BUCHI M-560 User Manual

Operation Manual

Melting Point

M 560

093251 en

Table of contents

Table of contents

1	About this manual					5
	1.1	Reference documents				5
	1.2	Abbreviations . . . . . . . . . . . . . .	. . . . . . . . . .	.		5
2	Safety					6
	2.1	User qualification . . . . . . . . . . . .	. . . . . . . . . .	.	.	6
	2.2	Proper use . . . . . . . . . . . . . .	. . . . . . . . . .	.	.	6
	2.3	Improper use . . . . . . . . . . . . . .	. . . . . . . . . .	.		6
	2.4	Warning notices used in this manual . . . . . .	. . . . . . . . . .	.		7
	2.5	Product safety				7
	2.5.1	Instrument-related hazards . . . . . . . . .	. . . . . . . . . .	.		. 7
	2.5.2	Other hazards				7
	2.5.3	Safety measures . . . . . . . . . . . .	. . . . . . . . . .	.	.	8
	2.5.4	Safety elements				8
	2.6	General safety rules . . . . . . . . . . . .	. . . . . . . . . .	.		8
3	Technical data . . . . . . . . . . . . . . . .		. . . . . . . . . .	.		9
	3.1	Scope of delivery . . . . . . . . . . . .	. . . . . . . . . .	.	.	9
	3.1.1	Standard accessories . . . . . . . . . . .	. . . . . . . . . .	.		. 9
	3.1.2	Optional accessories . . . . . . . . . . .	. . . . . . . . . .	.		11
	3.2	Technical data overview				12
	3.3	Materials used				13
4	Description of function . . . . . . . . . . . .		. . . . . . . . . .	.	. 14
	4.1	Melting Point . . . . . . . . . . . . . .	. . . . . . . . . .	.		14
	4.2	Boiling Point				14
	4.3	Controls and connections				15
5	Putting into operation					16
	5.1	Installation site				16
	5.2	Commissioning . . . . . . . . . . . . .	. . . . . . . . . .	.		16
	5.2.1	Unpacking and installation				16
	5.2.2	Power connection				18
	5.2.3	Calibration				18

Read this manual carefully before installing and running your system; take particular note of the safety precautions in section 2. Keep the manual in the immediate vicinity of the instrument, so that it can be consulted at any time.

No technical modifications may be made to the instrument without the prior written agreement of BUCHI. Unauthorized modifications may affect system safety or result in accidents. This manual is copyrighted. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited.

The English manual is the original language version and serves as basis for all translations into other languages. Other language versions can be downloaded at www.buchi.com.

3	Melting Point M-560 Operation Manual, Version D

Table of contents

6	Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . .			19
	6.1	Basic operating principles		19
	6.1.1	Display during idle		19
	6.1.2	Display during a process or in menus . . . . . . . . . . . . . . . .	.	20
	6.1.3	Entering text		21
	6.1.4	Using the external keyboard		21
	6.2	Melting point determination . . . . . . . . . . . . . . . . . . . .		22
	6.2.1	Sample preparation . . . . . . . . . . . . . . . . . . . . . .	.	22

6.2.2Determination without pre-registered melting point method . . . . . . . . . . 23

6.2.3	Creating a method . . . . . . . . . . . . . . . . . . . . . .	.	26
6.2.4	Using and handling methods . . . . . . . . . . . . . . . . . . .		. 26
6.2.5	Adjusting parameters during a determination . . . . . . . . . . . . . .		27
6.2.6	Printout . . . . . . . . . . . . . . . . . . . . . . . . . .	.	27
6.3	Boiling point		28
6.3.1	Sample preparation . . . . . . . . . . . . . . . . . . . . . .	.	28

6.3.2Determination without pre-registered boiling point method . . . . . . . . . . 28

	6.3.3	Creating a method . . . . . . . . . . . . . . . . . . . . . .	.	30
	6.3.4	Adjusting parameters during a determination . . . . . . . . . . . . . .		30
	6.3.5	Printout . . . . . . . . . . . . . . . . . . . . . . . . . .	.	31
	6.4	Calibration		32
	6.4.1	Calibration principle . . . . . . . . . . . . . . . . . . . . . .	.	32
	6.4.2	Calibration procedure . . . . . . . . . . . . . . . . . . . . . .		32
	6.4.3	Printout . . . . . . . . . . . . . . . . . . . . . . . . . .	.	34
	6.4.4	Verification		35
	6.5	Settings, SysInfo, Test		35
	6.5.1	Test protocol . . . . . . . . . . . . . . . . . . . . . . . .	.	37
	6.5.2	SysInfo protocol		38
7	Maintenance			39
	7.1	Housing		39
	7.2	Glass window		39
	7.3	Upkeep . . . . . . . . . . . . . . . . . . . . . . . . . .	.	39
	7.4	Cleaning the heating block . . . . . . . . . . . . . . . . . . . .		39
8	Troubleshooting . . . . . . . . . . . . . . . . . . . . . . . . . .			41
	8.1	Malfunctions and their remedy		41
	8.1.1	Setting the printer baud rate		43
	8.2	Customer service . . . . . . . . . . . . . . . . . . . . . . .		. 43
9	Shutdown, storage, transport, and disposal . . . . . . . . . . . . . . .			. 44
	9.1	Storage and transport		44
	9.2	Disposal		44
10	Spare parts			45
11	Declarations and requirements			46
	11.1	FCC requirements (for USA and Canada) . . . . . . . . . . . . . . .		. 46
	11.2	Declaration of conformity . . . . . . . . . . . . . . . . . . . .	.	47

4	Melting Point M-560 Operation Manual, Version D

1  About this manual

1 About this manual

This manual describes the Melting Point M-560 and provides all the information required for its safe operation and to maintain it in good working order.

It is addressed in particular to laboratory personnel and operators.

NOTE

The symbols pertaining to safety (WARNINGS and ATTENTIONS) are explained in section 2.

1.1Reference 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

1.2Abbreviations

Chemicals:

PTFE	Polytetrafluoroethylene
PP	Polypropylene
PE	Polyethylene
EPDM	Ethylene-propylene-diene rubber
POM	Polyoxymethylene
PUR	Polyurethane
Miscellaneous:
mp	Melting point
bp	Boiling point
pharm.	Pharmacopoeia
therm.	Thermodynamic
L	Sample left
C	Sample center
R	Sample right

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2  Safety

2 Safety

This section highlights the safety concept of the Melting Point M-560 and contains general rules of behavior and warnings about hazards concerning the use of the product.

The safety of users and personnel can only be ensured if these safety instructions and the 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.

2.1User 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.

2.2Proper 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.

2.3Improper use

Applications beyond those described above are improper. Furthermore, applications which do not comply with the technical data are also considered improper. The operator bears the sole risk for any damages caused by such improper use.

The following applications in particular are expressly forbidden:

•Use in rooms requiring explosion-proof equipment.

•Extraction of samples which may explode or ignite as the result of a blow, friction, heat, or spark (e.g. explosives).

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2  Safety

2.4Warning 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.

2.5Product safety

The Melting Point M-560 is designed and built in accordance with current state-of-the-art technology. However, risks to users, property, and the environment can arise when the instrument is used carelessly or improperly.

The manufacturer has determined residual dangers emanating from the instrument

•if the instrument is operated by insufficiently trained personnel.

•if the instrument is not operated properly.

Appropriate warnings in this manual serve to alert the user to these residual dangers.

2.5.1Instrument-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.

2.5.2Other hazards

WARNING

Certain solvents within or in the vicinity of the Melting Point M-560 can form peroxides and/or are highly inflammable.

•Always be aware of the explosion risk when working with hazardous substances or with substances of unknown composition.

•Always use the instrument in an adequately ventilated work area.

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2  Safety

2.5.3Safety measures

Always wear personal protective equipment such as protective goggles and protective clothing, when working with the instrument.

2.5.4Safety elements

Anti-seismic tie-down

•The instrument is equipped with a fixture to tie it down in areas at risk of an earthquake (see bottom side of the instrument).

2.6General 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-560 Operation Manual, Version D

3  Technical data

3 Technical data

This section introduces the reader to the Melting Point M-560 and its main components. It contains technical data, requirements and performance data.

3.1Scope 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.

3.1.1Standard accessories

Table 3-1: Standard accessories

Product	Order number
Melting Point M-560	051999

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

Compaction wire	036721
Operation Manual:
English	93251
German	93252
French	93253
Italian	93254
Spanish	93255

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3  Technical data

3.1.2Optional accessories

Table 3-2: Optional accessories

Product	Order number
Sample Loader M-569	051997

Verification set M-560/M-565

11055019

(3 substances; benzil, p-anisic acid, phenolphthalein)

Melting point capillaries, 1000 units	001759

Mortar and pestle, agate	041867

Compact keyboard German (CH)	029509
Compact keyboard English (USA)	029508

Serial dot matrix printer (including ribbon, 11055438 paper roll, and cables)

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3  Technical data

Table 3-2: Optional accessories (cont.)

Product	Order number
Ribbon for printer	044306

Paper roll for printer	038684

A) Boiling point tubes, 100 units	019007
B) Boiling point capillaries, 100 units	051890

Protective cover	051935

3.2	Technical data overview
		Table 3-4: Technical data of the Melting Point M-560
				Melting Point M-560
		Manual melting point determination		√
		Manual boiling point determination		√
		Automatic melting point determination		–
		Automatic boiling point determination		–
		Homogeneous sample loading		–
		Positions for melting capillaries		3
		Positions for boiling capillaries		1
		Precision magnifying lens		√
		Magnification of lens		2.5×
		Display		Colour, TFT, 320×240, 3.5˝
		Determination temperature range		Ambient +10 °C to 400 °C
		Temperature resolution		0.1 °C
		Accuracy of melting point at 0.5 °C/min
		up to 250 °C		±0.3 °C

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3  Technical data

Table 3-4: Technical data of the Melting Point M-560

	Melting Point M-560
250 °C to 400 °C	±0.3 °C to ±0.5 °C
Repeatability of melting point at 0.5 °C/min	±0.1 °C
Accuracy of boiling point at 1.0 °C/min up to 400 °C	±0.5 °C
Repeatability of boiling point at 1.0 °C/min	±0.3 °C
Temperature gradients, °C/min	0.1, 0.2, 0.5, 1, 2, 3, 5, 10, 20
Heat-up time (50 °C–350 °C) at 25 °C	~4 min
Cool-down time (350 °C–50 °C) at 25 °C	~13 min
Electrical supply	100–240 V (±10 %), 50–60 Hz
Power consumption	150 W
Contact termination	L, N, PE
Approval	CE, CSA, UL
Dimensions (W×H×D), mm	190×200×370
Weight, kg	4.5
Environmental conditions	For indoor use only
Temperature	5–40 °C
Altitude	up to 2000 m a.s.l.
Humidity	Maximum relative humidity 80 % for temperatures up to
	31 °C, decreasing linearly to 50 % relative humidity at 40 °C
Overvoltage category	II
Degree of protection	IP20
Pollution degree	2
Storable methods for melting point	50
Storable methods for boiling point	50
Compliant with Pharmacopeia methods	PH. EUR. 6.1.2.2.60, USP XXI 741 and JP

NOTE

Temperature measuring accuracy refers to pharmacopoeia melting point.

3.3	Materials used
		Table 3-5: Materials used
		Component	Material designation
		Print holder	PA
		Heating block	Aluminium
		Lenses	Glass
		Axial fan	Aluminium
		Housing	PU, Stainless Steel, Glass
		Cover	POM, Ceramic, Aluminium, Stainless Steel

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4  Description of function

4 Description of function

This section explains the basic principle of the Melting Point M-560 and provides a functional description of the assemblies.

4.1Melting Point

The Melting Point M-560 is an instrument for manual (visual) determination of melting point, melting range, and boiling point at ambient temperatures +10 °C up to 400 °C. The melting point of three samples can be determined at the same time. The boiling point can be determined for one sample. Samples have to be observed through the lens.

The melting point capillary sits in a hollow of the metal block, which is heated electrically and controlled by a temperature sensor. The heating block is capable of being maintained accurately at a pre-defined temperature by the heating element, and of being heated at a defined rate.

4.2Boiling Point

The boiling point is determined by the “Siwoloboff” method.

The Melting Point M-560 can be used to determine the boiling point of a small amount of liquid. The heating block has one insert available for boiling point tubes (outside left). The moment of boiling is determined visually.

The process for boiling point determination is analogous to that for determining a melting point:

•The start temperature is set 5 to 10 °C lower than the expected boiling point.

•The sample is put into the heating block as soon as the start temperature is reached.

•A delay time allows the equilibrium between oven temperature and sample temperature. During this delay time some air bubbles escape from the boiling point capillary.

•Starting from the start temperature, the sample is heated at a temperature gradient of 1 °C/min.

•As the temperature rises, bubbles of gas rise slowly and regularly from the immersed end of the boiling point capillary.

•The boiling point of the liquid has been reached when the flow of steam bubbles reaches a frequency of 0.6 Hz [Hertz].

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4  Description of function

4.3Controls and connections

a Power switch; turns the instrument on/off b Start; starts process

c Stop; stops process, starts/stops ventilation, returns to idle screen

d 3 Select and Set buttons

e Rotary knob for navigation through the menu and for select characters

f Display

f

ba

c d e

Fig. 4.1: Front view

	f
	d
	USB
a	b PS/2
e	c
	RS232

a Mains plug

b PS/2 connection for keyboard

c RS 232 connection for serial printer d USB connection: required for service e Housing cooling fan

f Heating block cooling fan

Fig. 4.2: Rear view

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