BUCHI M-565 User Manual

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

6.2.2Determination 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

6.3.2Determination 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

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..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

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 safety-​ related 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..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).

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2  Safety

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.

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.

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2  Safety

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

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

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

Table 3-1: Standard accessories

Product	Order number
Melting Point M-565	11058004

Calibration set M-560/M-565

11055018

(4 substances; 4-nitrotoluene, diphenyl acetic acid, caffeine, potassium nitrate)

Melting point capillaries, 100 units	017808

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3  Technical data

Table 3-1: Standard accessories (cont.)

Product	Order number
Sample holder	11055014

		Cleaning tool	051978
	B	A) Boiling point tubes, 10 units	019697
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

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3  Technical data

3..1..2 Optional accessories

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

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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

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3  Technical data

3..2	Technical data overview
		Table 3-3: Technical data of the Melting Point M-565
			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	± 0,5 °C
		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,
			decreasing linearly to 50% relative humidity at 40 °C
		Over voltage category	II
		Degree of protection	IP 20
		Pollution degree	2

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3  Technical data

Table 3-3: Technical data of the Melting Point M-565 (cont.)

	Melting Point M-565
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

15	Melting Point M-565 Operation Manual, Version D

4  Description of function

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

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.

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4  Description of function

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.

mp[thermodyn.] = mp[pharma.]–(k × gradient)

k = thermodynamic factor

temperature		oven		temperature
		temperature
temperature	thermodynamic
at moment of
	correction				oven
detection
			sample	temperature	temperature
					thermodynamic
			temperature	at moment of
melting				detection	correction
temperature				melting	sample
					temperature
				temperature
	melting start	all molten:	time		time
Steep gradient		moment of		Flat gradient
		detection

Fig. 4.2: The amount of thermodynamic correction depends on the gradient selected: The smaller the gradient, the less the correction required.

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4  Description of function

4..1..2 Boiling points

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.

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].

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 temperature. The boiling point is calculated and corrected for current pressure.

18	Melting Point M-565 Operation Manual, Version D