Buchi B-540 User manual

1
Melting point B-540 Contents
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.
Contents
en, Version L (48 pages) Order No.
B-540 Instructions 96626
1Scope of delivery 2
2Safety 4
3Function 6
4Putting into operation 7
5Operation 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
6Maintenance 33
6.3 Calibration of the unit with calibrating substances 33
6.4Customer service 38
7Taking out of operation 39
8Spare parts 40
9Appendix 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
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

2
Melting point B-5401 Scope of delivery
1Scope of delivery
Figure 2: Accessories
2
1
3
5
6
4
7
10
i
8
Figure 1: Complete view of the unit
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:
a1 Oven, upper part of ceramic 34564
b1 Glass panel 34236
c1 Metal cover for heating range 36569
d2 Sample holders of glass 36110
e1 Set of 100 melting point capillaries,each 17808
f1 Set of 10 boiling point tubes, each 19007
g1 Set of 10 boiling point capillaries, each 01762
h2 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
i1 Brief operating instructions
German 96635
English 96636
French 96661
j1 Compaction wire 36721
1 Operating instructions
German 96625
English 96626
French 96627
Italian 96628
Spanish 96629
1 Packaging
Table 2: Enclosed parts

3
Melting point B-540 1 Scope of delivery
Optional accessories:
1Keyboard for simple parameter input
Swiss keyboard arrangement 29599
USA keyboard arrangement 29548
1Printer for documentation
incl. printer cable
230 V, 50/60 Hz 38706
115 V, 60 Hz 38707
1Printer cable 29547
1Melting point capillary (1000 off) 01759
1Boiling point tube (100 off) 19697
1Boiling point capillary (100 off) 19698
1Büchi Certificate for Calibration
at Works G/E/F 97722
Remote control Meltingpoint
(Manual incl. 3 1/2" diskette)
German 33758
English 33758
1Protective cover 36625
1Sample block for prepared
melting point capillaries 36629
Table 3: Optional accessories

4
Melting point B-5402 Safety
2Safety
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.).

5
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.

6
Melting point B-540
3 Function
3Function
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.
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).
Figure 3: Analysis flow chart
Heating phase Readiness Melt. det. phase Cooling phase
Sequence of analysis
Temperature
Time
Gradient
Max-
point
Setpoint

7
Melting point B-540 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 exten-
sion 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.
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.
4Putting into operation
Figure 4: Mounting the glass sample holder

8
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
Figure 5: Mounting the glass panel
Figure 7: Fitting the metal cover 5 Operation
The upper ceramic part of the oven is placed onto the metal
block.
The metal cover is placed over the heating area.

9
Melting point B-540 5 Operation
Please note that the unit has been commissioned correctly
according to the instructions in chapter 4 Commissioning.
5.1 Control, operating and display elements
aMaster switch
bMagnifying glass for viewing the samples
cDisplay for prompt facility
dSTART key to start a determination
eSTOP key to interrupt a determination
fMENU key to change displayed menu windows
gENTER key to change the cursor position vertically when
adjusting parameters on the display
hNEXT key to change the cursor position horizontally
when adjusting parameters on the display
iUP/DOWN keys to change adjustments of the relative
cursor position
jKeys to store measured values during a determination
5Operation
kSample holder for melting point capillaries and boiling point
tubes during determination
lReceptacle for unused melting point capillaries and boiling
point tubes
mReceptacle for used melting point capillaries and
boiling point tubes
nAppliance plug
oPlug for printer connection
pPlug for keyboard connection
qPlug for PC connection
rMain fuse
sPocket for brief instruction manual
Figure 9: Rear view, B-540
12
18
15
Figure 8: Front view, B-540
1
2
3
4
5
6
7
8
10
9
19
16
14
11
17
13

10
Melting point B-5405 Operation
Mainmenu 1 Mainmenu 2 Mainmenu 3
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.
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 pro-
gramwill run down.
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.
PRESS START
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 °C
SP 136 °C
TEMPERATURE 140 °C
GR 2.0 °C
MP 145 °C
TEMPERATURE: 135.6 °C
GR 2.0 °C
MP 145 °C
TEMPERATURE 100 °C
TEMPERATURE 145 °C
TEMPERATURE :25.0°C
SETPOINT :100°C
GRADIENT :2.0°C
MAXPOINT :120°C
TEMPERATURE :25.0°C
NAME :
ID# :

11
Melting point B-540 5 Operation
(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 determi-
nation.
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
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.
TEMPERATURE: 25.0 °C
RECALL CLEAR
STORE PRINT
MSAMP1 SAMP2 SAMP3
AXXX.X XXX.X XXX.X °C
NXXX.X XXX.X XXX.X °C
XXX.X XXX.X XXX.X °C
PRESS START
TEMPERATURE 25.0 °C
SP 136 °C
TEMPERATURE 135.6 °C
GR 2.0 °C
MP 145 °C
TEMPERATURE 140 °C
GR 2.0 °C
MP 145 °C
TEMPERATURE 145 °C
TEMPERATURE 100°C

12
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:
aIs the approximate melting point known ?
if not Rsee 5.7.2
bIs a sample name to be entered ?
if yes Rsee 5.6.1
cWhere is the SETPOINT of the determination located ?
SETPOINT input R5.5.1
dHow fast should the temperature rise (GRADIENT)
between SETPOINT and MAXPOINT ?
GRADIENT input Rsee 5.5.2
eIs the difference between SETPOINT and MAXPOINT to
be more than 15°C ?
Change MAXPOINT Rsee 5.5.3

13
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 trans-
mitted with the ENTER key. By way of example, a SETPOINT
of 180°C is to be adjusted.
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 se-
cond 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.
TEMPERATURE :25.0°C
SETPOINT :100°C
GRADIENT :2.0°C
MAXPOINT :120°C

14
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.
5 Operation
TEMPERATURE :25.0°C
SETPOINT :100°C
GRADIENT :2.0°C
MAXPOINT :120°C

15
Melting point B-540
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.
5 Operation
TEMPERATURE :25.0°C
SETPOINT :100°C
GRADIENT :2.0°C
MAXPOINT :120°C

16
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).
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.
5 Operation
TEMPERATURE :25.0°C
NAME :
ID# :

17
Melting point B-540 5 Operation
5.6.2 Storage of parameters
Press MENU to change to main menu 3.
Press NEXT until the cursor is on the STORE field.
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.
TEMPERATURE: 25.0 °C
RECALL CLEAR
STORE PRINT
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

18
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.
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.
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.
5 Operation
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
TEMPERATURE :25.0°C
SETPOINT :100°C
GRADIENT :2.0°C
MAXPOINT :120°C
TEMPERATURE :25.0°C
MEMORY EMPTY !
PRESS ENTER