Teachware
Metrohm AG
CH-9100 Herisau
teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.
Documentation in additional languages can be found on
http://products.metrohm.com under Literature/Technical documenta-
Figure 4Mounting accessories for the air supply (rear of the instrument) ...... 11
Figure 5Equipping the reaction and measuring vessels ................................. 14
Figure 6Equipping the reaction vessel for determining Delta T ...................... 51
Figure 7Accessories for GLP test Temperature ............................................ 145
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VI
743 Rancimat
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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 temperature. 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 743Rancimat. Up to 4 instruments can be connected to each PC, hence
allowing a maximum of 32 samples to be analyzed. The evaluation algorithm of the PC program determines the break point of the Rancimat
curve fully automatically and hence the induction time. Besides the induc-tion 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
conductivity 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 particular, the induction times can be converted to the default temperatures of
the corresponding standards.
1 Introduction
Each Rancimat curve can also be evaluated manually. A PC-supported
tangential method is available for this, in which you can position the tangents 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, recalculation 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 temperature, 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 stating whether the GLP tests have been fulfilled. Metrohm
743 Rancimat
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1
1.2 Rancimat method
offers a GLP test set to carry out these tests (see Optional accessories,
page 185).
1.2 Rancimat method
The decay of vegetable and animal fats, which can be perceived in the initial stage through a deterioration of odor and taste (rancidity), is to a
great extent the result of chemical alterations caused by the effect of
atmospheric 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 multiple stages resulting in diverse decomposition products, in particular peroxides as primary oxidation products and alcohols, aldehydes and
carboxylic 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 induction period, which is a good indicator for the oxidation stability.
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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.
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
second to the instrument part in the figure.
MethodDialog text, parameter in the software
Instruction step
Carry out these steps in the sequence shown.
743 Rancimat
File ▶ New
Menu or menu item
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3
1.4 Safety instructions
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[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
1.4 Safety instructions
1.4.1 General notes on safety
Warning
This instrument may only be operated in accordance with the specifications 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
This symbol draws attention to a possible damage of
instruments or instrument parts.
Note
This symbol marks additional information and tips.
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4
Warning
The reaction vessels can become very hot.
Avoid any contact with the hot reaction vessels. Place these in the vessel holders provided for cooling down.
743 Rancimat
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1 Introduction
Flammable substances
Warning
The oven of the 743 Rancimat can be heated to 220 °C.
Flammable substances may ignite at these temperatures.
Adjust the maximum heating temperature of the oven to the sample
being examined.
Defective glass vessels
Warning
Caution with defective glass vessels.
An overflow of flammable samples into the heating block can be dangerous.
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).
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
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.
Warning
Warning
743 Rancimat
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5
1.4 Safety instructions
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Mains voltage
Warning
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains 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.
Always pull the mains cable out of the mains connection socket before
connecting or disconnecting electrical appliances on the rear panel 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. laboratory
flue).
■Keep all sources of flame far from the workplace.
■Clean up spilled fluids and solids immediately.
■Follow the safety instructions of the chemical manufacturer.
1.4.4 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.
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6
743 Rancimat
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743
Rancimat
11
10
9
8
7
6
5
4
3
2
1
2 Overview of the instrument
2 Overview of the instrument
Figure 2Front 743 Rancimat
743 Rancimat
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7
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Molecular sieve flask
Filter
Air out
2
Air/N in
Pt 100
RS 232
WARNING - Fire Hazard -
with the same type and rating of fuse
For continued protection replace only
100-115V: 4A(TH)
Fuse
Made by Metrohm Herisau Switzerland
From
flask
To
flask
220-240V: 2A(TH)
Type:
Nr.:
U:
f:
S:
14
3
4
5
6
89 10
1315
16
181920
1
2
Pilot lamp
1
Lights up when the instrument is switched
on.
Temperature display
3
Flashes when the heating is switched on.
Lights up when the temperature has been
reached.
Instrument number display
5
Indicates the number of the instrument.
Lights up if the instrument is registered.
Flashes (all LEDs) if the connection to the PC
is interrupted.
Measuring vessel cover (6.0913.130)
7
Contains an integrated conductivity measuring cell.
Silicone tubing (6.1816.010)
9
For connecting the reaction vessel to the
measuring vessel.
Reaction vessel (6.1429.040)
11
Gas flow display
2
Flashes when the gas flow is switched on.
Lights up when the gas flow has been
reached.
Error display (red)
4
Lights up or flashes when a fault has occurred in the instrument (see TroubleshootingChapter).
FEP tubing 250 mm (6.1805.080)
6
For supplying air into the reaction vessel.
Measuring vessel (6.1428.100)
8
Reaction vessel cover (6.2753.107)
10
Figure 3Rear 743 Rancimat
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8
743 Rancimat
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2 Overview of the instrument
Collection tube holder
1
For fastening the optional exhaust collection
tube (6.2757.000).
Air supply connection
3
For connecting the FEP tubing 250 mm
(2-6).
Mains connection socket
5
For important information on the mains connection, see Chapter 3.3.
Type plate
7
Contains specifications concerning mains
voltage and serial number.
Pt100 connector
9
For connecting an external temperature sensor.
Drying flask (6.1608.050)
11
FEP tubing 250 mm (6.1805.080)
13
For supplying the air from the internal pump
to the drying flask.
Electrode connector
2
For connecting the conductivity measuring
cell integrated in the measuring vessel cover
(2-7).
Mains switch
4
For turning the instrument on and off.
I = ON / 0 = OFF.
Fuse holder
6
Replacing fuses, see Chapter 3.3.2.
RS-232 connector
8
For connecting the PC.
Drying flask cover (6.1602.145)
10
Cover for the drying flask.
Flask holder
12
For fastening the drying flask.
FEP tubing 250 mm (6.1805.080)
14
For supplying the air from the drying flask to
the reaction vessel (2-11).
"From Flask" connection
15
FEP tubing 130 mm (6.1805.010)
17
For connecting the Air out connection to
the Air/N2 in connection during normal
operation with the internal air pump.
"To Flask" connection
19
"Air/N2 in" connection
16
"Air out" connection
18
Dust filter (6.2724.010)
20
743 Rancimat
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9
3.1 Setting up the instrument
3 Installation
3.1 Setting up the instrument
3.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately 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 complete 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.
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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 fluctuations and direct sunlight.
Note
In order to improve accessibility for the measuring positions, the instrument 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:
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10
743 Rancimat
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Molecular sieveflask
Filter
Air out
2
Air/N in
From
flask
To
flask
8
9
10
12
11
1
2
3
6547
3 Installation
Figure 4Mounting accessories for the air supply (rear of the instru-
ment)
Drying flask cover (6.1602.145)
1
Cover for the drying flask.
Flask holder
3
For fastening the drying flask.
FEP tubing 250 mm (6.1805.080)
5
For supplying the air from the internal pump
to the drying flask.
"From Flask" connection
7
"To Flask" connection
9
FEP tubing 130 mm (6.1805.010)
11
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
■If the laboratory air is heavily contaminated, a tubing for supply-
Drying flask (6.1608.050)
2
Filter tube (6.1821.040)
4
FEP tubing 250 mm (6.1805.080)
6
For supplying the air from the drying flask to
the reaction vessel (2-11).
Dust filter (6.2724.010)
8
"Air out" connection
10
"Air/N2 in" connection
12
on the rear of the Rancimat.
ing fresh air can be connected to the dust filter.
743 Rancimat
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11
3.2 Mounting accessories
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Note
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 filter 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).
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12
Note
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).
743 Rancimat
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3 Installation
■Screw the other end of the FEP tubing onto the Air/N
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).
in con-
2
Note
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 39).
3.2.3 Equipping the reaction and measuring vessels
The following figure shows in detail, how the accessories parts for measuring the oxidation stability have to be mounted and connected to one
another.
743 Rancimat
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13
3.2 Mounting accessories
2
1
3
4
5
6
7
8
9
10
20
16
12
11
13
14
15
17
18
19
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Figure 5Equipping the reaction and measuring vessels
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743 Rancimat
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3 Installation
FEP tubing 250 mm (6.1805.080)
1
For supplying air into the reaction vessel.
Thread adapter M8 / M6 (6.1808.090)
3
Air tube (6.2418.100)
5
Connection
7
For connecting the thread adapter M8 / M6.
Foam barrier (6.1451.010)
9
Tubing adapter M8 / olive (6.1808.050)
11
For connecting the silicone tubing to the
opening In (5-13).
Opening "In"
13
For supplying the air to the measuring vessel.
Connector plug
15
Silicone tubing (6.1816.010)
2
For connecting the reaction vessel to the
measuring vessel.
Tubing connector
4
For connecting the silicone tubing.
O-ring (6.1454.040)
6
Reaction vessel cover (6.2753.107)
8
Reaction vessel (6.1429.040)
10
Opening "Out"
12
For removing the air from the measuring
vessel.
Labeling field
14
For entering the cell constant.
Measuring vessel cover (6.0913.130)
16
Contains integrated conductivity measuring
cell.
PTFE tube (6.1819.080)
17
For supplying the air to the measuring solution.
Protection ring
19
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)
■Screw the tubing adapter M8 / olive (5-11) into the opening In of
■Place the measuring vessel cover (5-16) on the measuring vessel
2
Mount the reaction vessel cover
■Insert the air tube (5-5) from below into the connection (5-7) of
■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-
Electrode
18
Measuring vessel (6.1428.100)
20
of the measuring vessel cover.
the measuring vessel cover.
(5-20).
the reaction vessel cover.
tion (5-7) and, at the same time, press the air tube against the
thread adapter M8 / M6.
743 Rancimat
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15
3.2 Mounting accessories
■Now fix the air tube onto the reaction vessel cover by firmly pull-
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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 (5-9) is at least 7 cm above the base of
the reaction vessel (5-10).
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 reaction vessel cover.
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16
743 Rancimat
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■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.
Note
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 measuring vessel 6.1428.020 can also be cleaned with acetone.
3.2.5 Mounting the exhaust collection tube (optional accessories)
The optionally available exhaust collection tube 6.2757.000 can be mounted on the 743 Rancimat for targeted removal of the exhaust air. In addition 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
3 Installation
■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).
743 Rancimat
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17
3.3 Mains connection
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.
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
Service.
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.
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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 voltage 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
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18
743 Rancimat
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4
Insert the fuse holder
■Push the fuse holder back into the instrument until it latches into
place.
3.3.3 Mains cable and mains connection
Mains cable
The mains cable optionally supplied for the instrument
■6.2122.020 with plug SEV 12 (Switzerland)
■6.2122.040 with plug CEE(7), VII (Germany, …)
■6.2122.070 with plug NEMA 5-15 (USA, …)
is three-core and provided with a plug with grounding pin. If another plug
has to be mounted, the yellow/green conductor (IEC standard) must be
connected to the protective ground (protection class I).
Warning
3 Installation
Any interruption to the grounding within or outside the instrument can
make it dangerous!
Mains connection
Plug the mains cable into the mains connection socket of the Rancimat.
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.
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.
743 Rancimat
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
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19
3.4 Connecting a PC
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 25pin 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 systemWindows 2000, Windows XP Professional, Win-
RAM256 MB (Windows 2000 / Windows XP)
ProcessorPentium III or higher
Memoryapprox. 20 MB for program files
RS-232 interfaceone free RS-232 interface (COM)
The windows user must have administrator rights in order to be able to
install 743 Rancimat.
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dows Vista
1 GB (Windows Vista)
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 >].
■■■■■■■■
20
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
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 will be installed.
7
Complete the installation
■Click on the [Finish] button after the successfully completed
The installation program will be exited.
3.4.2.3 Windows Vista
3 Installation
the program icon is to be inserted and confirm with [Next >].
installation.
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 Microsoft 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:
■Exit 743 Rancimat if you have started the software after the instal-
1
lation.
■Start the installation file by double-clicking and follow the instruc-
tions of the installation program.
743 Rancimat
■■■■■■■■
21
3.4 Connecting a PC
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 19).
■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 Rancimat.
■■■■■■■■■■■■■■■■■■■■■■
The login window for the Administrator opens:
3
Set Administrator password
■Do not enter a password, instead click on [OK].
■Confirm the displayed message with [OK].
The following dialog window appears:
■■■■■■■■
22
■Leave the Old password field empty.
■Enter a new password for the Administrator in the New pass-
word field.
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
■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].
3 Installation
Establishing the device communication
Follow the instructions in Section 4.2.1.
1
743 Rancimat
■■■■■■■■
23
4.1 Fundamentals of 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:
Note
■■■■■■■■■■■■■■■■■■■■■■
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
■In the Windows Start menu under Pro-
grams ▶ Metrohm ▶ Rancimat, click on the menu item Rancimat.
The following dialog window appears:
2
Log in
■Select the required User.
■Enter the Password and confirm with [OK].
3
Close program
■■■■■■■■
24
■Click on the menu item File ▶ Exitor the symbol in the upper
right corner of the dialog window.
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4.1.2 Terms
4 Operation
For opening and closing the Results window, see page 28.
Control windowThe 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.
MethodA method comprises all parameters for carrying
out and evaluating a determination.
DeterminationDetermination refers to the automatic determi-
nation of the induction time and/or stability time
for a sample. In order to carry out a determination, a method suitable for the samples must be
selected.
ResultsThe results of a determination are automatically
saved in the database Repos.mrd and can be
viewed in the Results window.
ReevaluationReevaluation refers to the subsequent revision of
RecalculationThe recalculation can be used to subsequently
ExtrapolationExtrapolation can be used to convert the results
4.1.3 Control window
The dialog window 743 Rancimat Control serves for controlling the
devices, managing methods, displaying the live curves and accessing various 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.
a determination, in particular the manual specification of the induction time using tangents.
recalculate results, formulas and standards.
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.
743 Rancimat
■■■■■■■■
25
4.1 Fundamentals of 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:
FileCreate new methods, open existing methods,
manage methods, open Results window, print,
new login, close program.
ViewActivate/Deactivate toolbar and status bar, dis-
play instrument information, change live parameters, display status overview, display event logging, select instrument.
ToolsManage cell constants, perform GLP tests, set
timer, set gas flow control, start all channels,
determine Delta T, record temperature, perform
service diagnosis.
■■■■■■■■
26
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4 Operation
OptionsCarry out general settings, set instrument config-
uration, manage access rights.
HelpCall up program-specific Online help.
Symbols
New method
Open method
Method Manager
Print
ResultsOpen Results window (see "Opening and closing the Results window", page
Create a new method (see Chapter 4.5.1, page 55).
Open an existing method (see Chapter 4.5.1, page 55).
Open, rename and delete methods (see Chapter 4.5.1, page 55).
Print results (see Chapter 4.7.6, page 128).
28).
Live parametersDisplay live parameters which can be changed for a current determination (see
Chapter 4.6.6, page 84).
Status overviewDisplay status overview for the instruments connected (see Chapter 4.3.2, page
44).
Instrument information
GLP status
Instrument information (see Chapter 4.3.1, page 42).
Display GLP status (see Chapter 4.8.3, page 144).
Instrument 1…4
Start all channels
Block A
Start all channels
Block B
Help topics
Select instrument 1…4.
Start all channels of Block A (see Chapter 4.6.4, page 83).
Start all channels of Block B (see Chapter 4.6.4, page 83).
Call up the Online help.
4.1.4 Results window
The dialog window 743 Rancimat Results serves for displaying, outputting 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.
743 Rancimat
■■■■■■■■
27
4.1 Fundamentals of 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.
■■■■■■■■
28
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4 Operation
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:
The toolbar of the Results window contains the following symbols:
Print results, curves and overview lists (see Chapter 4.7.6, page 128).
Copy data to clipboard.
Format determination overview (see Chapter 4.7.1, page 87).
Display determination overview (see Chapter 4.7.1, page 87).
Display all methods and determination data of the selected determination (seeChapter 4.7.2, page 103).
Search in the database (see Chapter 4.7.1, page 87).
Sort column in ascending order (see Chapter 4.7.1, page 87).
Descending
Selection-based filter
743 Rancimat
Sort column in descending order (see Chapter 4.7.1, page 87).
Filter by selection (see Chapter 4.7.1, page 87).
■■■■■■■■
29
4.1 Fundamentals of operation
■■■■■■■■■■■■■■■■■■■■■■
Special filter
Apply filter
Remove filter
Delete filter
Filter selection
Selection not in filter
Single graph
Multiple graph
Live graph with
reevaluation
Export to Word
Define filter (see Chapter 4.7.1, page 87).
Apply filter (see Chapter 4.7.1, page 87).
Remove filter (see Chapter 4.7.1, page 87).
Delete content of the filter (see Chapter 4.7.1, page 87).
Only display selected determinations (see Chapter 4.7.1, page 87).
Hide selected determinations (see Chapter 4.7.1, page 87).
Display single graph (see Chapter 4.7.3, page 112).
Display multiple graph (see Chapter 4.7.3, page 112).
Reevaluate live graph (see Chapter 4.7.3, page 112).
Export Determination overview to Word (see Chapter 4.7.6, page 128).
Export to Excel
Export measured values
Export determination
and method data
Tile vertically
Tile horizontally
Return to main program
4.1.5 File types
Export Determination overview to Excel (see Chapter 4.7.6, page 128).
Export measured values to a TXT file (see Chapter 4.7.6, page 128).
Export determination and method data to a TXT file (see Chapter 4.7.6, page
128).
Arrange subwindows on top of each other (see Chapter 4.7.8, page 141).
Arrange subwindows beside each other (see Chapter 4.7.8, page 141).
Close Results window and return to main program.
The following file types are generated by the program 743 Rancimat:
*.mrdDatabase 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.
■■■■■■■■
30
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
*.melEvent file
*.txtText file
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 Operation
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.
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.
4.1.7 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-
■Keeping the left mouse button pressed down, pull the cursor to
The cursor assumes the form of a magnifying glass.
2
Release mouse button
■Release the mouse button in order to magnify the selected area
nified.
the lower right corner of the sector.
to the full size of the window.
743 Rancimat
■■■■■■■■
31
4.1 Fundamentals of 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 textcan be clicked on. This takes you to another help
topic.
Violet textmarks menu items, parameters or buttons in the
program.
Blue textmarks titles and important information.
■■■■■■■■
32
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4.2 Instrument and Program Settings
4.2.1 Establishing the instrument communication
Up to four instruments can be controlled with the program 743 Rancimat. 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....
The following dialog window appears:
4 Operation
■Enter the number of connected instruments and confirm with
[OK].
The following dialog window appears:
2
Select interface
■Under COM port, select the serial interface of the PC to which
the instrument is connected.
743 Rancimat
■■■■■■■■
33
4.2 Instrument and Program Settings
■If a softswitch is used, activate the option Softswitch in use and
select the serial interface of the softswitch to which the instrument is connected under Softswitch port.
■Confirm the entry with [OK].
3
Restart program
■Close the program with the menu item File ▶ Exit.
■In the Windows Start menu under Pro-
grams ▶ Metrohm ▶ Rancimat, click on the menu item Rancimat.
■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, allowing 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, individual Users can be assigned to a specific group.
Note
User lists are best created and passwords are best entered immediately
after the first program start.
■■■■■■■■
34
The setup for the users and their access rights is carried out in the following order:
1.Add a new group
2.Adjust rights for this group
3.Create users in this group
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4 Operation
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
■In the Control window, click on the menu item
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:
1
Open Users and groups manager
■In the Control window, click on the menu item
Options ▶ User permissions....
2
Open Properties dialog
■Right click on the relevant group whose access rights are to be
adjusted to select the menu item Properties....
The following dialog window appears:
743 Rancimat
■■■■■■■■
35
4.2 Instrument and Program Settings
■■■■■■■■■■■■■■■■■■■■■■
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:
1
Open Users and groups manager
■In the Control window, click on the menu item
Options ▶ User permissions....
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].
■■■■■■■■
36
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
Deleting a user
Proceed as follows to delete an existing user:
1
Open Users and groups manager
■In the Control window, click on the menu item
Options ▶ User permissions....
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:
1
Open Users and groups manager
■In the Control window, click on the menu item
Options ▶ User permissions....
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 Operation
4.2.3 Timer
743 Rancimat
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 running.
Two different examples will explain how to program the timer.
■■■■■■■■
37
4.2 Instrument and Program Settings
Proceed as follows to automatically start the heating of block A at a specific time:
■■■■■■■■■■■■■■■■■■■■■■
Starting heating block A once automatically
1
Open dialog window
■In the Control window, click on the menu item Tools ▶ Timer
function....
The following dialog window appears:
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 specific day of the week, at a specific time:
1
Open dialog window
■In the Control window, click on the menu item Tools ▶ Timer
function....
The following dialog window appears:
■■■■■■■■
38
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
2
Set automatic start time
■Under Start heating select the option Daily.
■Click on the button [Which days...].
The following dialog window appears:
4 Operation
■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 vessels 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
2
Switch off
■Click on the menu item Tools ▶ Gas flow control ▶ Gas flow
on.
off.
743 Rancimat
■■■■■■■■
39
4.2 Instrument and Program Settings
Proceed as follows:
■■■■■■■■■■■■■■■■■■■■■■
Displaying the gas flow
1
Open dialog window
■Click on the menu item Tools ▶ Gas flow control ▶ Display
gas flow....
The following dialog window appears:
Note
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 containing the following values:
t(s)Time in seconds.
Block [°C]Temperature measured in the heating block.
Ext. Sensor [°C]Temperature measured with the external tem-
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.
perature sensor.
■■■■■■■■
40
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
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 compress the program, so that this file no longer has any superfluous data and
the program runs faster again.
4 Operation
The file size of the database Repos.mrd can make access to existing
determinations considerably slower. If you regularly work with the program and carry out a large amount of determinations, you should optimize 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 24).
2
Optimize program
■In the windows Start menu, click on the menu item Pro-
grams ▶ Metrohm ▶ Rancimat ▶ Optimize ▶ Program.
743 Rancimat
■■■■■■■■
41
4.3 Program information
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 133).
■Close the Results window and the program Rancimat (see Chap-
ter 4.1.1, page 24).
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:
1
Open dialog window
■In the Control window, click on the menu item View ▶ Unit
information….
The following dialog window appears:
■■■■■■■■
42
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
2
Print instrument information
■Click on the button [Print report…].
4 Operation
Serial number
Program number
Last maintenance
Last calibration
Unit operating hours
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 of the selected instrument.
Number of the EEPROM program of the selected instrument.
Date of the last maintenance with signature of the service technician who
has carried out the service work.
Date of the last instrument adjustment with signature and code of the
responsible body.
Number of hours during which the instrument was switched on.
Pump operating hours
743 Rancimat
Number of hours during which the internal pump was in operation.
■■■■■■■■
43
4.3 Program information
The block Service diagnosis is password-protected and only accessible for trained service personnel.
4.3.2 Status overview
Displaying the status overview
Proceed as follows to display and adjust the status overview:
1
Open dialog window
■In the Control window, click on the menu item View ▶ Status
The following dialog window appears:
■■■■■■■■■■■■■■■■■■■■■■
Note
overview.
Unit
Block
Channel
Method
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.
■In the Control window, click on the menu item
Options ▶ Save settings now.
Meaning of the columns in the status overview
Instrument number (1…4).
Instrument block (A or B).
Channel (1…4).
Name of the method loaded.
■■■■■■■■
44
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
Sample ID1
Status
Stab. time
Induc. time
4 Operation
Sample identification 1.
Status of the channel.
ready: No active measurement. The channel is ready for starting a determination.
running: Instrument is measuring.
finished: Determination finished. The channel is ready for starting a new
determination.
error: Communication error between instrument and PC.
Stability time determined.
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 connected to the PC:
1
Open current log file
■In the Control window, click on the menu item View ▶ Event
log overview.
The following dialog window appears:
743 Rancimat
■■■■■■■■
45
4.3 Program information
■■■■■■■■■■■■■■■■■■■■■■
Note
You can find the meaning of the symbols and columns in the
event overview at "Meaning of the symbols and columns in theevent overview", page 47.
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
■In the dialog window Open, select the required file and confirm
or the menu item File ▶ Open….
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").
■■■■■■■■
46
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
■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
4 Operation
■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:
1
Open dialog window
■In the Control window, click on the menu item
Options ▶ Event log….
The following dialog window appears:
Type
Date
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
- Information on correctly executed events.
- Indication of a special event.
- Error message for error event.
Date of the event. The format depends on the settings defined in Windows in Control Panel ▶ Country settings ▶ Date.
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47
4.4 Calibration functions
Time
Time of the event. The format depends on the settings defined in Windows 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 "Conductivity". The cell constants can thereby be entered manually or deter-
mined automatically using a defined standard solution (see Optional
accessories, page 185).
Entering cell constants manually
Proceed as follows if you wish to enter the cell constants manually:
1
Open dialog window
■Click on the menu item Tools ▶ Cell constants ▶ Manual....
The following dialog window appears:
■■■■■■■■
48
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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
4 Operation
Proceed as follows if you wish to enter the cell constants automatically:
1
Open dialog window
■Click on the menu item Tools ▶ Cell constants ▶ Automatic....
The following dialog window appears:
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2
Select channels and define conductivity
■Activate the check boxes of those channels, for which the cell
constant is to be determined.
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49
4.4 Calibration functions
■■■■■■■■■■■■■■■■■■■■■■
■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:
TemperatureConductivity
18 °C
19 °C
20 °C
21 °C
22 °C
23 °C
24 °C
25 °C
127 µS/cm
130 µS/cm
133 µS/cm
136 µS/cm
138 µS/cm
141 µS/cm
144 µS/cm
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].
4.4.2 Determining Delta T
The temperature correction Delta T indicates the deviation of the current 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
60). It can automatically be determined with the calibrated, external temperature sensor (part of the optionally available GLP test set, see Optionalaccessories, page 185).
■■■■■■■■
50
If you wish to maintain the old values, click [Cancel].
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1
3
4
5
6
7
8
9
2
9
10
4 Operation
Figure 6Equipping the reaction vessel for determining Delta T
FEP tubing 250 mm (6.1805.080)
1
For supplying air into the reaction vessel.
Thread adapter M8 / M6 (6.1808.090)
3
Air tube
5
Connector
7
For connecting the thread adapter M8 / M6.
Spacer (6.2042.040)
9
Pt100 temperature sensor
2
Opening for temperature sensor
4
For inserting the temperature sensor.
O-ring (6.1454.040)
6
Reaction vessel cover (6.2753.107)
8
Reaction vessel (6.1429.040)
10
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4.4 Calibration functions
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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
■■■■■■■■
52
Note
Create a unique method for both blocks, so that you can separately 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 81).
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4 Operation
■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
■Click on the menu item Tools ▶ Gas flow control ▶ Gas flow
on.
■Click on the button [Heat to xx °C].
Executing a Delta T determination
After you have prepared everything for determining Delta T (see "Preparing Delta T determination", page 52), 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.
The following dialog window appears:
■Enter a Sensor name.
■Enter the calibration data (temperature and resistance) for Points
1 to 3 and confirm with [OK].
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4.4 Calibration functions
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Note
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.
The following dialog window appears:
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 of ext. sensor
Delta T
Temperature which has been measured in the
heating block with the internal temperature
sensor.
Temperature which has been measured in the
reaction vessel with the external temperature
sensor.
Temperature correction which is determined
from the difference between the block temperature and the temperature of the ext. sensor.
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54
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Note
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...
appears in the message box.
As soon as the temperature defined in the method has been
reached, the message Measuring temperature. Please wait...
appears in the message box.
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 corresponding method. It is automatically saved with the changed value
of Delta T.
4 Operation
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
item File ▶ New method.
The following dialog window appears:
or the menu
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4.5 Methods
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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.
Note
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].
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56
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4 Operation
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 60).
■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
■In the Control window, click on the symbol
or the menu
item File ▶ Open method....
The dialog window Open method appears.
■Click on the required method and confirm the selection with
[Open].
The dialog window "Method name" appears.
2
Adjust parameters and save changes
■Adjust the parameters (see Chapter 4.5.2, page 60).
■Confirm the changes with [Save].
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4.5 Methods
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Renaming an existing method
Proceed as follows to rename an existing method:
Note
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
■In the Control window, click on the symbol
or the menu
item File ▶ Method manager....
The following dialog window appears:
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.
■■■■■■■■
58
Saving a method under a new name
Proceed as follows to save an existing method under a new name:
1
Open method
■In the Control window, click on the symbol
or the menu
item File ▶ Open method....
The dialog window Open method appears.
■Click on the required method and confirm the selection with
[Open].
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4 Operation
The dialog window "Method name" appears.
2
Save it with a new name
■If necessary, adjust the parameters (see Chapter 4.5.2, page
60).
■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:
Note
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
■In the Control window, click on the symbol
or the menu
item File ▶ Method manager....
The following dialog window appears:
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].
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4.5 Methods
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Printing parameters of a method
Proceed as follows to print the parameters of an existing method:
1
Open method
■In the Control window, click on the symbol
item File ▶ Open method....
The dialog window Open method appears.
■Click on the required method and confirm the selection with
[Open].
The dialog window "Method name" appears.
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 carrying out the measurement are set using this tab. The settings affect the
progression of the measurement curve recorded.
or the menu
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60
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4 Operation
Temperature
Delta T
Setpoint temperature of the sample.
Range
50 ... 220 °C
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
50).
Note
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).
Range
-9.9 ... 9.9 °C
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4.5 Methods
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Table 1Approximate values for determining Delta T
Setpoint temperatureDelta T
Gas flow
Use internal pump
80 °C
90 °C
100 °C
110 °C
120 °C
130 °C
140 °C
150 °C
160 °C
+1.1 °C
+1.3 °C
+1.4 °C
+1.5 °C
+1.6 °C
+1.7 °C
+1.8 °C
+1.9 °C
+2.0 °C
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 decisive.
Range
7 ... 25 L/h
on | off (Default value: on)
Start options
Start delay
Start mode
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).
Waiting time until starting the measurement.
Range
0 ... 1000 min
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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Stop criteria
Time
4 Operation
per block
The 4 channels of a block can be started and stopped jointly.
on | off (Default value: off)
Time until the automatic stop of the determination.
Range
0.1 ... 9999 h
Conductivity
on | off (Default value: off)
Conductivity limit value. If this value is reached, the determination is
ended automatically.
Range
1 ... 400 µS/cm
Endpoint(s)
on | off (Default value: off)
Automatic stop of the determination, as soon as every active channel has
reached all endpoints (induction time and stability time).
Table 2Overview of stop criteria
TimeConductivityEndpoint(s)Analysis stops...
not automatically.
✔
after the time entered, independently of reach-
ing the induction/stability time (endpoint).
✔✔
✔
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✔
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 induction/stability time (endpoint).
✔
after reaching the first criterion (time or endpoint). If the time entered has been reached,
there is no further measuring until the induction/stability time (endpoint) has been reached.
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63
4.5 Methods
TimeConductivityEndpoint(s)Analysis stops...
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✔✔
✔✔✔
Actions at end of determinations...
Shut off heater
on | off (Default value: off)
Automatic deactivation of the heating at the end of the determination.
Shut off gas flow
on | off (Default value: off)
Automatic deactivation of the gas flow at the end of the determination.
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/stability time (endpoint) has been reached.
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 suction 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 (seeChapter 4.7.3, page 112).
Caution
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64
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4 Operation
Evaluate induction time
on | off (Default value: on)
Determination of the induction time (see "Induction time", page 66).
Evaluate stability time
on | off (Default value: off)
Determination of the stability time (see "Stability time", page 67).
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.
Range
Options for induction time
Note
1 ... 400 µS/cm
Evaluation delay
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Waiting time until starting the curve evaluation.
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65
4.5 Methods
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Range
Evaluation suppression
Start
Time from the start of the determination to the start of the evaluation
suppression.
Range
End
Time from the start of the determination to the end of the evaluation suppression.
Range
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 second derivative. Higher values require a higher maximum.
0 ... 100 h
0 ... 100 h
0 ... 100 h
Range
0.1 ... 9999
Induction time
The induction time is the time to the break point of the curve conductivity 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 tangents at the extended straight branches of the curve (see "Setting tan-gents manually", page 116).
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2nd derivative
Time
Conductivity
Induction time
End
Start
Evaluation
suppression
Evaluation
delay
Stability time
Time
Delta
Kappa
Conductivity
4 Operation
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 certain range.
Stability time
The stability time is the time which is necessary in order to attain a specified conductivity change Delta Kappa.
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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67
4.5 Methods
■■■■■■■■■■■■■■■■■■■■■■
Time axis (x)
End value
Conductivity axis (y)
End value
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 of the time axis with manual scaling.
Range
Selection
0.5 ... 100 h
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 of the conductivity axis with manual scaling.
■■■■■■■■
68
Range
10 ... 400 µS/cm
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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 measurement, a post-calculation or recalculation is possible at any time in the
determination overview (see Chapter 4.7.5, page 121).
4 Operation
Formula 1 for induction time:
on | off (Default value: off)
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:
on | off (Default value: off)
If this option is activated, the automatically determined stability time will
be calculated with the entered values. The result will be saved under the
name entered in the field "R2".
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69
4.5 Methods
Formula 3 for stability time:
on | off (Default value: off)
If this option is activated, the automatically determined stability time will
be calculated with the entered values. The result will be saved under the
name entered in the field "R3".
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-calculation or recalculation is possible at any time in the determination overview (see Chapter 4.7.5, page 121).
■■■■■■■■■■■■■■■■■■■■■■
Calculate standard time
Formula according to...
■■■■■■■■
70
on | off (Default value: off)
Activation/Deactivation of the calculation of the standard time according
to the following formula:
Standard time = Factor
Selection
(Temperature - Target temperature)/10
x induction time
AOCS Cd12b-92 | AOM | free
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Formula parameters
Factor
4 Operation
AOCS Cd12b-92
Formula calculation according to standard AOCS Cd12b-92 with Target temperature = 110 °C.
AOM
Formula calculation according to standard AOM with Target temperature = 97.8 °C.
free
Formula calculation with freely selectable Target temperature.
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 117) of results, which
have been recorded at different temperatures.
Range
Target temperature
Target temperature for the calculation of the standard time.
Range
4.5.2.6 "Documentation" tab
This tab contains parameters for the automatic report output.
0.001 ... 100
20 ... 300 °C
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4.5 Methods
Include in report...
Header
Method parameters
Curve(s)
Method description
■■■■■■■■■■■■■■■■■■■■■■
on | off (Default value: on)
Output of the header with company settings (see ""Company settings"tab", page 137), date of the printout, sample identifications, instrument
information, determination date, user, cell constant and serial number.
on | off (Default value: on)
Output of the method parameters.
on | off (Default value: on)
Output of the curves.
on | off (Default value: off)
Output of the method description entered on the tab Description.
Results
on | off (Default value: on)
Output of the selected results.
Selection
Automatic report output
Send to printer immediately
on | off (Default value: on)
Automatic printout of the report defined under Include in report... after
finishing the determination.
Send to file
on | off (Default value: off)
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....
Induction time | Stability time | Standard time
| Formula 1 | Formula 2 | Formula 3
■■■■■■■■
72
Browse…
Selection of the directory for saving this file.
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3.26
0
5
10
15
20
25
30
0.00.51.01.52.02.53.03.5
h
GLP test passed.
09.09.2006 09:34:03
Printing date
ID 1
Peanut oil
ID 2
DBG2307
Determination date
23.06.2006 13:25:52
Unit
1
Block
A
Channel
1
Cell constant
1
User
Administrator
Serial number
01109
h
Induction time
3.26
Method name
Oil 120°C
Creator
Administrator
Creation date
23.06.2006 08:27:20
Temperature
120
Start delay
0
Stop time
0.00
Stop at conductivity
0
Stop at endpoint
Evaluation delay
0.00
Evaluation delay start
0.00
Evaluation delay end
0.00
Delta Kappa
0
Send to file
Gas flow
20°CL/h
µS/cm
h
h
h
min
h
µS/cm
Delta T
1.60 °C
per channel
per 2 channels
per block
Start mode
µS/cm
4 Operation
Example of an automatically printed report
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4.5 Methods
4.5.2.7 "Description" tab
You can enter a comment on the method in this tab.
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Prepare samples
Prepare instrument and accessories
Select method
Modify method parameters
Start heating
Enter sample identifiers
Temperature
reached?
no
yes
Insert and connect reaction vessels
Start determination
Stop crit.
reached?
no
yes
Modify live parameters
Stop determination manually
Determination finished
Automatic report output
Result display
Clean vessels and accessories
4.6 Determinations
Standard sequenceOptional stepsFurther information
4 Operation
Section 4.6.1
Section .4.6.2
Section 4.6.3
Section 4.5.2
Section 4.6.3
Section 4.6.3
Section 4.6.3
Section 4.6.4
Section 4.6.6
Section 4.6.7
743 Rancimat
Section 4.5.2.6
Section 4.7
Section 4.6.5
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4.6 Determinations
4.6.1 Preparing samples
This section contains information on how to prepare the following samples:
■Pure, clear oils (see page 76)
■Non-liquid, pure fats (see page 76)
■Samples containing oil and fat (see page 77)
■Emulsion fats (see page 79)
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 sufficiently deeply. If this is not the case, add more sample material.
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Note
■■■■■■■■
76
Preparing non-liquid, pure fats
Prepare non-liquid, pure fat as follows:
1
Weigh in the sample
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.
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4 Operation
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 material.
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).
Note
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.
Note
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, allowing for a certain transfer loss (for more than two determinations
accordingly more is necessary).
743 Rancimat
■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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4.6 Determinations
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Note
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.
Note
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 Na
2SO4
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.
Note
If the isolated oil/fat samples are not immediately measured out,
you have to store the samples in a cool place and protectedfrom 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 preservation in many cases.
■■■■■■■■
78
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 Publish-ers, London and New York, 1983.
743 Rancimat
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4 Operation
Preparing emulsion fats
You can use water-soluble fats as pure substances and prepare them as
follows:
1
Weigh in the sample
■Weigh in the sample.
Note
As the water evaporates right at the beginning of the analysis and
is carried away by the air blown through, you have to use correspondingly more sample material.
2
Mount foam barrier
■Mount the foam barrier (see figure 5, page 14), as the samples
can significantly foam.
Note
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
uncontrolled 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 prerequisite for reliable, reproducible and correct analysis results. Even the
slightest contamination could catalytically accelerate the oxidative decomposition 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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4.6 Determinations
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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
Note
Only use measuring vessels and accessories which are absolutely 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).
4
Weigh in the sample
■■■■■■■■
80
Note
Use new reaction vessels and air tubes for each measurement. 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 76).
743 Rancimat
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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 fatfilm 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
4 Operation
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.
Note
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 57.
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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4.6 Determinations
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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.
Note
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
Note
The temperature defined in the method must be reached, before
you insert the reaction vessels, i.e. the frame of the button [Heatto 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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82
743 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 86).
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 displayed for every channel:
4 Operation
.
As soon as a stop criterion defined in the method (see table 2, page
63) 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
Note
Always clean the vessels and accessories directly after each
determination (see Chapter 4.6.5, page 83).
4.6.5 Cleaning the instrument and accessories
743 Rancimat
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!). Preclean with washing-up liquid in the case of severe contamination.
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83
4.6 Determinations
■■■■■■■■■■■■■■■■■■■■■■
■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 electrodes.
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.
Note
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
■In the Control window, click on the symbol
item View ▶ Live parameters....
The following dialog window appears:
or the menu
■■■■■■■■
84
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4 Operation
2
Adjust the parameters
■Adjust all required parameters (see Chapter 4.5.2.1, page 60).
■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 stopped 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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85
4.6 Determinations
4.6.8 Status of the live curve
Before a determination:
■■■■■■■■■■■■■■■■■■■■■■
No active measurement.
The channel is ready for starting a
determination.
During a determination:
Determination started.
The first measured value is measured.
After a determination:
No active measurement.
Communication error between
instrument and PC.
Current measurement.
Measured value and time are displayed above the live curve.
■■■■■■■■
86
Determination finished.
The channel is ready for starting a
new determination.
743 Rancimat
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4.7 Results
4.7.1 Determination overview
The determination overview displays selected information on all determinations 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 column 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 95).
4 Operation
Displaying the determination overview
Proceed as follows to open a determination overview:
1
Open Results window
■In the Control window, click on the symbol
or the menu
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].
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87
4.7 Results
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Formatting the determination overview
Proceed as follows to format the determination overview.
A detailed description of the parameters can be found at "Parameterdescription", page 95.
1
Select fields
■Click on the symbol
or the menu item Format ▶ Select
fields.
The following dialog window appears:
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.
The following dialog window appears:
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88
743 Rancimat
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■Under Column width, enter the number of characters of a col-
umn and confirm with [OK].
or
■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....
The following dialog window appears:
4 Operation
■Carry out the required settings and confirm with [OK].
743 Rancimat
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89
4.7 Results
4
Change the font
■Click on the menu item Format ▶ Fonts....
The following dialog window appears:
■■■■■■■■■■■■■■■■■■■■■■
■Carry out the required settings and confirm with [OK].
Selecting determinations
Proceed as follows to select one or more lines of the determination overview:
1
Select a line
■Place the mouse button on the left edge of the line to be selec-
ted.
The cursor assumes the following form:
■Click on the line.
2
Select several lines
■Place the mouse button on the left edge of the line to be selec-
ted.
The cursor assumes the following form:
■Keep the mouse button pressed down and move over the left
edge of all lines to be selected.
■■■■■■■■
90
743 Rancimat
■■■■■■■■■■■■■■■■■■■■■■
4 Operation
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 100.
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.
■Click on the symbol or the menu item Determina-
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.
■Click on the symbol or the menu item Determina-
tion ▶ Sort ▶ Descending.
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91
4.7 Results
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 90.
2
Display selected determinations only
■Click on the symbol
or the menu item Determination ▶ Fil-
ter ▶ Filter selection.
3
Remove the filter again
■Click on the symbol
or the menu item Determination ▶ Fil-
ter ▶ Remove filter/sorting.
All entries are once again displayed in the dialog window.
4
Hide selected determinations
■Click on the symbol
or the menu item Determination ▶ Fil-
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").
■Click on the symbol or the menu item Determination ▶ Fil-
ter ▶ Selection based filter.
Only the entries with the Determination date "12.2005" are displayed in the dialog window.
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92
743 Rancimat
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