (see
3 Select data
￭ Select the option Determination according to settings.
4 Carry out settings

￭ Click on the [Settings] button.
The dialog window Program settings appears.
￭ Carry out the required settings (see tab "Report settings", page
137) and confirm with [OK].
5 Print report
￭ Click on the [Print] button.
The report will be printed.
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Printing extrapolation results
Proceed as follows to print the extrapolation graph (normal and

detailed view), the extrapolation results and the overview of the deter-
minations used for the extrapolation with the fields ID 1, ID 2, tempera-
ture and result:
1 Display extrapolation results

￭ See "Extrapolation of several results", page 119.
2 Print extrapolation results

The extrapolation results will be printed.
Exporting the determination overview to Word or Excel
Proceed as follows to export the determination overview to Word or Excel:
1 Select determinations
If you do not select any determinations, the entire overview is
exported.
2 Select export program

tion ▶ Export ▶ Export to MS Word.
The data is copied to a RTF file to be opened automatically by
Microsoft Word.
or

tion ▶ Export ▶ Export to MS Excel.
Microsoft Excel will be opened automatically.
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Exporting determination and method data to a TXT file
Proceed as follows to export the determination and method data of one

or several determinations to a TXT file:

￭ Select the determination of which the data is to be exported (see
3 Export data
tion ▶ Export ▶ Determination and method data.
The dialog window Save to export file appears.
￭ Select memory location, enter file name and confirm with [Save].
The determination and method data will be exported.
Exporting determinations to another database
You can export determinations from a database to another existing data-

base or a newly created database. Proceed as follows:

￭ Select the determination to be exported (see "Selecting determi-
nations", page 91).
3 Select database
￭ Click on the menu item Determination ▶ Export ▶ Export to
database.
The dialog window Export data to... appears.
￭ Select an existing database.
or
Under File name enter the name for the new database.
￭ Confirm the selection or entry with [Save].
The following message appears (only for the Administrator):
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4 Keep or delete determination

￭ Click on [No] to also keep the exported determination in the
original database.
￭ Click on [Yes] to delete the exported determination in the origi-
nal database.
Opening the database in Microsoft Access 97
NOTICE
Each database is password-protected. The password is generated auto-

matically by the program and can only be read by the Administrator.
The databases are saved in the installation directory of the 743 Ranci-
mat program at C:\Program Files\Metrohm\Rancimat\Database.

item File ▶ Results....
The Results window appears.
2 Read out database password

￭ In the Results window, click on the menu item
Options ▶ Administrator ▶ Database password.
The dialog window Open appears.
￭ Select the required database and confirm with [Open].
The dialog window Password appears with the password for the
previously selected database.
3 Open database in Microsoft Access 97

￭ Start Microsoft Access 97.
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￭ Open the required database by entering the previously read out

password.
Exporting the measured value list
Proceed as follows to export a list of all measured values to a TXT file:

￭ Select the determination of which the data is to be exported (see
3 Export data
tion ▶ Export ▶ List of measured values.
The dialog window Save to export file appears.
￭ Select the memory location, enter the file name and confirm with
[Save].
The measured values list will be exported.
4.7.7 Program settings
Carrying out settings for the representation and output of

results
You can carry out settings for the representation and output of results as
follows:

￭ In the Results window, click on the menu item Options ▶ Set-
tings.
2 Carry out settings

￭ See the following "Report settings" tab.
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4.7.7.1 Parameter description
"Report settings" tab

On the Report settings tab, you can carry out the settings for the report
output.
Definition of elements for report output
Header
Output of the header with company settings (if defined, see "Company
settings" tab), date of the printout, sample identifications, instrument
information, determination date, user, cell constant and serial number.
Results
Output of the results selected in the Results tab (see page 139).
Curve
Method parameters
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Method description
Output of the method description entered in the tab Description.
Definition for multiple graph printing
with offset
If this option is activated, the curves are arranged with an offset above
one another in the case of an output of multiple graphs. Instead of the
usual lettering of the conductivity axis, the difference of the entire axis is,
in this case, printed in µS/cm.
"Company settings" tab

On the Company settings tab, you can carry out the settings for the
output of company logo and company text in the header.
[Company-logo…]
Open the window Find company logo for selecting the graphics file
with the company logo. Only WMF or BMP files can be used. After click-
ing on [Open], the logo is displayed in the adjoining window.
[Remove logo]
Remove the embedded company logo.
Logo on the...
Selection left side | right side
left side
The company logo is printed out on the left edge of the header.
right side
The company logo is printed out on the right edge of the header.
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Company text
The text entered here is printed out on the side of the header opposite the
company logo.
Entry Characters
"Results" tab
On the Results tab, you can carry out the settings for the result output.
Output of the following results on the reports:
Induction time
Stability time



Standard time
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"Scaling" tab
On the Scaling tab, you can carry out the settings for scaling the curve
axes.
Acc. to method
Axis scaling in accordance with the settings defined in the method under
Curve representation (see chapter 4.5.2.3, page 68).
Autoscaling
Automatic definition of the start and end values of the curve axes.
Manual scaling
Manual definition of the start and end values of the curve axes.
X Start
Start value of the time axis in hours.
X End
End value of the time axis in hours.
Y Start
Start value of the conductivity axis in µS/cm.
Y End
End value of the conductivity axis in µS/cm.
"Extrapolation" tab
On the Extrapolation tab, you can carry out the settings for the extrapo-
lation.
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Induction time
The induction time is used for extrapolation. If the induction time has
been determined manually, this value will be used and not the automati-
cally determined induction time.
Stability time
The stability time is used for extrapolation.

The result calculated with formula 1 is used for extrapolation.


Target temperature
Temperature, for which the selected result is to be converted. The conver-
sion is realized using the regression straight line (from the extrapolation).
Input range freely selectable - °C
"Live graph" tab

On the Live graph tab, you can carry out the settings for displaying the
live graph.
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Retain zoom at determination change

The selected zoom range is retained when changing the determination in
the determination overview.
Live graph always on top

The Live graph window is always displayed in the foreground.
4.7.8 Arranging windows

In the Results window, you can arrange the opened dialog windows either
above one another, beside one another or overlapping. Proceed as
follows:
1 Open windows
￭ Open all required dialog windows.
The following dialog windows can be opened in the Results win-
dow:
– Determination overview (View ▶ Determination over-
view)
– Graphs (Determination ▶ Graphics ▶ Single/Multiple/
Live graph)
– GLP window (View ▶ GLP)
2 Arrange windows
￭ Click on the menu item Window ▶ Tile vertically or Win-
dow ▶ Tile horizontally or Window ▶ Cascade.
The opened dialog windows are correspondingly arranged.
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4.8 GLP functions

4.8.1 General information on GLP and validation
GLP (Good Laboratory Practice) requires, amongst other things, the peri-
odical testing of analytical measuring devices for their reproducibility and
correctness on the basis of Standard Operating Procedures (SOP).
An example of such a standard operating procedure for the 743 Rancimat
is available from Metrohm under the title Application Bulletin No. 278 –
Validation of Metrohm Rancimats.
The operating software for the 743 Rancimat contains prepared GLP
tests for temperature, conductivity and gas flow measurement. The user
can determine whether and which tests have to be carried out. In addi-
tion, the time interval between the tests and the accuracy requirements
can be specified. If the GLP function is activated, each results report
receives a comment whether the GLP tests are fulfilled. Metrohm offers a
GLP test set to carry out these tests .
Further information on the subject of QA, GLP and validation can also be
found in the brochure Quality Management with Metrohm available from
your Metrohm representative.
Electronic and mechanical functional groups in Metrohm instruments can
and should be checked as part of regular service by specialist personnel of
the manufacturing company. All Metrohm instruments are provided with
start-up test routines which check the perfect functioning of the relevant
assemblies when switching on the instrument. If no error message is dis-
played, it can be assumed that the instrument functions without fault.
The 743 Rancimat also contains an integrated diagnostic program which
enables the service technician to check certain assemblies if any faults or
incorrect functioning occur and localize the fault.
4.8.2 GLP monitoring
Activating/Deactivating GLP monitoring
Proceed as follows to either activate or deactivate the GLP monitoring for

the temperature, the conductivity and the gas flow:

￭ If several instruments are connected: In the Control window,
use the menu item View ▶ Unit x to select the required instru-
ment.
￭ Click on the menu item Tools ▶ GLP test ▶ Properties....
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The dialog window GLP properties for unit with serial no. x
appears.
2 Activate monitoring
￭ In the Temperature tab, activate the option Enable GLP moni-
toring.
￭ Carry out the remaining settings (see "Parameter description",
page 144) and confirm with [OK].
3 Deactivate monitoring
￭ Open the dialog window GLP properties for unit with serial
no. x (see step 1).
￭ In the required tab (Temperature, Conductivity, Gas flow),
deactivate the option Enable GLP monitoring and confirm with
[OK].
Enable GLP monitoring

Activate/Deactivate automatic GLP monitoring.
GLP alert interval

Number of days until the implementation of the next GLP test.
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Tolerance
Indication of the tolerance value for the relevant GLP test. If the result is
within the range Setpoint ± Tolerance, the test is regarded as passed. If
you click on [Set default], the specified standard value is entered in this
field.
Additional alert message text

Additional message text which is to be added during the prompt for carry-
ing out the next GLP test.
4.8.3 GLP status
Displaying the GLP status
Proceed as follows to display the status of the GLP monitoring:

￭ If several instruments are connected: In the Control window,
use the menu item View ▶ Unit x to select the required instru-
ment.
￭ Click on the menu item Tools ▶ GLP test ▶ Status....
The dialog window GLP status for unit with serial no. x appears.
Test type
Type of GLP test (Temperature, Conductivity or Gas flow).
Next test due date

Date on which the next GLP test is to be carried out. If the GLP monitoring
is not activated, Disabled appears in this column.
Due in
Number of days until the next GLP test.
Last test result

Indication whether the test has been passed (Ok) or not (Not Ok!).
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4.8.4 Carrying out GLP tests

4.8.4.1 Temperature
For the GLP test for temperature measurement the calibrated tem-
perature sensor and the measuring insert are required (part of the option-
ally available GLP test set, ). For this, the temperature sensor must be con-
nected to the Pt100 connector on the rear of the 743 Rancimat.
5
Figure 7 Accessories for GLP test Temperature
1 Pt100 temperature sensor 2 PTFE cylinder
3 Hexagon screw 4 Hexagon key (6.2621.120)
5 Aluminum cylinder
Preparing the GLP test set
Proceed as follows in order to prepare the GLP test set according to Figure
7:
1 Assemble accessories
￭ Insert the temperature sensor from above into the opening of the
PTFE cylinder.
￭ Place the PTFE cylinder on the aluminum cylinder in such a way
that the temperature sensor fits into this opening.
￭ Push the temperature sensor into the aluminum cylinder as far as
the limit stop.
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2 Screw on accessories
￭ Use the hexagon key to lightly tighten the hexagon screw.
Carrying out the GLP test for the temperature measure-

ment
Proceed as follows to carry out the GLP test:
NOTICE
Before starting the GLP test, ensure that the temperature of the inserted
GLP test set is stable. If the GLP test set is used in a cold heating block,
this condition is fulfilled after the normal heating up time of the heating
block and the GLP test set. If the GLP test set, on the other hand, is
used in an already heated heating block, it is necessary to wait at least
30 min before starting the GLP test.
1 Select instrument and method

￭ In the Control window, use the menu item View ▶ Unit x to
select the instrument for which the GLP test is to be carried out.
￭ Under Unit x Block A and B, click on the symbol in order to
select the method whose temperature is required for the test.
￭ If required, adjust the temperature (see "Opening a selected

method and adjusting parameters", page 58).
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2 Enter calibration points of the temperature sensor

￭ Click on the menu item Tools ▶ GLP test ▶ Temperature... and
confirm with [Next >].
￭ Enter a Sensor name for the temperature sensor.

￭ Under Point 1…3, enter the Temperature and the Resistance
of the calibration point.
￭ Confirm the entry with [Next >].
3 Enter test parameters

￭ Under Channels used for test, select the required channels.
One channel per block has to be selected at least.
￭ Under Test duration per channel, enter the required test dura-
tion and confirm with [Next >].
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4 Insert GLP test set and start measurement

￭ Insert the prepared test set (see "Preparing the GLP test set",
page 146) in the channel of Block A to be checked.
￭ Connect the temperature sensor to the Pt100 connector on the
rear of the 743 Rancimat.
￭ In the dialog window GLP test for unit with serial no. x, click
on [Next >].
The test measurement is started.
As soon as the temperature defined in the method has been reached,
the following message appears:
Ext. temperature The temperature measured with the exter-

nal temperature sensor.
Measuring time The time elapsed since the start of the
temperature measurement.
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5 Carry out measurement for further channels
WARNING
The aluminum cylinder of the GLP test set is very hot. Do not
touch!
￭ As soon as the message appears with the prompt to insert the

external temperature sensor together with the measuring insert in
the next selected channel, rapidly carry out the change.
￭ Carry out measurement for each of the selected channels.
After the last measurement is completed, the dialog window with
the test results appears.
6 Confirm or reject results
✓ Test passed: The deviation of the measured temperatures

is within the specified tolerance.
✗ Test failed: The deviation of the measured temperatures is
greater than the specified tolerance.
￭ Confirm the results with [Finish].

or
￭ Reject the results with [Cancel].
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4.8.4.2 Conductivity
The GLP test for conductivity measurement can be carried out either
with a standard solution with a known conductivity or with the test
resistor 6.2109.030. The test resistor is part of the optionally avaiable
GLP test set . The test resistor must be connected during measurement at
the electrode connector (3-2) of the 743 Rancimat.
Carrying out the GLP test for the conductivity measure-

ment
NOTICE
Before carrying out the GLP test with standard solution for the first
time, the cell constants of the conductivity measuring cells must be
determined (see chapter 4.4.1, page 49).
1 Select instrument
￭ Carrying out the GLP test with the test resistor: continue with
step 2.
Carrying out the GLP test with the standard solution: continue
with step 3.
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2 Carry out GLP test with test resistor

￭ Click on the menu item Tools ▶ GLP test ▶ Conductivity... and
￭ Select the option Use test resistor.

￭ Under Resistance, enter the value of the test resistor in Ohms
(10000 Ω for 6.2109.030) and confirm with [Next >].
￭ Connect the test resistor to the electrode connector (3-2) indica-
ted in the dialog window and confirm with [Next >].
￭ Continue with step 4.
3 Carry out GLP test with standard solution

￭ Insert a measuring vessel, each filled with 60 mL standard solu-
tion, together with the measuring vessel cover at all measuring
position (see chapter 4.6, page 76).
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￭ Click on the menu item Tools ▶ GLP test ▶ Conductivity... and

￭ Select the option Use standard solution.

￭ Under Conductivity of standard solution, enter the conductiv-
ity in µS/cm and confirm with [Next >].
c(KCl) = 1 mmol/L can be used as a standard solution. This is
derived from the optionally available conductivity standard
6.2301.060 (KCl 0.1 mol/L) through dilution with distilled water. The
conductivity of this diluted solution is:
Temperature Conductivity
18 °C 127 µS/cm
19 °C 130 µS/cm
20 °C 133 µS/cm
21 °C 136 µS/cm
22 °C 138 µS/cm
23 °C 141 µS/cm
24 °C 144 µS/cm
25 °C 147 µS/cm
The conductivity is measured sequentially at all channels.

After the last measurement is completed, the dialog window with
the test results appears.
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✓ Test passed: The deviation of the measured conductivities

is within the specified tolerance.
✗ Test failed: The deviation of the measured conductivities is
greater than the specified tolerance.

or
4.8.4.3 Gas flow

For the GLP test for gas flow measurement, you require a gas flow
measuring device (not available from Metrohm), which can be used to
measure the gas flow at every channel.
Carrying out the GLP test for the gas flow measurement
1 Select instrument and start test

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￭ Click on the menu item Tools ▶ GLP test ▶ Gas flow... and
￭ Enter the Gas flow and confirm with [Next >].

2 Test all channels

￭ Measure the gas flow sequentially for all channels and enter the
values in the corresponding fields K1…K4 in L/h.
￭ After finishing the measurement, confirm the entries with
[Next >].
The dialog window with the test results appears.
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✓ Test passed: The deviation of the measured gas flow val-

ues is within the specified tolerance.
✗ Test failed: The deviation of the measured gas flow values
is greater than the specified tolerance.

or
4.8.5 GLP results
Printing the GLP certificate
NOTICE
To be able to print a test certificate, you have to activate the GLP moni-
toring (see "Activating/Deactivating GLP monitoring", page 143).
For the selected instrument, you can print a GLP certificate, which con-
tains the following information:
Print date, serial number of the instrument, results of the last GLP tests
(with date, test person and test results).
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Proceed as follows to print out a test identification:
1 Print GLP certificate

￭ In the Control window, click on the menu item Tools ▶ GLP
test ▶ Print GLP results....
Displaying the GLP results
NOTICE
If you want an overview of all GLP tests carried out with the connected
units, the database Repos.mrd must be open. If another database is
open, only those GLP tests are displayed which have also been exported
into this database during export of the determinations.
Proceed as follows to display the GLP results:
1 Open dialog window with overview

￭ Open the Results window (see "Opening and closing the Results
window", page 29).
￭ In the Results window, click on the menu item View ▶ GLP
and select the required test results (Temperature, Conductivity,
Gas flow).
The following dialog windows appear, depending on the selection
previously made.
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2 Display detailed results

￭ Double click on the required GLP test within the fields Date,
Serial number or Channel.
The dialog window GLP Temperature, GLP Conductivity or GLP
Gas flow appears.
Printing GLP results
NOTICE
To be able to print out the GLP results, you have to activate the GLP
monitoring (see "Activating/Deactivating GLP monitoring", page 143).
Proceed as follows to print the GLP results:
1 Open dialog window with overview

￭ Open the Results window (see "Opening and closing the Results
window", page 29).
￭ In the Results window, click on the menu item View ▶ GLP
and select the required test results (Temperature, Conductivity,
Gas flow).
2 Select data
￭ In the Results window, click on the menu item File ▶ Print....
If the database contains GLP test results which have been attained
with different instruments, the dialog window Select unit
appears.
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￭ Select the Serial number of the required instrument and confirm

with [OK].
￭ Select the required printing option and confirm with [OK].
Printing options
Selection Last certificate | Certificate of date | All tem-
perature GLPs | All conductivity GLPs | All gas
flow GLPs
Last certificate
Printout of the last GLP certificate of the selected overview window.
The printout contains the Serial number of the instrument, the Date,
the Tester and the Test result.
Certificate of date
Printout of the GLP certificate for the entered date. The printout con-
tains the Serial number of the instrument, the Date, the Tester and
the Test result.
All temperature GLPs
Printout of the detailed results for all GLP tests for temperature mea-
surement.
All conductivity GLPs
Printout of the detailed results for all GLP tests for conductivity mea-
surement.
All gas flow GLPs
Printout of the detailed results for all GLP tests for gas flow measure-
ment.
743 Rancimat ￭￭￭￭￭￭￭￭ 159

5.1 General information ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
5 Handling and maintenance
5.1 General information

5.1.1 Care
The 743 Rancimat requires appropriate care. Excess contamination of the
instrument may result in functional disruptions and a reduction in the ser-
vice life of the sturdy mechanics and electronics.
Spillages of chemicals and solvents should be cleaned up immediately.
Above all, the plug connections on the rear of the instrument (in particular
the mains connection socket) should be protected from contamination.
CAUTION
Although this is extensively prevented by design measures, the mains

plug should be unplugged immediately if aggressive media has penetra-
ted the inside of the instrument, so as to avoid serious damage to the
instrument electronics. In such cases, the Metrohm Service must be
informed.
5.1.2 Maintenance by Metrohm Service

Maintenance of the 743 Rancimat is best carried out as part of an annual
service, which is performed by technicians of the Metrohm company. If
working frequently with caustic and corrosive chemicals, a shorter mainte-
nance interval could be necessary.
The Metrohm service department offers every form of technical advice for
maintenance and service of all Metrohm instruments.
160 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Handling and maintenance
5.2 Replacing the dust filter

The dust filter (3-20) is mounted in the opening marked with Filter on
the rear of the instrument and serves for filtration of the air sucked in
through the air pump. It must be checked at periodic intervals and
replaced in the case of more intense contamination (order number:
6.2724.010).
5.3 Regenerating or replacing the molecular sieve
NOTICE
Regenerate the molecular sieve regularly.

The intervals at which you have to regenerate the molecular sieve
depends on the air humidity in the laboratory and also on the fre-
quency of use of the instrument.
The molecular sieve filled in the drying flask (3-11) serves for adsorption
of disruptive oxidizing gases as well as of the water from the sucked in air.
You can regenerate the molecular sieve in the drying oven at approx.
+140…+180 °C for 24 to 48 h. You can order a new molecular sieve
under the order number 6.2811.000.
CAUTION
Do not fill the hot molecular sieve directly into the drying flask after
regeneration, as otherwise the plastic filter on the filter tube will melt.
Wait until the molecular sieve has cooled down before filling.
743 Rancimat ￭￭￭￭￭￭￭￭ 161

5.4 Self test when switching on ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
5.4 Self test when switching on

An internal hardware self test executes after switching on the instrument.
Each one of the 7 test steps lasts around one second and is displayed on
the instrument number display (2-5) by a combination sample of the 4 dis-
play lamps. In the case of an error, the corresponding LEDs flash.
Display Cause Remedy

Device
LED test. If not all LEDs Notify Metrohm Service.
light up during this test,
an LED is defective.
Device
RAM test error. Switch the instrument
off and on again. If the
error occurs again,
please notify Metrohm
Service.
Device
PROM checksum test Switch the instrument
error. off and on again. If the
error occurs again,
Service.
Device
BUSY test error. Switch the instrument
error occurs again,
Service.
Device
ADC test error. Switch the instrument
error occurs again,
Service.
Device
EEPROM test error. Switch the instrument
error occurs again,
Service.
Device
Defective mains voltage Check power supply.
(deviation > 10 %).
162 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting
6 Troubleshooting
6.1 Problems
Problem Cause Remedy
The pump is louder The air flow is blocked ￭ Check dust filter (3-20) and, if necessary,
than normal. somewhere before or after replace.
the pump. ￭ Check filter tube (4-4) on the drying flask
cover for blockages and, if necessary, free
with a gentle tap.
￭ Examine FEP tubings (2-6), (3-13),(3-14)
and (3-17) for blockages and, if necessary,
replace.
Extra air is sucked in at ￭ Check FEP tubings (3-13), (3-14) and

somewhere else other than (3-17) for cracks, kinks etc. and tighten. If
the dust filter. There is a necessary, replace.
leak somewhere in the sys- ￭ Place the drying flask cover (3-10) correctly
tem before the pump. on the drying flask and screw tight.
No air flow can be The air supply is blocked. ￭ Remove FEP tubing (5-1) from the thread
detected in the reac- adapter (5-3). A slight air flow must be dis-
tion vessel (it does cerned here. If this is not the case, please
not bubble), contact Metrohm Service.
although the pump ￭ Check FEP tubing (2-6) for blockages. If
is running. necessary, clean or replace.
￭ Check thread adapter (5-3) and air tube
(5-5) on the reaction vessel cover for
blockages. If necessary, clean or replace.
The FEP tubing for the air Check FEP tubing (2-6) for cracks, kinks etc. If
supply is defective. necessary, replace.
The FEP tubing for the air Tighten FEP tubing (2-6) on both sides.
supply is not connected
correctly.
The air tube (5-5) does not ￭ Push reaction vessel cover (5-8) down as
immerse in the sample. far as the limit stop.
￭ Use more sample.
743 Rancimat ￭￭￭￭￭￭￭￭ 163

6.1 Problems ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

No air flow can be The connection is blocked. ￭ Check tubing connector (5-4) on the reac-
detected in the mea- tion vessel cover for blockages and, if nec-
suring vessel (it does essary, clean.
not bubble), ￭ Check silicone tubing (5-2) for blockages
although an air flow and, if necessary, clean.
can be discerned in ￭ Check tubing adapter (5-11) and PTFE
the reaction vessel. tube (5-17) on the measuring vessel cover
for blockages and, if necessary, clean.
The connection is leaking. Check silicone tubing (5-2) for leakages and, if
necessary, replace.
The reaction vessel cover ￭ If the reaction vessel cover is oblique or not
(5-8) is not mounted cor- completely mounted, press down as far as
rectly or is too loose. the limit stop.
￭ If the reaction vessel cover is loose on the
reaction vessel despite correct assembly,
the cover has to be replaced.
The connection is wrongly ￭ Ensure that the PTFE tube (5-17) is moun-
connected. ted to the air supply at the opening In
(5-13) of the measuring vessel cover.
￭ Ensure that the silicone tubing (5-2) is
mounted on the tubing adapter, which is
mounted in the opening In (5-13).
￭ Ensure that the reaction vessel is connected
to the measuring vessel belonging to the
corresponding measuring place.
The conductivity is The conductivity of the Check the conductivity of the water used and,
displayed in the water used is too high. if necessary, use deionized water from another
upper part of the source.
Live window during
startup. The conductivity measuring Check cell constant of the measuring cell. The
cell is contaminated. cell constant should be between 1.0 and 1.2.
If this is not the case, the measuring cell must
be cleaned (see chapter 4.6.5, page 84).
The induction times The reaction vessels used ￭ Free the reaction vessel of particles (dust,
are not reproducible are not clean. cardboard, glass fragments etc.) with com-
for multiple determi- pressed air before weighing in the sample.
nations. ￭ Only use new, unused reaction vessels.
164 ￭￭￭￭￭￭￭￭ 743 Rancimat


The reaction vessels used Only use new, unused reaction vessels.
are scratched on the
inside.
The reaction vessel cover ￭ If the reaction vessel cover is oblique or not
(5-8) is not mounted cor- completely mounted, press down as far as
rectly or is too loose. the limit stop.
￭ If the reaction vessel cover is loose on the
reaction vessel despite correct assembly,
the cover has to be replaced.
The connection to the Ensure that no air can escape through leaks
measuring vessel is not when transferring from the reaction vessel to
mounted correctly. the measuring vessel.
The temperature in differ- Check temperature in the different positions

ent channels of a heating (see chapter 4.8.4.1, page 146). If necessary,
block differs, as there are carefully remove the impurities from the cold
burn marks at one or more heating block.
places in the opening of
the heating block.
The temperature in differ- Determine the temperature correction Delta T

ent heating blocks differs. for each block separately (see chapter 4.4.2,
page 51).
The sample is not homoge- Homogenize sample.

nous.
The stability times The cell constant was not ￭ Determine cell constant (see chapter 4.4.1,
are not reproducible determined or does not page 49).
for multiple determi- correspond to the value ￭ Ensure that the measuring cell is always
nations. entered. used in the same channel, so that the cell
constant determined once also corre-
sponds to the measuring cell.
￭ Ensure that the measuring cell is not con-
taminated. If necessary, clean (see chapter
4.6.5, page 84).
The conductivity measuring Check measuring cell (see chapter 4.8.4.2,

cell is contaminated. page 151) and, if necessary, clean.
See also: The induction

times are not reproducible
for multiple determina-
tions.
743 Rancimat ￭￭￭￭￭￭￭￭ 165

6.1 Problems ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

The induction time The temperature is not ￭ Ensure that the correct method for the
is longer/shorter selected correctly. determination has been selected.
than expected. ￭ Check that Temperature and Delta T
have been specified correctly in the
method (see chapter 4.5.2.1, page 61).

times are not reproducible
for multiple determina-
tions.
The stability time is Delta Kappa is not defined Ensure that the value of Delta Kappa defined
longer/shorter than correctly. in the method is correct (see chapter 4.5.2.2,
expected. page 65).
See also: The stability times

are not reproducible for
multiple determinations.

time is longer/shorter than
expected.
The measurement The air supply for the mea- Loosen tubing adapter (5-11) on the measur-
curves are extremely suring solution is directed ing vessel cover, turn the PTFE tube (5-17) in
noisy. to the conductivity measur- such a way that the air is no longer directed to
ing cell. the measuring cell and fix in this position.
Gas bubbles adhere to the ￭ Ensure that the measuring cell is clean and
conductivity measuring cell free of fat. If necessary, clean thoroughly
during measurement. (see chapter 4.6.5, page 84).
￭ In some cases ultra pure water contains a
large proportion of dissolved air which
escapes during measurement. In this case,
degas the ultra pure water before the mea-
surement for 5 to 10 min in a vacuum.
During the measurement, ￭ Keep the measuring time as short as possi-

sample evaporates in the ble, by about 4 to 6 h. The induction time
reaction vessel and con- can be reduced by about half by increasing
denses in the measuring the temperature by 10 °C.
vessel. This results in con-
tamination of the conduc-
tivity measuring cell, which
in turn promotes adher-
ence of gas bubbles.
166 ￭￭￭￭￭￭￭￭ 743 Rancimat


￭ Reduce the temperature so that less sample
evaporates or no sample at all. However,
this can substantially extend the measuring
time. The induction time approximately
doubles by reducing the temperature by 10
°C.
The curve shows a Side reactions occur at the ￭ In the method, use the option Evaluation
step which means start or during the mea- delay or Evaluation suppression (see
that the induction surement, which cause the chapter 4.5.2.2, page 65).
time is no longer conductivity in the measur- ￭ Do not use Endpoint(s) as a stop criterion
determined cor- ing cell to rise. in the method, but instead a defined Con-
rectly. ductivity (e.g. 200 µS/cm) (see chapter
4.5.2.1, page 61). The curves can then also
be evaluated manually after finishing the
determination.
The curve shows a The reaction vessel cover ￭ Thoroughly clean the reaction vessel cover
step at the start of (5-8) and/or the tubing and the silicone tubing (see chapter 4.6.5,
the measurement, (5-2) still contain residues page 84).
which has not occur- which are transported into ￭ Replace the reaction vessel cover and the
red in previous the measuring vessel silicone tubing from time to time.
measurements. through the warm air flow
when a new measurement
is started.
The induction time The option Evaluate Activate the evaluation of the induction time in
is not evaluated induction time is deacti- the method (see chapter 4.5.2.2, page 65).
automatically, vated in the method.
although a signifi-
The option Evaluation Deactivate the corresponding option in the
cant break point can
delay or Evaluation sup- method (see chapter 4.5.2.2, page 65).
be noticed in the
pression is defined in the
curve.
method, which prevents
the evaluation of the curve
in the corresponding time
period.
Automatic detection of the Keep the determination running until the

induction time is not yet induction time is automatically found.
possible.
The curve progression is Do not use Endpoint(s) as a stop criterion in

too flat with the result that the method, but instead a defined Conductiv-
automatic detection of the ity e.g. 200 µS/cm (see chapter 4.5.2.1, page
induction time is not possi- 61). Evaluate the curves afterwards manually
ble.
743 Rancimat ￭￭￭￭￭￭￭￭ 167

6.1 Problems ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

using tangents (see "Setting tangents man-
ually", page 117).
The measurement The measurement has been Keep the measurement running until the end-
aborts without an stopped manually. point is automatically found.
endpoint being
found. A time or conductivity is Deactivate time or conductivity as a stop crite-
defined as a stop criterion rion in the method (see chapter 4.5.2.1, page
in the method, which was 61) or increase the corresponding value for the
reached before the end- time or conductivity.
point.
Error The heating is defective. Switch the instrument off and on again. If the
error occurs again, please contact Metrohm
Service.
The maximum temperature Switch the instrument off and on again. If the
(220 °C) has been error occurs again, please contact Metrohm
exceeded by 10 °C. Service.
Error Error during self test. Switch the instrument off and on again. If the
error occurs again, please contact Metrohm
Service.
168 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications
7 Technical specifications
7.1 General data

Number of instru- 1…4
ments that can be
connected
Number of sam- 1…8 (4 each per heating block)
ples per instru-
ment
Sample amount Several grams / several milliliters
7.2 Temperature regulation and measurement

Range setpoint 50…220 °C
temperature
Temperature cor- 0…±9.9 °C
rection (Delta T) (can be entered manually or determined automatically using the exter-
nal temperature sensor)
Temperature mea- 0…250 °C
suring range
Resolution 0.1 °C
Max. deviation of ±0.3 °C
the heating block
temperature from
the set value
(50…220 °C)
Reproducibility of typ. < 0.2 °C
the set tempera-
ture
Max. temperature typ. < 0.3 °C
difference
between different
measuring posi-
tions per block
Temperature fluc- typ. < 0.1 °C
tuations (at attained operating temperature, inserted and identically filled reac-
tion vessels and 20 L/h air throughput)
743 Rancimat ￭￭￭￭￭￭￭￭ 169

7.3 Conductivity measurement ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Shutdown temper- 260 ± 11 °C

ature (if this temperature is exceeded, the heating is shut down, and
switched on again at 210 ± 11 °C)
Heating up time approx. 45 min (from 20 °C to 120 °C)
for the instrument approx. 60 min (from 20 °C to 220 °C)
Instrument exter- < 50 °C
nal temperature (at operating temperature 220 °C)
7.3 Conductivity measurement

Sensor Conductivity measuring cell, integrated in the measuring vessel cover
6.0913.130
Structure Conductivity measuring cell with 2 steel electrodes
Measuring princi- AC current measurement with 1 kHz frequency and approx. 1.7 V
ple amplitude (peak to peak)
Cell constant 1.00…1.20
(the exact value can be entered manually or determined automatically)
Measuring range 0…400 µS/cm
Resolution 0.1 µS/cm
Maximum error ±1 % ± 0.5 µS/cm
7.4 Gas flow regulation

Pump Membrane pump
Adjustable range 7…25 L/h
Max. deviation ±10 %
from the set range
170 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications
7.5 GLP test set

External tempera-
ture sensor
Type Pt100 casing element ⌀1.9 mm, in 4-conductor technology; DIN IEC
751 Class B
Calibration 0…90 °C: ±0.02 °C
accuracy 90…220 °C: ±0.03 °C
Max. deviation ±0.3 °C
of the mea-
sured tempera-
ture from the
true value (50…
220 °C)
Test resistor 10 kΩ
7.6 RS-232 interface

Plug Sub-D plug, 9-pin (male)
Basic settings 9600 Baud, 8 Bit, 1 stop bit, no parity, XON/XOFF
7.7 Mains connection

Voltage 2.743.0014: 220…240 V ± 10 %
2.743.0015: 100…120 V ± 10 %
Frequency 50…60 Hz
Power consump- 450 W
tion
Fuse Diameter 5 mm, length 20 mm
100…120 V: 2.0 ATH (slow-acting)
220…240 V: 4.0 ATH (slow-acting)
743 Rancimat ￭￭￭￭￭￭￭￭ 171

7.8 Ambient temperature ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
7.8 Ambient temperature

Nominal function +5…+45 °C
range (at 20…80 % humidity)
Storage –20…+70 °C
Transport –40…+70 °C
7.9 Housing
Cover material Polyurethane hard foam (PUR) with flame retardation for fire class
UL94VO, CFC-free
Base material Steel, painted
Width 405 mm
Height 268 mm (without accessories)
353 mm (with accessories)
Depth 466 mm
Weight 20.2 kg (without accessories)
27.6 kg (with accessories)
172 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Accessories
8 Accessories
Up-to-date information on the scope of delivery and optional accessories
for your product can be found on the Internet. You can download this
information using the article number as follows:
Downloading the accessories list
1 Enter https://www.metrohm.com/ into your Internet browser.
2 Enter the article number (e.g. 743) into the search field.
The search result is displayed.
3 Click on the product.

Detailed information regarding the product is shown on various tabs.
4 On the Included parts tab, click on Download the PDF.

The PDF file with the accessories data is created.
NOTICE
Once you have received your new product, we recommend download-

ing the accessories list from the Internet, printing it out and keeping it
together with the manual for reference purposes.
743 Rancimat ￭￭￭￭￭￭￭￭ 173

Index ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
Index
A Determination .......................... 26 Filter
Access rights Delete ................................ 95 Determinations ................... 93
Adjust ................................ 36 Filter ................................... 93 Formulas .................................. 70
Manage ............................. 35 Prepare ............................... 82 Fuse
Accessories Recalculate ....................... 122 Replace .............................. 18
Mount ................................ 10 Search ................................ 92
Administrator password Select ................................. 91 G
Set ..................................... 22 Sequence ........................... 76 Gas flow
Air purification Sort .................................... 92 Method .............................. 63
Mount accessories .............. 10 Start ................................... 84 Range ............................... 170
Air supply external Stop manually .................... 86 Switch on / off .................... 40
Mount accessories .............. 13 Determination data GLP monitoring
Air supply internal Display ............................. 104 Activate / Deactivate ......... 143
Mount accessories .............. 10 Export .............................. 134 Display status ................... 145
Print ................................. 130 GLP test
C Determination overview Conductivity ..................... 151
Calibration data ........................ 54 Display ............................... 88 Gas flow ........................... 154
Cell constant Export .............................. 133 Results .............................. 156
Determine .......................... 49 Format ............................... 88 Temperature ..................... 146
Clean Print ................................. 130 Graph
Accessories ......................... 84 Device information ................... 43 Print ................................. 131
Measuring vessel ................ 84 Diagnosis ................................. 43 Group
Reaction vessel ................... 85 Drying flask Add .................................... 36
Tubings .............................. 85 Mount ................................ 12 Adjust access rights ............ 36
Computer Dust filter Delete ................................ 38
Connect ............................. 20 Mount ................................ 11
Conductivity measurement Replace ............................ 161 H
Measuring range .............. 170 Heating
Resolution ........................ 170 E Range ............................... 169
Connect Electrostatic charge .................... 6 Start automatically .............. 39
Power grid .......................... 19 Emulsion fat ............................. 77 Start manually .................... 82
Control window ....................... 26 Evaluation ................................ 65 Turn off .............................. 83
Menus ................................ 27 Event overview ......................... 46 Heating up duration ................. 83
Structure ............................ 26 Export Heating up time ..................... 170
Symbols .............................. 28 Determination and method
Curves ...................................... 68 data ................................. 134 I
Determination overview .... 133 Induction time .......................... 66
D Measured value list ........... 136 Live graph ........................ 115
Database To another database ......... 134 Multiple graph .................. 114
Open .................................. 88 External temperature .............. 170 Recalculate ....................... 122
Open in Microsoft Access 97 Extrapolation .................... 26, 118 Single graph ..................... 114
......................................... 135 Extrapolation results Instrument communication ....... 34
Optimize ............................ 42 Print ................................. 133 Instrument information ............. 43
Repos.mrd .......................... 29
Delta T F L
Determine .......................... 51 Fat Live graph
Method .............................. 62 Emulsion fats ...................... 77 Display ............................. 113
Derivative Non-liquid, pure fats ........... 77 Print ................................. 131
Second derivative ............. 115 File types .................................. 31 Log file ..................................... 46
174 ￭￭￭￭￭￭￭￭ 743 Rancimat

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index
Login GLP results ....................... 158 Print ................................. 131

For the first time ................. 22 Instrument information ....... 43 Software
Method parameters ............ 61 Installation ......................... 20
M Program Start ................................... 25
Measuring vessel Optimize ............................ 42 Stability time ............................ 66
Equip .................................. 13 Program number ...................... 44 Live graph ........................ 115
Method .................................... 26 Program start ........................... 25 Multiple graph .................. 114
Create ................................ 56 For the first time ................. 22 Recalculate ....................... 123
Delete ................................ 60 Protocol ................................... 32 Single graph ..................... 114
Open .................................. 58 Standard time
Rename .............................. 58 R Recalculate ....................... 124
Save ................................... 57 Reaction vessel Standart time ........................... 71
Method data Equip .................................. 13 Start delay
Display ............................. 104 Recalculation .................... 26, 122 Method .............................. 63
Export .............................. 134 Reevaluation ..................... 26, 117 Start mode
Print ................................. 130 Report Method .............................. 63
Method parameters Print instrument information Start options
Adjust .......................... 57, 61 ........................................... 44 Method .............................. 63
Adjust during the determina- Print method information ... 72 Status overview ........................ 45
tion .................................... 85 Results ...................................... 26 Stop criteria
Print ................................... 61 Results window ........................ 28 Method .............................. 64
Molecular sieve Close .................................. 29 Supply voltage ............................ 6
Regenerate ................. 12, 161 Menus ................................ 30 Switch off ................................. 19
Mouse functions ...................... 32 Open .................................. 29 Switch on ................................. 19
Multiple graph Structure ............................ 29 System requirements ................ 20
Display ............................. 113 Symbols .............................. 30
Print ................................. 131 Rights T
Activate/Deactivate ............. 37 Temperature
O Method .............................. 62
Oil S Record ................................ 41
Pure, clear oils .................... 77 Safety instructions ...................... 4 Temperature correction
Sample identification Determine .......................... 51
P Clear list ............................. 83 Temperature measuring
Parameter description Enter .................................. 83 Measuring range .............. 169
Determination overview ...... 96 Samples, prepare ...................... 77 Reproducibility .................. 169
Method .............................. 61 Emulsion fats ...................... 80 Resolution ........................ 169
Parameters Non-liquid, pure fats ........... 77 Timer ........................................ 38
Adjust .......................... 57, 61 Pure oil ............................... 77
Adjust during the determina- Samples containing oils and U
tion .................................... 85 fats ..................................... 78 User
Print ................................... 61 Self test .................................. 162 Add .................................... 37
Password Sensor calibration data ............. 54 Delete ................................ 38
Set ..................................... 22 Serial number ........................... 44 User group
PC Service ....................................... 5 Add .................................... 36
Connect ............................. 20 Service diagnosis ...................... 43 Adjust access rights ............ 36
Power connection .................... 19 Shutdown temperature .......... 170 Delete ................................ 38
Print ....................................... 129 Single graph
Extrapolation results ......... 133 Display ............................. 113 Z
GLP certificate .................. 156 Zooming .................................. 32
743 Rancimat ￭￭￭￭￭￭￭￭ 175

743 Rancimat: Manual

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743 Rancimat: Manual

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743 Rancimat

This documentation is protected by copyright. All rights reserved.

2 Overview of the instrument 7

743 Rancimat ￭￭￭￭￭￭￭￭ III

4.1.7 Mouse functions .................................................................... 32

IV ￭￭￭￭￭￭￭￭ 743 Rancimat

5 Handling and maintenance 160

7 Technical specifications 169

743 Rancimat ￭￭￭￭￭￭￭￭ V

VI ￭￭￭￭￭￭￭￭ 743 Rancimat

1.1 Instrument description

743 Rancimat ￭￭￭￭￭￭￭￭ 1

1.2 Rancimat method

2 ￭￭￭￭￭￭￭￭ 743 Rancimat

Figure 1 Measuring arrangement (schematic representation)

1.3 About the documentation

Please read through this documentation carefully before putting the

1.3.1 Symbols and conventions

Cross-reference to figure legend

743 Rancimat ￭￭￭￭￭￭￭￭ 3

[Next] Button or key

1.4 Safety instructions

Operate this instrument only according to the information contained in

Hot reaction vessels

The reaction vessels can become very hot.

4 ￭￭￭￭￭￭￭￭ 743 Rancimat

Defective glass vessels

Caution with defective glass vessels.

1.4.2 Electrical safety

Only personnel qualified by Metrohm are authorized to carry out service

Never open the housing of the instrument. The instrument could be

743 Rancimat ￭￭￭￭￭￭￭￭ 5

An incorrect supply voltage can damage the instrument.

Protection against electrostatic charges

Electronic components are sensitive to electrostatic charges and can be

1.4.3 Flammable solvents and chemicals

All relevant safety measures are to be observed when working with

1.4.4 Recycling and disposal

6 ￭￭￭￭￭￭￭￭ 743 Rancimat

2 Overview of the instrument

Figure 2 Front 743 Rancimat

1 Pilot lamp 2 Gas flow display

3 Temperature display 4 Error display (red)

5 Instrument number display 6 FEP tubing 250 mm (6.1805.080)

7 Measuring vessel cover (6.0913.130) 8 Measuring vessel (6.1428.100)

743 Rancimat ￭￭￭￭￭￭￭￭ 7

9 Silicone tubing (6.1816.010) 10 Reaction vessel cover (6.2753.107)

11 Reaction vessel (6.1429.040)

Molecular sieve flask

Made by Metrohm Herisau Switzerland Filter

1 Collection tube holder 2 Electrode connector

3 Air supply connection 4 Mains switch

5 Mains connection socket 6 Fuse holder

7 Type plate 8 RS-232 connector

8 ￭￭￭￭￭￭￭￭ 743 Rancimat

9 Pt100 connector 10 Drying flask cover (6.1602.145)

11 Drying flask (6.1608.050) 12 Flask holder

13 FEP tubing 250 mm (6.1805.080) 14 FEP tubing 250 mm (6.1805.080)

15 "From Flask" connection 16 "Air/N2 in" connection