88928001EN
88928001EN
88928001EN
Manual
8.892.8001EN / v6 / 2024-01-09
Metrohm AG
CH-9100 Herisau
Switzerland
+41 71 353 85 85
info@metrohm.com
www.metrohm.com
Manual
8.892.8001EN / v6 / 2024-01-09
Technical Communication
Metrohm AG
CH-9100 Herisau
Disclaimer
Deficiencies arising from circumstances that are not the responsibility of
Metrohm, such as improper storage or improper use, etc., are expressly
excluded from the warranty. Unauthorized modifications to the product
(e.g. conversions or attachments) exclude any liability on the part of the
manufacturer for resulting damage and its consequences. Instructions and
notes in the Metrohm product documentation must be strictly followed.
Otherwise, Metrohm's liability is excluded.
■■■■■■■■■■■■■■■■■■■■■■ Table of contents
Table of contents
1 Introduction 1
1.1 Device description ................................................................ 1
1.2 Displaying accessories .......................................................... 2
1.3 Symbols and conventions .................................................... 3
2 Safety 4
2.1 Responsibility of the operator ............................................. 5
2.2 Requirements for operating personnel ............................... 5
2.3 Electrical safety ..................................................................... 6
2.4 Tubing and capillary connections ........................................ 7
2.5 Flammable solvents and chemicals ..................................... 7
2.6 Danger from biological substances ..................................... 7
4 Installation 13
4.1 Setting up the device ......................................................... 13
4.1.1 Packaging .............................................................................. 13
4.1.2 Checks .................................................................................. 13
4.1.3 Setup location ....................................................................... 13
4.2 Mounting accessories ......................................................... 14
4.2.1 Mounting the internal air supply ............................................ 14
4.2.2 Mounting the external air supply ........................................... 16
4.2.3 Assembling the reaction and measuring vessels ..................... 17
4.2.4 Inserting vessels / Establishing tubing connections ................. 20
4.2.5 Mounting the exhaust air collection tube ............................... 21
4.2.6 Mounting the oil separator .................................................... 22
4.3 Power connection ............................................................... 24
4.3.1 Connecting the instrument to the power grid ........................ 24
4.3.2 Replacing fuses ...................................................................... 25
4.3.3 Switching the instrument on and off ...................................... 26
4.4 Connecting a computer ...................................................... 27
4.4.1 Connecting the 892 Professional Rancimat and the com-
puter ..................................................................................... 27
5 Operation 29
5.1 Rancimat method ............................................................... 29
5.2 Calibration functions .......................................................... 30
5.2.1 Determining the cell constant ................................................ 30
5.2.2 Determining the temperature correction ................................ 31
5.3 Determinations ................................................................... 34
5.3.1 Preparing a sample ................................................................ 34
5.3.2 Preparing the instrument and the accessories ......................... 38
5.3.3 Preparing the determination .................................................. 39
5.3.4 Cleaning the accessories ........................................................ 41
5.3.5 Cleaning the oil separator ...................................................... 42
7 Troubleshooting 48
7.1 Problems .............................................................................. 48
Index 58
Table of figures
Figure 1 Front 892 Professional Rancimat ........................................................ 9
Figure 2 892 Professional Rancimat rear ........................................................ 10
Figure 3 Instrument display ........................................................................... 11
Figure 4 Mounting accessories for the air supply ........................................... 14
Figure 5 Drying flask - Individual parts ........................................................... 15
Figure 6 Drying flask mounted in place ......................................................... 16
Figure 7 Equipping the reaction and measuring vessels ................................. 18
Figure 8 Mounting the air tube: correct - incorrect ........................................ 20
Figure 9 Mounting the foam barrier .............................................................. 20
Figure 10 Mounting the oil separator .............................................................. 23
Figure 11 Instrument display with instrument name ........................................ 26
Figure 12 Instrument display with "no connection" symbol ............................. 26
Figure 13 Instrument display without instrument name and symbol ................ 26
Figure 14 Instrument display with serial number ............................................. 27
Figure 15 Measuring arrangement (schematic representation) ......................... 30
Figure 16 Assembling the reaction vessel for determining the temperature correc-
tion ................................................................................................. 32
Figure 17 Oil separator (6.2753.200), disassembled ........................................ 42
Figure 18 Dust filter - conditions ..................................................................... 46
1 Introduction
NOTE
2 Safety
WARNING
WARNING
Flammable substances
WARNING
WARNING
WARNING
Supply voltage
WARNING
WARNING
CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing con-
nections. Damaged tubing ends lead to leakage. Appropriate tools can
be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.
WARNING
WARNING
1 5
2 6
3 7
4 8
892_1
10 5
9 8 7 6
Figure 3 Instrument display
4 Installation
4.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
CAUTION
Heat accumulation
Placing the instrument in a tight space or covering the housing may
lead to overheating and subsequent damage to the instrument.
■ Set the device up freestanding, to allow the air to circulate around
the instrument.
■ Do not cover the device.
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation and free of vibrations and which provides protection against
corrosive atmosphere and contamination by chemicals to the extent possi-
ble.
The instrument should be protected against excessive temperature fluctua-
tions and direct sunlight.
NOTE
10
11
12
NOTE
The dust filter serves for filtering the air aspirated through the air
pump and must be replaced at periodic intervals (see chapter 6.2,
page 46).
1
I II III
3 Bottle (6.1608.050)
■ [I] – Fill the molecular sieve (6.2811.000) into the drying flask.
■ [II] – Screw the filter tube on the bottom side of the drying flask
cap into the opening marked with a dot (on the upper side).
■ [III] – Screw the drying flask cap with mounted filter tube onto
the drying flask and insert it in the bottle holder on the rear of the
892 Professional Rancimat.
■ Screw one end of the FEP tubing 250 mm to the opening on the
drying flask cap marked with a dot.
■ Screw the other end of the FEP tubing to the From flask connec-
tor on the rear of the 892 Professional Rancimat.
■ Screw one end of the second FEP tubing 250 mm to the second
opening on the drying flask cap.
■ Screw the other end of the second FEP tubing to the To flask
connector.
NOTE
NOTE
3
11
4
12
5
13
6
7 14
8
15
9
16
10
17
18
19
20
Figure 7 Equipping the reaction and measuring vessels
Proceed as follows to mount the measuring vessel and the reaction vessel:
NOTE
When mounted without foam barrier, the air tube must be in a vertical
position in the reaction vessel.
WARNING
The foam barrier can melt if it projects too deeply into the heating
block.
Ensure that the foam barrier is at least 7 cm above the base of the
reaction vessel.
NOTE
NOTE
NOTE
NOTE
The oil separators must be cleaned after each measurement (see chap-
ter 5.3.5, page 42).
4 5
WARNING
WARNING
NOTE
WARNING
Ensure that the instrument is never put into operation with fuses of
another type, otherwise there is a risk of fire!
NOTE
5 Enter the instrument information into the dialog fields of the 892
Professional Rancimat configuration.
NOTE
5 Operation
NOTE
The figure shows in detail how the accessory parts are to be assembled for
the determination of the temperature correction. Proceed as follows:
NOTE
5.3 Determinations
5.3.1 Preparing a sample
NOTE
Use new reaction vessels and air tubes for each measurement.
Blow out the reaction vessels with nitrogen before use.
or
■ Place the reaction vessel on a scale using a 6.2628.000 holder.
■ Weigh in the fat as solid.
For this, weigh in 3 g sample material directly in the reaction
vessel and insert it briefly in the heated block of the 892 Pro-
fessional Rancimat, so that the fat melts.
Oils and fats made from products containing oil and fat must be extracted
with petroleum ether (low-boiling) while being protected from light as fol-
lows:
NOTE
2 Extraction
■ Prepare a 300 mL Erlenmeyer flask with standard ground-joint.
■ Weigh in between 50 and 100 g (depending on the oil/fat con-
tent) of the sample in powder form (e.g. milk powder, cocoa
powder, hazelnut powder) or the finely ground material.
■ Cover the sample material with a layer of approx. 1 cm of petro-
leum ether (low-boiling).
■ Extract the oil or fat while continuously stirring for around 12 h
and keeping it protected from light.
NOTE
NOTE
NOTE
■ Dry the oil/fat sample after the distillation has been completed for
approx. 30 min at a pressure of < 1,330 Pa (13.3 mbar).
■ Filtrate the oil/fat sample now present together with water-free
Na2SO4 with a folded filter. If necessary, work in the drying oven
at a temperature exceeding the melting point of this fat by 10 °C.
NOTE
You can find further information on the treatment of oil and fat samples in
Rancidity in Foods, Allen J.C., Hamilton R.J., Applied Science Publishers,
London and New York, 1983.
You can use emulsion fats like pure substances and prepare them as fol-
lows:
NOTE
NOTE
Alternatively you can melt 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.
NOTE
4 Weighing in samples
NOTE
Use new reaction vessels and air tubes for each measure-
ment. Blow out the reaction vessels with nitrogen before use so
that any adhering particles are removed.
NOTE
NOTE
If you wish to switch off the heating, click on the [Stop] button.
NOTE
The Info 2 and Info 3 info fields can be activated in the sub-
window Properties - Sample data in the Method program
part.
NOTE
NOTE
1 Body 2 Base
Body with the IN and OUT connectors. Base with O-ring (6.1454.050) used for seal-
ing the oil separator.
NOTE
NOTE
Do not allow the oil separator bases to come into contact with
acetone for extended periods of time.
NOTE
CAUTION
WARNING
WARNING
Prerequisites
■ The product is disconnected from the power grid.
NOTE
If the suspicion arises that liquids have found their way into the
product, disconnect the instrument from the power grid and con-
tact your Metrohm service engineer.
NOTE
NOTE
NOTE
The molecular sieve filled in the drying flask (2-9) serves to adsorb disrup-
tive oxidizing gases as well as of the water from the aspirated air.
You can regenerate the molecular sieve in the drying oven at
approx. +140 - +180 °C for 24 to 48 h. You can order a new molecular
sieve under the order number 6.2811.000.
CAUTION
Do not fill the hot molecular sieve directly into the drying flask after
regeneration, as otherwise the plastic filter on the filter tube will melt.
Wait until the molecular sieve has cooled down before filling.
7 Troubleshooting
7.1 Problems
Problem Cause Remedy
The pump is louder The air flow is blocked ■ Check dust filter and replace it if necessary.
than normal. somewhere before or after ■ Check filter tube on the drying flask cap for
the pump. blockages and, if necessary, gently tap on it
to remove them.
Extra air is aspirated from ■ Check the FEP tubing for cracks, kinks, etc.
elsewhere other than the and fasten it tightly. Replace it if necessary.
dust filter. There is a leak ■ Place the drying flask cap correctly on the
somewhere in the system drying flask and screw tight.
before the pump.
No air flow can be The air supply is blocked. ■ Remove the FEP tubing from the thread
detected in the reac- adapter. Here, a slight air flow must be per-
tion vessel (it does ceptible. If this is not the case, please con-
not bubble), tact Metrohm Service.
although the pump ■ Check FEP tubing for blockages. If neces-
is running. sary, clean or replace.
■ Check the thread adapter and the air tube
on the reaction vessel cover for blockages.
If necessary, clean or replace.
The FEP tubing for the air Check the FEP tubing for cracks, kinks etc. If
supply is defective. necessary, replace.
The FEP tubing for the air Tighten the FEP tubing on both sides.
supply is not connected
correctly.
The air tube does not ■ Press the reaction vessel cover all the way
immerse in the sample. down.
■ Use more sample.
No air flow can be The connection is blocked. ■ Check the tubing connector on the reac-
detected in the tion vessel cover for blockage and, if neces-
measuring vessel (it sary, clean.
does not bubble), ■ Check the silicone tubing for blockage and,
although an air flow if necessary, clean.
can be discerned in ■ Check the tubing adapter and the PTFE
the reaction vessel. cannula on the measuring vessel cover for
blockage and, if necessary, clean.
The reaction vessel cover ■ If the reaction vessel cover is oblique or not
does not sit correctly or completely mounted, press it all the way
tightly enough. down.
■ If the reaction vessel cover is loose on the
reaction vessel despite correct assembly,
the cover has to be replaced.
The connection is wrongly ■ Make sure that the PTFE cannula for air
connected. supply is connected to the In opening of
the measuring vessel cover.
■ Make sure that the silicone tubing is
connected to the tubing adapter that is
mounted on the In opening.
■ Make sure that the reaction vessel is
connected to the measuring vessel that
belongs to the corresponding measuring
position.
The induction times The reaction vessels used ■ Clean the reaction vessels of particles (dust,
are not reproducible are not clean. cardboard, etc.) with nitrogen before
for multiple determi- weighing in the sample.
nations. ■ Only use new, unused reaction vessels.
The reaction vessels used Only use new, unused reaction vessels.
are scratched on the
inside.
The reaction vessel cover ■ If the reaction vessel cover is oblique or not
does not sit correctly or completely mounted, press it all the way
tightly enough. down.
■ If the reaction vessel cover is loose on the
reaction vessel despite correct assembly,
the cover has to be replaced.
The connection to the Ensure that no air can escape through leaks
measuring vessel is not when transferring from the reaction vessel to
mounted correctly. the measuring vessel.
The stability times The cell constant was not ■ Determine the cell constant.
are not reproducible determined or does not ■ Make sure that the assignment of the con-
for multiple determi- correspond to the value ductivity sensors is correct, so that the
nations. entered. determined cell constant actually corre-
sponds to the measuring cell used.
■ Make sure that the measuring cell is not
contaminated. Clean if necessary.
The induction time The temperature is not ■ Make sure that the correct method for the
is longer/shorter selected correctly. determination has been selected.
than expected. ■ Check whether the Sample temperature
and the Temperature correction are indi-
cated correctly in the method.
The stability time is The conductivity change is Make sure that the value defined for the con-
longer/shorter than not correctly defined. ductivity change in the method is correct.
expected.
See also: The stability times
are not reproducible for
multiple determinations.
Gas bubbles adhere to the ■ Make sure that the measuring cell is clean
conductivity measuring cell and free of fat. If necessary, clean
during measurement. thoroughly.
■ In some cases, ultrapure water contains a
large proportion of dissolved air. In this
case, degas the ultrapure water before the
measurement for 5 to 10 min in a vacuum.
The curve shows a Side reactions occur at the ■ Use the Evaluation suppression in the
step which means start or during the method.
that the induction measurement. These reac- ■ In addition to Endpoint(s) activate also
time is no longer tions cause the conductiv- Conductivity (e.g. 200 µS/cm) as stop cri-
determined cor- ity in the measuring cell to terion in the method and select the Stop
rectly. rise. once all the criteria have been fulfilled
option. The evaluation parameters can be
optimized on the basis of this curve, or the
curve can be evaluated manually.
■ Increase the Evaluation sensitivity
method parameter.
The induction time The Evaluate induction Activate the evaluation of the induction time in
is not evaluated time option is deactivated the method.
automatically, in the method.
although a signifi-
The Evaluation suppres- Deactivate the corresponding option in the
cant break point can
sion option preventing the method.
be noticed in the
evaluation of the curve in
curve.
the corresponding time
period is defined in the
method.
An inappropriately high Enter a lower value (e.g. 1.0) for the Evalua-
value was used in the tion sensitivity option in the method.
method for the Evalua-
tion sensitivity. This value
makes a curve evaluation
impossible.
The measurement The measurement has been Keep the measurement running until the end-
aborts without an stopped manually. point is automatically found.
endpoint being
found. A time or conductivity ■ Activate the Stop once all the criteria
defined as a stop criterion have been fulfilled option in the method.
in the method is reached ■ Increase the value for time or conductivity.
before the endpoint. ■ Deactivate time or conductivity as stop cri-
terion.
9 Technical specifications
9.9 Dimensions/Material
Width 383 mm
Height 277 mm (without accessories)
Depth 462 mm
Weight 16.1 kg (without accessories)
Lid material Baydur®110 FR-6 with flame retardation for fire class UL94VO, CFC-
free
Base material Steel sheet, coated
Index
A Emulsion fat ............................. 34 Oil/fat
Accessories External air supply Samples containing oil and fat
Mount ................................ 14 Mount accessories .............. 16 ........................................... 34
Air purification External temperature ................ 55
Mount accessories .............. 14 P
Assemble F Power connection .............. 24, 25
Oil separator ....................... 43 Fat Prepare sample
Autoxidation ............................ 29 Emulsion fats ...................... 34 Non-liquid, pure fats ........... 34
Non-liquid, pure fats ........... 34 Pure, clear oils .................... 34
C Fuse Samples containing oil and fat
Cell constant Replace .............................. 25 ........................................... 35
Determine .......................... 30 Prepare the sample
Clean G Emulsion fats ...................... 37
Accessories ......................... 41 Gas flow
Measuring vessel ................ 41 Range ................................. 56 R
Oil separator ....................... 43 Reaction vessel
Reaction vessel ................... 41 H Assemble ............................ 17
Tubing ................................ 42 Heater
Computer Start manually .................... 40 S
Connect ............................. 27 Switch off ........................... 40 Safety instructions ...................... 4
Conductivity measurement Heating Sample
Measuring range ................ 55 Range ................................. 54 Prepare ............................... 34
Resolution .......................... 55 Heating period ......................... 40 Sample identification
Connect Heating time ............................ 55 Enter .................................. 40
Power grid .......................... 24 Service ....................................... 6
I Shutdown temperature ............ 55
D Induction time .......................... 29 Solid samples ............................ 34
Determination Internal air supply Stability time .............................. 1
Prepare ............................... 39 Mount accessories .............. 14 Supply voltage ............................ 6
Disassemble Switch on ................................. 26
Accessories ......................... 42 M
Oil separator ....................... 42 Measuring vessel T
Drying flask Assemble ............................ 17 Temperature correction
Mount ................................ 15 Molecular sieve Determine .......................... 31
Dust filter Regenerate ................... 16, 47 Temperature measurement
Mount ................................ 14 Measuring range ................ 54
Replace .............................. 46 O Reproducibility .................... 54
Oil Resolution .......................... 54
E Pure, clear oils .................... 34
Electrostatic charge .................... 6