IKA C 6000 User Manual

43 459 00 a

IKA® C 6000 global standards IKA

C 6000 isoperibol

052014 Reg.-No. 4343-01

Operating instructions EN

Source language: German

Contents

Page

CE Declaration of conformity 04

Explication of warning symbols 04

Safety instructions 05

Correct use 07

User instructions 07

System features 07

Warranty and liability 08

Transport and storage 08

Transport and storage conditions 08 Unpacking 09

Scope of supply 09

Description of system components 10

C 6000 calorimeter global standards/isoperibol 10

IKA

Hoses 11

Commissioning 11

Place of installation 11 Connection to the condenser 12 Connection to the water 12 Connection to the oxygen supply 13 Connection to the mains power supply 13 Connection of peripherals 14 On/off switch 15

Display and operating elements 16

Explanation of the screen display 16

Working with the IKA® C 6000 global standards/isoperibol calorimeter 20

Switching on the device 20 System test 20 Switching off the device 21 The standard calorimetric procedure 22

- Caloriﬁ c value determination 22

- Corrections 23

- Note on the sample 24

- Complete combustion 25

- Calibration (only IKA® C 6000 global standards) 25

- Calibrating 26

- Instructions on calibration 26 Preparation for measurement 27 Charging the decomposition vessel 29 Calorimetric measurement without automatic decomposition vessel detection 29 Starting the measurement 30 Evaluation 32

Menu (main overview) 33

Library 34 Method of operation, decomposition vessels and calibration 35 Servicing the decomposition vessel 38

Contents

Other Settings 38

Evaluation 38 Measurement 39 Ignition aids 40 Combustion aid 41 Balance 41 Printer 42 Other 42

Help and servicing system 44 Displaying / hiding the sample rack 46 Cleaning 48

Cleaning the system 48 Cleaning the ﬁ lter 48

Troubleshooting 49

Fault rectiﬁ cation 51 Checks 55

Accessories and consumables 56

Accessories 56

Technical data 57

Technical data IKA® C 6000 global standards 57 Technical data IKA® C 6000 isoperibol 59

EC-Declaration of conformity

We declare under our sole responsibility that this product corrosponds to the regulations 2006/95/EG, 2004/108/EG and 2011/65/EU and conforms with the standards or standardized documents EN 61010-1:2010, EN 61010-2-051:2003 and EN 61 326-1:2006.

Explication of warning symbols

General hazard

This symbol indicates information which is essential for the safety of your health.

DANGER

WARNING

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.

ATTENTION

Contents

This symbol indicates information which is important for ensuring that calorimetric measurements are performed eﬃ ciently and for using the calorimeter system.

Failure to observe this information can result in inaccurate measurements.

Safety instructions

Read the operating instructions in full before starting up and follow the safety instructions.

Keep the operating instructions in a place where they can be accessed by everyone. Ensure that only trained staff work with the appliance. Follow the safety instructions, guidelines, occupational health and safety and accident prevention regulations.

The IKA® C 6000 global standards/isoperibol calorimeter system may be used only in conjunction with the decomposition vessels C 6010 or C 6012 for determination of the caloriﬁ c values of solid and liquid substances to national and international standards (such as DIN 51900, BS 1016 T5, ISO 1928, ASTM 5468, ASTM 5865 and ASTM 4809).

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 (23 MPa) must not be exceeded. The maximum permitted operating temperature must not exceed 50 °C.

When burning substances containing metals, ensure that the maximum energy input is not exceeded!

Only ﬁ ll the decomposition vessel with oxygen to a maximum pressure of 40 bar (4 MPa). Check the pressure setting on the pressure reducer for your oxygen supply. Perform a leakage test before each combustion process (see section „Leaktightness testing“).

with a low vapour pressure (e.g. tetramethyl dihydrogen disiloxane) must not directly touch the cotton thread!

DANGER

example, is possible in the inner wall of the decomposition vessel.

Observe the accident prevention requirements applicable to the activity and the work station. 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 ﬂ ammable – explosive – bacteriologically contaminated – toxic

Please observe the relevant regulations when handling oxygen.

Warning: oxygen as a compressed gas is oxidising; intensively aids combustion; can react violently with ﬂ ammable materials.

DANGER

Tubes and screwed joints for oxygen must be kept free of grease.

Furthermore, toxic combustion residue in the form of gases, ashes or condensation, for

Do not use oil or grease!

Some materials tend to explode when combusted (e.g. due to formation of peroxides), which could cause the decomposition vessel to crack. The

IKA® C 6000 global standards/isoperibol calorimeter 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 ﬁ rst pressed. Oven-dry dust and powder such as splints, hay, straw etc. explode when combusted! Always wet these materials ﬁ rst! Highly ﬂ ammable liquids

Safety instructions

Combustion gases are hazardous to

health, therefore the venting hose must be connected to a suitable gas cleaning system or extraction system.

At the end of the work period, close the main valve for the oxygen supply.

Perform servicing work only when the equipment is depressurised.

When using stainless steel crucibles thoroughly check their condition after each experiment. If the material gets thinner, the crucible may catch ﬁ re 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 notiﬁ ed body. The decomposition vessel is a category III pressure device. The decomposition vessel has undergone an EC prototype test. The CE declaration of conformity conﬁ rms that this decomposition vessel corresponds to the pressure device described in the EC prototype test certiﬁ cate. The decomposition vessel has undergone a pressure test with test pressure of 33 MPa and a leakage test with oxygen at 3 MPa.

Refer also to the operating instructions for the C 6010/ 6012 decomposition vessel, see chapter „maintenance of the decomposition vessel“.

Decomposition vessels are experiment autoclaves and must be tested by a technical expert after each use.

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

A pressure test must be performed after a decomposition vessel has reached or exceeded the recommended number of ignition cycles. Once the pressure test has been performed a release code can be entered to enable the decomposition vessel to be used for further measurements (see the sections “Maintenance of the Decomposition Vessel” and “Inputting a Service Code”). The warning message will then disappear!

Note: You can then continue to use the device / decomposition vessel.

Contact the IKA® Service Department to perform the pressure test. Comply with the safety instructions in this respect. The user will be given speciﬁ c instructions on the relevant screen.

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

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 decompositionvessel.

The declaration of conformity becomes invalid if mechanical modiﬁ cations 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).

In particular the threads on the pressure vessel and the union nut are subject to considerable stress 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 the operating instructions for the C 6010/ 6012 decomposition vessel, section „Leaktightness testing“).

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 suﬃ ciently 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.

If the maintenance, and especially the pressure testing, is not performed or is performed incorrectly, there is a risk the decomposition vessel may burst or an uncontrolled internal ﬁ re may occur at the electrodes which could burn away the seals (oxyacetylene torch effect), thus posing a risk to life and limb.

Only technical experts may perform pressure tests and service work on the decomposition vessel.

Safety instructions

Correct use

The IKA® C 6000 global standards/isoperibol calorimeter system is used for caloriﬁ c value determination of solid and liquid substances. This is done by placing a known quantity of a substance in a decomposition vessel which is surrounded by a water jacket. The sample is then combusted in an oxygen atmosphere . The caloriﬁ c value of the sample can then be calculated from the resulting increase in temperature, the sample

User instructions

In this chapter you can ﬁ nd out how to work through these Operating Instructions most effectively to be able to work reliably with the calorimeter system.

The instructions in the section „Safety instructions“ must be complied with.

The chapters are designed for you to work through them in order. The section „Transport, storage“ is relevant for system reliability and for ensuring high measuring accuracy. The section „Description of system components“ describes the system components,

mass and the known thermal capacity of the overall system.

The IKA calorimeter system is subject to the Pressure Vessel Directive 97/23/EC. Comply with the safety instructions accordingly.

For adaptation to individual laboratory tasks, use original IKA® consumables and accessories.

and the section „The standard calorimetric procedure“ describes the essentials of calorimetry.

The calorimeter system is ready to perform measurements once you have completed the procedures in the section „Setting up and commissioning“: - „Preparing a measurement“ and „Starting a measurement“.

Numbers 1, 2, 3 etc. indicate operating instructions in the following sections. These must always be carried out in the speciﬁ ed sequence.

C 6000 global standards/isoperibol

System properties

The calorimeter system IKA® C 6000 global standards/isoperibol is routinely used for determination of gross caloriﬁ c values of solid and liquid substances. The accessories of the system ensure customized adaptation to laboratory tasks.

The system is characterized by the following features:

• Relieves you of routine tasks through automated

measurement procedure

• Integral oxygen ﬁ lling/degassing

• Automatic detection of decomposition vessel

• Operation without the cooling unit: Connection

to a water faucet with the pressure valve IKA

C 25; temperature range 12 °C upto 27 °C;

water consumption per measurement about 4 l; water pressure max. 1 bar upto 1,5 bar.

• Operation with active cooling unit 17-27 °C

(e.g. IKA® KV 600; optional)

• Measurement and calculation of gross caloriﬁ c

value according to DIN 51900, ISO 1928, ASTM D240, ASTM D4809, ASTM D5865, ASTM D1989, ASTM D5468, ASTM E711

• Calculation of net caloriﬁ c value according to

DIN 51900, ASTM D240, ASTM D4809, ASTM D5865, ASTM D1989, ASTM D5468, ASTM E711

• Measurement range: max. 40.000 J (This

corresponds to an increase in temperature in the decomposition vessel of approx. 5 K).

• PC-operation of one or several calorimeters

(Software CalWin®)

• A sample rack can be connected

• USB printer port is available

Correct use

• Operating mode based on the adiabatic, isoperibolic or dynamic principle at 22 °C, 25 °C or 30 °C (the beginning temperature of the

water in the inner vessel) depending on the cooling water temperature.

Cooling water Mode of operation Mode of operation

temperature C 6000 global standards C 6000 isoperibol

12 °C bis 20 °C Adiabatic 22 °C Isoperibolic 22 °C Isoperibolic 22 °C Dynamic 22 °C Dynamic 22 °C 20 °C bis 23 °C Adiabatic 25 °C Isoperibolic 25 °C Isoperibolic 25 °C Dynamic 25 °C Dynamic 25 °C 23 °C bis 27 °C Adiabatic 30 °C Isoperibolic 30 °C Isoperibolic 30 °C Dynamic 30 °C Dynamic 30 °C

Differences between the room temperature and working temperature have an inﬂ uence on accuracy in dynamic mode; as a result, the working temperature should always be kept similar to the room temperature.

Warranty and liability

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 direct to our factory, enclosing the delivery invoice and giving reasons for the claim. You will be liable for freight costs.

Please read these operating instructions carefully.

IKA

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.

Transport and storage

Transport and storage conditions

The warranty does not cover worn out parts, nor does it apply to faults resulting from improper use, insuﬃ cient care or maintenance not carried out in accordance with the instructions in this operating manual.

The calorimeter system may be opened only by an authorised Service Agent or Customer Service Centre.

If service is required, we recommend that you contact our customer service department

Furthermore, we refer you to the applicable safety conditions and accident requirements.

is not responsible for damages or costs

IKA

resulting from accident, improper use of the device or impermissible modiﬁ cations, repairs or renovations.

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%.

The appliance must be completely emptied before storing and transportation.

In case of repair the device has to be cleaned and free from any materials which may constitute a health hazard.

User instructions

For this use the „certiﬁ cate of compliance“, download the form from the IKA® website www.ika. com.

If you require servicing, return the appliance in its original packaging. Storage packaging is not suﬃ cient. Please also use suitable transport packaging.

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.

In the case of any damage a fact report must be sent immediately (post, rail or forwarder).

Scope of supply

Calorimeter IKA® C 6000 global standards/isoperibol

• Calorimeter IKA® C 6000 global standards/isoperibol

• Attachment set

• Stylus for touch screen operation

• Discharge hose (1.5 m)

• Connection tube O

• Venting hose

• Mains connection cable

• Warranty card

• Water inﬂ ow pipe

• Water return pipe

• Operating instructions

Transport, storage, place of installation

Description of system components

Calorimeter IKA® C 6000 global standards/isoperibol

Interfaces

Lift

Decomposition vessel Stylus for

operating the touch screen

Touch Screen

Water ﬁ lter

Mains power supply

Water Oxygen

Description of system components

Hoses

• Discharge hose

(empty)

• Inﬂ ow pipe

(in)

• Return pipe

(out)

• Venting hose

(out)

Condenser

C 6000

• O2 connection tube

(in)

Commissioning

Place of installation

A constant ambient temperature is an important requirement for ensuring the high measuring accuracy of the system. The following conditions must therefore be fulﬁ lled at the place of installation:

•

No direct solar radiation

• No draughts (e.g. beside windows, doors, air

conditioning)

• Suﬃ cient distance to radiators and other heat

sources

• The minimum distance between the wall and

the rear side of the device must be at least 25 cm.

M8x1

C 6000

For operation of the system the following must be available at the place of installation:

- A power supply corresponding to the nameplates on the system components,

- An oxygen supply (99.95 % pure oxygen, quality

3.5; pressure 30 bar) with pressure gauge.

A shut-off valve for the oxygen supply must be installed. Observe the instructions on handling oxygen given in the chapter „Safety instructions“. Please read these operating instructions carefully.

consider themselves responsible for the

IKA

safety, reliability and performance of the appliance only when

• the device has been operated in accordance

with the operating instructions,

• The system must not have laboratory hardware

such as shelves, wire ducts, ring lines, etc. installed above it.

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

• The system must be set up on a horizontal

surface.

Description of system components

• the speciﬁ cations for the place of

installation have been met.

Do not use distilled or demineralized water (increased risk of corrosion)! Fill the cooler

according to the cooler operating instructions. is recommended in drinking tap water quality. Mix in (max. 1 ml for 4-5 l of water) of the supplied water additive. Thus, the durability of the water is improved.

Connection to the condenser

Rear view without hoses attached

Make sure the ﬁ lter casing is always securely closed (see „Servicing and cleaning the ﬁ lter“)!

Insert the inﬂ ow pipe into the „IN“ port until it clicks home. Connect the other end of the pipe to the „OUT“ port of the condenser (water pressure max 1.5 bar).

Insert the return pipe into the „OUT“ port until it clicks home. Connect the other end of the pipe to the „IN“ port of the condenser.

Connection to the water

Operatrion is only allowed with the pressure valve IKA® C 25! The IKA® C 25 pressure valve is absolutely essential on the water faucet for operation of the calorimeter,

The connection „EMPTY“ is intended only for emptying the device, e.g. for transport purposes. In normal operation the discharge hose need not be inserted!

and it must be preset to an output pressure of approximately 1.5 bar. The valve is installed into the line of the water connection, see operating instruction IKA

C 25.

Commissioning

Connecting the oxygen supply

Insert the O2 connection tube into the calorimeter „IN“ port until it clicks home and connect the free end to the pressure reducer, using the adapters supplied if necessary. IKA® C 29. Removal entails the same operations performed in the reverse sequence.

Note: The O2 connection tube can be removed only after it has been depressurised.

Screw the venting hose to the screw coupling (8 AF) on the calorimeter and position the free end under the extractor hood or connect it to a gas washing device. Comply with the applicable safety regulations in this respect.

IKA® C 29

The venting hose discharges the combustion gases from the decomposition vessel after every combustion trial. When laying the venting hose ensure that it is not crushed or kinked.

Connection to the mains power supply

Check that the available mains power supply matches the mains power supply particulars listed on the rating plate.

O2 connection tube IN max. 4 MPa

Venting hose

Combustion gases are

DANGER

therefore the venting hose must be connected to a suitable gas cleaning system or extraction system.

hazardous to health,

Commissioning

Connection of peripherals

Standard setting : Baud rate: 9600

Note: While the peripheral devices are being connected, they and the calorimeter must be turned-off on the mains power switch!

RS232 PC: Serial connection for controlling the calorimeter using CALWIN or operating with serial printer C1.50.

Data bits: 8 Stop bits: 1 Parity: none Handshake: none

RS232 BALANCE: Interface for connecting scales (Mettler, Ohaus, Sartorius, Kern)

Standard setting : Baud rate: 1200 Data bits: 7 Parity: odd Stop bits: 1 Handshake: none

ETHERNET:

USB-DEVICE: USB interface (only for service).

USB-HOST: Interface for connection of a printer or with a USB mouse.

SAMPLE-RACK: Interface for connection of the C 5020 sample rack.

Network connection for data transfer via the network, e.g. to a network printer.

Commissioning

On/off switch

The device is switched on and off via the on/off switch located on the righthand side.

Switch the device off at the on/off switch. � Lift moves upwards.

Switch the appliance off only by using the menu commands. � Lift moves downwards.

Data may be lost if the

ATTENTION

other than by following the menu commands.

Note: Switch the device off at the on/off switch only when directed to do so by the menu command.

appliance is switched off

Commissioning

Display and operating elements

Explanation of the screen display

Schematic representation of he display components

After the IKA® C 6000 global standards/ isoperibol calorimeter has been switched on, the touch screen display is active and can be operated using the stylus or ﬁ nger.

Pos. Designation

A Tab C Arrow symbol, tabs D Arrow symbol, vertical scroll bar E Vertical scroll bar F Info line G Arrow symbol, horizontal scroll bar H Horizontal scroll bar I Control button

Other view-based presentations of display components are described in the relevant section.

Display and operating elements

List display

The contents of the screen display are often distributed over several tabs. You can switch between tabs at any time by clicking on them. Thus for instance the screen display during the calorimetric standard procedure consists of the three views „Measurements“, „Device“ and

„Graphics“.

Status symbols

Green tick Measurement completed but not yet evaluated, or selection acknowledgement.

Pocket calculator Measurement completed end evaluated, evaluation inputs can no longer be changed.

Blank tick Measurement prepared but not yet performed.

Report ﬁ eld

Yellow X Field property not selected, or cancelled before ignition.

Red X Cancellation after ignition.

Circle Measurement selected.

List displays and report ﬁ elds have scroll bars. Clicking on the pale areas of the scroll bar scrolls the list display or report ﬁ eld. Clicking in the dark area and dragging it allows you to move continuously through the display, as does clicking on the arrow symbols and maintaining the selection.

Display and operating elements

Note: Greyed-out ﬁ elds cannot be selected.

The view „Graph“ shows the temperature by time.

The most important actions available at any point in time are gathered together as clickable buttons along the bottom edge of the screen.

Switch

Selection box

Switch

To initiate an action it is suﬃ cient to click on one of the discrete areas showing the relevant images or text. For instance during the „Preparation for measurement“ dialogue the most important actions are explained below.

Weighted sample Permits manual input of a weight value using the virtual keyboard.

Calibration Selection ﬁ eld for marking a calibration (on/off).

Decomposition vessel Manual selection box when decomposition vessel detection is inactive.

Name Alphanumeric editable ﬁ eld

User Alphanumeric editable ﬁ eld

Properties Alphanumeric editable ﬁ eld

IKA® thread

Selection box which allows a selection list to be opened.

Display and operating elements

Weighted sample

Input of a numerical value, such as weighted sample:

The entire area with the exception of the „Balance“ button is available to be clicked here. A numerical virtual keyboard is opened and can be used to input the value:

After the virtual keyboard has been closed with „OK“, the value in the input ﬁ eld is loaded. Alternatively, clicking on the „Balance“ button automatically loads a value from a connected balance.

Selection box

Shift key for upper and lower case letters and special characters

Input of an alphanumeric value, such as „Designation“ :

Here again the entire area is available to be clicked. A complete virtual keyboard is opened.

Note: The maximum input is 23 characters.

After the virtual keyboard has been closed with „OK“, the value in the input ﬁ eld is loaded.

Select from a selection box, e.g. for the ignition aid:

Display and operating elements

After the selection box has been clicked, a list of the options is displayed. The option that is clicked is selected.

Single selection ﬁ eld, such as calibration :

Clicking on the entire area allows the prepared measurement to be marked as a calibration.

Working with the IKA® C 6000 global standards/isoperibol calorimeter

Switching on the device

The IKA switched on with the On/off switch. The cover opens automatically. A start screen appears for about 30 seconds, during which the hardware is initialised and the software is loaded.

System test

The system test is performed automatically every time the IKA switched on.

During the system test the start screen is shown again; clicking on the „Show details“ button provides detailed information.

C 6000 global standards/isoperibol is

Safety instructions regarding information on and activation of the calorimeter are then shown on

the IKA

Homepage.

The system test includes the following steps:

- Testing the external water circuit with the circulation pump and heater (approx. 30 to 45 seconds).

- Testing the internal water circuit with the condenser and water supply, plus the heater once again (approx. 30 to 45 seconds).

- Testing whether the temperature of the cooling waters is correct for the selected function of the

IKA® C 6000 global standards/isoperibol. (ap-

prox. 60 to 180 seconds).

If any one of these steps is not performed successfully, the system test stops with an error message. After all the components have been checked the system test can be restarted the same as after a manual cancellation. To do this, press the „Restart“ button.

With the system test in standby, no measurements can be made. However it is possible to select some menu options.

Working with the IKA® C 6000 global standards/isoperibol calorimeter

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