Operation Manual
Melting Point
M�560
093251
en
Table of contents
Table of contents
1 About this manual . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5
1.1 Reference documents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .5
1.2 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2 Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6
2.1 User qualification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.2 Proper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3 Improper use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.4 Warning notices used in this manual . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5 Product safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7
2.5.1 Instrument-related hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.5.2 Other hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .7
2.5.3 Safety measures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
2.5.4 Safety elements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .8
2.6 General safety rules . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
3 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.1.1 Standard accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.1.2 Optional accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2 Technical data overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
4.1 Melting Point . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
4.2 Boiling Point. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
4.3 Controls and connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
5.2 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
5.2.1 Unpacking and installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
5.2.2 Power connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
5.2.3 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Read this manual carefully before installing and running your system; take particular note of the safety
precautions in section 2. Keep the manual in the immediate vicinity of the instrument, so that it can be
consulted at any time.
No technical modifications may be made to the instrument without the prior written agreement of
BUCHI. Unauthorized modifications may affect system safety or result in accidents. This manual is
copyrighted. Information from it may not be reproduced, distributed, or used for competitive purposes,
nor made available to third parties. The manufacture of any component with the aid of this manual
without prior written agreement is also prohibited.
The English manual is the original language version and serves as basis for all translations
into other languages. Other language versions can be downloaded at www.buchi.com.
3 Melting Point M-560 Operation Manual, Version D
Table of contents
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
6.1 Basic operating principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
6.1.1 Display during idle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
6.1.2 Display during a process or in menus . . . . . . . . . . . . . . . . . . . . . . . . . 20
6.1.3 Entering text. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
6.1.4 Using the external keyboard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
6.2 Melting point determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.2.1 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
6.2.2 Determination without pre-registered melting point method . . . . . . . . . . . . . . 23
6.2.3 Creating a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.2.4 Using and handling methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.2.5 Adjusting parameters during a determination . . . . . . . . . . . . . . . . . . . . . 27
6.2.6 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
6.3 Boiling point . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
6.3.1 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
6.3.2 Determination without pre-registered boiling point method . . . . . . . . . . . . . . 28
6.3.3 Creating a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
6.3.4 Adjusting parameters during a determination . . . . . . . . . . . . . . . . . . . . . 30
6.3.5 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
6.4 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.4.1 Calibration principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.4.2 Calibration procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.4.3 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
6.4.4 Verification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.5 Settings, SysInfo, Test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
6.5.1 Test protocol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
6.5.2 SysInfo protocol. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
7.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
7.2 Glass window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
7.3 Upkeep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
7.4 Cleaning the heating block . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
8.1 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
8.1.1 Setting the printer baud rate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
8.2 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
9 Shutdown, storage, transport, and disposal . . . . . . . . . . . . . . . . . . . . . . . 44
9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
9.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 46
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
4 Melting Point M-560 Operation Manual, Version D
1 About this manual
This manual describes the Melting Point M-560 and provides all the information required for its safe
operation and to maintain it in good working order.
It is addressed in particular to laboratory personnel and operators.
NOTE
The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in section 2.
1.1 Reference documents
For more information regarding melting point, refer to the corresponding literature:
• The Laboratory Assistant 94187
• Melting Point M-560, Operating Manual numbers 93251–93255
• Melting Point M-565, Operating Manual numbers 93256–93260
1 About this manual
1.2 Abbreviations
Chemicals:
PTFE Polytetrafluoroethylene
PP Polypropylene
PE Polyethylene
EPDM Ethylene-propylene-diene rubber
POM Polyoxymethylene
PUR Polyurethane
Miscellaneous:
mp Melting point
bp Boiling point
pharm. Pharmacopoeia
therm. Thermodynamic
L Sample left
C Sample center
R Sample right
5 Melting Point M-560 Operation Manual, Version D
2 Safety
This section highlights the safety concept of the Melting Point M-560 and contains general rules of
behavior and warnings about hazards concerning the use of the product.
The safety of users and personnel can only be ensured if these safety instructions and the safetyrelated warnings in the individual sections are strictly observed and followed. Therefore the manual
must always be available to all persons performing the tasks described herein.
2.1 User qualification
The instrument may be used only by laboratory personnel or other persons whose training or professional experience give them an overview of the dangers which can develop when operating the
instrument.
Personnel without this training or persons who are currently being trained require careful supervision.
This Operation Manual serves as a basis for training.
2 Safety
2.2 Proper use
The instrument has been designed and built for laboratory use only. It is intended to be used to determine melting and boiling points and melting ranges at ambient temperatures up to 400 °C.
2.3 Improper use
Applications beyond those described above are improper. Furthermore, applications which do not
comply with the technical data are also considered improper. The operator bears the sole risk for any
damages caused by such improper use.
The following applications in particular are expressly forbidden:
• Use in rooms requiring explosion-proof equipment.
• Extraction of samples which may explode or ignite as the result of a blow, friction, heat, or spark
(e.g. explosives).
6 Melting Point M-560 Operation Manual, Version D
2.4 Warning notices used in this manual
WARNING
Generally, the triangular warning symbol indicates the possibility of personal injury or even loss of life
if the instructions are not followed.
WARNING
Hot surface.
WARNING
Electrical hazard.
WARNING
Biohazard.
ATTENTION
The “read this” symbol for ATTENTION indicates that equipment damage, malfunctions, or incorrect
processes may result if the instructions are not followed.
2 Safety
NOTE
Useful tips to facilitate operation of the instrument.
2.5 Product safety
The Melting Point M-560 is designed and built in accordance with current state-of-the-art technology.
However, risks to users, property, and the environment can arise when the instrument is used carelessly or improperly.
The manufacturer has determined residual dangers emanating from the instrument
• if the instrument is operated by insufficiently trained personnel.
• if the instrument is not operated properly.
Appropriate warnings in this manual serve to alert the user to these residual dangers.
2.5.1 Instrument-related hazards
Pay attention to the following safety notices:
WARNING
Potentially hot surfaces during operation, especially the heating oven (up to 400 °C).
• Always be aware of the danger of being burned.
2.5.2 Other hazards
WARNING
Certain solvents within or in the vicinity of the Melting Point M-560 can form peroxides and/or are
highly inflammable.
• Always be aware of the explosion risk when working with hazardous substances or with
substances of unknown composition.
• Always use the instrument in an adequately ventilated work area.
7 Melting Point M-560 Operation Manual, Version D
2.5.3 Safety measures
Always wear personal protective equipment such as protective goggles and protective clothing, when
working with the instrument.
2.5.4 Safety elements
Anti-seismic tie-down
• The instrument is equipped with a fixture to tie it down in areas at risk of an earthquake (see
bottom side of the instrument).
2.6 General safety rules
2 Safety
Responsibility of the operator
The head of laboratory is responsible for training the lab personnel.
The operator shall inform the manufacturer without delay of any safety-related incidents that occur
during the operation of the instrument. Legal regulations, such as local, state, and federal laws
applying to the instrument, must be strictly followed.
Duty of maintenance and care
The operator is responsible for ensuring that the instrument is operated only in a proper manner and
that maintenance, service, and repairs are performed with care, on schedule, and by authorized
personnel only.
Spare parts to be used
Use only recommended consumables and spare parts for maintenance in order to ensure continued
optimum system performance and reliability. Modifications to the spare parts used are allowed only
with the prior written permission of the manufacturer.
Modifications
Modifications to the instrument are permitted only after prior consultation with and written approval
from the manufacturer. Modifications and upgrades should be carried out only by an authorized
BUCHI technical engineer. The manufacturer reserves the right to decline any claim resulting from
unauthorized modifications.
8 Melting Point M-560 Operation Manual, Version D
3 Technical data
This section introduces the reader to the Melting Point M-560 and its main components. It contains
technical data, requirements and performance data.
3.1 Scope of delivery
Check the scope of delivery according to the order number.
NOTE
For detailed information on the listed products, see www.buchi.com or contact your local dealer.
3.1.1 Standard accessories
3 Technical data
Table 3-1: Standard accessories
Product Order number
Melting Point M-560 051999
Calibration set M-560/M-565
(4 substances; 4-nitrotoluene, diphenyl
acetic acid, caffeine, potassium nitrate)
11055018
Melting point capillaries, 100 units 017808
9 Melting Point M-560 Operation Manual, Version D
3 Technical data
Table 3-1: Standard accessories (cont.)
Product Order number
Sample holder 11055014
Cleaning tool 051978
A) Boiling point tubes, 10 units 019697
B
B
B) Boiling point capillaries, 10 units 051850
A
A
Compaction wire 036721
Operation Manual:
English 93251
German 93252
French 93253
Italian 93254
Spanish 93255
10 Melting Point M-560 Operation Manual, Version D
3.1.2 Optional accessories
3 Technical data
Table 3-2: Optional accessories
Product Order number
Sample Loader M-569 051997
Verification set M-560/M-565
11055019
(3 substances; benzil, p-anisic acid,
phenolphthalein)
Melting point capillaries, 1000 units 001759
Mortar and pestle, agate 041867
Compact keyboard German (CH) 029509
Compact keyboard English (USA) 029508
Serial dot matrix printer (including ribbon,
11055438
paper roll, and cables)
11 Melting Point M-560 Operation Manual, Version D
3 Technical data
Table 3-2: Optional accessories (cont.)
Product Order number
Ribbon for printer 044306
Paper roll for printer 038684
A) Boiling point tubes, 100 units 019007
B) Boiling point capillaries, 100 units 051890
3.2 Technical data overview
Table 3-4: Technical data of the Melting Point M-560
Manual melting point determination √
Manual boiling point determination √
Automatic melting point determination –
Automatic boiling point determination –
Homogeneous sample loading –
Positions for melting capillaries 3
Positions for boiling capillaries 1
Precision magnifying lens √
Magnification of lens 2.5×
Display Colour, TFT, 320×240, 3.5˝
Determination temperature range Ambient +10 °C to 400 °C
Temperature resolution 0.1 °C
Accuracy of melting point at 0.5 °C/min
up to 250 °C ±0.3 °C
Protective cover 051935
Melting Point M-560
12 Melting Point M-560 Operation Manual, Version D
3 Technical data
Table 3-4: Technical data of the Melting Point M-560
Melting Point M-560
250 °C to 400 °C ±0.3 °C to ±0.5 °C
Repeatability of melting point at 0.5 °C/min ±0.1 °C
Accuracy of boiling point at 1.0 °C/min up to 400 °C ±0.5 °C
Repeatability of boiling point at 1.0 °C/min ±0.3 °C
Temperature gradients, °C/min 0.1, 0.2, 0.5, 1, 2, 3, 5, 10, 20
Heat-up time (50 °C–350 °C) at 25 °C ~4 min
Cool-down time (350 °C–50 °C) at 25 °C ~13 min
Electrical supply 100–240 V (±10 %), 50–60 Hz
Power consumption 150 W
Contact termination L, N, PE
Approval CE, CSA, UL
Dimensions (W×H×D), mm 190×200×370
Weight, kg 4.5
Environmental conditions For indoor use only
Temperature 5–40 °C
Altitude up to 2000 m a.s.l.
Humidity Maximum relative humidity 80 % for temperatures up to
31 °C, decreasing linearly to 50 % relative humidity at 40 °C
Overvoltage category II
Degree of protection IP20
Pollution degree 2
Storable methods for melting point 50
Storable methods for boiling point 50
Compliant with Pharmacopeia methods PH. EUR. 6.1.2.2.60, USP XXI 741 and JP
NOTE
Temperature measuring accuracy refers to pharmacopoeia melting point.
3.3 Materials used
Table 3-5: Materials used
Component Material designation
Print holder PA
Heating block Aluminium
Lenses Glass
Axial fan Aluminium
Housing PU, Stainless Steel, Glass
Cover POM, Ceramic, Aluminium, Stainless Steel
13 Melting Point M-560 Operation Manual, Version D
4 Description of function
This section explains the basic principle of the Melting Point M-560 and provides a functional description of the assemblies.
4.1 Melting Point
The Melting Point M-560 is an instrument for manual (visual) determination of melting point, melting
range, and boiling point at ambient temperatures +10 °C up to 400 °C. The melting point of three
samples can be determined at the same time. The boiling point can be determined for one sample.
Samples have to be observed through the lens.
The melting point capillary sits in a hollow of the metal block, which is heated electrically and
controlled by a temperature sensor. The heating block is capable of being maintained accurately at a
pre-defined temperature by the heating element, and of being heated at a defined rate.
4 Description of function
4.2 Boiling Point
The boiling point is determined by the “Siwoloboff” method.
The Melting Point M-560 can be used to determine the boiling point of a small amount of liquid. The
heating block has one insert available for boiling point tubes (outside left). The moment of boiling is
determined visually.
The process for boiling point determination is analogous to that for determining a melting point:
• The start temperature is set 5 to 10 °C lower than the expected boiling point.
• The sample is put into the heating block as soon as the start temperature is reached.
• A delay time allows the equilibrium between oven temperature and sample temperature. During
this delay time some air bubbles escape from the boiling point capillary.
• Starting from the start temperature, the sample is heated at a temperature gradient of 1 °C/min.
• As the temperature rises, bubbles of gas rise slowly and regularly from the immersed end of the
boiling point capillary.
• The boiling point of the liquid has been reached when the flow of steam bubbles reaches a
frequency of 0.6 Hz [Hertz].
14 Melting Point M-560 Operation Manual, Version D
4.3 Controls and connections
f
4 Description of function
a Power switch; turns the instrument on/off
b Start; starts process
c Stop; stops process, starts/stops ventilation,
returns to idle screen
d 3 Select and Set buttons
e Rotary knob for navigation through the menu
and for select characters
f Display
b
c
Fig. 4.1: Front view
a
e
d
f
e
d
b
c
a
a Mains plug
b PS/2 connection for keyboard
c RS 232 connection for serial printer
d USB connection: required for service
e Housing cooling fan
f Heating block cooling fan
USB
PS/2
RS232
Fig. 4.2: Rear view
15 Melting Point M-560 Operation Manual, Version D
5 Putting into operation
This section describes the installation of the Melting Point M-560 and gives instructions for initial startup.
NOTE
Inspect the instrument for damage during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company, or transport company. Keep the original
packaging for future transport.
5.1 Installation site
Place the instrument on a stable, horizontal surface adequate for the maximum product dimensions.
It is advisable to place the instrument in a fume hood due to the fact that it will be used to measure
chemical substances. For safety reasons and to ensure sufficient cooling in the electronic compartment, the unit must be placed at least 30 cm away from rear walls or other objects. No containers,
chemicals, or other appliances should be placed behind the unit.
5 Putting into operation
General hazards arise from:
• Mixtures of unknown composition or contaminations
• Combustible gases or solvent vapor in the immediate vicinity of the unit
• Damaged glass components
• Insufficient distance from back of the unit to the wall
• Burning by touching hot parts of the heater
5.2 Commissioning
5.2.1 Unpacking and installation
• Unpack the instrument and place it on a table. Remove the packing, and make sure that the
following parts are installed:
16 Melting Point M-560 Operation Manual, Version D
5 Putting into operation
• Glass window • Glass window with glass holder
• Install the glass window with glass holder on
the front side of the heating block.
• Press the glass holder down.
Accessories
• Place the melting point capillaries in the hole of the housing. The second hole is a reservoir for
used capillaries.
• Install the cover.
17 Melting Point M-560 Operation Manual, Version D
5.2.2 Power connection
ATTENTION
Make sure that the voltage of the socket corresponds to the voltage given on the type plate of the
instrument. Ensure that the instrument is grounded. External connections and extension cables must
be provided with a grounded conductor lead (3-pole couplings, cable, or plug equipment) as the
mains lead has a molded plug to avoid risks due to inadvertently defective wiring. Make sure that no
electric sparks form in the instrument or its surroundings as they may damage the instrument. Make
sure that the mains connector is freely accessible at any time.
5.2.3 Calibration
NOTE
Before use it is recommended to calibrate the apparatus. Use supplied calibration substances only.
Calibration is carried out in accordance with section 6.4 of these operating instructions.
5 Putting into operation
18 Melting Point M-560 Operation Manual, Version D
6 Operation
This section explains the operating elements and possible operating modes. It gives instructions on
how to operate the Melting Point M-560 properly and safely.
ATTENTION
Before use it is recommended to calibrate the apparatus. Use supplied calibration substances only.
The calibration mode is described in section [6.4 Calibration].
6.1 Basic operating principles
WARNING
The heating oven can reach temperatures of up to 400 °C.
6 Operation
6.1.1 Display during idle
After switching on, the display shows the menu for melting point.
a
b
c
e
d
a Function category with main setting
parameters
b Advice
c Parameters used after pressing START
d Shows current heating block temperature
and time
e Functions selectable by the keys below
19 Melting Point M-560 Operation Manual, Version D
6 Operation
Different menus can be accessed by turning the rotary knob. Each menu has its own symbol. These
idle screens are the starting points for all actions. The corresponding symbol is displayed during all
processes.
Melting Point Boiling Point
Calibration Tools
6.1.2 Display during a process or in menus
c
a
b
a Shows where you are and gives advice and
instructions.
b Working area shows:
• items to select
• samples during measurement
• specific information in connection with
the current menu
c Functions selectable by the keys below.
20 Melting Point M-560 Operation Manual, Version D
6 Operation
Screen during melting point
determination
6.1.3 Entering text
Settings menu Result indication
(numeric result)
Text can be entered by using the rotary knob,
an external keyboard.
Rotary knob:
• Turn the rotary knob to select a character
and press Enter. Press Save after entering all
characters.
6.1.4 Using the external keyboard
NOTE
The instrument can be operated using an external keyboard.
For the softkeys, the following keys of the external keyboard are assigned:
• ENTER = right softkey
• Alt = center softkey
• Esc = left softkey
• In the method menu: To navigate quickly to a method name press the initial letter.
21 Melting Point M-560 Operation Manual, Version D
6.2 Melting point determination
NOTE
For exact melting point determination, use original capillaries from BUCHI only. If other capillaries are
used, the results may be inaccurate. Use the following items:
Fig. 6.1: Melting point capillaries
6 Operation
Product Order number
Melting point capillaries, 100 units 017808
Melting point capillaries, 1000 units 001759
6.2.1 Sample preparation
NOTE
Use only capillaries from BUCHI. They are precise and adequate for this kind of operation. Other
capillaries have other dimensions and wall thicknesses. Using others may result in results that are
incorrect.
Each sample has to be prepared.
The following methods to compact the samples are recommended:
• Using the Sample Loader M-569
• Knocking the capillaries on a hard surface.
NOTE
Sample preparation by letting the capillaries fall through a tube is not advised, because cross
contamination may occur.
Preparation of the samples:
• The samples being investigated must be fully dry, homogenous and in powdered form. Moist
samples must be dried first (the pharmacopoeias prescribe that the substance needs to be dried
in a vacuum for 24 hours over silica gel R). Coarse crystalline samples and non-homogeneous
samples are finely ground in a mortar.
• To fill the capillary tubes with the sample, the open ends of the tubes are pressed into the
substance. The substance is moved to the bottom of the tubes by repeatedly tapping the tubes
against a hard base.
• Enough substance must be filled into the glass capillary to form a compact column 4–6 mm in
height. (A height of 4–5 mm is recommended for precision measurements.) To ensure comparable results, it is important to fill all three capillary tubes to the same height and to compact the
substance well in the tubes using the Sample Loader M-569.
22 Melting Point M-560 Operation Manual, Version D
6.2.2 Determination without pre-registered melting point method
• Choose the menu for melting point determination.
• Make sure that all samples are removed.
• Press START to begin the determination process immediately with the last parameters used. They
always remain saved in the instrument and are indicated in the green field in the lower part of the
screen.
NOTE
If the current parameters do not meet your requirements, press Edit and set start temperature, stop
temperature, and temperature gradient.
a Start temperature
b Stop temperature
c Temperature gradient
d Edit
• To adjust the desired melting parameters,
a b c
press Edit.
6 Operation
d
• Chose start temperature
with the rotary knob, and
press Next.
NOTE
Insert samples only when the start temperature is reached (as soon as prompted).
• Chose stop temperature
with the rotary knob, and
press Next.
• Chose temperature
gradient with the rotary
knob, and press Save.
23 Melting Point M-560 Operation Manual, Version D
6 Operation
• Press START to begin the
determination, and follow
the on-screen instructions.
• To register additional
temperature stamps, manually press the SET button
for the related sample. Each
button can be pressed
three times. Registered
temperature stamps are
displayed in green.
• The instrument requests a
sample ID during preheating
(for details on entering text
see 6.1.3). This request can
be switched off by changing
the setting “Sample ID
request” (see 6.5).
• Insert samples and press
START to begin the determination.
24 Melting Point M-560 Operation Manual, Version D
6 Operation
• To run through the result,
turn the rotary knob up and
down.
• Press End or STOP to
return to the idle screen.
NOTE
The last result is stored in the device until a new measurement is started or the instrument is
switched off.
• After turning back to idle,
the last result can be
checked again by pressing
Result.
• Press START to measure
again with the identical
measuring parameters.
• The result is printed out
automatically if a printer is
connected.
25 Melting Point M-560 Operation Manual, Version D
6.2.3 Creating a method
Instead of entering and using the parameters directly from the idle screen, it is also possible to store
parameter sets as methods.
6 Operation
• To enter the method menu,
press Method.
• Adjust a parameter and
press Next. Then Save.
6.2.4 Using and handling methods
• To create a new method,
press Options New
then OK.
• Enter a method name. To
finish press Save.
• Turn the rotary knob to
select a method.
• Press START to start the
determination.
• Use Edit to adjust method
parameters.
26 Melting Point M-560 Operation Manual, Version D
• Press the Options key to
access further functions:
• New: Creates a new
method.
• Delete: Deletes the
method.
• Rename: Changes the
method name.
6.2.5 Adjusting parameters during a determination
NOTE
Measuring parameters can be modified during preheating or a determination. This function is
possible only if enabled by the setting “Param. adj. during meas.” (see 6.5).
6 Operation
a
6.2.6 Printout
NOTE
The result is printed out if a printer is connected.
• Turn the rotary knob to
display the current parameter set.
• Adjust the parameters by
pressing Edit. Adjusting the
parameters does not affect
the saved method.
a
b
c
• If the temperature gradient
is changed during a measurement, the result shows
CHANGED (a) for the
temperature gradient.
Printout
a Instrument type
b Determination parameters
c Manual pressed results
d General information
e Signature of person making the
determination
d
e
27 Melting Point M-560 Operation Manual, Version D
6.3 Boiling point
NOTE
For exact boiling point determination, use boiling point tubes and capillaries from BUCHI only. If other
glass parts are used, incorrect or no results may be obtained. Use the following items:
B
Fig. 6.2: Boiling point tube and capillary
6 Operation
Product Order number
B
A
A) Boiling point tubes, 10 units 019697
A) Boiling point tubes, 100 units 019007
B) Boiling point capillaries, 10 units 051850
B) Boiling point capillaries, 100 units 051890
A
6.3.1 Sample preparation
In preparation, the boiling point tubes are filled with 5 to 10 mm of liquid sample. We recommend
using a syringe for simple filling. Insert a boiling point capillary into the boiling point tube with its open/
thick end down. Put the sample immediately into the heating block.
6.3.2 Determination without pre-registered boiling point method
• Choose the menu for boiling point determination.
• Make sure that all samples are removed.
• Press START to begin the determination process immediately with the last parameters used. They
are always saved in the instrument and are indicated in the green field in the lower part of the
screen.
If the current parameters do not meet your needs, press Edit and set the start temperature, stop
temperature, and temperature gradient.
a Start temperature
b Stop temperature
c Temperature gradient
d Edit
• To adjust the boiling parameters, press Edit.
a b c
d
28 Melting Point M-560 Operation Manual, Version D
6 Operation
• Use the rotary knob to
choose the start tempera-
ture and press Next.
NOTE
Insert sample only when the instrument has reached the start temperature.
• Press START to begin the
determination and follow
the instructions on the
screen.
• Use the rotary knob to
choose the stop tempera-
ture and press Next.
• The instrument requests a
sample ID during preheating
(for details on entering text
see 6.1.3). This request can
be switched off by changing
the setting “Sample ID
request” (see 6.5).
• Use the rotary knob to
chose the temperature
gradient and press Save.
• Bar P: Enter the current
barometric pressure.
• This request can be
switched off by changing
the setting “Barometric
pressure request” (see 6.5).
• Insert sample and press
START to begin the determination.
29 Melting Point M-560 Operation Manual, Version D
6 Operation
• Delay: to ensure equilibrium
between oven temperature
and sample temperature.
During this delay time some
air bubbles escape from the
boiling point capillary. This
request can be changed in
the setting “Boiling sample
conditioning” (see 6.5). Bubble
frequency is an indicator.
When frequency of air bubbles
coming out of the capillary is
equal the indicator press Set.
6.3.3 Creating a method
NOTE
The process of creating a boiling point method is identical that used to create a melting point method
(see 6.2.3).
6.3.4 Adjusting parameters during a determination
• To run through the result,
turn the rotary knob up and
down.
• Press End or STOP to
return to the idle screen.
• Press START to measure
again with the identical
measuring parameters.
During preheating or a determination, measuring parameters can be modified. This function is possible
only if enabled by the setting “Param. adj. during meas.” (see 6.5).
a
• Turning the rotary knob
displays the current parameter set.
• Adjust the parameters by
pressing Edit. Adjusting the
parameters does not affect
the saved method.
30 Melting Point M-560 Operation Manual, Version D
• If the temperature gradient
is changed during a measurement, the result shows
CHANGED (a) for the
temperature gradient.
When a measurement is completed, the last method parameters are always retained in the instrument.
To start the same method, just press START.
NOTE
Results are stored in memory until a new measurement is started or the instrument is switched off.
6.3.5 Printout
6 Operation
a
b
c
d
e
Boiling temp. = Temperature sample boiled.
Boiling point = Boiling temp. corrected according entered
barometric pressure.
If a barometric pressure of 1013 mbar is entered
boiling temperature and boiling point results are
equal.
Printout
a Instrument type
b Determination parameters
c Manual pressed results
d General information
e Signature of person making the de-
termination
31 Melting Point M-560 Operation Manual, Version D
6.4 Calibration
NOTE
BUCHI recommends calibrating each new instrument after installation. Furthermore it is recommended that the instrument be recalibrated every year.
6.4.1 Calibration principle
NOTE
The instrument is calibrated using melting point standards. The calibration is valid for boiling points
as well.
Use the calibration set (11055018). This calibration set contains the melting point standards listed
below. Each standard is shipped with a certificate of analysis and an MSDS (material safety data
sheet).
The calibration set contains the following substances:
• 4-Nitrotoluene: approx. 52 °C
• Diphenyl acetic acid: approx. 148 °C
• Caffeine: approx. 237 °C
• Potassium nitrate: approx. 335 °C
6 Operation
From each substance, a minimum of 6 determinations have to fulfill a standard deviation of less than
+/- 0.2 °C, otherwise the instrument will not move on to the next substance. The maximum number of
samples for each substance to reach the deviation of +/- 0.2 °C is limited to 12 samples. The instrument automatically chooses the best 6 results from the determinations performed.
After a successful calibration is performed, it can be checked using the verification set (11055019).
Each standard of the set contains a certificate of analysis and the MSDS.
The verification set contains the following substances:
• Benzil: approx. 94 °C
• p-Anisic acid: approx. 182 °C
• Phenolphthalein: approx. 261 °C
6.4.2 Calibration procedure
To start calibration, turn the rotary knob to Calibration. Press START and follow the instruction on
display.
32 Melting Point M-560 Operation Manual, Version D
6 Operation
• The instrument auto-
matically heats to the start
temperature of the first
substance. In the meantime,
prepare at least 6 samples of
the given substance. For this
process, follow section 6.2.1 .
After each run the current
result is indicated.
• Press START to perform
next measurement.
• Choose the correct pharmacopoeia melting point
value with the rotary knob.
The pharmacopoeia melting
point is written on the
certificate of analysis. Press
Save.
After 6 results are obtained
within a standard deviation of
+/- 0.2 °C, the process moves
on to the next substance. The
process is identical for the
subsequent substances.
• To register temperature
stamps manually press the
Set button for the related
sample. Each button can
be pressed once. Registered temperature stamps
are displayed green.
As soon as a complete
calibration is obtained, the
new calibration date is saved
automatically.
• Press OK. All results
obtained are displayed.
• The rotary knob can be
used to display all the
results of the calibration.
• The Print key is used to
print out the data.
• Back exits this menu.
33 Melting Point M-560 Operation Manual, Version D
The calibration date is now
saved and indicated on the
idle screen.
6.4.3 Printout
6 Operation
a
b
c
d
Printout
a Instrument type
b General information regarding
calibration
c Results 4-nitrotoluene
d Results diphenylacetic acid
e Results caffeine
f Results potassium nitrate
g General information
h Signature of person performing the
calibration
e
f
g
h
NOTE
The Average is calculated on the basis of the temperature values with two positions after the decimal
point. Thus, the value indicated for the Average might deviate from the value you calculate on the
basis of the temperature values on the printout, as there is just one position after the decimal point.
34 Melting Point M-560 Operation Manual, Version D
6.4.4 Verification
To verify the calibration, proceed as follows:
• Measure all standards (BUCHI recommends using the verification set (11055019) but it is also
possible to use your internal standards.
NOTE
The verification is not a guided process.
• When all measuring results were within the required tolerances, click on Verified. The following
screen appears:
6 Operation
• Enter the following password: VER. The current date is now indicated under “Last verification”.
6.5 Settings, SysInfo, Test
Test: Functional test of the instrument. To
perform the test of several functions follow
carefully the on-screen instuctions. If a function
test does not show ok, please contact the customer service. The Test protocol is described in
section 6.5.1.
SysInfo: Instrument gives information regarding
settings and connected devices. The SysInfo
protocol is described in section 6.5.2.
Settings: This menu can be used to change
parameters.
35 Melting Point M-560 Operation Manual, Version D
6 Operation
• Press the Test button to
enter the functional test,
and follow the instructions.
Table 6-1: Setting parameters
Language English, German, French, Italian, Spanish, Japanese, Chinese
Param. adj. during meas. disabled, enabled: Whether or not it is possible to change parameters
Calibration interval 0–36 months: default 12 months. BUCHI recommends calibration or
Sample ID request enabled: After the start of determination, the sample ID window is
Barometric pressure request Has impact only on boiling point determination.
Boiling sample conditioning 0–600 s: The default value is set to 60 seconds. This is needed to
Company name The name of a company can be entered.
Date (DD.MM.YYYY) XX.XX.XXXX
Time (24 h) XX:XX
Date format DD.MM.YYY, MM/DD/YYYY, YYYY-MM-DD
Time format 24 h, AM/PM
Temperature unit °C, °F, K
Pressure unit hPa, mbar, Torr, mmHg
• Press the SysInfo button
to open the system information menu.
Printout is possible if a printer
is connected.
(start temperature, stop temperature and temperature gradient)
during a determination.
verification after 12 months using the calibration set and the verification set.
displayed.
disabled: The sample ID window is not automatically displayed. In
combination with the Melting Point Monitor software, it is advisable to
turn this feature off.
never: No pop-up screen is shown.
daily: Enter current barometric pressure once a day.
always: Enter current barometric pressure every time the instrument
heats up to the start temperature for boiling point determination.
ensure a temperature equilibrium between heating block and liquid
in the boiling point tube. If this value is set too low, the result can be
incorrect or no automatic boiling point detection.
• Press the Settings button
to enter the settings menu.
36 Melting Point M-560 Operation Manual, Version D
Table 6-1: Setting parameters
Buzzer volume 0, 1, 2, 3, 4
External Keyboard CH, USA
Display brightness 0–100 %
6.5.1 Test protocol
a
6 Operation
a Power supply voltage
b Signature of person carrying out the test
b
37 Melting Point M-560 Operation Manual, Version D
6.5.2 SysInfo protocol
a
6 Operation
a Setting parameters
b Calibration correction values
c Date of factory tests
b
c
38 Melting Point M-560 Operation Manual, Version D
7 Maintenance
This section provides instructions on all maintenance work to be performed to keep the instrument in
good working condition.
WARNING
All maintenance and repair work requiring the opening or removal of the instrument housing must be
carried out by trained personnel and only with the tools provided for this purpose.
WARNING
Electrical hazard:
• Prior to any maintenance work on the instrument, switch off the power supply.
ATTENTION
Use only genuine BUCHI consumables and spare parts for any maintenance and repair work in order
to assure continued system performance and reliability. Any modifications to the spare parts used
should be carried out only with the prior written permission of the manufacturer.
7 Maintenance
7.1 Housing
Check the housing of your melting point instrument for defects (controls, plugs). The housing is coated
with paint and should be cleaned only with a rag moistened in a soapy solution.
ATTENTION
Never use any halogenated solvents, acetone, or similar chemicals, because such cleaning agents
may damage the instrument.
7.2 Glass window
Remove the glass window from the heating block periodically and wipe it clean with alcohol or
acetone. Replace the window with a new one if it will not come clean completely.
7.3 Upkeep
The upkeep of the unit is mainly limited to:
• Periodic calibration of the temperature.
7.4 Cleaning the heating block
Remove broken capillaries from the heating block.
ATTENTION
• Wait for the heating block to cool down before touching it!
39 Melting Point M-560 Operation Manual, Version D
• Remove the cover.
• Follow the instructions mentioned below on the use of the cleaning tool 051978.
• If a melting point capillary is broken and is stuck
in the heating block, use the cleaning tool
(Order number: 051978).
• Remove the cover and glass holder with glass
window.
7 Maintenance
• If glass parts of a melting point capillary are
stuck in a hole of the metal heating block, use
the cleaning tool as shown in the picture.
40 Melting Point M-560 Operation Manual, Version D
8 Troubleshooting
The following section describes how to resume operation of the instrument in the event of any minor
problem. It lists some possible occurrences, their probable cause, and suggests how to remedy
the problem. The troubleshooting table below lists possible instrument malfunctions and errors and
describes courses of action that can be used by operators to correct some of those problems. The
appropriate course of action is listed in the column “Remedy”.
More complicated malfunctions or errors are usually handled by a BUCHI technical engineer who has
access to the official service manuals. In this case, please contact your local BUCHI customer service
agent.
8.1 Malfunctions and their remedy
Table 8-1: General malfunctions and their remedy
Malfunction Possible cause Remedy
Instrument does not work Main switch off Switch on mains switch
No or unreadable printout Not activated in the settings Activate automatic printout in the
No or wrong result Sample-specific preparations:
Instrument does not heat Heating defective Contact BUCHI customer service.
8 Troubleshooting
Instrument is not connected to mains
supply
Bad cable connection Check cable connection
Printer switched OFF Switch ON printer
No paper Replace paper roll
Baud rate settings of printer faulty See section 8.1.1
Sample is not dry or is contaminated
by another substance
Sample decomposes during the
melting process (formation of
bubbles, sample turns brown, etc.)
Apparatus parameters:
Apparatus is not or is poorly calibrated
Setting point is too close to the
melting point
Check mains connection
settings
Sample should be dried before use
Regular calibration of apparatus with
BUCHI calibration standards or check
with verification standards
Select setting point 5–10 °C below
melting point
Table 8-2: Warning messages
Warning number Possible cause Remedy
Warning 01 Calibration outdated. Calibrate or verify device.
Warning 02 Housing temperature too high. Cool down device and check clearance of vent
holes and fans.
Check ambient temperature.
Warning 03 Device not calibrated. Calibrate device.
41 Melting Point M-560 Operation Manual, Version D
8 Troubleshooting
Table 8-3: Error messages
Error number Possible cause Remedy
Error 01 Memory data loss, all data are reset. Calibrate device.
In case of recurrence contact customer service.
Error 02 Automatic restart, firmware problem possible. In case of recurrence contact customer service.
Error 03 Board temperature sensor defective. Contact customer service.
Error 04 Temperature sensor defective. Contact customer service.
Error 05 Heating defective. Contact customer service.
Error 06 Cooling fan defective. Contact customer service.
Error 07 Housing fan defective. Contact customer service.
Error 08 Camera defective, communication loss. Contact customer service.
Error 09 24 V fuse defective. Contact customer service.
Error 10 24 V input voltage missing. Contact customer service.
Error 11 Internal clock, power loss. Contact customer service.
Error 13 5 V input voltage missing Contact customer service.
NOTE
If several errors are pending, the one with the highest priority will be displayed.
42 Melting Point M-560 Operation Manual, Version D
8.1.1 Setting the printer baud rate
8 Troubleshooting
• Open compartment on the bottom of the
printer.
8.2 Customer service
Only authorized service personnel are allowed to perform repair work on the instrument. They have
comprehensive technical training and knowledge of possible dangers that might arise from the instrument.
Contacts for official BUCHI customer service offices are available on the BUCHI website at: www.
buchi.com. If malfunctions occur on your instrument or you have technical questions or application
problems, please contact one of these offices.
Customer Service offers the following:
• Spare part delivery
• Repairs
• Technical advice
• The following setting should be selected.
1,2,3,4,5,7,8,9,10 = ON
6 = OFF
43 Melting Point M-560 Operation Manual, Version D
9 Shutdown, storage, transport and disposal
9 Shutdown, storage, transport, and disposal
This section provides instructions on how to shut down the instrument, how to pack it for storage or
transport, and specifies the storage and shipping conditions.
9.1 Storage and transport
WARNING
Biohazard:
• Remove all dangerous substances from the instrument, and clean it thoroughly.
• Store and transport the instrument in its original packaging.
WARNING
Electrical hazard:
• Always remove the power cord from the socket first to avoid having live cables in the laboratory.
9.2 Disposal
To dispose of the instrument in an environmentally friendly manner, a list of materials is given in
section 3.3, please ensure that the components are separated and recycled correctly. Please follow
current regional and local laws concerning disposal.
44 Melting Point M-560 Operation Manual, Version D
10 Spare parts
This section lists spare parts, accessories and optional extras, including all of the relevant order
information for ordering from BUCHI. Always state the product designation and part number when
ordering any spare parts.
To ensure optimum system performance and reliability, use only genuine BUCHI consumables and
spare parts for maintenance and repair. Prior written permission of the manufacturer should be
obtained before any modifications are made to the spare parts used.
10 Spare parts
051900
051848
Fig. 10.1: Spare parts
051847
051849
11055017
Table 10-1: Spare parts
Product Order number Product Order number
Cover 051900 Ring 051848
Glass holder 051847 Rotary knob 11055017
Glass window 051849
45 Melting Point M-560 Operation Manual, Version D
11 Declarations and requirements
11.1 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,
pursuant 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 likely to cause harmful interference, in which case
users will be required to correct the interference at their 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 réglementations FCC ainsi qu’à la réglementation des interférences
radio du Canadian Department of Communications. Ces limites sont destinées à fournir une protection adéquate contre les interférences néfastes lorsque l’appareil est utilisé dans un environnement
commercial.
Cet appareil génère, utilise et peut irradier une énergie à fréquence radioélectrique, il est en outre
susceptible d’engendrer des interférences 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 néfastes, auquel cas l’exploitant sera amené à prendre les
dispositions utiles pour palier aux interférences à ses propres frais.
11 Declarations and requirements
46 Melting Point M-560 Operation Manual, Version D
11.2 Declaration of conformity
11 Declarations and requirements
47 Melting Point M-560 Operation Manual, Version D
BÜCHI Labortechnik AG
CH-9230 Flawil 1/Schweiz
T +41 71 394 63 63
F +41 71 394 65 65
www.buchi.com Quality in your hands
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