Buchi B-540 Operation Manual

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Melting point B-540 Contents

Contents

1 Scope of delivery 2

2 Safety 4

3 Function 6

4 Putting into operation 7

5 Operation 9

5.1 Control, operating and display elements 9

5.2 Operating setup of the menus 10

5.3 Definition of concepts on displays 10

5.4 Preparation of samples 12

5.5 Determination of a melting point 12

5.5.1 Determination of the SETPOINT 13

5.5.2 Determination of the GRADIENT (temperature rise) 14

5.5.3 Determination of the MAXPOINT 15

5.6 Program management 16

5.6.1 Assignment of a sample identification 16

5.6.2 Storage of programs 17

5.6.3 Calling stored programs 18

5.6.4 Cancelling stored programs 19

5.6.5 Printing of results 20

5.7 Running a melting point determination 21

5.7.1 Melting point determination with known melting point 21

5.7.2 Determination of the melting point with unknown melting point 22

5.7.3 Modifications of parameters during the determination of a melting point 25

5.8. Boiling point determination 27

5.9 Adjustment of subparameters 28

Please read these instructions thoroughly before using the Melting Point B-540 Unit. The instructions should be kept near the unit for general reference.

Chapter 2 contains important notes on safety which must be observed if the Melting Point Unit is to be operated safely.

Due to continuous improvement and updating, technical specifications may be altered without prior notice. No part of this document may be reproduced, copied or transmitte in any way by using electronic or optical systems without prior agreement and written permission of Büchi Labortechnik AG. All rights reserved. © Büchi Labortechnik AG, 1995, 2001

6 Maintenance 33

6.3 Calibration of the unit with calibrating substances 33

6.4 Customer service 38

7 Taking out of operation 39

8 Spare parts 40

9 Appendix 41

9.1 Connecting a keyboard 41

9.2 Connection of a printer 41

9.3 Interface configuration 41

9.4 Menu chart 42

9.5 Print-Out 45

9.6 Error messages 46

9.7 Technical data 46

9.8 Materials used 47

9.9 FCC requirements (for USA and Canada) 47

9.10 Declaration of EC conformance 48

en, Version L (48 pages) Order No. B-540 Instructions 96626

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Figure 1: Complete view of the unit

Melting point B-5401 Scope of delivery

1 Scope of delivery

Description

Appliance models: Order No.

Melting Point Unit B-540, 220-230 V, 50 or 60 Hz 36580

Melting Point Unit B-540, 100-120 V, 50 or 60 Hz 36581

Table 1: Versions of the unit

Accessories:

a 1 Oven, upper part of ceramic 34564 b 1 Glass panel 34236 c 1 Metal cover for heating range 36569 d 2 Sample holders of glass 36110 e 1 Set of 100 melting point capillaries,each 17808 f 1 Set of 10 boiling point tubes, each 19007 g 1 Set of 10 boiling point capillaries, each 01762 h 2 Spare fuses 20083

1 Mains cable PNE, 2.5 m:

Type CH 10010 Type earthed (shock-proof) 10016 Type GB 17835 Type USA 10020 Type AUS 17836

i 1 Brief operating instructions

German 96635 English 96636 French 96661

j 1 Compaction wire 36721

1 Operating instructions

German 96625 English 96626 French 96627 Italian 96628 Spanish 96629

1 Packaging

Table 2: Enclosed parts

Figure 2: Accessories

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Melting point B-540

1 Scope of delivery

Optional accessories:

1 Keyboard for simple parameter input

Swiss keyboard arrangement 29599 USA keyboard arrangement 29548

1 Printer for documentation

incl. printer cable 230 V, 50/60 Hz 38706

115 V, 60 Hz 38707 1 Printer cable 29547 1 Melting point capillary (1000 off) 01759 1 Boiling point tube (100 off) 19697 1 Boiling point capillary (100 off) 19698

1 Büchi Certificate for Calibration

at Works G/E/F 97722

Remote control Meltingpoint (Manual incl. 3 1/2" diskette)

German 33758 English 33758

1 Protective cover 36625

1 Sample block for prepared

melting point capillaries 36629

Table 3: Optional accessories

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Melting point B-5402 Safety

2 Safety

This unit has been designed in accordance with the state of engineering and the recognised rules of safety. Nevertheless, it can still be a source of risks and hazards:

• If used by persons with insufficient training

• If used for purposes other than that for which it is intended.

2.1 Symbols

Stop

Information about hazards which can lead to serious material damage or cause serious or potentially fatal injury.

Warning

Information about hazards which can be harmful to your health or lead to material damage.

Please note

Information about technical requirements. Non-observance can lead to malfunctions, inefficiency and lost production.

2.2 Requirements to be met by the customer

The device must only be operated by persons who have the training or professional experience to comprehend the hazards that can arise when using the unit. Personnel without such training or persons currently undergoing a course of training require thorough instruction. This Instruction Manual should form the basis of these instructions.

2.3 Proper use

The unit is designed and built for use in laboratories. It is intended to be used to determine the melting and boiling points at ambient temperatures of up to 400°C.

2.4 Improper use

Any use other than those already listed, and any application that does not conform with the technical data is deemed to be a case of mis-use. The customer shall bear sole responsibility for any damage due to such mis-use. The following applications in particular are inadmissible:

• Use in rooms requiring an explosion-proof equipment.

• Extraction of samples which may explode or ignite by a blow, friction, heat or spark (e.g. explosives, etc.).

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Melting point B-540

2 Safety

2.5 General hazards

General hazards arise from:

• Mixtures of unknown composition or contaminations.

• Combustible gases or solvent vapours in the immediate vicinity of the unit.

• Damaged glass components.

• An insufficient distance from the back of the unit to the wall (see chapter 4, Commissioning the unit).

• Burnings by touching hot parts of the heater.

Apart from authorised maintenance personnel, no one is allowed to remove any safety devices and covers with a standard tool. The unit must not be put into operation with damaged glass components.

Touching life parts may result in fatal injury!

2.6 Safety measures

Personal protective garments must be worn, such as goggles and a laboratory coat.

This Instruction Manual is a component of the melting point unit and as such it must remain available at any time to the operating staff where the unit is operated. This also applies to manuals in other languages which are available on request.

2.7 Modifications

Modifications on the unit or on the spare parts or accessories as well as the use of any other spare parts or accessories as those indicated in this Manual are only permitted after consulting with Büchi Labortechnik AG and obtaining its written consent.

2.8 Responsibility of the operator

The operator is responsible for instructing his personnel. For that purpose, this Manual can be supplied in other languages. The operator shall inform the manufacturer without delay on any events relevant to safety which may occur with operating the Melting Point Unit.

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3 Function

Sequence of analysis

Heating phase Readiness Melt. det. phase Cooling phase

Melting point B-540

3 Function

The Melting Point Unit B-540 is a unit to determine melting and boiling points at ambient temperatures of up to 400°C. Three different samples can be determined at the same time. Values can be detected by viewing the samples.

Operating principle

The Melting Point Unit B-540 provides the melting point in agreement with pharmacopoeia methodologies and the boiling point according to Silowopov.

Temperature

Setpoint

Figure 3: Analysis flow chart

Gradient

Max-

point

For every determination the procedure is as follows:

1. Selection of the SETPOINT; temperature which is 10°C below the melting point to be expected.

2. Selection of the temperature GRADIENT; temperature GRADIENT within the range of the melting point.

3. Selection of the MAXPOINT; temperature at which the determination can be interrupted automatically.

4. Storage of the parameters selected (if needed).

Time

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Melting point B-540 4 Putting into operation

4 Putting into operation

Check the unit for any damages immediately after opening the packaging. It is important that damage incurred during transit is determined and reported immediately. If this is the case, a full statement of facts must be made immediately (and reported to the post office, railway or transport firm).

It is advisable to keep the original packaging for future transport.

4.1 Location of unit

The unit must be erected on a stable, clean and even surface.

For safety reasons and to ensure sufficient cooling in the electronic compartment, the side walls of the unit must be placed at least 30 cm away from the walls or other objects. No containers, chemicals or other appliances should be placed behind a unit.

4.2 Power connections

Check that the voltage of the socket is identical to the voltage specified on the unit plate. Only connect the Melting Point Unit to a plug which is earthed. External couplings and extension cables must be earthed (3-contact couplings, cables and connectors). Any interruption of the earth wire is prohibited. Risks caused by possible internal defects are thus prevented.

4.3 Mounting of accessoires

The sample holders of glass are inserted into the opening of the housing cover.

Figure 4: Mounting the glass sample holder

The glass sample holders protect the apparatus from dust and smaller particles and the operator from contact with electric parts.

Therefore, the apparatus should never be operated without the sample holders inserted.

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Figure 5: Mounting the glass panel

Melting point B-5404 Putting into operation

The glass panel is placed into the metal heating block, taking care to touch the panel only laterally.

Figure 6: Inserting the upper ceramic part

The upper ceramic part of the oven is placed onto the metal block.

The metal cover is placed over the heating area.

Figure 7: Fitting the metal cover 5 Operation

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Melting point B-540

5 Operation

Please note that the unit has been commissioned correctly according to the instructions in chapter 4 Commissioning.

Figure 8: Front view, B-540

5.1 Control, operating and display elements

a Master switch b Magnifying glass for viewing the samples c Display for prompt facility d START key to start a determination e STOP key to interrupt a determination f MENU key to change displayed menu windows g ENTER key to change the cursor position vertically when

adjusting parameters on the display

h NEXT key to change the cursor position horizontally

when adjusting parameters on the display

i UP/DOWN keys to change adjustments of the relative

cursor position

j Keys to store measured values during a determination

Figure 9: Rear view, B-540

k Sample holder for melting point capillaries and boiling point

tubes during determination

l Receptacle for unused melting point capillaries and boiling

point tubes

m Receptacle for used melting point capillaries and

boiling point tubes

n Appliance plug o Plug for printer connection p Plug for keyboard connection q Plug for PC connection r Main fuse s Pocket for brief instruction manual

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Mainmenu 1 Mainmenu 2 Mainmenu 3

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0°C

NAME : ID# :

TEMPERATURE : 25.0°C

RECALL CLEAR STORE PRINT

Melting point B-5405 Operation

5.2 Operating setup of the menus

5.2.1 Main menus

The user may move through these menus for every new melting point determination.

TEMPERATURE 25 °C

TEMPERATURE 140 °C

SP 136 °C

GR 2.0 °C MP 145 °C

TEMPERATURE: 135.6 °C

GR 2.0 °C MP 145 °C

PRESS START

TEMPERATURE 145 °C

TEMPERATURE 100 °C

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

5.2.2 Graphics

These graphics will accompany the user during a melting point determination and explain which part of the heating profile is activated.

5.3 Definition of concepts on displays

5.3.1 Main menus

Basic condition (main menu 1)

Temperature: Current temperature inside of the oven.

SETPOINT: Temperature

• at which the sample capillaries are inserted into the unit;

• as from which the adjusted temperature programwill run down.

TEMPERATURE : 25.0°C

NAME : ID# :

GRADIENT: Temperature rise from 0.1/0.2/0.5/1.0/2.0/5.0/

10.0/20° C/min, at which the unit will be heated

up as from SETPOINT to MAXPOINT.

MAXPOINT: Maximum temperature to be reached for the

current determination. This is set automatically at 15°C above the SETPOINT but may also be adapted.

Storage menus (main menu 2)

Temperature: Current temperature inside of the oven. Name: Name of the method under which the

parametersare to be stored for a melting point determination.

ID#: Assignment of a sample name to a current

determination which should appear equally on a subsequent printout.

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Melting point B-540 5 Operation

TEMPERATURE: 25.0 °C

RECALL CLEAR STORE PRINT

M SAMP1 SAMP2 SAMP3 A XXX.X XXX.X XXX.X °C N XXX.X XXX.X XXX.X °C

XXX.X XXX.X XXX.X °C

(Main menu 3)

Temperature: Current temperature inside of the oven.

RECALL: Calling stored methods for melting point determi-

nation

STORE: For storing new methods for melting point deter-

mination

CLEAR: For cancelling stored methods of a melting point

determination

PRINT: For switching on and off the automatic printout of

thevalues obtained from a melting point determination.

5.3.2 Display of values

Manuell display This display permits to read off the melting points after a determination. A maximum of three values will be displayed per sample capillary which are arranged in vertical order.

5.3.3 Graphics

TEMPERATURE 25.0 °C

TEMPERATURE 135.6 °C

PRESS START

TEMPERATURE 140 °C

TEMPERATURE 145 °C

TEMPERATURE 100°C

SP 136 °C

GR 2.0 °C MP 145 °C

The unit heats up to the preselected SETPOINT:

The unit has reached the preselected SETPOINT and waits for the temperature program to be started.

With the preselected GRADIENT, the unit heats up to the maximum point of the temperature program (MAXPOINT).

The unit has reached the highest point of the temperature program (MAXPOINT) and cools down to the previously selected SETPOINT.

The unit cools down to room temperature.

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Melting point B-5405 Operation

5.4 Preparation of samples

Granular crystalline and inhomogenous samples are crushed in the mortar and then filled into the melting point capillary to at least 4-6 mm. In order to obtain comparable results, it is essential that all three capillaries are filled to the same height and that the substance is compacted.

Compaction is obtained either by knocking the capillary on a hard base or letting the capillary drop onto the table through a glass tube of approx. 1 m length.

5.5 Determination of a melting point

The following items must be known before a melting point can be determined:

a Is the approximate melting point known ?

if not R see 5.7.2

b Is a sample name to be entered ?

if yes R see 5.6.1

c Where is the SETPOINT of the determination located ?

SETPOINT input R 5.5.1

d How fast should the temperature rise (GRADIENT)

between SETPOINT and MAXPOINT ? GRADIENT input R see 5.5.2

e Is the difference between SETPOINT and MAXPOINT to

be more than 15°C ? Change MAXPOINT R see 5.5.3

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Melting point B-540 5 Operation

5.5.1 Determination of the SETPOINT

The SETPOINT can be adjusted in the main menu. This is done on every individual digit of the relative number. The SETPOINT is adjusted with keys UP/DOWN and NEXT, the number is transmitted with the ENTER key. By way of example, a SETPOINT of 180°C is to be adjusted.

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

Actuate ENTER until the cursor is on the SETPOINT field.

Increase or reduce the value until the number 1 is in the first digit.

NEXT until the cursor is on the second digit.

Increase or reduce the value until the number 8 is in the second digit.

NEXT until the cursor is on the third digit.

Increase or reduce the value until the number 0 is in the third digit.

ENTER to transmit the complete SETPOINT temperature.

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5 Operation

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

Melting point B-540

5.5.2 Determination of the GRADIENT (temperaturerise)

The gradient is the heating rate at which heating is continued as from reaching the SETPOINT temperature to MAXPOINT. Adaptation of the gradient is made in 0.1/0.2/0.5/1/2/5/10/ 20°C/min in the main menu. By way of example, a gradient of 1°C is to be selected.

Actuate the ENTER key until the cursor is on the gradient field.

Increase or reduce the temperature rise until the value of 1°C/min is displayed.

Actuate ENTER to transmit the selected temperature rise.

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Melting point B-540

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

5 Operation

5.5.3 Determination of the MAXPOINT

Normally, the temperature of the MAXPOINT is adjusted automatically at 15°C above the SETPOINT. If this temperature differential exceeds 15°C in an individual case, the MAXPOINT may be adapted manually. The MAXPOINT is equally adapted in the main menu. By way of example, the MAXPOINT temperature of 195°C is to be increased to 230°C.

Actuate ENTER until the cursor is on the MAXPOINT field.

Increase or reduce the value until the number 2 is in the first digit.

NEXT until the cursor is on the second digit.

Increase or reduce the value until the number 3 is in the second digit.

NEXT until the cursor is on the third digit.

Increase or reduce the value until the number 0 is in the third digit.

ENTER to transmit the MAXPOINT temperature.

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5 Operation

Melting point B-540

5.6 Program management

5.6.1 Assignment of a sample identification

If similar parameters are used all over again, it is recommended to store them with sample names. By simply calling them up from the memory, their repeated entering becomes dispensable. As far as necessary, an identification (e.g. batch number or test number) may be assigned to this method. The name and the sample identification will then be printed out. A sample name and the sample identification are entered into the menu of the memory. The name used may consist of letters, figures or a combination of figures with letters.

For easy entering of sample names and sample identifications we recommend to use a keyboard (Büchi Art. No. 29599).

TEMPERATURE : 25.0°C

NAME : ID# :

Actuate ENTER until the cursor is on the NAME field for entering the method name.

Actuate NEXT until the cursor is on the correct position of the horizontal which is to be modified.

An individual cursor position can be changed by actuating UP/DOWN.

Press ENTER to transmit the method name. Enter the identification again with UP/DOWN and NEXT.

Press ENTER to transmit the sample identification.

The name and sample identification are now printed out. But the method has not yet been stored. If the method is to be stored in the memory, change over to main menu 3.

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Melting point B-540 5 Operation

5.6.2 Storage of parameters

Press MENU to change to main menu 3.

TEMPERATURE: 25.0 °C

RECALL CLEAR STORE PRINT

Press NEXT until the cursor is on the STORE field.

TEMPERATURE : 25.0°C

MEMORY FULL !

PRESS ENTER

TEMPERATURE : 25.0°C

NO NAME - NOT STORED !

PRESS ENTER

TEMPERATURE : 25.0°C

NAME EXISTS ALREADY

PRESS ENTER

By pressing ENTER, the program is stored with the selected parameters under the entered name and the display will change to main menu 1. The sample identification is not stored.

Possible error messages.

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5 Operation

Melting point B-540

5.6.3 Recalling stored programs

If similar parameters are used all over again, it is recommended to store them with sample names. By simply recalling them from the memory, their repeated entering becomes dispensable.

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0 °C

RECALL CLEAR STORE PRINT

TEMPERATURE : 25.0 °C RCL: XXXXXX q

XXXXXX XXXXXX Q

Stored programs can only be recalled from main menu 3.

Press the MENU key twice to enter the main menu 3.

The NEXT key is pressed until the cursor is on the RECALL field.

By pressing the ENTER key, the stored programs are listed.

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0°C

MEMORY EMPTY !

PRESS ENTER

Choose the selected program with UP/DOWN keys (e.g. benzoic acid).

Recall the selected program by pressing the ENTER key. The unit is now ready for the next determination with the recalled method.

Possible error message.

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Melting point B-540 5 Operation

5.6.4 Cancelling stored programs

If stored programs are no more needed or if the capacity of storage locations is exhausted, programs may be cancelled (erased).

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0 °C RCL: XXXXXX q

XXXXXX XXXXXX Q

Stored programs can only be cancelled from the main menu.

Press MENU twice to return to the storage menu.

Press NEXT until the cursor is on the CLEAR field.

By pressing ENTER, the stored programs are listed.

Select the program to be cancelled with UP/DOWN (e.g. benzoic acid).

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0°C

MEMORY EMPTY!

PRESS ENTER

Press ENTER to cancel the selected program. If necessary, further programs may be cancelled now.

By pressing MENU, return to the main menu.

Possible error message.

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5 Operation

Melting point B-540

5.6.5 Printing of results

1. Automatic printout after every determination

When a determination is complete, results and selected parameters can be printed out automatically. If this automatic printout is required, it is necessary to accesss configuration menu 3.

The menu key is pressed for 3 seconds access the first submenu.

Press the menu key tweice to access the 2nd configuration menu.

AUTOPRINT : XXX PRINTER : XXXXX KEYBOARD : XX

TEMPERATURE : 25.0 °C

RECALL CLEAR STORE PRINT

The connected printer is selected in the PRINTER box.

In the AUTOPRINT bix it is stipulated that for:

YES: there will be an automatic printout after

every determination.

NO: there will not be a printout after every

determination.

2. Manual printout after every determination.

The user can stipulate for which determination he wishes to have a printout.

No must then be selected for AUTOPRINT in configuration menu 3.

If a printout is required after completion of a determination, the PRINT box is accessed with the MENU key and confirmed with ENTER.

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Melting point B-540

5 Operation

5.7 Running melting point determination

5.7.1 Melting point determination with a known melting point

TEMPERATURE : 25.0°C SETPOINT ; 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE 25.0 °C

TEMPERATURE : 135.6 °C

PRESS START

TEMPERATURE : 140 °C

SP 136 °C

GR 2.0 °C MP 145 °C

The melting point determination may be started from any main menu. The SETPOINT, GRADIENT and MAXPOINT must first have been defined as described in 5.5.1–5.5.4.

By pressing START, the unit will heat up to the previously selected SETPOINT. The display shows the temperature gradient graphically.

The user is informed acoustically when the SETPOINT has been reached. The graphic will change at the same time. Samples are introduced into the sample holder.

By pressing START again, the temperature program is started between SETPOINT and MAXPOINT and the display changes to the detection phase.

M SAMP1 SAMP2 SAMP3 A XXX.X XXX.X XXX.X -C N XXX.X XXX.X XXX.X -C

XXX.X XXX.X XXX.X -C

A maximum of three modifications of condition per sample may be transmitted to the memory. If keys are pressed more than 3x, the last three temperature values will be retained.

When the preselected MAXPOINT has been reached, the unit will cool down automatically to the previously used SETPOINT. The temperature program may be stopped before reaching the MAXPOINT temperature by pressing STOP. Even in this case, the unit will cool down to the previously selected SETPOINT and display the values obtained.

Samp 1: Determinated value for substance in capillary 1

Samp 2: Determinated value for substance in capillary 2

Samp 3: Determinated value for substance in capillary 3

By pressing MENU, the determination can be repeated.

By pressing STOP, the unit will cool down to ambient temperature.

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5 Operation

Melting point B-540

5.7.2 Melting point determination with unknown melting point

If the user has no information about the location of the melting point of his substance it can be found out by means of a previous fast determination. For that purpose, it is recommended to select the SETPOINT as low as possible and the temperature GRADIENT as high as possible. Here, the MAXPOINT should be selected to ensure that it is definitely above the melting point. A fast determination can only be started from the main menu.

A sample designation is dispensable. The SETPOINT, GRADIENT and MAXPOINT must be defined. By way of example, a melting point is to be determined which is between the ambient temperature and 300°C. For this, it is sufficient to determine the approximate melting point with one capillary only.

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

Establishing the SETPOINT

(with unknown melting point)

Press ENTER until the cursor is on the SETPOINT field.

Increase or reduce the value until the number 0 is in the first digit.

Press NEXT until the cursor is on the second digit.

Increase or reduce the value until the number 3 is in the second digit.

Press NEXT until the cursor is on the third digit.

Increase or reduce the value until the number 0 is in the third digit.

ENTER to transmit the SETPOINT temperature. The cursor will jump to the next line.

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Melting point B-540 5 Operation

Adjusting the temperature program (GRADIENT)

(with unknown melting point)

Increase or reduce the temperature program until the value of 20°C/min is displayed.

Press ENTER to transmit the selected temperature program. The cursor jumps to the next line.

Adjusting the MAXPOINT

(with unknown melting point)

Increase or reduce the value until the number 3 is in the first digit.

Press NEXT until the cursor is on the second digit.

Increase or reduce the value until the number 0 is in the second digit.

Press NEXT until the cursor is on the third digit.

Increase or reduce the value until the number 0 is in the third digit.

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TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

Melting point B-5405 Operation

Press ENTER to transmit the MAXPOINT temperature.

By pressing START, the unit will heat up to the previously selected SETPOINT. The display will show the temperature gradient graphically.

TEMPERATURE 25.0 °C

TEMPERATURE : 135.6 °C

PRESS START

TEMPERATURE : 135.6 °C

M SAMP1 SAMP2 SAMP3 A XXX.X XXX.X XXX.X °C N XXX.X XXX.X XXX.X °C

XXX.X XXX.X XXX.X °C

SP 136 °C

GR 2.0 °C MP 145 °C

The user is informed acoustically that the SETPOINT has been reached. At the same time, the graphic will change. The samples are introduced into the sample holder.

By pressing the START key again, the temperature program is started between SETPOINT and MAXPOINT and the display changes to the detection phase. (If Auto-Start had been switched off, refer to 5.9).

The samples are viewed through the magnifying glass as required. The melting point is retained by pressing SAMPLE keys 1/2/3. Every pressing of the SAMPLE keys is acknowledged with a beep and confirmed with an indication on the screen. A maximum of three modifications of condition per sample may be transmitted to the memory. If keys are pressed more than 3x, the last three temperature values will be retained.

The melting point thus determined is 25°C too high for a more accurate determination (see chapter 5.5.5).

By pressing MENU, the determination can be repeated.

By pressing STOP, the unit will cool down to ambient temperature.

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Melting point B-540

5 Operation

5.7.3 Modifications of parameters during a melting point determination

Quite frequently, the user will find out during an actual determination that his selected parameters have to be adapted, e.g. because the SETPOINT or the MAXPOINT are too low or because the GRADIENT runs too slowly. In order to adapt these parameters, it is not necessary to start the determination again from the beginning.

The following modifications are possible:

Modifications before reaching the SETPOINT

The SETPOINT can be adapted. The determination can be aborted. Cooling down to ambient temperature.

TEMPERATURE 25.0 °C

SP 136 °C

Modifications in the ready mode

The MAXPOINT can be adapted. The GRADIENT can be adapted. The determination can be aborted. Cooling down to ambient temperature.

Modifications between SETPOINT and MAXPOINT

The MAXPOINT can be adapted. The GRADIENT can be adapted. The determination can be aborted. Cooling down to ambient temperature.

Modifications before reaching the SETPOINT

Problem: The SETPOINT has been selected too low.

The field for SETPOINT temperature begins to flash and may be rised by actuating UP/DOWN.

The new SETPOINT temperature is confirmed with ENTER and the unit returns to the determination mode.

Problem: The determination is to be aborted.

The determination is to be aborted and the unit is to be cooled down to ambient temperature.

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5 Operation

Melting point B-540

Modifications in the ready mode

Modifications between SETPOINT and MAXPOINT

TEMPERATURE 135.6 °C

PRESS START

GR 2.0 °C MP 145 °C

TEMPERATURE : 140 °C

GR 2.0 °C MP 145 °C

Problem: The temperature GRADIENT and/or MAXPOINT have been selected too low.

The field for temperature GRADIENT begins to flash and can be increased via UP/DOWN.

The new temperature GRADIENT is acknowledged with ENTER and the MAXPOINT temperature flashes.

The MAXPOINT temperature can be increased via UP/DOWN.

The newly selected MAXPOINT is confirmed with ENTER and the unit returns to the determination mode.

Problem: The determination is to be aborted.

The determination is aborted and the user returns to the main menu.

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Melting point B-540 5 Operation

Siedepunkt 100 °C Boiling point 100 °C Point d'ébullition 100 °C

20 °C

95 °C

100 °C

5.8 Boiling point determination

The sample liquid is filled into the capillary of 3.2 mm internal diameter to a height of 5-10 mm. Use a syringe for easy filling. The boiling capillaries are plunged into the sample with their thick end. Switch the master switch on. Place the sample capillary into the sample holder. The position for boiling point determination is either fully to the left or to the right of the sample holder.

If the approximate boiling point is not known, the SETPOINT should be selected as low as possible and the temperature GRADIENT and the MAXPOINT as high as possible (analogously to the melting point determination, section 5.6, a quick determination for orientation is carried out). If the approximate boiling point is known, enter the SETPOINT, GRADIENT and MAXPOINT (analogously to melting point determination with known melting point, section 5.5.5).

The boiling point has been reached when a quick continuous flow of bubbles (like a string of pearls) is formed at the plungedin end of the capillary.

Figure 10: Boiling point determination

Page 30

Melting point B-5405 Operation

5.9 Adjustment of subparameters

Sub-parameters are main-settings which have to be presetted by the user when using the insrument the first time. The presettings are located in the sub-menu (Configuration).

Press and hold the MENU-key for 3 seconds to enter in this sub-menu. After being in the menu it can be switched through the window menu by pressing the MENU-key.

5.9.1 Parameter menus

TIME : XX:XX DATE : XX.XX.XX NAME : XXXXX

AUTOPRINT : XXX PRINTER : XXXXX KEYBOARD : XX

RS232 C : XXXX XXX

CONTRAST : XXX % BUZZER : XXX AUTOSTART : XXX

TIME : HH:MM DATE : DD:MM:YY UNIT : °X LANGUAGE : ENGLISH

Menu window for setting data which are to appear on the printout. Time: Time Date: Date Name: Company name

Menu window for adjusting the displays to be printed out. Autoprint: Automatic printing after every determination

yes/no

Printer: Selection of the printer to be used

Menu window for adjusting the serial interface to the PC connection.

Menu window for adjustments of the unit Contrast: Adjustments of the LCD display Buzzer: Beep yes/no

Menu window for basic adjustments Time: Time subdivided into 12 or 24 steps Date: American or European date Unit: Temperature in °C or °K Language: Language as displayed

SW-VER. : VX.XX LAST CAL : XX.XX.XX

CALIBRATION INTERVAL : XX MONTH PASSWORD :

SW version: Indication of the software installed Last cal.: Date of the last calibration

Interval: Time interval before the unit informs the user

that calibration should be re peated.

Password: Entering the menu level for calibrating the unit

by the user.

Page 31

Melting point B-540 5 Operation

5.9.2 Modification of time, date and company name

If you connect the unit to a printer, the melting points may be printed out with other parameters. In order to permit a better assignment of the printouts, each printout will bear the following:

• the name of the own company

• the time of melting point determination

• the date of melting point determination

Press MENU for three seconds to return to the range of submenus.

TIME : XX:XX DATE : XX.XX.XX NAME : XXXXX

By pressing UP/DOWN, the individual digits are changed; by pressing NEXT, the horizontal cursor position is changed.

By pressing ENTER, the date field will be displayed and this is then adapted in the same way as described above.

By pressing ENTER, the field for the company name is displayed and this is then adapted in the same way as described above.

By pressing ENTER, the newly entered company name will be used for all new determinations.

In order to return to main menu 1, press MENU again for three seconds.

Page 32

Melting point B-5405 Operation

5.9.3 Automatic printout after every determination, selection of the printer

In this menu, the following adjustments can be carried out:

• Automatic printout after every determination

• Automatic printout of the transmission curve after every

determination

• Selection of the connected printer

Press MENU for three seconds to return to the range of submenus.

Press MENU twice to go to the menu window.

AUTOPRINT : XXX GRAPHIC : XXX PRINTER : XXXXX

By pressing UP/DOWN, the automatic printout will be activated after every determination, and made inoperative with NO.

Press ENTER to change to the printer field.

Press UP/DOWN to select the printer to be used.

• CITIZEN • EPSON (also Canon and Seiko)

• HP • STAR • NONE

By pressing ENTER, the newly entered printer will apply for all new determinations.

In order to return to the main menu, press MENU again for three seconds.

Page 33

Melting point B-540 5 Operation

5.9.4 Definition of the RS-232 C interface

In this menu, you can change the following setting:

• Transfer speed (baud rate)

• Data word length

• Parity

• Number of stopbits

Press MENU for three seconds to return to the range of submenus.

Press MENU twice to change to the menu window.

RS232 C : XXXX XXX

Press UP/DOWN to select the correct RS-232 C interface.

When pressing ENTER, the newly selected RS interface will be displayed for all determinations.

Press MENU again for three seconds to return to mainmenu 1

Page 34

5 Operation

Melting point B-540

5.9.5 Display adjustments, switching on/off, beep

In this menu, the following adjustments can be carried out:

• Increase/reduce background illumination on the display

• Switch the beep on/off

Press the MENU key for three seconds to return to the range of submenus.

Press the MENU key three times to change to the menu window.

CONTRAST : XXX % BUZZER : XXX AUTOSTART : XXX

Menu window to unit adjustments CONTRAST: LCD display adjustments BUZZER: Beep on/off

By pressing the UP/DOWN key, the background illumination will be increased or reduced.

By the pressing the ENTER key, the user return to the buzzer field.

By pressing the UP/DOWN key, the beep will remain with YES and be made inoperative with NO.

Press the MENU key again for three seconds to return to the main menu.

Page 35

Melting point B-540

Temperature

Temperature Displayed by apparatus

Display in calibration sub-menu

of the apparatus

CAL: 83°C+0.0°C+0.0°C

Correction by user

Temperature

Temperature Displayed by apparatus following calibration

Display in calibration sub-menu

of the apparatus

CAL: 83°C+0.5°C+0.0°C

Corrections following calibration: +0.5°C

Correction by user

First calibration following

installation

Correction = +0.5°C

Second calibration after one

yearCorrection = -0.4°C

Temperature

Temperature Displayed by apparatus following calibration

Corrections following 2nd calibration: -0.4°C

Correction by user

Display in calibration sub-menu

of the apparatus

CAL: 83°C+0.1°C+0.0°C

5 Maintenance

6 Maintenance

All instructions intended to keep the Melting Point Unit in a fully operative condition should be duly noted. This also includes a periodic cleaning and checking for any damages. It is also recommended to calibrate the unit periodically with adequate calibration substances.

6.1 Cleaning

The housing of the Melting Point Unit B-540 is coated with paint. It must only be cleaned with a rag to be either dry or moistened with alcohol. Do not use any chlorinated solvents, acetone or similar chemical to clean the magnifying glass.

6.2 Upkeep

The upkeep of the unit is mainly limited to:

• a periodical calibration of the transmission

6.3 Calibration of the unit with calibrating substances

The unit is to be checked frequently by means of reference substances. We recommend to use the following reference substances for calibrating the Melting Point Unit B-540:

Vanilline Rated melting point approx. 83°C

Phenacetine Rated melting point approx. 136°C

Caffeine Rated melting point approx. 237°C

We recommend to use the reference substances from the calibration kit, Büchi order number 37454.

Figure 11: Schematic correction factors

Page 36

Melting point B-5406 Maintenance

6.3.1 Melting point determination procedure for the calibration

• The instrument should be calibrated at least once a year.

• The reference substances should be stored protected from

light in a desiccator over desiccant at room temperature (15-25°C).

• The expiry date must be checked and the reference

replaced if necessary.

• The theoretical melting points of the reference substances

are known. An analysis certificate is provided and describes how the theoretical melting points are determined.

• Three measurements are performed simultaneously for

each reference substance.

Recommendation:

Filling height: 4-5mm, as compact as possible by knocking

the filled capillaries on a hard surface, the

substances are ground in a mortar. Gradient: 0.5°C/min Setting point: 5°C below the expected melting point

Determine the clear melting point (sample melted completely clear).

6.3.2 Evaluation of the melting point

determination

All measurements should be evaluated in accordance with strict criteria and checked for their usability. For this we recommend that at least the following parameters be checked and the measurement repeated in the case of doubt.

• The melting procedure complies with the requirements.

• There should not be any bubbles which hinder visual eva-

luation of the melting procedure.

• The samples should not become discoloured.

• The samples melt within a narrow temperature range of

1°C.

The mean value is calculated and the standard deviation from 3 measurements is:

Vanilline <0.3°C

Phenacetine <0.5°C

Caffeine <0.5°C

Page 37

Melting point B-540 6 Maintenance

• No systematic deviation from the individual melting points due to the particular position in the heating element shall exceed 0.4°C.

For example (repeated measurements):

Position 1 Position 2 Position 3 Acceptable yes/no

83.0°C 83.0°C 83.4°C acceptable

82.3°C 82,9°C 83,5°C unacceptable

82.5°C 82,3°C 82,0°C acceptable

After the melting value mean values have been carefully checked, these will be compared with the expected theoretical values and the corresponding corrections made if necessary.

We recommend correction only in the case of errors > +/-

0.3°C.

CALIBRATION INTERVAL : XX MONTH PASSWORD :

6.3.3 Correction inputs

If it is ascertained during a routine check of the temperature display, that the actual and rated values of the calibration substances differ, the unit may be recalibrated by the user as follows:

Press the MENU key for three seconds.

Press the MENU key again six times to change to the calibration window.

Press the ENTER key to change to the PASSWORD field. The password for the calibration may then be entered: CAL.

Press the ENTER key to get to calibration.

Page 38

6 Maintenance

Melting point B-540

Correction calculation

The theoretical melting point is stated for the reference substance. If an interval is given, the mid-point is the theoretical melting point.

Correction = Theoretical melting point display

Examples:

• The theoretical melting point of vanillin is 83.0°C. The Büchi Melting Point B-540 found a melting point of 82.3°C. Correction: 83.0°C = +0.7°C

• The theoretical melting point of vanillin is 83.0°C. The Büchi Melting Point B-540 found a melting point of 83.0°C. Correction: 83°C = -0.3°C

CAL: 83°C + X.X + X.X °C

136°C + X.X + X.X °C 237°C + X.X + X.X °C

STORE CALIBRATION:XXX

Now the pertinent corrections can be entered for the three types of calibration substances. The left column indicates the last correction, the right column is used to enter the new corrective value.

By pressing the UP/DOWN/NEXT keys, the necessary corrective value at 83°C is entered.

By pressing the ENTER key, change to the 2nd temperature value and adapt this analogously.

Then press the ENTER key to change to the 3rd temperature value and adapt this analogously.

Press the ENTER key to change to the STORE CALIBRATION field and press the UP/DOWN key to obtain YES.

By pressing the ENTER key, the new calibration is confirmed.

05.09.95 WILL BE THE

NEW CALIBRATION DATE.

REALLY STORE : XXX

DONE. VERIFY CAL.

05.09.95 WILL BE THE

NEW CALIBRATION DATE.

REALLY STORE : XXX

DONE. VERIFY CAL.

For reasons of safety, the user is inquired again whether the corrective factors should be stored. If this is the case, set the display to YES and confirm with the ENTER key.

Checking of the calibration with the same parameters under the recommendation (see above).

Page 39

Melting point B-540 6 Maintenance

Press the MENU key to leave the calibration menu.

After entering the values, the correction factors for the middle and right hand columns are added together and entered in the middle column. Thus, the values in the middle column alter following each calibration and the right hand column is then free for the next calibration.

6.3.4 Control measurement

The calibration is checked with verification substances. For this we recommend the Set of verification substances, Büchi Item No. 37667. It allows checks at the following temperatures using four different substances:

Substance Melting Point* Melting Point

Deviation*

4-Acetyl benzonitrile ca. 60°C ± 0.2°C

m-Toluic acid ca. 110°C ± 0.2°C

Sulfanilamide ca. 165°C ± 0.2°C

Phenolphthalein ca. 260°C ± 0.2°C

* The exact values are specified on the packing as well as on the certificate from the manufacturer of the substance (Fluka AG).

The measurements are performed with the measurement parameters recommended in section 6.3.1. The melting point of each reference substance must be checked in at least three measurements. The standard deviations should be less than 0.3°C. The maximum permitted deviations of the mean value from the theoretical melting point are as follows:

Substance Melting Point Measuring Total

Deviation Accuracy Deviation

4-Acetyl benzonitrile ± 0.2°C ± 0.3°C > ± 0.5°C

m-Toluic acid ± 0.2°C ± 0.5°C > ± 0.7°C

Sulfanilamide ± 0.2°C ± 0.5°C > ± 0.7°C

Phenolphthalein ± 0.2°C ± 0.8°C > ± 1.0°C

All measurement results of the calibration, the correction factors entered and control measurement values should be recorded. This allows the calibration to be checked and repeated at a later date.

Page 40

Melting point B-5406 Maintenance

6.4 Customer service

Work on or in the unit may only be carried out by authorised service personnel, i.e. skilled technicians who are familiar with the operating instructions and current regulations with regard to work safety and accident prevention.

Büchi customer service depots have device-specific service manuals which are only available to authorised personnel.

Addresses of official Buchi customer service offices are given on the Buchi website under: www.buchi.com. Please contact one of these depots if the unit develops any faults, or you have any technical enquiries or application problems.

The Büchi customer service will be pleased to provide you with the following services:

• Spare parts service (when placing an order, please use the article numbers printed in this manual)

• Repair service

• Maintenance service

• Technical hotline

Page 41

Melting point B-540 7 Taking out of operation

7 Taking out of operation

The unit must be cleaned thoroughly.

7.1 Storage/Transport

The unit should be stored and transported in its original packaging and in clean condition.

7.2 Disposal

To ensure the disposal of the Melting Point Unit is as ecofriendly as possible, you will find a list of the materials used, some of which are marked with material codes, in Chapter 9, Appendix. This ensures that components can be separated and, where appropriate, recycled. Care must be taken that regulations are complied with, when disposing of electrical components. Furthermore, all methods of disposal should comply with regional and local legislations.

Page 42

Melting point B-5408 Spare parts

8 Spare parts

Only original Büchi accessories and spare parts guarantee the operational safety and reliability of this unit. Use of any spare parts or accessories other than Büchi is only permitted with the express permission of the manufacturer. For assembly and dismantling purposes, spare parts should only be used as described in chapter 6 of this instruction manual. The reproduction or manufacture of any parts found in this manual is equally prohibited.

Description Order no.

Protective cover 36625 Brief instruction manual in German 96635 Brief instruction manual in English 96636 Brief instruction manual in French 96661 Compaction wire 36721 Capillary holder of plastic 36629 Spare bulbs 29573 Spare fuse 110 – 120 V 19660 Spare fuse 220 – 240 V 20083 Upper ceramic part of oven 34564 Glass panel 34236 Metal cover for heating area 36569 Glass beaker 36110 Paper retainer for printer IDP-562 33751 Ribbon for printer Citizen IDP-562 37303 Paper roll for printer Citizen IDP-562 28261 Ribbon for printer Citizen IDP-460 38683 Paper roll for printer Citizen IDP-460 38684 Battery 29570

Table 4: Spare parts

Page 43

Melting point B-540

9 Appendix

9.1 Connecting a keyboard

We recommend to use a keyboard for a simple input of the sample names and sample identifications.

STOP

Figure 12: Functionkey-line

SAMPLE 2

SAMPLE 1

SAMPLE 3

CONFIG MENÜ

MENÜ

START

9.2 Connection of a printer

We recommend to use a printer model Star Printer 512 MC-42 parallel. The printer is connected using the communication cable supplied with the printer.

All printers are connected through the parallel V24 interface which is connected via the communication cable (centronic) to the printer (see section 5.1).

Appropriate printer settings are selected in the configuration menu of the melting point apparatus. The interface is automatically correctly configured by the melting point apparatus.

9.3 Interface configuration

Parallel interface: RS232 Baud rate: 9600 Data bits: 8 Stop bits: 1 Parity: none

Page 44

9 Appendix

Melting point B-540

9.4 Menu chart

The menu chart of the Melting Point B-540 can be subdivided in 2 main parts:

Main menu

Press "MENU"-key for 3 seconds

Configuration-

menu 1

.....

Figure 13: Menu chart

Main menu

.....

Configurations-

menus

.....

Main menu

.....

• the 3 main menus (Chapter 9.4.1)

• the 7 configuration submenus (Chapter 9.4.4)

Page 45

Melting point B-540 9 Appendix

9.4.1 Main menus 1-3

TEMPERATURE : 25.0°C SETPOINT : 100°C GRADIENT : 2.0°C MAXPOINT : 120°C

TEMPERATURE : 25.0°C NAME : ID# :

TEMPERATURE : 25.0 °C

RECALL CLEAR STORE PRINT

TEMPERATURE 25.0 °C

TEMPERATURE : 135.6 °C

PRESS START

TEMPERATURE : 135.6 °C

SP 136 °C

GR 2.0 °C MP 145 °C

Actual temperature Setting range: 25 - 400°C Parameter: 0.1 / 0.2 / 0.5 / 1.0 / 2.0 / 5.0 / 10.0 / 20.0 Automatic; SETPOINT + 15°C or variable to 410°C

Actual temperature Program name (max. 15 digits) Sample identification number (max. 15 digits)

Actual temperature RECALL/CLEAR: Recalling/deleting the stored program STORE: Store the program PRINT: Print the measure results on a connected printer

9.4.2 Heating-/Cooling phase

Quick heating (approx. 70°C/min.) to SETPOINT.

SP = SETPOINT

SETPOINT reached. Continue with the START-key.

GR = GRADIENT MP = MAXPOINT

Slow heating with selected Gradient to MAXPOINT; or early stopping with the STOP-key (manual)/auto detection. GR = GRADIENT MP = MAXPOINT

TEMPERATURE : 145 °C

TEMPERATURE : 100 °C

TEMPERATURE : 25.0 °C RCL: XXXXXXq

TEMPERATURE : 25.0 °C CLR: XXXXXXq

XXXXXX XXXXXX Q

Quick cooling down to SETPOINT.

Quick cooling to ambient temperature.

9.4.3 Program memory

RCL = Recall = Recalling the programs stored

CLR = Clear = Clearing the programs stored

Page 46

Melting point B-5409 Appendix

German French

ZEIT : XX:XX DATUM : XX.XX.XX NAME : XXXXX

AUTO PRINT : XXX DRUCKER : XXXXX TASTATUR : XX

RS232 C : XXXX XXX RS232 C : XXXX XXX RS232 C : XXXX XXX

KONTRAST : XXX % PIEPSER : XXX

ZEIT : HH:MM DATUM : DD:MM:YY EINHEIT : °X SPRACHE : DEUTSCH

SW-VER. : VX.XX LETZ. KAL. : XX.XX.XX

HEURE : XX:XX DATE : XX.XX.XX NOM : XXXXX

IMPR. AUTO : XXX IMPRIMANTE : XXXXX CLAVIER : XX

CONTRASTE : XXX % BUZZER : XXX

HEURE : HH:MM DATE : DD:MM:YY UNITE : °X LANGAGE : FRANCAIS

SOFT. VER. : VX.XX DERNIER CAL : X.XX.XX

English

TIME : XX:XX DATE : XX.XX.XX NAME : XXXXX

AUTOPRINT : XXX PRINTER : XXXXX KEYBOARD : XX

CONTRAST : XXX % BUZZER : XXX

TIME : HH:MM DATE : DD:MM:YY UNIT : °X LANGUAGE : ENGLISH

SW-VER. : VX.XX LAST CAL : XX.XX.XX

9.4.4 Configuration menus

Time: 12 (AM/PM) and 24 hours clock. HH = hours, MM = minutes Date: DD = day, MM = month, YY = year User name (max. 8 digits)

Automatic printing: (YES/NO) Printers: - CITIZEN - EPSON (also Canon and Seiko)

- HP - STAR - NONE

Serial interface to PC-Connection. Baud rates: 1200 / 2400 / 4800 / 9600 Baud

Parity Start / Stop Bit

Contrast: 10-90% (basic value 50%) Buzzer: ON/OFF (at start and end of the determination)

Time: 12 (AM/PM) and 24 hours clock. HH = hours, MM = minutes Date: DD = day, MM = month, YY = year Temperature unit: °C or F° eligible

Language: Deutsch (basic setting), English, Français

SW Version: Indication of the software installed Date of last calibration

KALIBRATION INTERVALL : XX MONATE PASSWORT :

CAL: 83°C + X.X + X.X °C

136°C + X.X + X.X °C 237°C + X.X + X.X °C

SPEICHERN KAL :XXX

05.09.95 WIRD ALS

KAL. DATUM GESETZT.

WIRKLICH : XXX

GEMACHT. KAL. PRUEFEN

CALIBRATION INTERVAL : XX MOIS PASSWORD :

CAL: 83°C + X.X + X.X °C

136°C + X.X + X.X °C 237°C + X.X + X.X °C

MEMORISER CAL: XXX

05.09.95 DATE DE CAL. CONFIRMER LA

CALIBRATION: XXX

VERIFIER LA CAL.

CALIBRATION INTERVAL : XX MONTH PASSWORD :

CAL: 83°C + X.X + X.X °C

136°C + X.X + X.X °C 237°C + X.X + X.X °C

STORE CALIBRATION:XXX

05.09.95 WILL BE THE

NEW CALIBRATION DATE.

REALLY STORE : XXX

DONE. VERIFY CAL.

Calibration screen: Calibration interval: 1 to 36 months. Password (for the calibration with calibrating substances; chapter

6.3).

3 calibration substances were recommended. (Calibrating substances: Vanilline, Phenacetine, Coffein) Left column: shows the actual correction Right column: insert the new correction.

Storage the correction factors: (YES/NO)

Checking the calibration with the recommended parameters (see chapter 6.3).

Page 47

Melting point B-540 9 Appendix

9.4.5 Error messages

TEMPERATURE : XXX.X°C

MEMORY EMPTY !

PRESS ENTER

TEMPERATURE : XXX.X°C

NAME EXIST ALREADY

PRESS ENTER

TEMPERATURE : XXX.X°C

NO NAME - NOT STORED!

PRESS ENTER

TEMPERATURE : XXX.X°

MEMORY FULL !

PRESS ENTER

TEMPERATURE : XXX.X°C

NO PRINTER SELECTED

PRESS ENTER

STORED DATA LOST

PLEASE CHECK BATTERY AND SET TIME AND DATE

CALIBRATION INTERVAL

EXCEEDED!

LAST CAL.: XX.XX.XX

Memory is empty - no entries.

Program name exists already. Insert a new one.

Program not stored, no name has been inserted.

Memory full. Clear programs to obtain free memory space.

No printer selected. (Configuration menu)

Check the battery (Lithium cell in the unit) and set new time and date.

Calibration interval exceeded. (Keep pressing MENU-key to go on working)

Last calibration.

CALL SERVICE

ERROR: 001/099

Switch off the unit (main switch). Keep pressing the START-key and switch on the unit.

Call customer service (see chapter 6.4).

9.5 Print-Out

What Input/Change

○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○

Company name Configuration menu 2

Date of determination Configuration menu 2

Method name Main menu 2

Identification of the determination Main menu 2

○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○

Start temperature of the determination Main menu 1

Heating rate selected during the determination Main menu 1

End temperature of the determination Main menu 1

○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○

Determined melting points per capillary

○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○

Signature of the controller

Date of the last calibration

Figure 14: Print-Out

Page 48

Melting point B-5409 Appendix

9.6 Error messages

Fault Cause Remedy

STORED DATA LOST The battery is exhausted Press the Menu key for 5 seconds. PLEASE CHECK BATTERIE Order new battery and have it installed by techn. AND SET TIME AND DATE service. Date and time to be reprogrammed.

CALIBRATION INTERVAL The selected calibration Press the Menu key for 5 seconds. EXCEEDED! time has expired. Calibrate the unit. LAST CAL: XX:XX (See chapter 6, Maintenance)

The Citizen printer does Configuration The SEL key on the printer must not print be actuated whenever he printer is switched on.

CALLSERVICE Damage in the unit Switch off the unit (main switch). ERROR 001/099 Press START-key.

Switch on the unit and keep holding the START-key.

Wrong melting points. Wrong transmission. Always remove capillaries when

switching the unit on.

Calibration Calibrate the unit.

Table 5: Error messages

9.7 Technical data

Dimensions of the unit (width x height x depth) 170 x 210 x 340 mm

Dimensions of packaging (width x height x depth) 340 x 390 x 580 mm

Weight 5.4 kg

Temperature range 25 °C - 400°C

Cooling-down rate 350°C – 50°C max. 10 min

Heating-up speed 50°C – 350° C max. 7 min

Measuring accuracy up to 100°C +/- 0.3°C

Measuring accuracy up to 250°C +/- 0.5°C

Measuring accuracy up to 400°C +/- 0.8°C

Temperature ramps 0.1/0.2/0.5/1.0/2.0/5.0/10.0/20.0°C min.

Mains voltage 100 – 120 V/ 50 or 60 Hz

220 – 230 V/50 or 60 Hz

Power consumption approx. 200 W

Current consumption approx. 2 A (100-120 V) / 1 A (220-230 V)

Data saving with current failure The status of the unit is stored

Restarting is required

Ambient temperature 5 – 40°C

Table 6: Technical data

Page 49

Melting point B-540

9.8 Materials used

Designation Material Material code

Lens holder Grillamid PA 12

Diaphragm Grillamid PA 12

Spacer ring Grillamid PA 12

Collar Arosten PBT

Print holder Arosten PBT

Upper part of heater Ceramic

Heater plate Aluminium ALMGSI 1

Spacer PEEK

Housing Steel sheet ST 12

Axial fan - housing: Aluminium

- propeller: Ultem 254

Lens Glass

Conical handle Duroplast

Foot of the appliance Natural rubber NR

Insulation cover Saproplan

Table 7: Materials

9 Appendix

9.9 FCC requirements (for USA and Canada)

English:

This equipment has been tested and found to comply with the limits for a Class A digital device, pusuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.

This equipment generates, uses and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this equipment in a residential area is like to cause harmful interference in which case the user will be required to correct the interference at his own expense.

Français:

Cet appareil a été testé et s'est avéré conforme aux limites prévues pour les appareils numériques de classe A et à la partie 15 des règlementation FCC à la règlementation des radio-interférences du Canadian Department of communications. Ces limites sont destinées à fournir une protection odéquate contre les interférences nétastes lorsque l'appareil est utilisé dans un environnement commercial.

Cet appareil génère, utilise et peut radier une énergie à fréquence radioélectrique, il est en outre susceprible d'engendrer des interferences avec les communications radio, s'il n'est pas installé et utilisé conformément aux instructions du mode d'emploi. L'utilisation de cet appareil dans les zones résidentielles peut causer des interférences nèfastes, auquel cas l'exploitant sera amené à prendre les dispositions utiles pour polier aux interférences à ses propres frais.

Page 50

9 Appendix

9.10 Declaration of EC conformance

We BÜCHI Labortechnik AG

Postfach, CH-9230 Flawil Switzerland

declare under our sole responsibility that the product:

Melting Point B-540/B-545

to which this declaration relates is in conformity with the following standards:

EN 61010-1:1993 (~ IEC 1010-1, VDE 0411-1)

Safety requirements for electrical equipment for mesurement, control an laboratory use: General requirements

EN 55014:1993 Limits and methods of measurement of radio disturbance characteristics of electrical motoroperated and thermal Rotavapors for household and similar purposes, electric tools and similar electrical apparatus

Melting point B-540

EN 50082-1:1992 Electromagnetic compatibility - Generic immunity standard: Residential, commercial, light industry.

EN 60555-2:1987 (~ IEC 555-2) Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment: Harmonics

EN 60555-3:1987 (~ IEC 555-3) Disturbances in supply systems caused by hosehold Rotavapors and similar electrical equipment: Voltage fluctuations

EN 61000-3-2: 1995/1996 Limits for harmonic current emissions

EN 61000-3-3: 1995 Limitation of voltage fluctuations and flicker

EN 61000-3-2: 1995/1996 Limits for harmonic current emissions

EN 61000-3-3: 1995 Limitation of voltage fluctuations and flicker

following the provisions of EU-Directive: 73/23/EEC (Low voltage) 89/336/EEC (Electromagnnetic compatibility)

Flawil, 13.03.1995

BÜCHI Labortechnik AG Meierseggstrasse 40 9230 Flawil Schweiz

Tel +41 (0)71 394 63 63 Guido Worch Fax +41 (0)71 394 65 65 Qualitymanager buchi@buchi.com www.buchi.com