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
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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
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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
5 Operation
Please note that the unit has been commissioned correctly
according to the instructions in chapter 4 Commissioning.
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Figure 8: Front view, B-540
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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
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Figure 9: Rear view, B-540
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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.
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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.
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
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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