Operation Manual
Melting Point
M�565
093256
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 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
3.3 Materials used. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
4 Description of function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.1 Functional principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.1.1 Pharmacopoeia and thermodynamic melting points . . . . . . . . . . . . . . . . . . 17
4.1.2 Boiling points . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.2 Controls and connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5 Putting into operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.1 Installation site. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.2 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.2.1 Unpacking and installation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.2.2 Connecting to a PC with MeltingPoint Monitor software . . . . . . . . . . . . . . . . 22
5.2.3 Power connection . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
5.2.4 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
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-565 Operation Manual, Version D
Table of contents
6 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.1 Basic operating principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.1.1 Display during idle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
6.1.2 Display during a process or in menus . . . . . . . . . . . . . . . . . . . . . . . . . 24
6.1.3 Entering text. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
6.1.4 Using the external keyboard. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.2 Melting point determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.2.1 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
6.2.2 Determination without pre-registered melting point method . . . . . . . . . . . . . . 27
6.2.3 Creating a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
6.2.4 Using and handling methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
6.2.5 Adjusting parameters during a determination . . . . . . . . . . . . . . . . . . . . . 31
6.2.6 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
6.2.7 Melting result . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
6.3 Boiling point . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
6.3.1 Sample preparation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
6.3.2 Determination without pre-registered boiling point method . . . . . . . . . . . . . . 38
6.3.3 Creating a method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
6.3.4 Adjusting parameters during a determination . . . . . . . . . . . . . . . . . . . . . 40
6.3.5 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
6.4 Calibration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.4.1 Calibration principle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
6.4.2 Calibration procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 43
6.4.3 Printout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
6.4.4 Verification. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.5 Settings, SysInfo, Test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
6.5.1 Test protocol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
6.5.2 SysInfo protocol. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
7.1 Housing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
7.2 Glass window . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
7.3 Upkeep . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
7.4 Cleaning the heating block . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
8 Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
8.1 Malfunctions and their remedy. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
8.1.1 Setting the printer baud rate. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
8.2 Customer service . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
9 Shutdown, storage, transport, and disposal . . . . . . . . . . . . . . . . . . . . . . . 55
9.1 Storage and transport . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
9.2 Disposal. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
10 Spare parts. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
11 Declarations and requirements. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
11.1 FCC requirements (for USA and Canada) . . . . . . . . . . . . . . . . . . . . . . . 57
11.2 Declaration of conformity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
4 Melting Point M-565 Operation Manual, Version D
1 About this manual
This manual describes the Melting Point M-565 and provides all the information required for the 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 Polyoxymethylen
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-565 Operation Manual, Version D
2 Safety
This section highlights the safety concept of the Melting Point M-565, Sample Loader M-569 and the
MeltingPoint Monitor software 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 the 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, et cetera).
6 Melting Point M-565 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-565, Sample Loader M-569, and the MeltingPoint Monitor software are 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-565 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-565 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 the event 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-565 Operation Manual, Version D
3 Technical data
This section introduces the reader to the Melting Point M-565 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-565 11058004
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-565 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
Protective cover 051935
Compaction wire 036721
CD Demo Melting Point Monitor 051983
USB cable, 2.0 m 11055310
Operation Manual:
English 93256
German 93257
French 93258
Italian 93259
Spanish 93260
10 Melting Point M-565 Operation Manual, Version D
3.1.2 Optional accessories
3 Technical data
Table 3-2: Optional accessories
Product Order number
MeltingPoint Monitor software with
11055332
license
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
11 Melting Point M-565 Operation Manual, Version D
3 Technical data
Table 3-2: Optional accessories (cont.)
Product Order number
Compact keyboard German (CH) 029509
Compact keyboard English (USA) 029508
Serial dot matrix printer (including ribbon,
11055438
paper roll, and cables)
Ribbon for printer 044306
Paper roll for printer 038684
A) Boiling point tubes, 100 units 019007
B) Boiling point capillaries, 100 units 051890
12 Melting Point M-565 Operation Manual, Version D
3 Technical data
Table 3-2: Optional accessories (cont.)
Product Order number
IQ/OQ: After installation
OQ: For repeat use
For further information please contact
your local affiliate or distributor.
IQ/OQ M-565 English 11055 004
IQ/OQ M-565 German 11055 005
IQ/OQ M-565 French 11055 006
IQ/OQ M-565 Spanish 11055 007
IQ/OQ M-565 Italian 11055 008
OQ M-565 English 11055 009
OQ M-565 German 11055 010
OQ M-565 French 11055 011
OQ M-565 Spanish 11055 012
OQ M-565 Italian 11055 013
13 Melting Point M-565 Operation Manual, Version D
3.2 Technical data overview
Table 3-3: Technical data of the Melting Point M-565
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×
Digital camera √
Video function √
Magnification, display 6 x
Display Colour, TFT, 320×240, 3.5˝
Determination temperature range Ambient + 10 °C to 400 °C
Temperature resolution 0.1 °C
Accuracy melting point at 0.5 °C/min
up to 250 °C ± 0,3 °C
250 °C to 400 °C ± 0,3 °C to ± 0,5 °C
Repeatability melting point at 0.5 °C/min ± 0.1 °C
Accuracy boiling point at 1.0 °C/min up to
400 °C
Repeatability b oiling 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
Video run time 350 min at 1 °C/min, 700 min at 0.5 °C/min
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,
Over voltage category II
Degree of protection IP 20
Pollution degree 2
3 Technical data
Melting Point M-565
± 0,5 °C
decreasing linearly to 50% relative humidity at 40 °C
14 Melting Point M-565 Operation Manual, Version D
Table 3-3: Technical data of the Melting Point M-565 (cont.)
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 3-4: 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
3 Technical data
Melting Point M-565
15 Melting Point M-565 Operation Manual, Version D
4 Description of function
This section explains the basic principle of the Melting Point M-565 and provides a functional description of the assemblies.
4.1 Functional principle
The Melting Point M-565 is an instrument for automatic and visual (manual) 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 can be observed through the lens or on the color display.
Detection principle of the Melting Point M-565
4 Description of function
a
f
b
c
d
g
e
Fig. 4.1: Reflection mode due to Ph. Eur. 6.1 2.2.60.
a glass capillary tube
b sample
c camera
d temperature sensor
e heating block
f light source
g glass window
The melting point capillary sits in a hollow of a
metal block, which is heated electrically and
controlled by a temperature sensor. The heating
block can be maintained accurately at a predefined temperature by the heating element and
can be heated at a defined rate.
Detection is done as follows: The melting point
capillary is illuminated from the front and the
camera records the image. Melting and boiling
points are detected by image processing.
16 Melting Point M-565 Operation Manual, Version D
4.1.1 Pharmacopoeia and thermodynamic melting points
The melting process of a substance does not take place instantaneously - it requires a finite amount
of time. The melting process begins at the point where the first particles of the substance turn into the
liquid state (thermodynamic melting point). The end of the melt is reached when the last solid particles
have gone over into the liquid phase (pharmacopoeia melting point).
During the entire melting process of a pure compound, the temperature of the pure substance remains
constant while heat is constantly transferred from the heating block to the sample.
For pure substances the thermodynamic melting point can be approached by multiplying the thermodynamic correction factor by the square root of the gradient and subtracting the result from the
pharmacopoeia melting point.
4 Description of function
mp
[thermodyn.]
= mp
–(k × gradient)
[pharma.]
k = thermodynamic factor
temperature
temperature
at moment of
detection
melting
temperature
thermodynamic
correction
melting start
Steep gradient Flat gradient
Fig. 4.2: The amount of thermodynamic correction depends on the gradient selected: The smaller the
oven
temperature
all molten:
moment of
detection
sample
temperature
temperature
temperature
at moment of
detection
melting
temperature
oven
temperature
thermodynamic
correction
sample
temperature
timetime
gradient, the less the correction required.
17 Melting Point M-565 Operation Manual, Version D
4.1.2 Boiling points
Fig. 4.3: Boiling point
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 sample oven temperature and sample temperature.
During this delay time some air bubbles turns out of 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].
4 Description of function
The boiling point is determined by the “Siwoloboff” method.
The Melting Point M-565 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 automatically or visually.
Detection is done as follows:
The beam of light illuminates the boiling point tube from the front,
and the camera records the image.
The instrument records the curve and displays the result. At the beginning of the measurement, the
current pressure has to be entered to obtain correct results. The system detects the boiling tempera-
ture. The boiling point is calculated and corrected for current pressure.
18 Melting Point M-565 Operation Manual, Version D
4.2 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 in the menu and
for select characters
f Display
b
c
Fig. 4.4: Front view
a
Fig. 4.5: Rear view
f
d
e
e
d
b
c
a
RS232
USB
PS/2
a Mains plug
b PS/2 connection for keyboard
c RS 232 connection for serial printer
d USB connection to the PC if software Melting
Point Monitor is used, needed for service
e Housing cooling fan
f Heating block cooling fan
19 Melting Point M-565 Operation Manual, Version D
5 Putting into operation
This section describes the installation of the Melting Point M-565 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, of 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
NOTE
Do not expose the instrument to direct sunlight or very high illumination. This could influence the
automatic detection process.
General hazards arise from:
• Mixtures of unknown composition or contaminations
• Combustible gases or solvent vapors 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:
20 Melting Point M-565 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.
• Install the cover.
21 Melting Point M-565 Operation Manual, Version D
Accessories
• Place the melting point capillaries in the hole of the housing. The second hole is a reservoir for
used capillaries.
5.2.2 Connecting to a PC with MeltingPoint Monitor software
5 Putting into operation
The Melting Point M-565 can be operated
in connection with the MeltingPoint Monitor
software. In this case, connect the instrument
with the PC or laptop using the USB cable. For
detailed information check installation guide on
software CD.
Fig. 5.1: Connection of Melting Point M-565 with the MeltingPoint Monitor software.
5.2.3 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 might damage the instrument. Make
sure that the mains connector is freely accessable at any time.
5.2.4 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.
a Melting Point M-565
b Laptop or PC with MeltingPoint Monitor
software
22 Melting Point M-565 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-565 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 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 Hint
c Parameters used after pressing START
d Shows current heating block temperature
and time
e Functions selectable by the keys below
23 Melting Point M-565 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 hints 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.
24 Melting Point M-565 Operation Manual, Version D
6 Operation
Screen during melting point
determination
Result indication
(numeric result)
6.1.3 Entering text
Settings menu
Result indication
(replay)
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.
25 Melting Point M-565 Operation Manual, Version D
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.
6.2 Melting point determination
NOTE
For exact melting point determination, use original capillaries from BUCHI only. If other capillaries are
used, the results can be wrong. Use the following items:
6 Operation
Fig. 6.1: Melting point capillaries
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.
Product Order number
Melting point capillaries, 100 units 017808
Melting point capillaries, 1000 units 001759
NOTE
Sample preparation by letting the capillaries fall through a tube is not advised, because cross
contamination may occur.
26 Melting Point M-565 Operation Manual, Version D
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 pounding the tubes
against a hard base.
• Enough substance must be filled into the glass capillary to form a compact column 4 to 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.
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 start the determination process immediately with the last parameters used.
6 Operation
NOTE
If the current parameters do not meet your needs, 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
d
press Edit.
• Chose start temperature
with the rotary knob, and
press Next.
27 Melting Point M-565 Operation Manual, Version D
• Chose stop temperature
with the rotary knob, and
press Next.
• Chose temperature
gradient with the rotary
knob, and press Save.
NOTE
Insert samples only when the start temperature is reached (as soon as prompted).
6 Operation
• Press START to start the
determination, and follow
the instructions on the
screen.
• 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 start the determination.
NOTE
The result is indicated automatically after the melting point of each sample is detected.
28 Melting Point M-565 Operation Manual, Version D
6 Operation
• To run through the results,
turn the rotary knob up and
down.
• To replay the recorded
melting process, press
Replay.
• Press End or STOP to
return to the idle screen.
• Press START to measure
again with the identical
measuring parameters.
• The result is printed out
automatically if a printer is
connected.
NOTE
The last result is stored in the device until a new measurement is started or the instrument is
switched off.
• Back: Turns back to the
result menu.
• Sample: Switches between
sample left, middle, and
right.
• Play: Replays recorded
video automatically.
• Rotary knob: Changes
temperature value and its
corresponding picture of
the sample.
• Changes replay speed of
video using rotary knob.
• Stop: Stops replay mode.
• After turning back to idle,
the last result can be
checked again by pressing
Result.
29 Melting Point M-565 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.
30 Melting Point M-565 Operation Manual, Version D
6 Operation
• Turn the rotary knob to
select a method.
• Press START to start the
determination.
• Use Edit to adjust method
parameters.
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).
• Press the Options key to
get further functions:
• New: Creates a new
method.
• Delete: Deletes the
method.
• Rename: Changes the
method name.
a
6.2.6 Printout
NOTE
The result is printed out automatically if a printer is connected and automatic printing is configured in
the settings menu.
• 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.
If the temperature gradient
is changed during a measurement, the result shows
CHANGED (a) for the temperature gradient.
31 Melting Point M-565 Operation Manual, Version D
6.2.7 Melting result
NOTE
Changing the determination mode does not affect the principle of measurement, but it does influence
the interpretation and the appearance of the results. The mode can be selected in the settings menu.
The default and most frequently used mode is the pharmacopoeia melting point. Melting range is
convenient for substances with a wide melting range. The thermodynamic melting point should be
used for special application only. For detailed information see Section 4.1.1.
6 Operation
• In the settings, change the
melting result to Melting
point pharmacopoeia
and press Save.
Melting point pharmacopoeia
• In the settings, change the
melting result to Melting
point pharmacopoeia
and press Save.
• In the settings, change the
melting result to Melting
range and press Save.
• In the settings, change the
melting result to Melting
point thermodynamic
and press Save.
32 Melting Point M-565 Operation Manual, Version D
6 Operation
a
b
c
d
e
Printout
a Instrument type
b Determination parameters
c Automatically detected results
d Manual results
e Curve sample left
f Curve sample center
g Curve sample right
h General information
i Signature of person making the
determination
f
g
h
i
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.
33 Melting Point M-565 Operation Manual, Version D
6.2.7.2 Melting range
6 Operation
• In the settings, change the
melting result to Melting
range and press Save.
An additional parameter is
shown. The default value is
set to 15%. This value can be
used for most of substances.
Threshold: This value is
needed only for melting range
determination. The default
value is set to 15%. This value
can be used for 80% of substances.
• If the beginning of the
melting range differs from
that observed, increase or
decrease this value.
The result mode shows a
range for each sample:
XX.X–XX.X °C
34 Melting Point M-565 Operation Manual, Version D
In the replay mode, the melting range is shown in gray
backlit.
6 Operation
a
b
c
d
e
Printout
a Instrument type
b Determination parameters
c Automatically detected results
d Manual results
e Curve sample left
f Curve sample center
g Curve sample right
h General information
i Signature of person making the
determination
f
g
h
i
35 Melting Point M-565 Operation Manual, Version D
6.2.7.3 Melting point thermodynamic
6 Operation
• In the settings, change the
melting result to Melting
point thermodynamic
and press Save.
Experimental measurements
have shown that in most cases a good approximation to
the factor for thermodynamic
correction of the BUCHI Melt-
Empirical calculation for
thermodynamic correction is
recommended when more accurate results are required for
specific substances.
ing Point M-565 is a value of
~1.5.
In order to obtain a thermodynamic melting point result within the accuracy of the unit, the following
steps are advised:
• Perform complete automatic pharmacopoeia melting point determinations on your sample at three
different temperature ramping rates: 0.2, 0.5, 1.0 °C/min.
• Plot the resulting melting points versus the square root of their corresponding temperature ramping
rate (mp pharmacopoeia vs.
gradient
)–a linear dependence should be observed.
• The slope is the thermodynamic correction factor. Enter this value in the setting 6.6 “Thermodynamic correction.”
An example of this calculation procedure is shown below:
Gradient, r [°C/min] Melting Point [°C]
0.2 236.1
0.5 236.6
1.0 236.9
gradient
”
mp pharmacopoeia vs.
gradient
“Melting point temperature vs.
for a caffeine sample melted at 0.2, 0.5,
and 1.0 °C/min. The slope of the straight
236.9
236.8
236.7
236.6
236.5
236.4
236.3
236.2
236.1
236.0
0 0.2 0.4 0.6 0.8 1 1.2
y = 1.2684 x + 235.52
line, factor for thermodynamic correction
= 1.3, is programmed into the setting of
instrument for this compound.
gradient
Fig. 6.2: “Melting point temperature vs.
gradient
”
36 Melting Point M-565 Operation Manual, Version D
6 Operation
d
a
b
c
d
e
Printout
a Instrument type
b Determination parameters
c Correction factor for thermodynamic
determination
d Automatically detected results
e Manual results
f Curve sample left
g Curve sample center
h Curve sample right
i General information
j Signature of person making the deter-
mination
f
g
h
i
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.
37 Melting Point M-565 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 can be obtained. Use the following items:
B
Fig. 6.3: 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
38 Melting Point M-565 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 start 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 start the determination.
39 Melting Point M-565 Operation Manual, Version D
73.2 76.4
73.4 76.6
6 Operation
Delay: to ensure equilibrium
between oven temperature
and sample temperature.
During this delay time some
air bubbles turns out of the
• To run through the results,
turn the rotary knob up and
down.
Video replay is not available
for boiling point determination.
boiling point capillary. This
request can be changed in
the setting “Boiling sample
conditioning” (see 6.5).
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
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).
• Press End or STOP to
return to the idle screen.
• Press START to measure
again with the identical
measuring parameters.
a
• Turning the rotary knob
displays the current parameter set.
• Adjust the parameters by
pressing Edit. Adjusting the
If the temperature gradient
is changed during a measurement, the result shows
CHANGED (a) for the tem-
perature gradient.
parameters does not affect
the saved method.
40 Melting Point M-565 Operation Manual, Version D
When a measurement is done, 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
Printout
a Instrument type
b Determination parameters
c Automatically detected results
d Manual results
e General information
f Signature of person making the de-
termination
e
f
Boiling temp. = Temperature sample boiled.
Boiling point = Boiling temp. corrected according entered baro-
metric pressure.
If a barometric pressure of 1013 mbar is entered
boiling temperature and boiling point results are
equal.
41 Melting Point M-565 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 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 done, it may 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
42 Melting Point M-565 Operation Manual, Version D
6.4.2 Calibration procedure
To start calibration, turn the rotary knob to Calibration. Press START and follow the instruction on
display.
6 Operation
The instrument automatically
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 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
other substances.
• Choose the correct pharmacopoeia melting point
value with the rotary knob.
The pharmacopoeia melting
point is written on the
certificate of analysis. Press
Save.
As soon as a complete
calibration is obtained, the
new calibration date is saved
automatically.
• Press OK. All results
obtained are displayed.
Follow the instructions on the
display. After each run, the
current result is indicated.
• Press START to perform
the next measurement.
• 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.
The calibration date is now
saved and indicated on the
idle screen.
43 Melting Point M-565 Operation Manual, Version D
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 making 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.
44 Melting Point M-565 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 per-
form the test of several functions follow carefully
the instuction on the screen. If a function test
shows not 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.
Settings: This menu can be used to change
parameters. The SysInfo protocol is described
in section 6.5.2.
45 Melting Point M-565 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
Stop after detection disabled, enabled: If the instrument finds a melting point or boiling
Param. adj. during meas. disabled, enabled: Whether or not it is possible to change parameters
Result printout automatically disabled, enabled: After a measurement is finished, results will be
Result graph indication disabled, enabled: Each result contained is shown with a graphic.
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.
• Press the SysInfo button
to open the system information menu.
Printout is possible if a printer
is connected.
point for every detected sample, measurement stops automatically.
(start temperature, stop temperature, and temperature gradient)
during a determination.
printed automatically.
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 MeltingPoint Monitor software, it is advisable to
turn this feature off.
never: No pop-up screen is shown.
• Press the Settings button
to enter the settings menu.
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.
Boiling sample conditioning 0–600 s: The default value is set to 60 seconds. This is needed to
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.
Melting result acc. pharmacopoeia
thermodynamic
range
46 Melting Point M-565 Operation Manual, Version D
6 Operation
Table 6-1: Setting parameters (cont.)
Thermodynamic correction 0.0–3.0; default value: 1.1
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
Table 6-1: Setting parameters
Buzzer volume 0, 1, 2, 3, 4
External Keyboard CH, USA
Display brightness 0–100%
Automatic detection Enable or disable the automatic detection. If disabled, stop tempera-
ture of method is the end of the determination.
Statistic Enable or disable the statistic. If disabled, mean value and standard
deviation are not shown in the results.
Camera position Use the rotary knob to position the dashed rectangles at the bottom
part of the substance according to the example.
Change Direction to move vertically or horizontally.
47 Melting Point M-565 Operation Manual, Version D
6.5.1 Test protocol
a
6 Operation
a Power supply voltage
b Values for sample brightness
c Signature of person carrying out the test
b
c
48 Melting Point M-565 Operation Manual, Version D
6.5.2 SysInfo protocol
6 Operation
a Setting parameters
a
49 Melting Point M-565 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.
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 completely clean.
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 completely clean.
7.3 Upkeep
The upkeep of the unit is mainly limited to:
• Periodic calibration of the temperature.
50 Melting Point M-565 Operation Manual, Version D
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!
• Remove the cover.
• Follow the instructions mentioned below on the use of the cleaning tool 051978.
7 Maintenance
• 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.
• 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.
51 Melting Point M-565 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 melting curve is shown Not activated in the settings Activate graphic in the settings
In the automatic melting point determination, no value and no melting
curve are determined
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
No automatic detection of samples Manually register the melting point/
Measuring finished before detecting
a result for all samples
Sample is unstable, it decomposes,
turns brown, or melts non-uniformly
The temperature parameters have
been entered incorrectly and the
sample does not melt at all
Check mains connection
settings
boiling point
Turn off in the settings “Stop after
detection” and check stop temperature.
e.g. select higher maximum point
Automatic detection is disabled
Sometimes no results or only 1 or 2
results instead of 3 results
Unexpected results Sample-specific preparations:
52 Melting Point M-565 Operation Manual, Version D
START button was pressed before
insertion of all sample capillaries
Sample is not dry or is contaminated
by another substance
Enable the Automatic detection in the
Settings
Put all sample capillaries in the oven
first, then press the START button.
Do not move the sample capillaries
again.
Sample should be dried before use
8 Troubleshooting
Table 8-1: General malfunctions and their remedy
Malfunction Possible cause Remedy
Sample decomposes during the
melting process (formation of
bubbles, sample turns brown, etc.)
Apparatus parameters:
Apparatus is not or is poorly calibrated
Method “According to pharmaco-
Regular calibration of apparatus with
BUCHI calibrating substances
Alter the corresponding parameters
poeia” or “thermodynamic melting
point determination” is incorrectly
selected
No results Setting point is too close to the
melting point
No statistic Setting parameter Statistic is
Select setting point 5–10 °C below
melting point
Enable the Statistic in the Settings
disabled
Instrument does not heat Heating defective Contact BUCHI customer service.
Table 8-2: Malfunctions with Melting Point Monitor software
Malfunction Possible cause Remedy
No USB connection USB cable is not connected or defec-
tive.
Check USB connection, replace if
necessary.
Driver not found Device connected for the first time. Install recommended driver.
Table 8-3: 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.
Table 8–4: 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.
53 Melting Point M-565 Operation Manual, Version D
Table 8–4: Error messages
Error number Possible cause Remedy
Error 11 Internal clock, power loss. Contact customer service.
Error 13 5V input voltage missing Contact customer service.
NOTE
If several errors are pending, the one with the highest priority will be displayed.
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
54 Melting Point M-565 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.
55 Melting Point M-565 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
56 Melting Point M-565 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
57 Melting Point M-565 Operation Manual, Version D
11.2 Declaration of conformity
11 Declarations and requirements
58 Melting Point M-565 Operation Manual, Version D
BÜCHI Labortechnik AG
CH-9230 F lawil 1 / Swit zerland
T +41 71 394 63 63
F +41 71 394 65 65
www.buchi.com Quality in your hands
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