IKA

35 488 01

Calorimeter system C 200

Operating instructions

C 200 Vers. 01

Reg.-No. 4343-01

EN

Table of contents
Chapter

Page

Safety precautions

User information

2.1

Information regarding operating instructions

2.2

Warranty and liability

Transport, storage, place of installation

10

3.1

Conditions of transport and storage

10

3.2

Place of installation

10

3.3

Unpacking

10

3.4

Contents C 200

11

Installation and starting up

12

4.1

Calorimeter C 200

12

4.2

Installation

12

4.3

Switching on the system

14

4.4

Display and operating elements

14

4.5

Configuring the system

16

4.6

System settings

17

4.7

Filling the calorimeter for the first time

19

4.8

Switching off the system

20

4.9

Coding decomposition vessels

20

4.10

Oxygen station C 248

21

Calorimetric measurements

22

5.1

Determining the calorific value

22

5.2

Corrections

23

5.3

Information about the sample

24

5.4

Calibration

25

Preparing and performing measurements

26

6.1

Decomposition vessel C 5010

26

6.2

Preparing the decomposition vessel

27

6.3

Preparing the measurement

29

6.4

Performing the measurement

30

6.5

Cleaning the decomposition vessel

32

6.6

Errors in the measuring procedure

33

Service menu

36

7.1

Operation

36

7.2

Description of service menu options

37

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Table of contents
Chapter

Page

Cleaning and maintenance

38

8.1

Inner vessel filter

38

8.2

Filler

38

8.2a

Micro filter

38

8.3

Maintaining the water circulation

39

8.4

Decomposition vessels

40

8.5

Cleaning information

40

IKA accessories and consumablesl

41

9.1

Accessories

41

9.2

Consumables

41

10

Technical data

42

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DE

CE KONFORMITTSERKLRUNG
Wir erklren in alleiniger Verantwortung, dass dieses Produkt den Bestimmungen
der Richtlinien 89 / 336 EWG; 89 / 392 EWG und 73 / 23 EWG entspricht und mit
folgenden Normen und normativen Dokumenten bereinstimmt:
EN 61 010; EN 50 082; EN 55 014; EN 60 555.

EN

CE DECLARATION OF CONFIRMITY
We declare under our sole responsibility that this product corresponds to the
regulations 89 / 336 EEC; 89 / 392 EEC and 73 / 23 EEC and conforms with the
standards or standardized documents:
EN 61 010; EN 50 082; EN 55 014; EN 60 555.

FR

DCLARATION DE CONFORMIT CE
Nous dclarons sous notre responsabilit que se prodiut est conforme aux
rglementations 89 / 336 CEE; 89 / 392 CEE et 73 / 23 CEE et en conformit avec
les normes ou documents normaliss suivant:
EN 61 010; EN 50 082; EN 55 014; EN 60 555.

ES

DECLARACION DE CONFORMIDAD DE CE
Declaramos por nuestra responsabilidad propia que este produkto corresponde
a las directrices 89 / 336 CEE; 89 / 392 CEE y 73 / 23 CEE y que cumple las normas
o documentos normativos siguientes:
EN 61 010; EN 50 082; EN 55 014; EN 60 555.

IT

CE DICHIARAZIONE DI CONFORMIT
Dichiariamo, assumendone la piena responsabilit, che il prodotto conforme alle
seguenti direttive CCE 89 / 336 ; CCE 89 / 392 e CCE 73 / 23, in accordo ai seguenti
regolamenti e documenti:
EN 61 010; EN 50 082; EN 55 014; EN 60 555.

IKA-LABORTECHNIK Janke & Kunkel GmbH & Co. KG

Staufen, November 2005

IKA-WERKE C 200

Ver. 02/2.06

Safety precautions
Calorimeter system C 200 may only be used to determine the calorific value of solid and
fluid materials. Only the appropriate original IKA decomposition vessels may be used
for this purpose. For detailed information, please see the operating instructions for the
decomposition vessels.
The maximum extra energy added to the decomposition vessel must not exceed 40,000 J
(select the test mass accordingly). The permitted operating pressure of 230 bar must not
be exceeded. The maximum permitted operating temperature must not exceed 50C.
Do not overfill the decomposition vessel with sample. Only fill the decomposition vessel
with oxygen to a maximum pressure of 40 bar. Check the set pressure on the pressure
reducer. Perform a leakage test before each combustion process (follow operating
instructions for decomposition vessel!).
Some materials tend to explode when combusted (e.g. due to formation of peroxide),
which could cause the decomposition vessel to crack.
Standard decomposition vessels may not be used for testing explosive samples.
If the burning behaviour of a material is unknown, it must be tested before combustion
in the decomposition vessel (risk of explosion). If you are burning unknown samples,
leave the room or keep your distance from the calorimeter.
Benzoic acid may only be combusted in its pressed form! Flammable dust and powder
must be first pressed. Oven-dry dust and powder such as splints, hay, straw etc. explode
when combusted! Always wet these materials first! Highly flammable liquids with a low
vapour pressure (e.g. tetramethyl dihydrogen disiloxane) must not directly touch the
cotton thread!
Furthermore, toxic combustion residue in the form of gases, ashes or condensation, for
example, is possible in the inner wall of the decomposition vessel.
Please observe the accident prevention regulations applicable for the activity and the
workstation. Wear your personal protective equipment.
When handling combustion samples, combustion residue and auxiliary materials, please
observe the relevant safety regulations.
The following materials, for example, could pose a risk:

corrosive
highly flammable
explosive
bacteriologically contaminated
toxic

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Please observe the relevant regulations when handling oxygen.

Warning: oxygen as a compressed gas is oxidising; intensively aids combustion; can
react violently with flammable materials.
Do not use oil or grease!
Caution - magnetism! Beware of effects from the magnetic field (pacemakers, data media
etc.).
When using stainless steel crucibles thoroughly check their condition after each experiment. If the material gets thinner, the crucible may catch fire and damage the decomposition vessel. Crucibles must not be used for more than 25 combustions for safety reasons.
The decomposition vessel is manufactured in accordance with the directive for pressure
equipment 97/23/EC. This is indicated by the CE symbol with the ID number of the notified body. The decomposition vessel is a category III pressure device. The decomposition
vessel has undergone an EC prototype test. The CE declaration of conformity confirms
that this decomposition vessel corresponds to the pressure device described in the EC
prototype test certificate. The decomposition vessel has undergone a pressure test with
the test pressure of 330 bar and a leakage test with oxygen at 30 bar.
Decomposition vessels are experiment autoclaves and must be tested by a technical
expert after each use.
Individual use is understood here to include a series of experiments performed under
roughly the same conditions in terms of pressure and temperature. Experiment autoclaves must be operated in special chambers (C 2000, C 5000, C 7000, C 200).

The decomposition vessels must undergo repeated tests (internal tests and pressure
tests) performed by the technical expert. The frequency of these tests is to be determined by the operator on the basis of experience, type of operation and the material used
in the decomposition vessel
The declaration of conformity becomes invalid if mechanical modifications are carried
out to the experiment autoclaves or if tightness can no longer be guaranteed as a result
of major corrosion (e.g. pitting by halogens).
The threads on the body of the decomposition vessel and the union nut are subject to
considerable stress in particular and must therefore be checked regularly for wear.
The condition and function of the seals must be checked and ensured by way of a leakage test (see operating instructions for decomposition vessel!).
Only technical experts may perform pressure tests and service work on the decomposition vessel
We recommend that you send the decomposition vessel to our factory for inspection,
and if necessary, repair after 1000 tests or after one year or sooner depending on use.

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For the purposes of these operating instructions a technical expert is someone

1. who guarantees to conduct the tests properly on the basis of his training, knowledge
and experience gained through practical work,
2. who is sufficiently reliable,
3. who is not subject to any instructions in terms of the test activity
4. who has suitable test equipment if necessary
5. who can provide appropriate proof of the requirements listed in 1

National directives and laws must be observed for operating pressure vessels!
Anyone operating a pressure vessel must keep it in a proper condition, operate it properly, supervise it, carry out the necessary maintenance and repair work immediately and
implement the safety measures required in the circumstances.
Pressure vessels must not be used if they have defects which could pose a risk to staff or
third parties. The pressure equipment directive can be obtained from Carl Heymanns or
Beuth publishers.

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2
2.1

User information
Information regarding operating instructions
This symbol indicates information which is essential for the safety of your
health. Failure to observe this information can cause damage to health and
injuries.
This symbol indicates information which is important for ensuring that the
appliance functions without any technical problems. Failure to observe
this information could damage the calorimeter system.
This symbol indicates information which is important for ensuring that
calorimetric measurements are performed efficiently and for using the
calorimeter system. Failure to observe this information can result in inaccurate measurements.

TIPP

This symbol indicates references to the optimization of operatinal sequences are characterized.

Numbers , , etc. indicate guidelines in the following sections which must always
be carried out in order.

2.2

Warranty and liability

You have purchased an original IKA product, manufactured to the latest, highest quality
standards. According to IKA's conditions of warranty, this product is guaranteed for
12 months. To ensure the long-term precision and function of the calorimeter system,
we recommend that you conclude a maintenance agreement (annual maintenance) with
IKA or an authorised IKA workshop. If the first maintenance is carried out within
12 months of purchase, the warranty will be extended to 24 months.
In the case of a warranty claim, please contact the responsible representative or the supplier. You can also return the appliance directly to IKA-WERKE.
Please enclose the sales invoice and the reason for the claim and state the name of the
contact person at your company. Freight charges are to be paid by the sender.
Please read these operating instructions carefully.
IKA-WERKE only consider themselves to be responsible for the safety, reliability and
performance of the appliance when

the appliance has been operated in accordance with the operating instructions,
only persons authorised by the manufacturer interfere with the appliance,
only original parts and original accessories are used for repairs

IKA-WERKE do not accept liability for damage or costs resulting from accidents, misuse
of the appliance or unauthorised changes, repairs or upgrades.

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Transport, storage, place of installation

3.1

Conditions of transport and storage

The system must be protected against mechanical impact, vibrations, dust deposits and
corrosive ambient air during transportation and storage.
It is also important to ensure that the relative humidity does not exceed 80%.
Only the original packing may be used for transportation.
The appliance must be completely emptied before storing and transportation.

3.2

Place of installation

Please observe the respective country-specific regulations for operating pressure equipment when installing the appliance.
A constant ambient temperature is an important requirement for ensuring the high measuring accuracy of the system. The following conditions must therefore be fulfilled at the
place of installation:

No direct solar radiation

No draughts (e.g. beside windows, doors, air conditioning)

Sufficient distance to radiators and other heat sources

The (constant) room temperature should be around 20 C ... 25 C.

The system must be installed on a level surface.

An adequate power supply corresponding to the nameplates on the system components.

Oxygen supply (99.95 % pure oxygen, quality 3.5; pressure 30 bar) with pressure
display and shut-off device. (C29 reducing valve, accessories)

3.3

Unpacking

Please unpack the system components carefully and check for any damage. When you
unpack the equipment, check for any damages which may have occurred during transportation. Make a note of any damage and report it immediately (post, railway, shipping
company).

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3.4

Contents C 200

1 x basic device C 200

1 x decomposition vessel C 5010
1 x ignition adaptor
1 x attachment set
1 x table power supply
1 x plug
1 x operating instructions
1 x water emptying hose (length: 1 m)
1 x oxygen station C 248
1 x measuring cup (2 l)

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11

Installation and starting up

4.1

Calorimeter C 200

measuring cell cover

tank fillers
display
keyboard
fill level display

4.2

Installation

All the connections for draining as well as the peripherals are on the back of the
appliance.

Connecting the plug

Connect the calorimeter to the plug (4-pin plug ).
Check that the voltage information on the rating plate of the power supply unit matches
your mains supply.
Connect the power line of the plug to the voltage source.

PC connector
printer connector
ON/OFF switch

plug

plug connector

12

Connecting peripherals
When connecting peripherals make sure that both they and the calorimeter are
switched off at ON/OFF switch .

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Connecting the water drain

inner vessel emergency drain

tank drain
inner vessel drain

Insert the emptying hose (included in package contents) into plug-in coupling .
Place this in the mould so that it is sloping. This must always be connected for operation.
If the inner vessel ever requires emergency drainage, insert the emptying hose into plugin coupling .
To empty the tank container, insert the emptying hose into plug-in coupling .
(see service menu section 7.2)
If you use a thermostat to fill the tank, you can also hang the drain hose in the thermostat. Check that the thermostat is below the calorimeter. If the thermostat is self-priming

TIPP

in the return line, you can also install the thermostat beside the calorimeter.

Opening the calorimeter cover

The calorimeter cover is opened by hand by lifting the cover by the gripping groove and
raising it until it automatically swivels to the right and locks in position.

Raise

IKA-WERKE C 200

Swivel to right

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13

4.3

Switching on the system

Switch the calorimeter on at ON/OFF switch (back of appliance).

The appliance is now in standby mode.

Press ON (F1) to work with the appliance. The start screen will appear.
The operating console features the following elements:

4.4

Display and operating elements

Display elements during operation:

Status line: shows the current status of the appliance

Footer:

shows what the function keys currently do.

Exception: a progress bar is displayed during automatic measuring runs

Reading value: shows the current temperature increase in minute intervals during the
measurement or the measurement result after the measurement.

Current temperature value: shows the current temperature in second intervals at the
sensor in the inner vessel.

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Operating elements:

Function keys F1, F2, F3: what these keys do depends on the operating state of the
appliance. The footer of the display shows what the function
keys currently do.

Numerical keypad:
Delete button:

this is used to enter digits and the decimal point into

command lines
this key is used to delete the last character entered.

Display elements in menu mode:

If you press the Menu (F3) ) key, a menu will appear in the display which allows you to
enter settings. There are six submenus: GENERAL, CALIBRATION VALUES, UNIT OF
MEASUREMENT, LANGUAGE, MEASURING PROCEDURE and SERVICE.
Pressing the DOWN (F2) key selects the menu line below.
Double clicking (F2) allows you to switch between UP and
DOWN.
The current direction of movement is displayed in the footer.
BACK (F3) allows you to exit a menu without confirming
new settings.

TIPP

Selection menu (e.g. combustible crucible)

Menu header:

shows the name of the submenu and the currently selected menu
line of the total number of menu lines. (For example, 2/5: you are in
the second of five lines)

There are three different menu lines

Submenu line:

, and :

. . . this line indicates that a submenu is called up with OK (F1).

. . . : indicates that it is a selection menu.
If you press OK (F1) on a selection line 4 in this selection menu,
this selection will be confirmed and you will exit the menu. The current selection is marked with = and is displayed after the : in
the submenu line.

Command line:

IKA-WERKE C 200

this line allows you to directly enter numerical values using the keyboard. If you press OK (F1), the menu settings will be saved and you
will exit the menu.

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15

4.5

Configuring the system

In order to ensure that the appliance works properly, you must set some parameters the
first time you use it.

Select language
MENU (F3)
UP/DOWN (F2) to "Language"
OK (F1)
UP/DOWN (F2) select desired language
(default: English)
OK (F1)
BACK (F3)
The set language will appear in the "Language" submenu line.
Set date
MENU (F3)

UP/DOWN (F2) to "General"

OK (F1)
UP/DOWN (F2) to "Date"
Enter the date in the format dd.mm.yyyy
(e.g: 06.12.2005)

OK (F1)
BACK (F3)
Set time
MENU (F3)
UP/DOWN (F2) to "General"
OK (F1)
UP/DOWN (F2) to "Time"
Enter the time in the format hh:mm:ss (e.g: 16:32:51)
OK (F1)
BACK (F3)

Reference
In order to calibrate the appliance you must state the exact calorific value of the calibration substance used (usually benzoic acid).
MENU (F3)

UP/DOWN (F2) to "General"

OK (F1)
UP/DOWN (F2) to "Reference"
Enter the calorific value in the format xxxxx

16

(default: 26460)
OK (F1)
BACK (F3)

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Calibration values
Once you have calibrated the appliance, you will need to enter the calculated C-values
(calibration values) of all the decomposition vessels used.
MENU (F3)
UP/DOWN (F2) to "Calibration values"
OK (F1)
UP/DOWN (F2) select desired decomposition vessel
Enter the C-value in the format xxxx (default: 1)
OK (F1)
BACK (F3)
See the advice in section 5.4 Calibration.

4.6

System settings

In addition to the configuration described in section 4.5, you can apply other settings
which are not necessary for the correct functioning of the appliance or which are only
required for special applications

Combustible crucible
If you are using a combustible crucible, you can enter this here. The value for the external
energy QExternal1 will then be automatically reduced by 50 joules as no cotton thread is
used. The combustible crucible itself must be weighed and the resulting calculated energy
value manually entered under QExternal2 (see section . 6.3, ) so that it can be taken into
account as external energy when calculating the calorific value.
MENU (F3)
UP/DOWN (F2) to "General"
OK (F1)
UP/DOWN (F2) to "Combustible crucible"
OK (F1)
Select the options "with" oder "without"
(default: without)
OK (F1)
BACK (F3)

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17

Operator
You can assign each operator an ID number (0-9). This number will appear on the results
report.
MENU (F3)
UP/DOWN (F2) to "General"
OK (F1)
UP/DOWN (F2) to "Operator"
Enter ID code (default: 0)
OK (F1)
BACK (F3)

Unit of measure
You can set the unit of measure you want the measuring results to be displayed in.
The currently selected unit of measure is marked with "=".
MENU (F3)
UP/DOWN (F2) to "Unit"
OK (F1)
UP/DOWN (F2) select the desired unit
(default: J/g)
OK (F1)
BACK (F3)
Measuring procedure
You can choose between four measuring procedures:
MENU (F3)
UP/DOWN (F2) to "Measuring procedure"
OK (F1)

UP/DOWN (F2) select desired measuring procedure

(default: Isoperibol)

OK (F1)
BACK (F3)
Isoperibol
Calorimeter C 200 automatically performs the measurement according to the standard
for isoperibol calorimeters and calculates the provisional result for you. The measurement takes approx. 17 minutes with excellent result reproducibility.
Manual
This is student mode. You work according to the standard for isoperibol / isothermal
calorimeters. You read the temperature values off yourself every minute, calculate the
temperature drift before ignition, ignite and end the experiment by pressing F1, calculate
the temperature drift after the temperature increase and calculate the result itself.
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Dynamic
Calorimeter C 200 performs the measurement automatically and calculates the provisional result. The measuring time is reduced to approx. 8 minutes thanks to a dynamic correction process. It is still possible, however, to meet the accuracy specifications of the
international standards.
Time control
Calorimeter C 200 performs the measurement automatically according to a set period of
time and calculates the provisional result. The measuring time is set at 14 minutes.

4.7

Filling the calorimeter for the first time

Before using the calorimeter for the first time you must fill the outer vessel with tap
water. To do this, pour two litres of tap water into the filler of tank (see section 4.1)
using the measuring cup provided.
The water must first be maintained at a constant temperature. To ensure accurate results,
the initial temperature must not fluctuate too much.
Water temperature 18 C - 25 C with an accuracy of 1 C during a measurement series

You must now pump the water out of the tank into the outer vessel:
MENU (F3)
UP/DOWN (F2) to "Service"
OK (F1)
UP/DOWN (F2) to "Pump off"
OK (F1)
The surge will start
Keep an eye on the water by pulling the filler of tank (see section 4.1) out the top.
When the overflow causes the water to run back in the side of the tank, the outer vessel
is full and you must switch of the pump again by pressing OK (F1) once more.
You should change the water if it has been sitting for a long time. See section 8.3.

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TIPP

19

4.8

Switching off the system

Standby mode
In order to switch off the calorimeter system, the start screen must be displayed.
Press OFF (F1). The appliance will switch to standby mode.

Switching off
Only switch the appliance off in standby mode. To do this, press the ON/OFF switch
(see section 4.2) on the back of the appliance.

4.9

TIPP

Coding decomposition vessels

You can use several decomposition vessels (max. 4) when working with calorimeter C
200. You can code these to distinguish between them by sticking the black coding strips
into the special slots on the decomposition vessels.

Decomposition vessel no.:

(without coding)

Slot for coding strips

3

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4.10

Oxygen station C 248

The C 200 does not have an integrated oxygen filling point for the decomposition vessel.
You can use oxygen station C 248 for filling. For information on how to operate and connect the oxygen station, please see the accompanying operating instructions.
Operation:
Place decomposition vessel C 5010 on the marked position
Move the lever down and centre the decomposition vessel below the fill head
Lock the lever in place
Fill the decomposition vessel for approx. 30 secs.
Move the lever back to its original position

Lever

Fill head

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21

Calorimetric measurements
5.1

Determining the calorific value

Combustion is carried out in a calorimeter under specific conditions. The decomposition

vessel is filled with a weighed fuel sample, the fuel sample is ignited and the temperature
increase in the calorimeter system measured. The specific calorific value of the sample is
calculated as follows:

Ho = (C * DT - QExternal1 - QExternal2) / m

(1)

m
C
DT
QExternal1

Weight of fuel sample

Heat capacity (C-value) of calorimeter system
Calculated temperature increase of water in inner vessel of measuring cell
Correction value for the heat energy generated by the cotton thread as
ignition aid
QExternal2 Correction value for the heat energy from other burning aids
The decomposition vessel is filled with pure oxygen (99.95 %) to optimise the combustion process. The pressure of the oxygen atmosphere in the decomposition vessel is
max. 30 bar. Formula (1) for the calorific value of a material requires that combustion
takes place under specifically defined conditions. The relevant standards are based on
the following assumptions:

The temperature of the fuel and its combustion products is 25C.

The water contained in the fuel before combustion and the water formed whilst combusting the hydrogenous compounds of the fuel is in fluid form after combustion.
The atmospheric nitrogen has not oxidised.
The gaseous products after combustion consist of oxygen, nitrogen, carbon dioxide
and sulphur dioxide.
Solid materials may form (e.g. ashes).

In many cases, however, not just the combustion products referred to in the standards are
produced. In such cases the fuel sample and the combustion products must be analysed
to provide data for a revised calculation. The standard calorific value is then calculated
from the measured calorific value and the analysis data. The heat value Hu is the same
as the calorific value, minus the condensation energy of the water contained in the fuel
and formed through combustion. The heat value is the more important parameter from
a technical point of view because in all major, technical applications only the heat value
can be evaluated in terms of energy.
The complete bases of calculation for the calorific and heat value can be found in the
relevant standards (e.g.: DIN 51 900; ASTM D 240; ASTM D 5865..). They are also contained in the CalWin calorimeter software.

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5.2

Corrections

Due to the nature of the system a combustion test does not just produce the combustion
heat of the sample, but also heat from external energy (QExternal).
This can fluctuate considerably in relation to the heat quantity of the fuel sample.

Heat quantity from:

Fuel sample

External energy
(QExternal)
(QFremd)
Burning aid

Igniter
Formation of
sulphuric acid

Formation
of nitric
acid

The combustion heat of the cotton thread which ignites the sample and the electric ignition energy would distort the measurement. This influence is taken into account in the
calculation by way of a correction value
Note: in all the automatic calculations an extra 100 J have already been included for the
electric ignition energy. This value cannot be set.
Materials which are difficult to ignite or combust are combusted together with a burning
aid. The burning aid is first weighed and then put into the crucible with the sample.
The additional heat quantity can be determined from the weight of the burning aid and
its known specific calorific value. You must correct the test result by this heat quantity.
Combustible crucible C 14 is a combustible crucible, which can be used instead of a standard crucible. The combustible crucible burns without leaving any residue whatsoever.
When using a combustible crucible you do not need an extra cotton thread. The crucible
is placed directly on the permanent ignition wire in the decomposition vessel and ignited.
The cleanliness of the material used in the combustible crucible prevents chemical contamination of the sample (no blank values).
Decomposition vessels, in which the combustible crucible is used, must be fitted with an
extra part (support C 5010.4, see Accessories). The sample is weighed out into the combustible crucible as normal. In most cases no additional burning aid is required because
the combustible crucible itself serves as a burning aid.

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23

Virtually all of the materials to be studied contain sulphur and nitrogen. Under the conditions in calorimetric measurements, sulphur and nitrogen combust to SO2, SO3 and NOx.
Together with the water from combustion and moisture, sulphuric and nitric acid as well
as heat of solution are produced. In order to obtain the standard calorific value, the influence of the heat of solution on the calorific value is corrected. The calculation formulae
depend on the standard used. These are not taken into account in the calculation for
C 200. Use IKA's CalWin software for this.

5.3

Information about the sample

It is essential that the sample fully combusts to ensure correct determination of the calorific value. After each experiment check the crucible and all the solid residue for signs of
incomplete combustion.
As a rule the weighted sample must be selected in such a way that the temperature
increase during the measurement is below 4 K and comes close to the temperature increase of the calibration (max. extra energy: 40,000 J).
Normally solid materials in powder form can be combusted directly. Materials which
combust quickly (e.g. benzoic acid) must not be burnt loose. These materials tend to
splash and there is therefore no guarantee of complete combustion. Furthermore, this
can damage the inner wall of the decomposition vessel. IKA pelleting press C 21 and
IKA analytical mill A11 basic (see Accessories) are available for sample preparation.
Materials which are difficult to burn (materials with a high mineral content, low caloric
materials) can often only be fully combusted using IKA acetobutyrate capsules C 10,
IKA combustion bags C 12 or IKA combustible crucible C 14 (see Accessories). It is
also possible to use liquid burning aids such as paraffin oil.
Before filling the capsule or the combustion bag with the substance to be determined,
weigh them to calculate the extra external energy added by the burning aid from the
weight and the calorific value. This must be taken into account in QExternal2. You should
keep the amount of burning aid used to a minimum.
Most fluid substances can weighed out directly into the crucible. Highly volatile substances are poured into combustion capsules (IKA gelatine capsules C 9 or IKA acetobutyrate capsules C 10, see Accessories) and combusted together with the capsules.
The burning aids (e.g. cotton thread) must also fully combust. If there is any unburnt
residue, the test must be repeated.
When working with unknown substances, select very small weighted samples at the start
in order to determine the natural energy. If you are burning unknown samples, leave the
room or keep your distance from the calorimeter.

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After combustion the water produced is collected and the decomposition vessel is thoroughly rinsed with distilled water. The water used for rinsing and the solution produced
are combined and examined for their acidity. If the sulphur content of the fuel and the
nitric acid correction are known, it is not necessary to analyse the water.

5.4

Calibration

The calorimeter system must be calibrated before accurate measurements are possible.
This is done by combusting tablets made of certified benzoic acid (see Accessories) with
a known calorific value. The heat quantity required to raise the temperature of the calorimeter system by one Kelvin is used to determine the heat capacity of the so-called
"C-value" of the system. For this calculation the formula (1) (see section 5.1) is adapted:

C = (Ho * m + QExternal1 + QExternal2) / DT

(2)

This value is used for determining the following calorific values.

The heat capacity is determined by the measuring cell and the decomposition vessel (DV).
It has a significant influence on the calorific value to be calculated and must be redetermined in particular when using for the first time, after servicing and when parts are replaced. A monthly control measurement is recommended.
The system must be calibrated in every work mode used.
If a calorimeter is operated with several decomposition vessels, you will need to determine the heat capacity of the system for each decomposition vessel.
Ensure that calibration is carried out under the same conditions as the subsequent tests.
If substances are used in the decomposition vessel in combustion tests (e.g. distilled water or solutions), you must use exactly the same amount of this substance for calibration.
For more detailed information on calibration, please see the relevant standards.

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25

Preparing and performing measurements

The term "measurements" below refers to both the measurements to calibrate the calorimeter system (calibration measurements) and the actual measurements for determining
the calorific value. The difference lies in the calculation (cf. section 5, formulae (1) and (2)),
whereas preparation and performance are virtually identical.
Exact measurements are only possible when the individual test steps are carried out carefully. You must therefore follow the exact procedure described in section 1 "For your
safety and in the following sections
Please also see section 5 "Calorimetric measurements
Failure to observe these instructions could result in damage to the decomposition vessel. Damaged decomposition vessels could crack! Follow the operating instructions for
the decomposition vessel!

6.1

Decomposition vessel C 5010

Union nut
Oxygen valve

Electric ignition contact

Ignition wire

Cover
Crucible

Crucible holder

If several decomposition vessels are used, their individual parts must not be interchanged (see Stamping individual parts).
To prolong the life of wearing parts (o-rings, seals, etc.) we recommend that you always
work with a water trap.
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6.2

Preparing the decomposition vessel

Prepare the decomposition vessel as follows

Unscrew the union nut and remove the cover using the handle

Handle

Cover
Union nut

Attach a cotton thread to the centre of the ignition wire using a loop

Cotton thread

Weigh out the substance directly into the crucible with an accuracy of 0.1 mg. Note
the weight or enter directly into the calorimeter. (See section 6.3 "Preparing the
measurement")
Insert the crucible into the crucible holder

If necessary put some distilled water or a solution into the decomposition vessel.
See section 5.3 "Information about the sample" and section 1 "Safety precautions.

Using tweezers, align the cotton thread so that it hangs inside the crucible and is
immersed in the sample. This will ensure that the burning thread ignites the sample
during the ignition process.
Insert the cover into the decomposition vessel and hand tighten the union nut.

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27

Fill the decomposition vessel using oxygen station C 248. (See section 4.10

Slide the ignition adaptor onto the decomposition vessel

For information on how to operate the decomposition vessel, please see the operating
instructions provided.
Attaching the ignition adaptor

Detaching the ignition adaptor

1.
2.

Place the decomposition vessel into the inner vessel of calorimeter C 200.
The decomposition vessel must be placed between the three locating bolts.

Locating bolt

28

Magnetic stirring bar

Pour approx. 2 l tap water maintained at a constant temperature into the tank using
the measuring cup. Keep an eye on the level indicator!

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6.3

Preparing the measurement

The calorimeter is in waiting mode.

Selecting MEASUREMENT (F2) will take you to the "Prepare measurement" menu.

Enter the noted weighted sample in the marked "Einwaage" (weighted sample) field
with an accuracy of 0.0001 g using the keyboard.

You can access all the other options by pressing UP/DOWN (F2):

CALIBRATION
Enter "1" here to perform a calibration..
Check the other presettings:
DECOMPOSITION VESSEL
Enter the number of the decomposition vessel used for this test. If you are only
using one decomposition vessel, you can leave the "1" in the "decomposition vessel"
field.
QEXTERNAL1
Correction value for the heat energy generated by the cotton thread ignition aid. A
default value of 50 J is specified here. The default value for the combustible crucible
option is 0 J. If you use a burning aid other than the C 710.4 IKA cotton thread,
change this value.
QEXTERNAL2
Correction value for the heat energy from other burning aids e. g. combustible
crucible). The default value is 0.

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29

TESTNO
For each measurement the software automatically assigns a number in the form of
yymmddnn, with jj representing the year, mm the month, dd the day and nn a consecutive number. You can also assign your own numbers to the measurements.
Example: TestNo = 0509150 represents the first measurement on 15 September 2005

Press OK (F1) to apply your entries.

6.4

Performing the measurement

Once you have done all the necessary preparatory work as described above, the message
Tank gefllt? (Tank filled?) will appear. Check that the tank is filled with water maintained at a constant temperature and confirm by pressing CONTINUE (F1).
The message close cover will appear.

30

Close the cover by moving it to the left out of the locking position until it slides
down by itself. The decomposition vessel comes into contact with the igniters via
the ignition adaptor.
The "Fill" message will appear.

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The inner vessel will be filled with water (approx. 70 s). The measurement process
will begin as soon as it is full.

a)

b)

The measurement process is fully automatic for automatic measuring procedures

(isoperibol, dynamic and time-controlled, see section 4.6). The result will appear
once the measuring process is complete

With the manual measuring procedure the user decides when ignition is to take
place and when the measurement is complete.

To start ignition press IGNITE (F1)

Press the same key END (F1) again to end
the measurement

In the case of manual ignition / completion, "Preparing to ignite" or Preparing to

complete" will appear in the status line. Ignition/completion is only finished when
this display disappears (max. 60 sec.).

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31

6.5

After the measurement open the cover to automatically empty the inner vessel.
Remove the decomposition vessel and the ignition adaptor. To release tension in the
decomposition vessel use venting button under a fume hood or venting station
C 5030 available in our accessories range. See also section 1 "Safety precautions".
Open the decomposition vessel and check the crucible for signs of incomplete combustion. If combustion is incomplete, discard the test result. Repeat the test.

Cleaning the decomposition vessel

If you suspect that the combustion sample, the combustion gases produced or the combustion residue could be harmful to health, wear personal protective equipment (e.g.
protective gloves, breathing masks) when handling these materials. Harmful or polluting
combustion residue must be disposed of as hazardous waste. Express reference is made
to the applicable regulations.
In order to obtain accurate measurements it is essential that the decomposition vessel is
clean and dry. Impurities alter the heat capacity of the decomposition vessel and thus
cause inaccurate measuring results. It is important to thoroughly clean the inner walls of
the vessel, the internal fittings (brackets, electrodes etc.) and the combustion crucible
(inside and out!) after each combustion test.
In most cases, you will only need to remove condensate from the inner walls of the vessel and the internal fittings. It is sufficient to thoroughly wipe the parts with an absorbent, non-fibrous cloth. If the decomposition vessel cannot be cleaned in the above way
(e.g. due to baking, pitting, corrosion etc.), please contact the Technical Service.
The combustion residue in the crucible, e.g. soot or ashes, should also be wiped away
with an absorbent non-fibrous cloth.

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6.6

Errors in the measuring procedure

Errors in the measuring procedure are shown in the alarm line of the display and remain
there until they are appropriately acknowledged by the user.
Message:

Cover open

Cause:
User action:

the cover was opened during the measuring process.

the inner vessel will be emptied automatically, after which a new
measurement can be started.
if the cover was opened within a minute of ignition, automatic
emptying will be delayed by approx. 2 mins for safety reasons.

Note:

Cause:

no ignition contact during the measurement.

User action:

open the cover and check the ignition wire and ignition contacts.
If necessary, clean the ignition contacts or change the ignition wire.
Check that the ignition adaptor is in the right position.

Message:

No temperature increase
(appears if the value specified for the temperature increase is not
reached within one minute of ignition (0.05 K).

Cause:
User action:

sample not combusted.

(Cotton thread had no contact to sample)
open cover and remove decomposition vessel. If the cotton thread has
not combusted, check the ignition contacts and the ignition wire.
Otherwise, start a test and use ignition aid if necessary

Cause:
User action:

decomposition vessel may not have been filled with oxygen.

open the cover to cancel the test and perform a new measurement

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Message:

A/D converter error

Cause:
User action:

an error has occurred in the temperature measuring system.

if the measurement is still active, open the cover to cancel the test.
Then reinitialise the converter (see section 7.2 ReInit).
If this does not work, switch the appliance off and then back on again.
If this does not work either, please contact IKA Service.

34

Message:

Fill time exceeded

Cause:
User action:

no water in tank
check the fill level in the tank and top up with water if necessary.
Press CONTINUE (F1) to repeat the filling process and continue the
measurement.

Cause:
User action:

filter in inner vessel is dirty.

open the cover to cancel the test. Remove and clean the inner vessel
filter.

Cause:
User action:

pump for filling inner vessel is not working

open the cover to cancel the test. Switch on the pump in the service
menu (see section 7.2 Pump) and check water jet in tank. If there is
no water flow, please contact IKA Service.

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Message:

Start temperature outside

Cause:
User action:

start temperature of inner vessel is not in range 22 3 C

open cover to cancel measurement, or press CONTINUE (F1) to
continue the measurement anyway.

Note:

a measuring result obtained in this way does not correspond to the

standard conditions

User action:

check the water temperature for the tank. Check the temperature
shown. If it does not change within 5 to 10 secs, reinitialise the A/D
converter. (See section 7.2 ReInit)

Message:

Drift unstable

Cause:

there is no magnetic rod in the inner vessel or the magnetic rod is

outside of the magnetic field.
open the cover to cancel the test and check the position of the
magnetic rod. If necessary, insert the rod or position properly.
(See section 6.2, )

User action:

Cause:
User action:

the stirrer is not working.

open the cover to cancel the test. Half fill the inner vessel with water
(via Service menu see section 7.2) and then manually switch the stirring motor on and off (also via Service menu). If the stirring motor
does not work, please contact IKA Service.

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35

Service menu
7.1

Operation

This menu allows you to directly control and test various actions and statuses of the
calorimeter without performing a measurement. There are also menu items which can be
used to start up and shut down the appliance. The service menu can only be run if the
calorimeter displays the start screen.
Perform the desired action using:
MENU (F3)
UP/DOWN (F2) to "Service"
OK (F1)
There are now eight actions to choose from

select the desired action with UP/DOWN (F2)

OK (F1) starts the action
OK (F1) stops the action again

Please note that you must stop every started action.

Exceptions: The "Ignite action ends automatically after a set time period
(approx. 2 seconds).
With actions "Reset and "ReInit you will automatically exit the menu
after the actions have been performed.
If you exit the service menu, all the started actions will be stopped and the system will be
restored to its original state. This will allow you to continue without any errors.

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7.2

Description of service menu options

Ignition
This menu item allows you to check the ignition function
Requirement: there must be a decomposition vessel without sample, but with ignition
thread in the inner vessel and the cover must be closed.
Fill IV
This menu item allows you to fill the inner vessel manually.
Requirement: there must be enough water in the tank.
Empty IV
This menu item allows you to empty the inner vessel.
Requirement: the emptying hose must be locked in place in the plug-in coupling
(section 4.2).
Stirrer
This menu item allows you to switch on the stirrer drive and check that the magnetic rod
is also rotating in the inner vessel.
Requirement: there must be approx. 0.5 l water in the inner vessel
Pump
Switch the pump on with this menu item. The outer vessel will be filled and rinsed.
(See also section 4.7)
Requirement: check that there is water in the tank.
Empty outer vessel
This menu item allows you to empty the outer vessel.
Note: shut-down, completely empty appliance
Requirement: the emptying hose must be locked in place in plug-in coupling
(section 4.2)
Reset
This menu item allows you to restore the default settings.
Reinit
This menu item allows you to reinitialise the A / D converter.

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37

Cleaning and maintenance

In order to ensure trouble-free operation over a long period of time, it is important to
carry out the following maintenance work to the calorimeter system.

8.1

Inner vessel filter

Remove the filter element from the inner vessel and clean the inner vessel filter in clear
water or an ultrasonic bath if there is any dirt visible. Also clean the inner vessel, by removing the positioning mount for the decomposition vessel. Place the filter back on the
inner vessel connector after cleaning.
Operation without the filter element causes dirt in the valves and thus appliance failure.

8.2

Filler

There is also a filter in the filler. This prevents dirt in the storage container.
If the filter is dirty, remove the entire filler and clean the filter. (See section 4.1, )

8.2a Micro filter

38

In the back plate of the equipment is additionally a

micro filter. If the micro filter is dirty, the water flow in
the equipment is reduced. Thus the water filling time
of the inner vessel extends. Thereby if the upper time
limiting is exceeded by 120 seconds, the system
indicates the disturbance and breaks the measurement
off.

IKA-WERKE C 200

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For cleaning the micro filter you must empty the

outer vessel (chapter 7.2).

Screw the cover of the micro filter down and pull

you out the filter element.

Clean the filter element with clear water.

Insert the filter element after cleaning with the opening inward again into the housing of the micro filter and screw you on hand tight the cover.

Fill the outer vessel again with water (chapter 4.7).

Control the tightness after you the equipment
filling (chapter 6.6 fill time exceeded).

8.3

Maintaining the water circulation

In the case of discontinuous use with tap water (single measurements with long gaps) a
stabiliser must be added to the water circulation to prevent the formation of algae.
Add approx. 4 ml IKA-Aqua-Pro C 5003.1 to the tank (see Accessories). Switch the pump
on via the service menu (section Pump). Switch the pump off again after 30 - 60 s.
You can also add the 4 ml Aqua-Pro to the water maintained at a constant temperature in
the last measurement. (Before long gaps in measuring)

TIPP

If the appliance is not going to be in operation for a long period of time, it is advisable
to completely empty the calorimeter's water circulation.
The water must be drained out before transportation.
Empty the outer vessel via the service menu (section 7.2 Outer vessel). The emptying
hose must be locked in place in the plug-in coupling (section 4.2).
Empty the tank by locking the emptying hose in place in the plug-in coupling
(section 4.2). ). The tank will empty automatically.
Press the locking knob on the plug-in coupling to remove the hose.

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39

8.4

Decomposition vessels

Please see the operating instructions for C 5010 for information on decomposition
vessel maintenance!

8.5

Cleaning information

Only clean IKA appliances using these IKA approved cleaning agents:
Dirt

Cleaning agent

Dyes

Isopropanol

Building materials

Water containing detergent, isopropanol

Cosmetics

Water containing detergent, isopropanol

Food

Water containing detergent

Fuels

Water containing detergent

Other materials

Please consult IKA

Comment:
Do not place electrical appliances into the cleaning agents for cleaning purposes.
Stainless steel parts can be cleaned using standard stainless steel cleaning agents, but
do not use abrasives.
We recommend that you wear protective gloves for cleaning.
The operator is responsible for ensuring appropriate decontamination in the event that
dangerous material is spilt onto or into the appliance.
Before using a cleaning or decontamination method other than that recommended by
the manufacturer, check with the manufacturer that the intended method will not destroy
the appliance.

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IKA accessories and consumables

9.1

Accessories

C 5010
C 5010.4
C 5010.5
C 5010.6
C 5030
C 5040
C 248
C 21
C 29
C 200.1
A 11 basic

9.2

Consumables

C 710.4
C 5010.3

Cotton thread, cut to length (500 x)

Ignition wire, replacement (5 x)

C 5003.1
C4
C5

Aqua-Pro bath stabiliser (30 ml)

Quartz dish
VA combustion crucible set (25 x)

C
C
C
C
C
C
C
C

Quartz dish, large

VA combustion crucible set, large (25 x)
Gelatine capsules (100 x)
Acetobutyrate capsules (100 x)
Combustion bag, 40 x 35 mm (100 x)
Combustion bag, 70 x 40 mm (100 x)
Benzoic acid (NBS 39i, 30 g)
Benzoic acid (100 g)
Benzoic acid blister pack (50 x)

6
710.2
9
10
12
12A
43
43A

C 723
C 14
C 15

IKA-WERKE C 200

Decomposition vessel, standard

Support for combustible crucible
Support for large crucible
Venting button
Venting station
CalWin, calorimeter software
Oxygen station
Pelleting press
Reducing valve
Measuring cup
Analytical mill

Ver. 02/2.06

Combustible crucible (100 x)

Paraffin strips (600 x)

41

10 Technical data
Tischnetzteil (external):
Rated voltage/frequency

100 - 240 V AC 50 / 60 Hz

Input power max.

120 W

Calorimeter:
Rated voltage

24 V DC 5A

Input power max..

100 W

Fuses (internal)

1x 2.5 AT

On-time

Continuous operation

Protection class as per DIN EN 60 529

IP 21

Protection class

III

Overvoltage category

Level of contamination

II

Ambient temperature

20 C ... 25 C (constant)

Ambient humidity

80%

Use above sea level

2000 m above sea level

Size

400 x 400 x 400 (W x D x H)

Weight

21 kg

Measurement ranges

40,000 J

Measuring mode / measurement times:

Isoperibol / approx. 17 min

Dynamic / approx. 8 min
Time control / 14 min
Manual / approx. 17 min
1 x parallel (Centronics)

Interfaces

1 x serial (RS 232)

Subject to technical change!

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IKA

Europe
Middle East
Africa

IKA - WERKE GMBH & CO.KG

North America
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IKA Works, Inc.

Asia
Australia

IKA Works (Asia) Sdn Bhd

Japan

IKA Japan Y.K.

Janke & Junkel - Str. 10

D-79219 Staufen
Tel.:+49 7633 831-0
Fax:+49 7633 831-98
E-mail: [email protected]

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Wilmington, NC 28405-7419 USA
Tel.: 800 733-3037
Tel.: +1 910 452-7059
Fax: +1 910 452-7693
E-mail: [email protected]

No. 17 & 19, Jalan PJU 3/50

Sunway Damansara Technology Park
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E-mail: [email protected]

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E-mail: [email protected]

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IKA Works Guangzhou

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Tel.: +86 20 8222-6771
Fax: +86 20 8222-6776
E-mail: [email protected]

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