Buchi 540 Manual
Buchi 540 Manual
Buchi 540 Manual
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
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
Please read these instructions thoroughly 9 Appendix 41
before using the Melting Point B-540 Unit. 9.1 Connecting a keyboard 41
The instructions should be kept near the unit 9.2 Connection of a printer 41
for general reference. 9.3 Interface configuration 41
9.4 Menu chart 42
Chapter 2 contains important notes on safety 9.5 Print-Out 45
which must be observed if the Melting Point 9.6 Error messages 46
Unit is to be operated safely. 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
1
1 Scope of delivery Melting point B-540
1 Scope of delivery
Description
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
Figure 1: Complete view of the unit i 1 Brief operating instructions
German 96635
English 96636
French 96661
2 8 j 1 Compaction wire 36721
1
1 Operating instructions
3 German 96625
English 96626
4 French 96627
10
Italian 96628
Spanish 96629
1 Packaging
7 Table 2: Enclosed parts
i
6 5
Figure 2: Accessories
2
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
3
2 Safety Melting point B-540
2 Safety
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.
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:
4
Melting point B-540 2 Safety
2.7 Modifications
5
3 Function Melting point B-540
3 Function
Operating principle
Sequence of analysis
The Melting Point Unit B-540 provides the melting point in
Heating phase Readiness Melt. det. phase Cooling phase agreement with pharmacopoeia methodologies and the boiling
Temperature
6
Melting point B-540 4 Putting into operation
7
4 Putting into operation Melting point B-540
The glass panel is placed into the metal heating block, taking
care to touch the panel only laterally.
The upper ceramic part of the oven is placed onto the metal
block.
8
Melting point B-540 5 Operation
5 Operation
a Master switch
b Magnifying glass for viewing the samples
c Display for prompt facility
3 d START key to start a determination
4 6 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
8 7 adjusting parameters on the display
h NEXT key to change the cursor position horizontally
9
5 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
10 1
19
14 15
18 16
17
9
5 Operation Melting point B-540
TEMPERATURE 100 °C
SETPOINT: Temperature
• at which the sample capillaries are inserted
into the unit;
• as from which the adjusted temperature pro-
gramwill run down.
10
Melting point B-540 5 Operation
5.3.3 Graphics
TEMPERATURE 135.6 °C The unit has reached the preselected SETPOINT and waits
GR 2.0 °C
MP 145 °C
for the temperature program to be started.
PRESS START
TEMPERATURE 140 °C With the preselected GRADIENT, the unit heats up to the
GR 2.0 °C
MP 145 °C maximum point of the temperature program (MAXPOINT).
TEMPERATURE 145 °C The unit has reached the highest point of the temperature
program (MAXPOINT) and cools down to the previously
selected SETPOINT.
11
5 Operation Melting point B-540
12
Melting point B-540 5 Operation
TEMPERATURE : 25.0°C
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
13
5 Operation Melting point B-540
TEMPERATURE : 25.0°C
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
14
Melting point B-540 5 Operation
TEMPERATURE : 25.0°C
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
15
5 Operation Melting point B-540
TEMPERATURE : 25.0°C
NAME :
ID# :
Actuate ENTER until the cursor is on the NAME field for entering
the method name.
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.
16
Melting point B-540 5 Operation
TEMPERATURE: 25.0 °C
RECALL CLEAR
STORE PRINT
TEMPERATURE : 25.0°C
Possible error messages.
MEMORY FULL !
PRESS ENTER
TEMPERATURE : 25.0°C
TEMPERATURE : 25.0°C
17
5 Operation Melting point B-540
TEMPERATURE : 25.0°C Stored programs can only be recalled from main menu 3.
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
Possible error message.
MEMORY EMPTY !
PRESS ENTER
18
Melting point B-540 5 Operation
TEMPERATURE : 25.0°C
Stored programs can only be cancelled from the main menu.
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
TEMPERATURE : 25.0 °C
RCL: XXXXXX q
XXXXXX
XXXXXX Q
TEMPERATURE : 25.0°C
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
19
5 Operation Melting point B-540
..
20
Melting point B-540 5 Operation
TEMPERATURE : 25.0°C
The melting point determination may be started from any main
SETPOINT ; 100°C menu. The SETPOINT, GRADIENT and MAXPOINT must first
GRADIENT : 2.0°C
MAXPOINT : 120°C have been defined as described in 5.5.1–5.5.4.
TEMPERATURE 25.0 °C
SP 136 °C
TEMPERATURE : 135.6 °C The user is informed acoustically when the SETPOINT has
GR 2.0 °C
been reached. The graphic will change at the same time.
MP 145 °C Samples are introduced into the sample holder.
PRESS START
TEMPERATURE : 140 °C The samples are viewed through the magnifying glass as
GR 2.0 °C required. The melting point is retained by pressing SAMPLE
MP 145 °C keys 1/2/3. Every pressing of the SAMPLE keys is ack
nowledged with a beep and confirmed with an indication on
the screen.
21
5 Operation Melting point B-540
22
Melting point B-540 5 Operation
23
5 Operation Melting point B-540
TEMPERATURE : 25.0°C
SETPOINT : 100°C
GRADIENT : 2.0°C
MAXPOINT : 120°C
TEMPERATURE 25.0 °C
SP 136 °C
TEMPERATURE : 135.6 °C The user is informed acoustically that the SETPOINT has been
GR 2.0 °C reached. At the same time, the graphic will change. The samples
MP 145 °C are introduced into the sample holder.
PRESS START
TEMPERATURE : 135.6 °C
GR 2.0 °C
MP 145 °C
24
Melting point B-540 5 Operation
25
5 Operation Melting point B-540
26
Melting point B-540 5 Operation
27
5 Operation Melting point B-540
TIME : XX:XX Menu window for setting data which are to appear on the
DATE : XX.XX.XX
NAME : XXXXX printout.
Time: Time
Date: Date
Name: Company name
AUTOPRINT : XXX
Menu window for adjusting the displays to be printed out.
PRINTER : XXXXX Autoprint: Automatic printing after every determination
KEYBOARD : XX
yes/no
Printer: Selection of the printer to be used
RS232 C : XXXX XXX Menu window for adjusting the serial interface to the PC
connection.
28
Melting point B-540 5 Operation
TIME : XX:XX
DATE : XX.XX.XX
NAME : XXXXX
29
5 Operation Melting point B-540
AUTOPRINT : XXX
GRAPHIC : XXX
PRINTER : XXXXX
30
Melting point B-540 5 Operation
31
5 Operation Melting point B-540
Press the MENU key for three seconds to return to the range
of submenus.
CONTRAST : XXX %
Menu window to unit adjustments
BUZZER : XXX CONTRAST: LCD display adjustments
AUTOSTART : XXX
BUZZER: Beep on/off
By the pressing the ENTER key, the user return to the buzzer
field.
Press the MENU key again for three seconds to return to the
main menu.
32
Melting point B-540 5 Maintenance
6 Maintenance
6.1 Cleaning
6.2 Upkeep
The upkeep of the unit is mainly limited to:
• a periodical calibration of the transmission
Temperature
Temperature
Displayed by Correction by user
apparatus
following
calibration
33
6 Maintenance Melting point B-540
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
Vanilline <0.3°C
Phenacetine <0.5°C
Caffeine <0.5°C
34
Melting point B-540 6 Maintenance
CALIBRATION
INTERVAL : XX MONTH
PASSWORD :
35
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 Now the pertinent corrections can be entered for the three
136°C + X.X + X.X °C
237°C + X.X + X.X °C
types of calibration substances. The left column indicates the
last correction, the right column is used to enter the new
STORE CALIBRATION:XXX
corrective value.
05.09.95 WILL BE THE Checking of the calibration with the same parameters under
NEW CALIBRATION DATE. the recommendation (see above).
REALLY STORE : XXX
DONE. VERIFY CAL.
36
Melting point B-540 6 Maintenance
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.
* The exact values are specified on the packing as well as on the certificate from the manufacturer of the substance (Fluka AG).
37
6 Maintenance Melting point B-540
38
Melting point B-540 7 Taking out of operation
7.1 Storage/Transport
7.2 Disposal
39
8 Spare parts Melting point B-540
8 Spare parts
40
Melting point B-540 9 Appendix
9 Appendix
Ü
sample names and sample identifications.
EN
M
3
2
1
IG
E
E
E
PL
NF
PL
PL
T
Ü
OP
AR
EN
M
CO
M
M
SA
ST
ST
SA
SA
41
9 Appendix Melting point B-540
Configurations-
..... menus .....
42
Melting point B-540 9 Appendix
TEMPERATURE 25.0 °C
Quick heating (approx. 70°C/min.) to SETPOINT.
SP 136 °C
SP = SETPOINT
TEMPERATURE : 135.6 °C
SETPOINT reached. Continue with the START-key.
GR 2.0 °C GR = GRADIENT
MP 145 °C
PRESS START
MP = MAXPOINT
43
9 Appendix Melting point B-540
ZEIT : XX:XX HEURE : XX:XX TIME : XX:XX Time: 12 (AM/PM) and 24 hours clock. HH = hours, MM = minutes
DATUM : XX.XX.XX DATE : XX.XX.XX DATE : XX.XX.XX Date: DD = day, MM = month, YY = year
NAME : XXXXX NOM : XXXXX NAME : XXXXX
User name (max. 8 digits)
AUTO PRINT : XXX IMPR. AUTO : XXX AUTOPRINT : XXX Automatic printing: (YES/NO)
DRUCKER : XXXXX IMPRIMANTE : XXXXX PRINTER : XXXXX Printers: - CITIZEN - EPSON (also Canon and Seiko)
TASTATUR : XX CLAVIER : XX KEYBOARD : XX - HP - STAR - NONE
ZEIT : HH:MM HEURE : HH:MM TIME : HH:MM Time: 12 (AM/PM) and 24 hours clock. HH = hours, MM = minutes
DATUM : DD:MM:YY DATE : DD:MM:YY DATE : DD:MM:YY Date: DD = day, MM = month, YY = year
EINHEIT : °X UNITE : °X UNIT : °X
SPRACHE : DEUTSCH LANGAGE : FRANCAIS LANGUAGE : ENGLISH Temperature unit: °C or F° eligible
Language: Deutsch (basic setting), English, Français
SW-VER. : VX.XX SOFT. VER. : VX.XX SW-VER. : VX.XX SW Version: Indication of the software installed
LETZ. KAL. : XX.XX.XX DERNIER CAL : X.XX.XX LAST CAL : XX.XX.XX Date of last calibration
CAL: 83°C + X.X + X.X °C CAL: 83°C + X.X + X.X °C CAL: 83°C + X.X + X.X °C 3 calibration substances were recommended.
136°C + X.X + X.X °C 136°C + X.X + X.X °C 136°C + X.X + X.X °C (Calibrating substances: Vanilline, Phenacetine, Coffein)
237°C + X.X + X.X °C 237°C + X.X + X.X °C 237°C + X.X + X.X °C
Left column: shows the actual correction
SPEICHERN KAL :XXX MEMORISER CAL: XXX STORE CALIBRATION:XXX Right column: insert the new correction.
05.09.95 WIRD ALS 05.09.95 DATE DE CAL. 05.09.95 WILL BE THE Storage the correction factors: (YES/NO)
KAL. DATUM GESETZT. CONFIRMER LA NEW CALIBRATION DATE.
WIRKLICH : XXX CALIBRATION: XXX REALLY STORE : XXX
GEMACHT. KAL. PRUEFEN VERIFIER LA CAL. DONE. VERIFY CAL.
Checking the calibration with the recommended parameters
(see chapter 6.3).
44
Melting point B-540 9 Appendix
MEMORY EMPTY !
PRESS ENTER
TEMPERATURE : XXX.X° Memory full. Clear programs to obtain free memory space.
MEMORY FULL !
PRESS ENTER
TEMPERATURE : XXX.X°C
No printer selected. (Configuration menu)
NO PRINTER SELECTED
PRESS ENTER
9.5 Print-Out
What Input/Change
○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○
○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○
45
9 Appendix Melting point B-540
46
Melting point B-540 9 Appendix
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.
47
9 Appendix Melting point B-540
We BÜCHI Labortechnik AG
Postfach, CH-9230 Flawil
Switzerland
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
Flawil, 13.03.1995
BÜCHI Labortechnik AG
Meierseggstrasse 40
9230 Flawil
Schweiz
48