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
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