Method For The Determination of Crystallizing Point Method For The Determination of Melting Point A

BRITISH STANDARD BS 4633 &
4634:1970
Method for
The determination of
crystallizing point
Method for
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The determination of
melting point and/or
melting range
Copyright British Standards Institution

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BS 4633 & 4634:1970
Co-operating organizations
The Technical Committee which has been working under the supervision of the
Chemical Divisional Council, and which is responsible for the preparation of
these British Standards, consists of members representing the following
Industry Standards Committees:
Chemicals
Laboratory Apparatus
Pest Control Products
Petroleum
Pigments, Paints and Varnishes
Tar Products (other than Ammonia)
The committee entrusted with the preparation of these British Standards

consists of members nominated by the Technical Committee.
These British Standards, having

been endorsed by the Chairman
of the Chemical Divisional
Council, were published under
the authority of the Executive
Board on
23 October 1970
Amendments issued since publication
© BSI 11-1999
Amd. No. Date of issue Comments
The following BSI references
relate to the work on these 7715 July 1993 Indicated by a sideline in the margin
standards:
Committee references
C/40, C/40/-/1
Drafts for comment
67/8191 and 68/18936
ISBN 580 06273 2
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BS 4633 & 4634:1970
Contents
Page
Co-operating organizations Inside front cover
Foreword ii
BS 4633 Method for the determination of crystallizing point
1 Scope 1
2 Definition 1
3 Apparatus and materials 1
4 Preparation of sample 1
5 Procedure 2
Figure 1 — Apparatus for determination of crystallizing point 3
BS 4634 Method for the determination of melting point and/or
melting range
1 Scope 4
2 Definitions 4
3 Apparatus and materials 4
4 Procedure 5
5 Calculation 5
6 Reporting 5
Figure 1 — Device suitable for holding a number of capillary tubes in close
proximity to the thermometer 6
i
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© BSI 11-1999
BS 4633 & 4634:1970
Foreword
These standards make reference to the following British Standards:

BS 593, Laboratory thermometers.
BS 3218, Test tubes and boiling tubes.

These British Standards have been prepared under the authority of the Chemical
Divisional Council to provide general methods for the determination of
crystallizing point, and melting point and/or melting range, applicable to a wide
range of chemical products. They have been prepared taking into account
methods already adopted by other standardizing bodies and by technical
committees of the International Organization for Standardization (ISO). It is
hoped that they will be adopted not only by those preparing British Standards but
also by other bodies preparing specifications.
By agreement with the Standardization of Tar Products Test Committee,
hereinafter referred to as STPTC, the method of test and description of apparatus
for determination of crystallizing point have been adapted from STPTC Method
Serial No. PC 10–67 in the publication, “Standard methods for testing tar and its
products” (6th edition 1967). This method also has some features in common with
ISO 1392 “Determination of crystallizing point — General method”.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
pages 1 to 6 and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on the
inside front cover.
ii
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© BSI 11-1999
BS 4633 & 4634:1970
BS 4633 Method for the determination of crystallizing point

1 Scope
This British Standard describes a basic procedure for the determination of crystallizing point of chemical
products over the temperature range – 20 °C to + 260 °C.
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2 Definition
For the purposes of this British Standard the following definition applies:
crystallizing point
the temperature determined and recorded according to 5.2 at which crystallization takes place when a
liquid is being cooled down under the prescribed conditions of test
3 Apparatus and materials

The following apparatus and materials are required:
1) Crystallizing point apparatus, as shown in Figure 1. A glass test tube1) of nominal
size 150 mm × 25 mm is placed inside another glass test tube of nominal size 200 mm × 38 mm which
has been cut down in length to 160 mm × 38 mm. The latter tube is flanged so that it may be supported
by a metal cover plate centrally in a 1 000 ml tall-form beaker filled to within 20 mm of the top with
appropriate cooling medium. For crystallizing point temperatures between – 20 °C and + 10 °C, the
beaker is replaced by an unsilvered Dewar vessel of at least 80 mm inside diameter and 200 mm deep.
The wider tube is weighted with lead shot, or similar material, and the inner tube is closed by means of
a cork which carries a glass stirrer and, through its centre, the selected thermometer [see 3 2)]. The
stirrer is a rod attached to a loop of outside diameter 18 mm which surrounds the thermometer. The
thermometer is so fixed in the cork that the bottom of the bulb is about 15 mm from the bottom of the
inner tube. A thermometer for the cooling bath passes through a hole in the cover plate and is held by a
rubber ring.
2) Thermometer, accurately standardized of suitable range and accuracy, calibrated for 100 mm
immersion and complying with Series B of BS 5932), unless otherwise required by the specification for
the product being tested.
3) Thermometer, covering a convenient range to suit the temperature of the cooling bath.
4) Melting bath, suitable for raising the temperature of the sample to about 5 degC above the
crystallizing point.
5) Cooling media. The following cooling media are in common use:
For crystallizing temperatures down to – 20 °C: Crushed ice and calcium chloride, CaCl2.6H2O
For crystallizing temperatures down to – 12 °C: Crushed ice and salt
For crystallizing temperatures down to + 1 °C: Ice and water
For crystallizing temperatures up to 80 °C: Water
For crystallizing temperatures up to 150 °C: Liquid paraffin, density 0.87 g/ml to 0.89 g/ml
For crystallizing temperatures up to 260 °C: Silicone fluids
4 Preparation of sample
The sample may have to be dehydrated, or dealt with as received, or as otherwise required by the
specification for the product being tested.
1)
BS 3218, “Test tubes and boiling tubes”.
2) BS 593, “Laboratory thermometers”.
© BSI 11-1999
1
BS 4633 &4634:1970
5 Procedure
5.1 Carry out a trial experiment to determine the approximate crystallizing point. Fill the beaker or Dewar
flask [see 3 1)] with appropriate cooling medium to within 20 mm of the top and regulate the temperature
to between 6 degC and 8 degC below the expected crystallizing point. Remove the inner tube from the
crystallizing point apparatus and place the sample in the test tube (see the specification for the product
being tested). Insert the cork carrying the thermometer and stirrer. If the sample has commenced to
crystallize, warm the tube in the melting bath to about 5 degC above the approximate crystallizing point
so that the crystals melt except for a trace necessary for seeding. Replace the inner tube in its jacket with
the cooling medium maintained 6 degC to 8 degC below the expected crystallizing point. Stir the sample
gently and continuously, add traces of seeding crystals if necessary, and record thermometer readings
at 30 s intervals.
5.2 As soon as the temperature remains constant for five consecutive readings, record this temperature
(corrected for thermometer error) as the crystallizing point.
5.3 If supercooling occurs as shown by a rise in temperature followed by a constant temperature after the
rise, observe this temperature after the rise. A temperature rise of 1 degC is the maximum allowable. If
five consecutive readings constant within the required accuracy limit are not obtained, record six readings
commencing with the point at which the maximum temperature is first attained. Plot the complete cooling
curve of temperature against time, and draw a straight line to lie evenly between the first and second and
between the fifth and sixth points mentioned above. Extend this line to meet the section of the cooling curve
before the temperature rise. Report the temperature corresponding to the point of intersection, corrected
for the thermometer error, as the crystallizing point.
2 --`,,``,`-`-`,,`,,`,`,,`--- © BSI 11-1999

BS 4633 & 4634:1970
NOTE This drawing shows the apparatus required for crystallizing point temperatures between 10 °C and 260 °C; for crystallizing
point temperatures between – 20 °C and + 10 °C the beaker is replaced by a Dewar flask [see 3 1)].
Figure 1 — Apparatus for determination of crystallizing point
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© BSI 11-1999
3
BS 4633 &4634:1970
BS 4634 Method for the determination of melting point and/or melting range
1 Scope
This British Standard describes a procedure for the determination of melting point and/or melting range
of readily powdered substances that have a well defined melting point, or a well defined melting range; it
is applicable over the temperature range 50 °C to 260 °C.
2 Definitions
For the purposes of this British Standard the following definitions apply:
2.1
melting point
the temperature at which liquefaction of a substance occurs, as indicated by the formation of a definite
meniscus
2.2
melting range
the range between the temperature at which the substance collapses, or forms droplets on the wall of the
capillary tube, and the temperature at which it is completely melted as shown by the disappearance of the
solid phase
3 Apparatus and materials

The following apparatus and materials are required:
1) Melting point tube, thin walled, closed at one end, wall thickness of 0.10–0.15 mm, about 150 mm long
and 0.9–1.1 mm internal diameter. The melting point tube should preferably be stored sealed at both
ends, one end being cut off when required.
NOTE Since some compounds containing hydroxyl groups, or which are capable of muta-rotation or of undergoing hydrolysis or
keto-enol transformation, may melt at a lower temperature in soda glass tubes than in borosilicate glass tubes, the latter should
be used for such compounds.
2) Heating bath, of borosilicate glass, of suitable construction and capacity, and of such height as to hold
not less than a 140 mm depth of liquid. The bath should be provided with a suitable stirrer capable of
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rapidly mixing the liquid, and should be heated by a controllable source of heat, such as gas or electricity.
The use of a draught screen is recommended.
It has been shown that, at higher temperatures where gas heating is used, and the hot gases rise up the
sides of the melting point bath and heat the walls, an unacceptable temperature gradient may be set up
between the liquid in contact with the wall and the liquid at the centre of the bath. This can be
prevented by standing the bath on a sheet of non-asbestos, heat resistant board which projects
at least 100 mm beyond the walls of the bath. A hole slightly smaller than the base of the bath is cut in
the centre of the board so that the bottom of the bath can be heated.
Similarly if electric heating is used, the heating of the walls of the bath should be avoided.
3) Thermometers, accurately standardized of suitable range and accuracy, calibrated for 100 mm
immersion and complying with Series B of BS 5933), unless otherwise required by the specification for
the product being tested.
4) Mortar, of porcelain, glass or agate, approximately 50 mm diameter, with suitable pestle.
5) Magnifying glass (optional).
6) Heating media. The following heating media are in common use:
For temperatures up to 80 °C: Water
For temperatures above 80 °C and up to 150 °C: Liquid paraffin, density 0.87 g/ml to 0.89 g/ml
For temperatures above 150 °C and up to 260 °C: Silicone fluids
3)
BS 593,”Laboratory thermometers”.
4 © BSI 11-1999
BS 4633 & 4634:1970
4 Procedure
Grind the sample in the mortar to a fine powder, taking care to avoid any contamination, if necessary using
reduced pressure and/or a dessicant, and dry the powder at a temperature well below its melting point
unless otherwise required by the specification for the product being tested.
Transfer a sufficient quantity of the dried powder to a clean, dry melting point tube, and pack the powder
by tapping the tube on a hard surface or by rubbing the outside of the capillary tube with a file, so as to
form a compact column 4 mm to 6 mm high.
Fill the heating bath with the heating medium to the appropriate depth, insert the thermometer to the
proper immersion and heat the bath with constant stirring. When the temperature of the bath is 20 degC
below the expected melting point, adjust the rate of heat input so that the temperature of the bath increases
by 3 degC per minute or at such a rate as required by the specification of the product. At 10 degC below the
expected melting point attach the filled melting point tube to the thermometer in such a way that the
sample is in close proximity to the thermometer bulb. Use surface tension or some other means, e.g. a
rubber band or the device illustrated in Figure 1, to effect this attachment.
Continue heating at a rate of 2 degC per minute, with constant stirring, and record either the melting point
or the melting range as required. Record also the temperature of the emergent stem of the thermometer by
placing the bulb of a second thermometer in contact with the emergent stem at a point approximately
midway along the mercury thread in the emergent stem of the test thermometer.
If the recorded melting point or the lower temperature of the melting range is less than 7 degC above the
temperature at which the sample was inserted, repeat the determination, inserting the sample into the
bath at a correspondingly lower temperature.
5 Calculation
Correct the observed temperature(s) for any error in the calibration of the thermometer(s) and, if required,
for the difference in the emergent stem temperature under the conditions of calibration and of use, using
the following equation:
tc = 0.000 16 n (ts – td)
where tc = correction (positive or negative) to be applied to the observed temperature of the melting
point,
ts = mean temperature of the emergent stem when calibrated (see Note).
td = mean temperature of the emergent stem at the observed melting point, and
n = length of the exposed stem expressed in degrees Celsius.
NOTE The specified mean temperature for n degC of emergent stem of a partial immersion thermometer when calibrated may
usually be found by reference to the appropriate specification for the thermometer.
6 Reporting
Report the corrected temperature(s) to the nearest 0.1 degC, unless otherwise required, as the melting
point or the melting range of the sample, whichever is required, stating whether the result is on a “dried”
or “undried” basis.
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© BSI 11-1999
5
BS 4633 &4634:1970
Figure 1 — Device suitable for holding a number of capillary tubes in close proximity to the
thermometer
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6 © BSI 11-1999
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blank
BS 4633 &
4634:1970
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BRITISH STANDARD BS 4633 &

Copyright British Standards Institution

The committee entrusted with the preparation of these British Standards

These British Standards, having

ISBN 580 06273 2

Copyright British Standards Institution

These standards make reference to the following British Standards:

BS 3218, Test tubes and boiling tubes.

BS 4633 Method for the determination of crystallizing point

3 Apparatus and materials

2 --`,,``,`-`-`,,`,,`,`,,`--- © BSI 11-1999

3 Apparatus and materials

Copyright British Standards Institution

British Standards are updated by amendment or revision. Users of

In response to orders for international standards, it is BSI policy to supply the

BSI provides a wide range of information on national, European and

Subscribing members of BSI are kept up to date with standards developments

If permission is granted, the terms may include royalty payments or a licensing

Copyright British Standards Institution

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