Ika c1 Calorimeter Manual
Ika c1 Calorimeter Manual
Ika c1 Calorimeter Manual
C 1_042016
IKA® Calorimeter C 1
Operating instructions EN
EN
Declaration of Conformity
We declare under our sole responsibility that this product is in compliance with the regulations 2014/68/EC (article 3, (3)), 2011/65/EU,
2014/30/EU and 2014/35/EU and conforms to the standards or standardized documents: EN 61010-1, EN 61326-1, EN 60529 and EN ISO
12100.
Indicates a potentially hazardous situation, which, if not avoided, can result in death, serious injury.
WARNING
Indicates a potentially hazardous situation, which, if not avoided, can result in injury.
CAUTION
User notes
Read the operation instructions completely before The warranty does not cover worn out parts, nor does it apply
starting up and follow the safety instructions. to faults resulting from improper use, insufficient care or
Keep the operation instructions in a place where they can be maintenance not carried out in accordance with the instructions
accessed by everyone. in this operating manual.
Ensure that only trained staff work with the appliance.
Please read these operating instructions carefully. IKA only
®
Follow the safety instructions, guidelines, occupational health and consider themselves to be responsible for the safety, reliability
safety and accident prevention regulations. and performance of the appliance when
In this chapter you can find out how to work through these • the appliance has been operated in accordance with the
Operating Instructions most effectively to be able to work reliably operating instructions,
with the calorimeter system.
• only persons authorised by the manufacturer interfere with
The instructions in the section “Safety instructions“ must the
be complied with. appliance,
The chapters are designed for you to work through them in order. • only original parts and original accessories are used for repairs.
The section “Transport, storage“ is relevant for system reliability The calorimeter system may be opened only by an authorised
and for ensuring high measuring accuracy. Service Agent or Customer Service Centre.
The calorimeter system is ready to perform measurements once If service is required, we recommend that you contact our
you have completed the procedures in the section “Setting up customer service department. Furthermore, we refer you to the
and commissioning“: - “Preparing a measurement“ and “Starting applicable safety conditions and accident requirements.
a measurement“.
Numbers 1, 2, 3 etc. indicate operating instructions in the IKA is not responsible for damages or costs resulting from
®
following sections. These must always be carried out in the accident, improper use of the device or impermissible modifications,
specified sequence. repairs or renovations.
Page Page
Declaration of Conformity 02 Measurements 25
Explication of warning symbols 02 New measurements 25
User notes 02 Last result 25
Contents 03 System test 26
Safety instructions 04 Measurement archive 26
Correct use 05 Measurement archive: Edit 27
System properties 05 Measurement archive: Print 27
Transportation, Storage 06 Measurement archive: Delete 27
Transport and Storage conditions 06 Measurement archive: Delete all 28
Unpacking 06 Calibration archive 28
Scope of delivery 06 Calibration archive: Edit 28
Description of the system components 06 Calibration archive: C-Value selectin 29
Hoses 07 Calibration archive: Print 29
Calibration archive: Delete 29
Commissioning 07
Place of installation 07 Default settings 30
Cooler connection 08 Settings 30
Venting hose connection 08 Date / Time 30
Drain hose connection 08 Units 30
Oxygen supply connection 08 Display / Keypad 31
Power supply unit connection 09 Inverted menu view 31
Connection of peripherals 09 List view 31
Handling the unit 09 Language 31
Accessories 32
Control unit with display 10
Chiller test 32
Dialog box 11
System start 12 Maintenance 32
Maintenance menu 32
Switching on the system (in the open state) 12
Change seal 33
Selection of language 12
Stirrer test 33
Pressure test 13
O2 System blow 33
Oxygen pressure 13
Servo up 33
System check 13
Servo down 33
Heating detected 14
Factory settings 14 Informations 33
Calorimetric measurements 14 User information: Memory 34
Determination of gross calorific value 14 Prior to input a new measurement 34
Corrections 15 After input a new measurement 34
Notes on the sample 15 Exchanging off wear parts 34
Complete combustion 16 O2 Valve seal change 34
Calibration 16 Change ignition wire 35
Notes on calibration 16 Change ignition electrode 35
Overview Main menu 17 Change the main seal 35
Measurements 17 Change ground electrode 36
Default settings 17 Leak test with the system test 36
Settings 17 Fault and troubleshoot 36
Maintenance 18 E01 STIRRER 36
Informations 18 E02 COMMUNICATION 37
Preparing and performing measurements 18 E03 DRIFT ALARM 37
Performing the measurement 18 E04 MINTEMPDIFF 37
Placing the sample 19 E05 FILLWATER 37
Preparing a measurement 20 E06 EMPTYWATER 38
Close the calorimeter 20 E07 POSTWATERFILLING 38
Prerequisite checking for a measurement 21 E10 FILLWATER SENSOR 38
Measurement procedure 21 E11 SYSTEM OPEN 38
Cleaning the inner vessel 23 E12 PRESSURE 38
Follow-up measurement 23 E13 HEATER 39
Display the storage overview 23 E16 MAXTEMPDIFF 39
Use of a disposable crucible 23 Accessories and Consumables 39
Using a scale 24 Maintenance 40
Permissible weight entries 24 Warranty 40
Cancel a measurement 25 Technical data 41
3
Safety instructions
Read the operating instructions in full before start- Combustion gases are hazardous
ing up and follow the safety instructions. DANGER to health, therefore the venting
hose must be connected to a suita-
Keep the operating instructions in a place where they can be ble gas cleaning system or extrac-
accessed by everyone. tion system.
Ensure that only trained staff work with the appliance.
Caution! In case of failure Error 04
The calorimeter C 1 may only be used for the determination of DANGER ”Min.Temp.Diff.“ the combustion
calorific value of solid and liquid materials according to national chamber could be hot after an ig-
and international standards (eg DIN 51900, BS 1016 T5, ISO 1928, nition/combustion, even though
ASTM 5468, ASTM 5865 and ASTM 4809). the message ”No temperature in-
The pressure vessel is integrated into the calorimeter C 1. The crease!“ is displayed.
maximum extra energy added to the pressure vessel must not At the end of the work period, close the main valve for the oxygen
exceed 40,000 J (select the test mass accordingly). The permitted supply.
operating pressure of 142 bar (14.2 MPa) must not be exceeded.
The maximum permitted operating temperature must not exceed Perform servicing work only when the equipment is depressurised.
50 °C.
When using stainless steel crucibles thoroughly check their condi-
Only fill calorimeter system C 1 with oxygen to a maximum tion after each experiment.
pressure of 40 bar (4 MPa). Check the pressure setting on the If the material gets thinner, the crucible may catch fire and dama-
pressure reducer for your oxygen supply. Perform a leakage test ge the pressure vessel. Crucibles must not be used for more
before each combustion process (see section “Leaktightness than 25 combustions for safety reasons.
testing with system test“).
Some materials tend to explode when combusted (e.g. due to The EC Declaration of Conformity confirms that this pressure ves-
formation of peroxides), which could cause the decomposition sel was manufactured by the Pressure Equipment Directive
vessel to crack. The IKA C 1 calorimeter may not be used
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2014/68/EC. (Article 3, paragraph 3).
for testing explosive samples.
The pressure vessel has undergone a pressure test with test pressure
If the burning behaviour of a material is unknown, it must be
of 203 bar (20.3 MPa) and a leakage test with oxygen at 40 bar.
tested before combustion in the inner vessel (risk of explosion).
If you are burning unknown samples, leave the room or keep
Decomposition vessels are experiment autoclaves and must be tested
your distance from the calorimeter.
by a technical expert after each use. (see capture: “Maintenance“).
Benzoic acid may only be combusted in its pressed form! Flammable
dust and powder must be first pressed. Oven-dry dust and powder Individual use is understood here to include a series of experiments
such as splints, hay, straw etc. explode when combusted! Always performed under roughly the same conditions in terms of pressure
wet these materials first! Highly flammable liquids with a low and temperature. Experiment autoclaves must be operated in special
vapour pressure (e.g. tetramethyl dihydrogen disiloxane) must not chambers.
directly touch the cotton thread!
The pressure vessels must undergo repeated tests (internal tests and
pressure tests) performed by the technical expert. The frequency of
Please pay attention to the combustion of metal-containing
these tests is to be determined by the operator on the basis of experi-
substances, that the permissible total energy input is not exceeded!
ence, type of operation and the material used in the pressure vessel.
Furthermore, toxic combustion residue in the form of gases, ashes
or condensation, for example, is possible in the inner wall of the The declaration of conformity becomes invalid if mechanical
inner vessel. modifications are carried out to the experiment autoclaves or if
tightness can no longer be guaranteed as a result of major corro-
Observe the accident prevention requirements applicable to the
sion (e.g. pitting by halogens).
activity and the work station.
In particular the Thread on the lower part of the pressure vessel
Wear your personal protective equipment.
and the nut are subject to considerable stress and must therefore
When handling combustion sam- be checked regularly for wear. (see figure “Description of the sys-
DANGER ples, combustion residue and tem components“).
auxiliary materials, please observe The condition and function of the seals must be checked and en-
the relevant safety regulations. sured by way of a system test (see capture “system check“).
The following materials, for example, could pose a risk: Check the seals for damage before each use (see chapter
- corrosive “Maintenance“.
- highly flammable
- explosive If the maintenance, and especially
- bacteriologically contaminated DANGER the pressure testing, is not per-
- toxic. formed or is performed incorrectly,
there is a risk the decomposition ves-
Please observe the relevant regulations when handling oxygen. sel may burst or an uncontrolled in-
ternal fire may occur at the elec-
Warning: oxygen as a compressed gas is oxidising; intensively aids trodes which could burn away the
combustion; can react violently with flammable materials. seals (oxyacetylene torch effect),
Do not use oil or grease! thus posing a risk to life and limb!
Tubes and screwed joints for oxygen must be kept free of grease.
Only technical experts may perform pressure tests and service
work on the decomposition vessel.
4
We recommend that you send the C 1 calorimeter system National directives and laws must be observed for operating
to our factory for inspection, and if necessary, repair after pressure vessels!
1000 tests or after one year or sooner depending on use. Anyone operating a pressure vessel must keep it in a proper
For the purposes of these operating instructions a technical condition, operate it properly, supervise it, carry out the necessary
expert is someone maintenance and repair work immediately and implement the
1. who guarantees to conduct the tests properly on the safety measures required in the circumstances.
basis of his training, knowledge and experience gained A pressure container must not be operated if it exhibits defects
through practical work, that could endanger those working with it or third parties.
2. who is sufficiently reliable, You can obtain a copy of the pressure vessel regulation from
3. who is not subject to any instructions in terms of the test Beuth Press.
activity,
4. who has suitable test equipment if necessary,
5. who can provide appropriate proof of the requirements
listed in 1.
Correct use
software (accessories), from the acid corrections up to the calo- Automatic internal system checks enable the identification and
rific value according to DIN, ISO, ASTM, GB, and GOST standards monitoring
typed, corrected and calculated. By a transfer of the results to • the presence of oxygen pressure
Excel can quickly and easily adapt special or own calculations. • the controlled stirrer speed
The worldwide unique patented IKA calorimeter C 1 operates on
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• the the availability of water in the system
the globally applied isoperibolic measurement procedure at 22 °C • the input water temperature
and 30 °C. The temperature values are output every 12 seconds, • of inner vessel
and the calculation of the temperature correction according to • the correct shutter of the measuring cell with locking
standards Regnault Pfaundler. • Ignition counter with memory function for the next due
maintenance
Measurement times of the system:
- Sample preparation time: < 1 minute
- from the start of measurement until the start of the next: 12 minutes
- Pre-experimental period: Response of the system 3 minutes
- Main experiment: after ignition of the sample: 4 minutes
To a supply of cooling water, the calorimeter can with a conven-
tional thermostat / cooler operate for example such as the IKA ®
KV 600 (accessory).
5
Transportation, Storage
Transport and Storage conditions If you require servicing, return the appliance in its original packag-
The system must be protected against mechanical impact, vibra- ing. Storage packaging is not sufficient. Please also use suitable
tions, dust deposits and corrosive ambient air during transporta- transport packaging.
tion and storage. It is also important to ensure that the relative
Unpacking
humidity does not exceed 80%.
The appliance must be completely emptied before storing and Please unpack the system components carefully and check for
transportation. any damage. When you unpack the equipment, check for any
In case of repair the device has to be cleaned and free from any damages which may have occurred during transportation.
materials which may constitute a health hazard. In the case of any damage a fact report must be sent immediately
(post, rail or forwarder).
Scope of delivery
• IKA C 1 Calorimeter
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• Mains cable • 1 O-ring FPM 3.1 x 1.6 • 4 base
• Power supply unit • 1 Tool • 5 O-ring FPM 3.0 x 1.5 • O-ring-grease Molykote 55
• Inflow conduit • 5 O-ring FPM 11.0 x 2.0 • 5 O-ring FPM 48.0 x 2.0 • Handle
• Return conduit • 2 O-ring FPM 6.0 x 2.0 • 1 Quad-Ring NBR 92.0 x 4.5 • Operationg instructions C 1
• Discharge hose • 2 O-ring FPM 15.0 x 2.0 • 1 X-Ring NBR 6,07 x 1,78 • Safety instructions C 1/C 6000
• Round cable clamp • 5 O-ring FPM 10.0 x 2.5 • C 1.104 water bath additive • Technical information C 1
• Connection tube • 5 O-ring FPM 8.0 x 2.5 • C 723 Benzoic acid • Insert sheet C 1 (4 steps to use)
• Venting hose • 5 O-ring FPM 4.0 x 1.5 • C 1.1012 Organizer • Warranty card
Manual,
pivotable lift
Rotary
Threaded nut handle
Measuring cell as
a pressure vessel
Inner vessel (IB)
Ignition wire
Crucible
holder Interfaces on
rear of the unit
Ignition
electrode
C1
•
Discharge hose (overflow)
Cooler
•
Inflow conduit filter 10μm
Cooler (water in)
max. 1.5 bar C1
•
Return conduit C1
(water out)
Cooler
•
Venting hose
Exhaust C1
air
(degas)
SW8
•
Connection tube Adapter C1
Pressure reducer C 29 SW10
(O2)
Commissioning
Place of installation
A constant ambient temperature is an important requirement For operation of the system the following must be available at the
for ensuring the high measuring accuracy of the system. The place of installation:
following conditions must therefore be fulfilled at the place of - A power supply corresponding to the nameplates on the system
installation: components,
• No direct solar radiation - An oxygen supply (99.95 % pure oxygen, quality 3.5; pressure
• No draughts (e.g. beside windows, doors, air conditioning) 30 bar) with pressure gauge.
• Sufficient distance to radiators and other heat sources A shut-off valve for the oxygen supply must be installed. Observe
• The minimum distance between the wall and the rear side the instructions on handling oxygen given in the chapter “Safety
of the device must be at least 25 cm. instructions“.
• The system must not have laboratory hardware such as Observe the instructions on handling oxygen given in the chapter
shelves, wire ducts, ring lines, etc. installed above it. “Safety instructions“. Please read these operating instructions
• The (constant) room temperature should be around carefully. IKA consider themselves responsible for the safety,
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7
Cooler connection
1. Connect the inflow pipe to the 2. Connect the return pipe to the
quick coupling to the “water quick coupling to the “water
in“ (on the calorimeter) port. out“ (on the calorimeter) port.
Connect the other end of the Connect the other end to
radiator side of “water out“ “water in“ (on the cooler) and
and tighten the hose clamp. tighten the hose clamp.
Inflow pipe
Return pipe
8
Power supply unit connection
1. Connect the power supply The desktop power supply (scope of delivery) must not be placed
connecting cable (24 V) flat on the laboratory table. It must be protected against moisture
and water penetration and must not be wet.
NOTE: Note the correct inser-
tion position (flat side 2. Tape the supplied rubber feet
of the connector to the power supply.
pointing to the right). Place the power supply on the
rubber feet.
Connect the connection cable
to the DC power supply to
flat side of the connector your supply network
(100-240V AC 50/60 Hz).
Connecting cable
Connection of peripherals
h 1
h
Q
Q2
The closing of the unit in the reverse order
9
2. Removing the inner vessel 3. Removing the inner vessel base
Inserting the inner vessel takes place in the reverse
order
h h
Del button
10
Dialog box
Editable
Menu-heading Selected menu item input field
(blue) Scrollbar (yellow)
Status field
Menu-heading: • ‚Back‘:
The name of the currently displayed window Closing a info window without information input
values and return to the parent menu.
Selected menu item: Also possible using [ESC].
The blue background (cursor) marks the selected
item. The position can be changed by • ‚Accept‘:
turning the multifunction element. Closing a window. Changes made are saved by
the system.
Scrollbar: If a menu window more entries can be displayed as • ‚Start‘:
the current is displayed a scrollbar. Starting a measurement.
Turn the multi-function element, the other menu
items are visible. • ‚Details‘:
Detailed information during a running
User notifications: measurement.
Some windows have a field in the user notes will • ‚Graph‘:
be displayed. View graph during a running
Menu options: measurement.
They allow a “getting ahead“ from the current Editable input field:
window. They can be enabled for value entry by pressing
In the following example, the most frequently the multi-function element. The background color
displayed menu options are listed and described: of the active field is indicated in yellow. By using
• “Break off“: the numeric keys or by turning the multi-function
Closing a window, the changes made will not be element, the input values can be changed.
accepted by the system. Status field:
Also possible using [ESC]. Display the device status, which is important for
the user and operation.
11
System start
Switching on the system (in the open state)
After switching on the calorimeter, first the initial screen with the
IKA logo, the calorimeter-type and the software and firmware
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version.
Selection of language
12
Pressure test
NOTE:
The calorimeter C 1 required for functionality an oxygen
pressure of at least 20 bar.
Reproducible measurements for a working pressure
of 30 bar is required.
System check
13
Heating detected
NOTE:
Check that the heater is correctly connected and turned on.
Factory settings
Basic settings:
• C-value IB1: 0 • QExternally 1: 50
• C-value IB2: 0 • QExternally 2: 0
• Reference calorific value: 26457 • Controlled time: off
• Start temperature: 22 °C • O2 rinsing: off
• HO Combustible crucible: 19839 • Cooling: on
• Prolonged venting: 0
Calorimetric measurements
Determination of gross calorific value
Test condition • Solid substances may be formed (for example ash).
Combustion is carried out in a calorimeter under specific
conditions. Often, however, the combustion products that form the basis
of the standards are not the only products that are formed. In
The IKA C 1 is filled with a weighed fuel sample, the fuel sample
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The combustion aid is first weighed and then added to the crucible your nearest authorized dealer.
with the sample. From the weight of the combustion aid and its When calculating the energy value in C 1 external energies are
known specific gross calorific value, it is then possible to determine taken into account from kiln furniture, however, there is no
the quantity of heat that is introduced thereby. The result of the correction of acid. The calorific value is not calculated.
experiment must be corrected by this amount of heat.
The C 14 disposable crucible is a combustible crucible that can To do this, use the calorimeter software IKA CalWin .
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only if the individual steps of the trial are performed with care.
• Most liquid substances can be weighed directly into the cru-
The procedure as described in the “For your safety“ section 1 and
cible. Liquid substances exhibiting turbidity or containing water
in the following sections must therefore be adhered to exactly.
that will settle out must be dried or homogenized before they
If you are burning unknown samples, are weighed in. The water content of these samples must be
DANGER leave the room or keep well away determined.
from the calorimeter! • Highly volatile substances are placed in combustion capsules
A few points should be noted in respect of the substances to be (gelatin capsules or acetobutyrate capsules, see “Accessories“)
combusted: and undergo combustion together with the capsules.
• For substances with low flammability or low calorific substances
• Normally, solid substances can be burned directly in powder use combustion aids (see “Accessories“). Before the capsules or
form. Rapidly burning substances (for example benzoic acid) the combustion bag is fi lled with the substance to be deter-
must not undergo combustion in loose form. mined, it must be weighed in order to determine the additional
Benzoic acid must only be burned in the form of pellets! Com- extraneous energy introduced into the system from the weight
bustible dust and powder must be compressed into pellets and the gross calorific value. This is taken into consideration
before combustion. Oven-dry dust and powder such as wood with QExtern2. The amount of combustion aid should be as little
chips, hay, straw etc. burn in an explosive manner! They must as possible.
be moistened first! Readily combustible liquids with a low va-
por pressure must not be come in direct contact with the The external energy must be determined externally.
cotton thread (e.g. tetramethyl dihydrogen disiloxan).
15
• Under the conditions that prevail during calorimetric mea- These correction values can
not be entered in C 1. For this, use the
surements, sulfur and nitrogen un-dergo combustion and form IKA calorimeter software CalWin .
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SO2, SO3 and NOX. Sulfuric and nitric acid arise in combinati-
To increase the service life of parts to wear and tear (O rings,
on with the water resulting form combustion. Heat of solution
seals etc.) we recommend to work with water added to the
is also generated. This heat of solution is taken into conside-
experiment as a matter of general principle.
ration in calculating the gross calorific value. In order to quanti-
tatively record and determine all acids that have been formed,
Halogen rich substances can cause corrosion on the inner con-
about 5 ml of distilled water or another suitable substance can
tainer.
be added to the decomposition vessel before the experiment.
These substances must not be burned in C 1 with the
The calibration of the system must have been performed in
standard inner vessel.
accordance with the instructions!
In halogen-rich substances of special halogen-resistant
Remove after measuring the complete inner vessel. Turn the inner inner vessel C 1.12 must be used.
container upside down, loosen gently the internal container bot-
tom. Rinse thoroughly with distilled water, the inner area of the
inner container. The rinsing water and the solution formed from
the water that was added are combined and the acid content of
the combined solution is examined. If the sulfur content of the
combustion aid and the nitric acid correction are known, the water
does not need to be analyzed.
h
h
h
Handle
Complete combustion
To correctly determine the gross calorific value, it is of fundamen- undergo complete combustion only with the aid of combustion
tal importance that the sample undergoes complete combustion. capsules or combustion bags (C 10/ C 12 see “Accessories“). It is
After each experiment, the crucible and all solid residues must be also possible to use liquid combustion aids such as paraffin oil.
examined for any signs that combustion was not complete.
The combustion aids as well (for example the cotton thread) must
In case of using substances tending to squirt it is not possible to undergo complete combustion. If unburned residues are left over,
ensure complete combustion. the experiment must be repeated.
Substances with low flammability (substances with a high
content of mineral matterand low-calorific substances) will often
Calibration
To ensure precise, reproducible results of the measurement, the to calculate the heat capacity based on the increase in temperature
calorimeter system is calibrated after it is initially placed in service, of the calorimeter system. The reference substance for calorimetry
after service jobs, after parts are replaced and at specific time inter- on an international level is benzoic acid of the National Bureau of
vals. During calibration, the heat capacity of the calorimeter system Standards (NBS Standard Sample 39 J) with a guaranteed gross
is redetermined. calorific value.
Regular calibration is absolutely essential to obtain accurate For more detailed information on calibration please see the relevant
measurements! standards.
If the IKA C 1 is operated with several different decomposition
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Notes on calibration
Ensure that calibration is carried out under the same conditions as For determination of calorific values the increase in temperature
the subsequent tests. If substances are used in the decomposition must be about as great as for the calibration (± 30%). 1g benzoic
vessel in combustion tests (e.g. distilled water or solutions), you acid =˜ 6K. The optimum sample quantity must de determined by
must use exactly the same amount of this substance for calibration. several trials where necessary.
16
Overview Main menu
The user has two display modes are available.
Measurements
• New measurement
• Last result
• System test
• Measurement archive
• Calibration archive
• Memory overview
Default settings
• C-value IB1
• ID IB1
• C-value IB2
• ID IB2
• Ref. cal. value
• Ho Comb. cruc.
• Start temperature
• QExtern 1
• QExtern 2
• O2 rinse
• Cool Down
• Extend. O2 Emptying
Settings
• Date / Time
• Units
• Display / Keypad
• Language
• Accessories
• Cooler test
17
Maintenance
• Change seal
• Test stirrer
• O2 System blow
• Servo up
• Servo down
INFO: When performing maintenance programs, the system
must be open !
Information
• Software
• Firmware
• Serial number
• Service
• Pressure test
• Ignitions
• Next test
• Support
18
Input window NEW MEASUREMENT
Select and confirm the menu item “Sample weight“. Enter the
sample weight with numeric keypad and confirm.
INFO: A distinction is made between the use and non disposable
cup. Use of disposable crucible can be selected in Settings
" Accessories.
INFO: For automatic input of the weight may be a connected
scale can be used
INFO: The inputted weight values are checked for permissibility.
INFO: The existing store will be reviewed after the entry of a
new measurement / calibration and a user note displayed
if it is not possible to save the measurement / calibration.
NOTE:
Ensure that a maximum energy input of from 40,000 joules is not
exceeded.
NOTE:
For more, detailed descriptions of the individual menu items are
treated in the chapter “Calorimetric Measurements“.
INFO: If a scale is used in activation of the input field, the
weight is automatically queried. It can be pressed on the
scale alternatively, the transmit button.
Fill in the sample weight.
Calibration off.
When you are ready with your input, press “OK” button.
19
Preparing a measurement
The inner container base remains in the control of sample prepara- 1. Attach with a loop a cotton thread centered on the ignition
tion in the calorimeter. But you can also use it by pulling it out wire (at the open calorimeter).
individually, or for consequential - Analysis - determinations, refer
to the closed inner container. 2. Weigh the substance with an accuracy of 0.1 mg directly into
The following preparations must be made to prepare the system the crucible.
for a measurement: Where appropriate distilled water or a solution must be
presented in the inner vessel.
C 6 Quartz crucible
To increase the service life of wearing parts (O-rings, seals, To determine the potential energy initially very small sample
etc.) it is advisable to always work with a water template. weights (approx. 0.2g) must be chosen when working with
unknown substances. If you burn unknown samples, leave
Generally, the test sample must be selected so that the tempe- the room or keep your distance from the calorimeter.
rature elevation during the measurement is below 10 K and
the temperature increase of the calibration comes close (max. If distilled water or solutions presented in the decomposition
energy input: 40,000 J). Such exposure may damage the vessel during the combustion experiment, the calibration
calorimeter. with the same template must have been performed before.
When exceeding the maximum energy input is recommended
to return the calorimeter.
After the sample is loaded and the contact with the ignition wire
is present and the inner vessel was placed, the calorimeter is
sealed.
Note:
Can the inner container and / or closure ring with handle heavy
wire, please follow the instructions for oiling the seals!
20
Prerequisite checking for a measurement
Without • Ignition:
C 1.20 Checking whether ignition contact available
heating: • Oxygen pressure:
Check whether the system has sufficiently high oxygen pressure
has to make a measurement
• Water detected:
Check whether the system has detected water
• Limit ≤ Water ≤ Start temp:
Check whether there is the current water temperature within the
permissible temperature range
Measurement procedure
• Phase 1:
Filling the calorimeter with water
NOTE:
After switching on the calorimeter C 1 or after a break of 2
hours during the filling of the calorimeter C 1 is still carried
out an intermediate emptying (H2O - purge). Once the
water sensor detects water, the stirrer is switched on.
After a short waiting period begins phase 2.
• Phase 2:
Filling the calorimeter with oxygen (Note: If the option-O2
flushing under the main menu " Basic Settings is selec-
ted, the inner vessel is two times with Oxygen rinsed)
NOTE:
Alternatively, to display the graph may also have a detailed
view of be selected with the following information:
• Current temperature:
Mean value of the actual temperatures
• Ignition temperature:
the currently measured temperature
• Measurement time:
Display: duration of the measurement
• Fill time:
Filling the inner vessel with water.
The fill time is user specific and must be kept constant
on each measurement. Check the filter where long fill times
are used.
21
• Phase 3:
Filling with oxygen
• Phase 4:
Stabilizing the temperature and preliminary
• Phase 5:
The system ignites and thereby starts the main test
• Phase 6:
Post test
• Phase 7:
Venting, result is displayed
• Phase 8:
Cooling (if option under the main menu " Basic Settings
" cooling is enabled) and water emptying
NOTE:
With the “cooling“ option, the energy is absorbed (by the
combustion in the calorimeter entered).
Deactivation, the measuring time and the accuracy of the
calorimeter affecting (depending on the sample
throughput).
22
• Phase 9:
The system is completely emptied, and can be opened.
Follow-up measurement
23
Using a scale
This applies both to the initial sample weight of the sample and
the weight of the disposable crucible.
24
Cancel a measurement
After ignition, the system waits for 1 minute with the emptying,
as otherwise there is a risk that the sample is not completely
burned.
After confirm the cancellation, the system automatically emptied
and bring it to a safe state. The calorimeter can be opened and
you can return to the main menu.
Measurements
New measurements
• New measurement:
Preparing and starting a measurement
• Last result:
Displaying the result of the last measurement
• System test:
The functionality of the calorimeter is checked
• Measurement archive:
The system can store up to 100 measurements
• Calibration archive:
The system can be used for both modes of operation (22 °C,
and 30 °C) for each inner container (1 and 2) each
storing 15 calibrations.
• Memory Summary:
Display the memory summary
Last result
25
System test
Use for the system test one or two benzoic acid tablets.
Alternatively, however, for example, an appropriate amount of
sugar or an alternative fuel to be used.
The system test is used to test the functionality of the overall
system. For this purpose all switching operations are carried out,
which take place in a normal measurement. If the system test
performed without error, the functionality is guaranteed.
The system test can be used to create a quick ˝warm up“ the
system. It is faster than a normal measurement, since there is no
analysis and improves the accuracy of the first measurement so
that they need not be discarded
Measurement archive
26
Measurement archive: Edit
Print:
• Measurements can be selected and printed
Delete:
• Measurements can be selected and deleted
Delete all:
• All measurements are deleted
27
Measurement archive: Delete all
By clicking the “OK“ button, the following dialog appears:
Calibration archive
Displays the line number, the name of the calibration and the
result (C value).
Below the list of the current C-value of the system is shown (in
red). By confirming the multifunctional element details concerning
the measurement are displayed. For the C-value calculation, select
˝Edit“.
INFO: The C-value can also manually at Main Menu > Basic
settings entered alternative.
28
Calibration archive: C-Value selection
29
Default settings
NOTE:
When using a gas-washing station, the ventilation time
must be extended.
Settings
The setup menu contains the following menu items
• Date / Time
• Units
• Display / Keypad
• Language
• Accessories
• Chiller temperature
Date / Time
Units
• J/g
• cal/g
• BTU/lb
• MJ/kg
30
Display / Keypad
The user can access this menu
• select and change the background color of the display.
The background color can be selected either white or black
• the key tones on or off
• the appearance of the menus between animated view
and list view move
List view
Language
31
Accessories
Selection of accessories
• Heating:
Use of heating during the measurement C 1.2
• Combustible crucible:
yes / no
Weight input of the combustible crucible in the submenu “New
measurement“ can be done manually or by data transfer from
the balance.
• Printer:
Using a serial printer.
Selection option between:
• off: no expression
• briefly: expression
• standard: result expression with temperature values
• Service Information:
Service information is outputted via the serial interface
• Balance:
Selecting a balance type.
Selection option between:
• out
• Sartorius/Kern
• Mettler-Toledo
• Ohaus
Chiller test
Maintenance
Maintenance menu:
The maintenance menu can be reached at Menu > Maintenance and contains the following points
Viewing maintenance programs that can be performed by the
user at regular intervals.
Inner vessel and the inner vessel bottom lift out and set
aside.
32
Change seal:
1 In the Menu Maintenance press “change seal“ button. This 38 III
requires oxygen pressure be present at C 1.
2 Unscrew the piston (Pos. 38 III) with screwdriver
counterclockwise VI (8,0 x 2,5)
3 Remove the O-ring (Pos. 38 VI) 38
4 Put new O-ring on piston (Pos. 38 VI)
5 Screw in piston and tighten securely
6 “Change seal“ button again actuate pistons move to the O-ring
home position (Water inlet valve
seal)
Stirrer test
The stirrer is switched on and off for a visual check.
O2 System blow:
1 Lift out the inner vessel from the bottom and set aside
2 After about 20 seconds the button “O2 system blow“ button.
Keep openings with a paper towel or similar covered by hand Stirrer
3 After about 3 seconds, this state switches itself off again.
Servo up
The locking pin is extended.
locking pin
Servo down
The locking pin is retracted.
Informations
33
User information: Memory
Prior to input a new measurement
Information about the available space when you select the menu
item “New Measurement“
This information is displayed when there is a value in the
critical region is located, that is, from 95 out of 100 possible
measurements in memory or from 13 of 15 calibrations in store
for IB1, IB2 at 22 °C or 30 °C operating temperature.
The user can skip this message, then the following measurement or
calibration is not saved. However, it can also switch on the button
“Archive“ to the appropriate archive and then delete old or unused
measurements or calibrations.
40 (10,0x 2,5)
1 Bushing (Pos. 33) with the enclosed tool SW11
33
screw out 32/21
2 Lift piston (Pos. 32/21) with tweezers
3 Remove the O-ring (Pos. 40), insert a new O-ring and ensure
the correct position 32/8
4 Set piston (Pos. 32/21) back in the opening
5 Bushing (Pos. 33) screw with the enclosed tool SW11
(3,0 x 1,5)
handtight, paying attention to correct position of the
O-ring (Pos. 32/8)
34
Change ignition wire
I Safety note:
1 To release the ignition wire (Pos. 24) on the ignition electrodes 25 13 Use only original IKA ®
Inner vessel
h
Pos. 15 O-ring (48,0 x 2,0)
1x X-ring
Marked with rings must
be greased as needed with
the supplied grease.
35
Change ground electrode
17
(6,0x2,0)
22
14
(3,1x1,6)
E01 STIRRER
This error appears if the setpoint of the stirrer speed is not
reached.
A possible cause for this problem is a defective stirring motor.
36
E02 COMMUNICATION
If no internal communication between the software and firmware
are prepared COMMUNICATION ALARM appears..
E04 MINTEMPDIFF
E05 FILLWATER
Message appears when the system during filling with water after
50 seconds does not detect water in the upper water outlet.
Causes for this problem are:
• the cooler is not switched on or not connected
• Water valve seal defective
• no oxygen present (for switching the valves, the system
requires pressure)
• upper water sensor is defective
• the filter in the supply line is dirty
• Water valve tightly or defective
the water supply is not connect
• the water filter is clogged
37
E06 EMPTYWATER
Occurs when the lower water sensor during the emptying of
system after 60 seconds still detects water.
Possible causes for this problem are:
• the drain hose for sucking the air is in the water. Check the
hose laying on the cooler (see page 8).
• the pump is defective. Switch the device off and back on
and then run a system test. Disconnect the return flow line
and let the water drain into a lower lying container..
E07 POSTWATERFILLING
After 45 seconds in the post-water-filling state, the current
temperature is compared with the selected fill-water temperature.
If it falls below the Fill-water temperature, the oxygen filling is
started.
Otherwise, the system additionally waiting 180 seconds, if the
fill-water temperature is not reached.
A possible cause for this problem is set too high cooler temperature.
Check the cooler.
E12 PRESSURE
Oxygen pressure is too low (min. 20 bar).
The most common cause for this problem is an unopened or
empty oxygen bottle.
Check the oxygen supply!
NOTE:
20 bar, the minimal pressure necessary to keep the system
is able to work. A pressure < 30 bar may have measurement
errors in consequence.
38
E13 HEATER
When using the heater C 1.20 this is not detected.
The most common cause for this problem is a switched off or unplugged
heating during measurement.
Check the contact of the heating C 1.20.
E16 MAXTEMPDIFF
Temperature increase > = 10 °C detected.
39
Maintenance
Cleaning the water filter: - When cleaning, please do not allow moisture to get into the unit.
Clean the water filter in the water supply line every 2-3 days in - Wear the proper protective gloves during cleaning of the devices.
the beginning and define the regular intervals, depending on the - Before performing a non-recommanded method of cleaning or
degree of contamination for cleaning.
decontamination, the user must ascertain with IKA that this
®
Warranty
In accordance with IKA warranty conditions, the warranty period is 12 months. For claims under the warranty please contact your local
®
dealer. You may also send the machine directly to our factory, enclosing the delivery invoice and giving reasons for the claim. You will
be liable for freight costs.
The warranty does not cover worn out parts, nor does it apply to faults resulting from improper use, insufficient care or maintenance not
carried out in accordance with the instructions in this operating manual.
40
Technical data
Power supply unit (external)
Design voltage /-frequency 100–240 V AC 50/60 Hz
Power consumption max. 120 W
Calorimeter:
Design voltage 24 V DC 5A
Power consumption max. 120 W
41
IKA®-Werke GmbH & Co.KG
Janke & Kunkel-Str. 10
D-79219 Staufen
Tel. +49 7633 831-0
Fax +49 7633 831-98
[email protected]
www.ika.com 20005032d