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FUNKE Operating Instructions

GERBER
Funke-Dr.N.Gerber Labortechnik GmbH
Ringstraße 42
12105 Berlin

EC declaration of conformity
according to EU Directive Machines 89/392/EC,
Appendix II A
We hereby declare that the machine specified below complies with the
basic health and safety requirements of the EC Machines Directive in its
design and construction and in the configuration put on the market by us.
This declaration is invalid if the machine is modified without our agreement.

Machine description: CryoStar I


Machine type: Freezing point determination
machine (cryoscope)
Machine No. 7160-

Applicable EU Directives: EC Machines Directive i.d.f. 93/44/EEC


EC-EC Low Voltage Directive
EC-Electromagnetic Compatibility Directive
89/336/EC

International standards DIN / EN ISO 5764

Berlin, date
Funke-Dr.N.Gerber Labortechnik GmbH

Dipl.-Ing. K. Schäfer, CEO


CryoStar automatic
Article-No.:7160
As per November 2007
28 FUNKE FUNKE 1
GERBER CryoStar I - Operating Instructions GERBER CryoStar I - Operating Instructions
Freezing Point: Example:
A-calibration with 0.000°C
A-calibration with -0.557°C (Operating error)
The freezing point of pure water means the temperature at which Remeasurement B-solution: results in 0.000°C
ice and water are at equilibrium. Remeasurement A-solution: results in + 0.557°C

If soluble parts are added to this liquid, the freezing point will be 12.3. Defective thermistor
lower (colder) because of the reduced capacity of the water This is the most frequently occurring error. There are two possible causes:
molecules to escape from the water surface. Fat has no influence 1. The thermistor is (has been) broken off: This can be recognised by the
on the freezing point, because it is not soluble in water. display constantly, without any change, showing a negative value.
2. The glass shell of the thermistor is showing hairline cracks and is leaky:
This manifests itself with extremely unstable measuring behaviour. The
repeatability is very bad, e.g. fluctuations from approx. 20 m̊C to 100 m̊C.
Measuring Principle: In both cases, the thermistor must be replaced.

The milk is cooled down (undercooled) to a temperature of -3°C 12.4. Stirrer error
and excited by vibration to undergo crystallisation. As a result of a) The stirrer is not oscillating freely:
the freezing process, there is a rapid rise in temperature caused The agitator must be able to move freely in the slot provided for it. It must
by configurational energy released which stabilises at a certain never touch the thermistor at any point. This must be paid particular
plateau equal to the freezing point. attention to during thermistor replacement.
b) The stirrer amplitude is not large enough:
Cooling the sample is not performed evenly and clearly lasts longer than 1
FUNKE minute. With a correctly adjusted agitator, the cooling time is almost exactly
GERBER 1 minute. The agitator amplitude must be approx. 3 - 4 mm.
c) The stirrer amplitude is too large:
Premature freezing of the sample happens often.
FUNKE-DR.N.GERBER LABORTECHNIK GMBH The agitator must be readjusted if needed.
Ringstrasse 42 13 Guarantee conditions
12105 Berlin
Germany 13.1. Guarantee period
Phone: ++49 - 30 - 702 006 0 The guarantee period is 12 months from the date of invoice.
Fax: ++49 - 30 - 702 006 66
13.2 Guarantee terms
Replacement parts will be exchanged at no cost during this period. Other
costs for working time, transport etc. are not covered by the guarantee.

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GERBER CryoStar I - Operating Instructions GERBER CryoStar I - Operating Instructions
colder than +1 ̊C (which cannot be the case for a thermistor in a new, i.e. Table of Contents
still warm sample), the machine also does not start the measurement. Page
1 First time operation 5
12. Detection of errors during use 1.1 Unpacking 5
1.2 Components Included in the Delivery 5
Most of the errors made during use of freezing point determination 1.3 Place of Installation 5
equipment are miscalibrations. The calibration of a cryoscope is a 1.4 Filling with cooling bath liquid 6
necessary precondition for every use. It is necessary to use a thermistor for 1.5 Loading or unloading the Carousel 7
measuring the temperature of a sample for measuring technology reasons. 1.6 Ongoing care and maintenance 7
Thermistors have a very large temperature effect which is necessary for 1.7 Transporting the machine 7
resolutions of more than 1 m̊K. Unfortunately, the fluctuation range of the 2 Connections 7
resistance values of these components is so large for production 21 Mains connection 7
technology reasons that the temperature zero point (0̊C)in the cryoscope 22 Adjustment the alternating current 8
must usually be determined by a precalibration before the machine can be Printer connection 8
calibrated with a new thermistor. 24 PC connection 8
It must be assumed that the A-calibration cannot be performed successfully 3 Switching on 9
after a thermistor replacement. The reason for this is that the machine must 4 Operation / Menu structure 10
5 Settings 11
first reach the specified impact temperature and then recognise an increase
5.1 Freely adjustable calibration values: Example A-value 11
in the temperature after the impact (as an indication that the freezing has
5.2 B-calibration value 12
initiated). However, this is not guaranteed because the values of the new 5.3 Adjusting base value 12
thermistor after calculation with the calibration constants of the old 5.4 Adjusting impact temperature 12
thermistor result in wrong temperatures. Therefore, a so-called 5.5 Setting the mode 12
precalibration is necessary where the machine does not pay attention to the 5.6 Plateau / Selecting the modes 12
temperatures but instead carries out a purely time-controlled measuring 5.7 Language selection 13
procedure. Afterwards, the calibration constants are adapted to the 5.8 Adjusting the stirrer 13
characteristics of the new thermistor so that both the A as well as the B 5.9 System check 14
calibration can be carried out successfully. 5.10 Printing 15
Unfortunately, it is often the case that the sample glasss filled with the 5.11 Precalibration 15
calibration liquids are mixed up during the calibration. 5.12 Technical parameters 15
5.13 Recommended settings 16
12.1. Mixing up the A-solution with the B-solution: 6 Performing measurements 16
6.1 Pipetation / Preparing the carousel 16
Initially the A-calibration is made without any anomalies. During the B- 6.2 Starting the measurement 16
calibration, the machine reports the “not calibrated or defective thermistor” 7 Calibration 17
error and remains in an uncalibrated state. In every case, a new pre- 7.1 Preparing the calibration 18
calibration and then a correct calibration should be performed. 7.2 Performing the calibration 18
8 Precalibration 19
12.2. Mixing up A-calibration instead of B-calibration 9 Thermistor / Temperature measurement 19
9.1 Replacing thermistor 20
Afterwards, the complete temperature scale of the machine is shifted. 10 Analytics 20
During remeasurement of the calibration solutions, transposed values and a 10.1 Principle Freezing Point Determination 20
transposed leading sign are obtained. 10.2 Fixed time 22
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10.3 Plateau search 22 longer the cooling takes, the more time the sample has to freeze on its own.
10.4 Maximum search 22 Therefore, the cooling down must be completed as quickly as possible. Dirt
11 Sources of error / Error messages 22 in the sample can also initiate the freezing.
11.1 Errors during cooling 24
11.2 Frozen too early 24 11.3. Not frozen:
11.3 Not frozen 25
If the specified temperature for the supercooling (the “trigger temperature”)
11.4 Plateau not found 25
has been reached, the machine strikes against the glass wall of the sample
11.5 Not calibrated or thermistor defective 25
glass in order to initiate the freezing. Now, the temperature must rise. A
12 Detection of errors during operation 26
temperature increase of at least 0.1̊ C is valid as criterion for a successful
12.1 Mix-up of A-solution with B-solution 26
12.2 Mix-up of A-calibration instead of B-calibration 26
crystallisation. For water or calibration solutions, this is also always the
12.3 Defective thermistor 27
case if the agitator has been adjusted so that it strikes forcefully against the
12.4 Stirrer error 27
glass wall. This is sometimes not the case for milks. There are milks which
13 Guarantee conditions 27 freeze with difficulty. If this error only occurs occasionally for individual
milks, then heat the milk concerned to approx. 40 ̊C, let it cool down again
and measure again. Conversely, if this error occurs frequently, then it is
better to reduce the impact temperature so that the samples are
supercooled further and thus freeze more easily. If this error also occurs
with calibration liquids, the calibration of the machine is not correct or
cooling bath liquid has penetrated the sample.

11.4. Plateau not found:


This error can only occur if “Plateau Search” according to the reference
method for determining the freezing point (ISO/DIS 5764) is used. For this
method, the temperature value during the plateau must be within a
specified range for a specified time. Thereby, it can occur that a certain milk
does not satisfy this criterion. Then, a second sample of this milk must be
measured. If this error suddenly occurs frequently although the machine is
otherwise operating correctly, then the fault must be looked for in the
thermistor or external interference.

11.5. Not calibrated or defective thermistor:


When starting a measurement or calibration, the machine tests the current
value of the thermistor. Its electrical resistance is known as a function of
the temperature. This electrical resistance is converted to a number by an
ADC (analogue-digital converter) which is then further processed by the
machine. If the thermistor has a shirt-circuit or a failure, its resistance is null
or infinity, both of which cannot be the case for a functional thermistor. In tis
case, the machine does not start the measurement.
If the temperature which is produced from the current value of the
thermistor together with the calibration constants stored in the machine is

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GERBER CryoStar I - Operating Instructions GERBER CryoStar I - Operating Instructions
Error messages 1. First-time operation
The machine displays the following error messages:
1.1. Unpacking
11.1. Error during cooling:
If the heat removal from the sample is too low, then the cooling down takes After opening the carton, remove all accessory parts from the side areas of
too long. The cause for this is either the cooling bath or the agitator. The the carton. Afterwards, you can lift out the machine included the moulded
cooling bath liquid must be -6̊ C or colder and it must circulate well in order foam parts. Remove these moulded parts from the machine. Please keep
to be able to dissipate the heat from the sample. The agitator must agitate both the carton as well as these transport moulded parts in case the
evenly with an amplitude of approx. 3 mm - 4 mm. In the case of cooling machine has to be transported.
errors, first the temperature of the cooling bath must be measured, then the
cooling bath circulation must be checked with an empty sample glass. 1.2. Components Included in the Delivery
Afterwards, it must be checked whether the agitator can oscillate freely and The following components are included in the delivery:
is not bumping or grinding somewhere. Afterwards, the agitator amplitude is CryoStar automatic incl. Carousel
checked. There is also a special menu for the CryoStar I. No number on the Test record printer
display applies as a guideline value - this is only intended as a starting point Mains cable
- instead, you consider the tip of the oscillating agitator and adjust it so that Printer cable
the changeover points are approx. 3-4 mm apart. Then fill a sample glass 1 bottle of cooling bath liquid (500 ml)
with 2.5 ml of water and hold this under the thermistor so that the agitator 1 bottle of calibrating solution A (250 ml)
agitates the water and check whether the agitator also oscillates well in the 1 bottle of calibrating solution B (250 ml)
water. 1 pack containing 50 test tubes
When this has all been checked and correctly adjusted, carry out a sample 1 sample rack
measurement with water and observe the temperature value on the display 1 floppy disk
in doing so. The time which the machine needs to cool down a sample from 1 plastic syringe (to fill in the cooling bath)
room temperature (20 ̊C...25 ̊C) to -2 ̊C should be almost exactly 1 minute. 1 crosstip screwdriver
The cooling bath and agitator are then correctly adjusted. 1 Allan key
If the cooling takes less than 45 seconds, then the cooling bath is too cold This manual.
or the agitator is adjusted too strongly. Please check consignment for completeness upon delivery.
If the cooling takes longer than 75 seconds, then the cooling bath is too
warm or is circulating too badly or the agitator is too adjusted too weakly. 1.3 Place of Installation
If “Error during cooling” occurs after the cooling bath and agitator have been
checked for correct functioning, the thermistor and the machine calibration The equipment should be installed on a perfectly level horizontal surface in
must be checked. If the machine is grossly miscalibrated, it does not find its your laboratory. It should not be placed near ovens, water baths or any
temperature scale and thus cannot measure any correct temperatures. other source of heat or in a humid environment. The equipment needs lots
of cooling air which is sucked in on the right side and blown off on the left
11.2. Frozen too early: side. You should therefore make sure that the lateral slots for air inlet are
The condition of a sample is not stable if it is colder than its freezing point. clear and unobstructed at all times and that no other equipment, and
Thus it can occur that a sample freezes on its own or due to an unintended particularly no heat-emitting appliances, be placed within a distance of 20
influence before the machine initiates the freezing. There are several cm on either side of the CryoStar. Do not leave any loose sheets or similar
possible causes for this: If the agitation is too strong or the agitator is objects near the equipment. These might be carried along with the air
grinding somewhere, vibrations can occur and trigger the freezing. The current and obstruct the air inlet pathway.

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1.4. Filling with cooling bath liquid part of the sample is in the frozen state whereby both parts are in
equilibrium. Thus, the sample must be brought into exactly this condition for
The machine is connected and switched on first (see Chapters 2 and 3). As
measurement of the freezing point. A specified procedure is also required
soon as the measuring head has moved to the top, filling the cooling bath
which functions in the following way:
liquid can be started:
a) Carefully remove the grey foam part. This is only a safeguard
First, the sample must be cooled down while being agitated to below its
during transport.
actual freezing point. The agitation is necessary for 3 reasons:
b) Remove the carousel by pushing down the lock of the carousel.
● The sample is kept in motion so that it cannot freeze on its own.
c) Fill the plastic syringe with cooling bath liquid.
● The sample is well mixed so that all parts of the sample show the same
d) When the machine is running, fill the machine (cooling bath) with
temperature.
approx. 50 ml of cooling bath liquid from the plastic syringe.
● The heat in the sample is transported to the outside where it can be
discharged by the cooling apparatus.
If a liquid is colder than its actual freezing point, this condition is not stable.
This condition is called “metastable”. Small influences such as the impacts
on the glass wall with a hard object already have effects that the freezing
initiates and continues like an avalanche until the fusion heat released
during the freezing has increased the temperature of the sample so that the
freezing point of the sample has been reached and frozen parts are in
equilibrium with not yet frozen parts of the sample.

A cryoscope must then initiate the freezing when the sample is sufficiently
colder than its actual freezing point. What is “sufficiently colder”? The
objective is that so much ice forms during freezing that for the normal size
of ice crystals there are such crystals everywhere in the sample yet the
sample is not yet frozen solid too much. Over time, it has been optimally
proven for milks to initiate the freezing at approx. -2̊C to -3̊C.
e) Switch the machine off for a short time
(approx. 2-3 seconds); switch it on
After initiation of the freezing, the temperature of the sample increases
again afterwards so that air bubbles can
because the fusion heat is released during freezing. It then stabilises to a
escape from the pump system. Repeat
certain value which is called the plateau. The cooling bath continuously
this until there are no more air bubbles
draws heat outside from the sample and at the same rate as this happens
in the system.
further parts of the sample freeze and release their fusion heat. Thus, the
f) Check the filling level of the cooling
temperature remains the same - in any case for as long as still liquid parts
bath liquid. It should be just under the
of the sample are present. This plateau lasts for a few minutes. The
perforated ring. Correct the filling level if
cryoscope determines the freezing point from the temperature measured
needed by adding more or extracting
values of the plateau. There are also standards.
cooling bath liquid.
g) Replace the transparent cooling bath cover afterwards. After
Possible sources of error in the measuring process
completion of the cooling-down phase (approx. 8 – 15 minutes
A certain procedure is followed for determining the freezing point whereby
depending on the ambient temperature), the machine is ready for
errors can occur at any stage of the procedure.
use.
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10.2. Fixed time 1.5 Loading or Unloading the Carousel
Here, there is a fixed waiting time (freely configurable from 20 to 200
seconds) after triggering the freezing. After this time, the measured value Insert the Carousel into the guide as deeply as is necessary to have it
has set itself to a certain temperature which is then output as the freezing locked in place. Press to unlock, if you wish to remove the Carousel.
point value.
Advantage: relatively high sample throughput 1.6. Ongoing care and maintenance
Drawback: low repeatability for strongly fluctuating fat contents. Check the filling level of the cooling bath liquid once per day or after approx.
This method is only authorised for routine examinations. 50 measurements. Remove the carousel for this: the filling level should be
just under the perforated metal. Correct the filling level if needed by adding
10.3. Plateau search more or extracting cooling bath liquid.
With this method, it is set as a criterion that the temperature of the sample If the cooling bath liquid becomes contaminated by milk during operation,
must not change by more than a specified amount within a certain period. replace the cooling bath liquid immediately. Use the supplied plastic syringe
This can be imagined as a template with a window being placed over the for this. Replace the cooling bath liquid once per week and if the machine
cooling-down curve. The window width (20 to 23 seconds is usual) and the has not been used for a long time.
window height (0.2 m̊C to 1 m̊C is usual) are specified and the plateau is Check the internal cleanliness of the machine at least once per year. For
considered as found as soon as the temperature curve is within this window this, the power cable must be disconnected, the cover removed and the
without touching the top or bottom edge. inside of the machine must be cleared of dust and similar. While doing this,
also check the slideway of the measuring head lift. Contamination of the
Benefits: High repeatability. slideway can be removed with spirit.
Reference process
Drawbacks: Long measuring times 1.7. Transport of the apparatus
For some milk samples, no measurement value can be
found because the plateau criterion is not satisfied. The coolant circuit of the machine is open at the measuring point.
Therefore, it is necessary to suck out the cooling bath liquid for transporting
10.4. Maximum search the machine in order to avoid discharges and contamination. This could be
In this method, the warmest point of the temperature curve is searched for. dispensed with only if it can absolutely be ensured that the machine is
For this, the progress of the temperature curve must be followed until a horizontal and level during transport. For protecting the thermistor, place an
clear reduction of the temperature can be seen. Therefore this method empty sample glass at the measuring point, start a measurement (the
takes the longest time of all the methods. It is only used for scientific thermistor moves into the sample glass and is thus protected) and switch
purposes. off the machine. Do not press the measuring head manually downwards
into the cooling bath opening.
11. Sources of error / Error messages
2. Connections:
In order to be able to rectify possible errors, you must know the complete
measuring procedure and be able to correctly assign the individual error
messages. 2.1. Mains connection:

Measuring procedure 230 V / 50...60 Hz or 115 V / 50...60 Hz 180 VA


The freezing point of liquids is not just any temperature but it is exactly the
temperature at which a part of the sample is in the liquid state and another

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2.2. Adjusting the alternating current so, use is made of the fact that a liquid can be cooled down to below its
The machine is set to 230 V at the factory. If a voltage of 115 V is required, actual freezing point while being carefully stirred. This state is not stable.
the voltage can be changed to 115 V using the voltage selection switch. The freezing process can be triggered by vibrations, e.g. by impacts on the
The voltage selection switch is on the right-hand side of the machine. wall of the sample glass. The freezing is also triggered by introducing a
small ice crystal into the supercooled liquid. During freezing, the melting
heat of melting energy is released and the temperature rises until the
freezing point is reached. There, the fusion heat released by the freezing
solid stays in equilibrium with the heat
loss due to the surrounding cooling
bath until the sample is completely
frozen solid and the temperature then
drops.
The graph on the left shows the
principal temperature curve.
However, if the curve in the area of the
The mains connection, the fuse and the mains power switch are plateau is considered with higher
underneath. resolution (second graph), it can
clearly be seen that this plateau is not
completely flat. Therefore a binding
regulation (standard) is needed which
specifies how the freezing point must
be determined from the curve.
For this reason, it has been precisely
2.3. Printer connection: specified in the national and
The report printer is connected to the rear of the machine. You international standards how the
will find a parallel interface (printer connection) and a 6 V chronological progress of the
power supply for the small report printer here. Other PC- measurement curve must be
compatible printers can of course also be used. evaluated in order to determine the
standardised freezing point. The
currently applicable standard defines
the plateau as follows: The temperature value must not increase by more
than 0.5m̊C within a period of at least 20 seconds. The freezing point
2.4. PC connection determination equipment from Funke-Gerber can be freely adjusted in all
Serial interface the important parameters for the measurement. For this reason, the
The serial interface is also at the rear of the machine. Using equipment complies with all national and international standards and
this interface, the measured values, in each case after possible corresponding changes to the standards. The equipment from
completion of the individual measurement, are output to a PC. Funke-Gerber provide the possibility of being able to select from various
( ASCII format, 9,600 Baud). Using the software included in the methods:
scope of delivery, the temperature curves can be displayed on
the screen.

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9.1. Replacing the thermistor 3. Switching on:
Proceed as follows to replace the thermistor: The machine is switched on with the mains power switch (see 2.
• Remove the blue measuring head cover. Undo the Phillips screw on the Connections) on the right-hand side.
rear side of the measuring head for this. The cover can be lifted The following screen is displayed:
off afterwards. After a cooling-down phase of
• There is a hole on each side of the bottom part of the measuring head. In approx. 15 minutes, the
both these holes, there is an Allen screw which fastens the machine is ready for operation
thermistor. and the display changes
• Both the screws can be slackened (slacken only, do not undo automatically to the following
completely) using the small Allen key included in the scope of Main Menu.
delivery. Pull the thermistor connector out of the connection The Main Menu can also be
socket. The thermistor can be removed afterwards. Rotating the reached without waiting time by
thermistor slightly makes its removal easier. Now, you can start pressing the “Enter” key
installing the new thermistor. immediately. However, the
• The new thermistor is inserted into the bore provided with a slight rotary machine is not ready for
movement. operation until after completion
• ·Important: The slot in the thermistor case of the cooling-down phase, i.e.
must be aligned exactly parallel to after reaching the specified
the oscillation movement of the cooling bath temperature, e.g.
stirring rod (see Fig.). The stirring -6.7̊C .
rod must never touch the thermistor
case at any point. It must oscillate Main Menu:
completely freely.
• Now tighten both the Allen screws (grub
screws). Attention: do not screw too
tight or even with force! Afterwards,
plug the connector completely, i.e.
until the plug engages, into the connection socket. Carefully lay
the cable in the area of the rear coil so that it can never come
into contact with the moving parts of the agitator.
• Replace the measuring head cover afterwards.

10. Analytics
10.1. Principle of the freezing point determination
The freezing point is the temperature at which the solid phase and the liquid
phase of a substance or mixture of substances are present simultaneously
and are in equilibrium.
The best suitable method for determining the freezing point has proved to
be undercooling down the sample and then triggering the freezing. In doing
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8. Precalibration (see 5.11).
4. Operation / Menu structure
Using precalibration, the measuring device is put into a defined condition.
The machine is operated in the dialogue using 5 buttons. The Such a precalibration is necessary in particular cases, e.g. for a thermistor
desired function can be selected from the menu using the four change. Without precalibration, it would often not be possible to perform a
“arrow keys” (left, right, up and down). The selected function is normal calibration.
activated using the “Enter” button. An extensive choice of various Only one sample glass with calibration liquid “A” is needed for the
menu languages is available. precalibration. The precalibration can be started after the glass has been
placed in the cooling bath opening.
The most important menu options are:

4.1. Start measurement: The measurement is started (see 6). 9. Thermistor / Temperature measurement

4.2. A-calibration: The A-calibration is started(see 7). The thermistor measures the sample
temperature. There is a special
4.3. B-calibration: The B-calibration is started (see 7). semiconductor material in the tip
whose electrical resistance changes
with the temperature. This very
4.4. Settings: You reach the “Settings” submenu from here sensitive tip is fused into a thin glass
The following screen is displayed: shell. The electrical resistance is
measured and converted into the
corresponding temperature value by a
microprocessor and displayed.

Caution! The thermistor is made of


glass and can break off very easily.
Thermistors will age. Thin, hairline
cracks occur in their thin glass shell
over time where moisture can
penetrate and affect the electrical
values. This is recognised by the
repeatability becoming very bad: the
measured values for the same sample
can deviate very strongly (e.g. 20 m̊C
or more). In these cases, the
thermistor must be replaced.

All important parameters can be freely adjusted.

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7.1. Preparing for calibration: 5. Settings
Ensure that the machine is set to the correct calibration values. Otherwise, 5.1. Freely adjustable calibration values
the calibration values must be changed accordingly (see 5.1 and 5.2). The machine can be calibrated with any calibration solutions. Here,
Four glasses each are needed for the A and B calibration. Place the only the respective A and B calibration values have to be entered.
glasses in the sample rack; ensure that the sample glasss are separated Two different A calibration standards (0.000̊C and -0.408̊C) and two
from each other in the sample rack so that mix-ups between A and B are different B standards (-0.557̊C and -0.600̊C)can be obtained from
ruled out. Pipette 4 sample glasss each with 2,2 ml A-Standard and 4 Funke-Gerber.
Sample glasses each with 2.2 ml B-Standard.
Tip: In order to ensure that the glasses are really clean, or that the calibration Example: The A-value should be changed from 0.000̊C to -0.408̊C:
liquids in the vial correspond to 100% of their value, we recommend rinsing the
vials with the respective calibration fluid in advance.

7.2. Perform calibration


7.2.1. Adjust the machine to the calibration standard
The machine can be adjusted to different calibration standards (see
5.1 and 5.2).
7.2.2. Preparing the Carousel for Calibration
The following configuration is used to fill the carousel:

Spaces 1 to 4: These are the spaces where four test tubes are
placed for A calibration.
Space 5: This space is left unoccupied, without any test tube.
Spaces 6 to 9: These are the spaces where four test tubes are
placed for B calibration.

Once the test tubes are placed in the Carousel, they are filled with the
corresponding calibration solutions.
a) Using the arrow keys, the cursor (red border) is moved to the
7.2.3. Inserting Carousel into the Apparatus position “A: 0.000̊C”.
See section 1.5. b) After pressing the “Enter” button, the cursor changes to a hand with
index finger, the symbol for modifying the value. This hand with index finger
7.2.4. Start Calibration is moved left or right to the desired decimal position using the left and right
Use the two cursor keys to select "Calibration", then arrow keys
activate by pressing "Enter". Start calibration by c) The digit can be increased or decreased using the “Up” and ”Down”
pressing the "Enter" key again. arrow keys.
d) Press the “Enter” button to confirm and save the new value

All other parameters can be set or modified in the same way.

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5.2. B: -0.557̊C
Adjustment of the desired B-calibration value

5.3. Base value: -0.515̊C


Using the base value, the percentage content of the infiltration water
and/or the percentage deviation from this base value can be
calculated and displayed. Both the average freezing point value of
undiluted milk or a limit value, e.g. -0.520̊C, based on which the
percentage deviation is calculated, can be entered as the base
value.

5.4. Trigger: -2.00̊C


After reaching the impact temperature or triggering temperature, the After reaching the triggering The area undemeath the green
freezing process is triggered by impacting the agitator on the temperature (beat temperature), e.g. range represents the specified
sample glass wall. If the “not frozen” message is displayed several -2.00°C, the machine chenges over plateau criterion. Thus it can bee
times, it is recommended to reduce the impact temperature, e.g. to plateau display. This means the checked in a simple and
-2.50̊C. Conversely with “frozen too early”, the impact temperature temperature range is strongly retraceable way whether the
can be increased accordingly. magnified. specified plateau criterion is
Important: After such changes, the machine must be calibrated satisfied.
again.
If you want to look at one of the measured curves again, you navigate to the
5.5. Mode: Celsius blue field, where you can find the last results, select the desired result and
The machine must be set to Celsius or Hortvet (usual in some activate the curve by pressing the enter button.
countries) for freezing point determination.
7. Calibration (normal calibration)
Other possible settings are:
In order to obtain precise measurements, it is necessary to calibrate the
Osmol: Osmometer operation
Petrol: Determination of the solidification point machine. This is due to the physical ambient conditions such as the air
Alcmode: Determination of the alcohol content of alcoholic drinks. pressure. It is recommended to check the calibration at least once per day
and recalibrate if needed. The calibration can be checked easily using a
5.6. Plateau: Seek Plateau control standard. Funke-Gerber has such a control standard (-0.512̊C) in its
The machine can be set to the following operating modes: product range.
The machine is calibrated using two-point calibration, an A-calibration and a
Seek Plateau: This setting is for reference measurements B-calibration. Funke-Gerber provides two different A-calibration standards
according to the new DIN/ISO/IDF/CEN standards. (0.000̊C and -0.408̊C) and two different B standards (-0.557̊C and -0.600̊C).
At least 0.5 m̊C / 20 s must be set as the plateau criterion. This As the machine can be freely programmed, other calibration standards can
means that the temperature value is allowed to increase by a also be used.
maximum of 0.5 m̊C during a period of at least 20 seconds.
The displayed value of 0.4 m̊C / 22 s corresponds to more than the
required standard and is thus a more strict criterion.

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5.13 Recommended settings Fixed time: This is suitable for routine measurements. After
No. Designation Settings activating a freezing process, the measured value is displayed as
the freezing point value after expiration of a specified (modifiable)
51 A-calibration value 0.000°C or -0.408°C time.
52 B-calibration value -0.557°Cor -0.600°C Maximum: In this operating mode, the complete freezing point
53 Base value -0.520°C (EU limit value) curve is displayed until the milk sample is completely frozen and
there is no further temperature increase to display. The warmest
54 Impact temperature. -2.00°C ( -3.00̊C minimum) value, i.e. the highest point of the freezing curve, is taken as the
freezing point value. A measurement takes about 5 minutes. Thus,
55 Mode Celsius his operating mode is only suitable for research purposes.
56 Plateau Plateau search: 0.4 m°C / 22s
Fixed time: 50 s 5.7. Language: English
Maximum: 0.2 m°C There are many different menu languages available. The number of
languages is constantly being extended in cooperation with our
57 Language free choice distribution partners.
58 Agitator see description under 5.8. 5.8. Stirrer After pressing the “Enter” button, the following
If you modify the settings, the machine must be calibrated afterwards. submenu is displayed:

6. Performing measurements
6.1. Insert sample glass in the carousel
The milk sample to be measured is pipetted into a sample glass. The
sample quantity must be between 2.0 ml and 2.5 ml, preferably 2.2 ml. The
sample glass (one sample, up to 12 samples) is placed at any position in
the carousel. Insert the carousel --- now you are ready to start the
measurment!

6.2. Start measurement


Select the “Start measurement”
function using the arrow keys. Press
the “Enter” button after-wards to start
the measurement. The display
changes -- the cooling down curve is
displayed. The temperature values in Stir amplitude: The oscillation movement of the stirrer is
̊C are on the vertical axis. The time in adjusted here. The stirrer should be set to approx. 4 mm
seconds is displayed on the movement width. If the stirrer is considered from the side, the
horizontal axis. The measurement oscillation distance can be seen well. The stirrer amplitude should
can be stopped by pressing the be checked regularly and readjusted if needed.
“Enter” button again.
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Stir frequency: The stir frequency should not be changed. It has 5.10. Print
already been adjusted at the factory. In the case that the frequency Using this command, the printer prints out the complete machine status.
has to be adjusted, it should be set to 3 Hz higher than the This is helpful in the case of fault localisation or when the machine settings
resonance frequency. The resonance frequency is determined, e.g. have been completely modified (“Troubleshooting”). In principle, the
by starting at 80 Hz and constantly increasing the frequency measurement values are printed out automatically (without extra
afterwards (keep the “Up” arrow key pressed). The resonance commands) to the connected printer after each measurement.
frequency is at the point where the stirrer amplitude achieves a
maximum. Afterwards, the frequency is usually set to resonance 5.11. Precalibration
frequency + 3 Hz. The measuring technology is put into a defined position using
precalibration. In particular cases, e.g. thermistor change etc, such a
Test: The impact force is tested here. For this purpose, hold a precalibration is necessary. Without precalibration, it would often not be
sample glass filled with 2.5 ml of water on the measuring head so possible to perform a normal calibration.
that agitator and thermistor dip in the water and activate the agitator A sample glass filled with calibration fluid “A” is needed for the
by pressing the “Enter” button. On the one hand, the agitator should precalibration. The precalibration can be started after the vial has been put
strongly strike the glass wall of the sample glass so that the freezing into the cooling bath opening. After completion of the precalibration, a
process is well and quickly triggered: on the other hand it should not normal calibration must in principle be performed. This precalibration is
be too strong in order to prevent damaging the sample glass. usually not needed.

Beat amplitude: The “correct” beat amplitude can be adjusted


using the “Up” and “Down” arrow keys. 5.12. Technical parameters
The following submenu is displayed after pressing the “Enter” button:

5.9. Sys-Check The following submenu is displayed after pressing


the “Enter” button:

Some information about


the machine condition
(status) is displayed.

A detailed report is printed


using the “Print” command.

Analogously to the previous settings, you can change the date, time and the
cooling bath temperature.

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