Contents

Introduction 2

Methods of Measuring Melting Point 2

The Capillary Method 3

Techniques for refractory materials 4

Sample Preparation 5

References 5

Introduction:
1
Determining the melting point of a compound is one way to test if
the substance is pure. A pure substance generally has a melting
range (the difference between the temperature where the sample
starts to melt and the temperature where melting is complete) of
one or two degrees. Impurities tend to depress and broaden the
melting range so the purified sample should have a higher and
smaller melting range than the original, impure sample.

Methods of Measuring Melting Point:

There are a variety of methods that you can use to determine the
melting point of a sample. The most common and most basic
method of determination is the capillary method. This method
involves placing the sample in a capillary tube and running an
experiment that will heat the sample until it reaches melting
point. The melting point can then be recorded.

There are a few ways in which you can set up an experiment with
the capillary method. The first is a manual apparatus set up with
the aim of heating up a sample inside a capillary tube whilst
visually looking for when the sample has melted. The concept
involves placing a small amount of the substance in a capillary
tube and joining this to a thermometer. The capillary tube is then
placed into a heating bath and the experiment is conducted. If you
don’t have a heating bath, you can use Mineral Oil in a Thiele
Tube and heat the tube with a Bunsen Burner. It is important to
heat the sample slowly using this method so that a thermal
equilibrium can be established.

2
A more modern way of using the capillary method is to use a
device called a Melting Point Apparatus. This device uses the same
concept of heating a sample in a capillary tube but makes the
process far simpler and quicker. There are many different types of
Melting Point Apparatus machines and they range in functionality
and accuracy. At a basic level, the machine is designed so that a
capillary tube with the sample can be inserted into the device and
rapidly heated to a set temperature. Generally, you will heat the
capillary tube to near melting point and then decrease the speed
of the temperature increase so that you can observe when the
sample melts. Observation is generally conducted through a
viewing eyepiece. A Melting Point Apparatus will more than likely
have the temperature displayed in digital format for easy
recording of data.

The Capillary Method:

The melting point measurement is usually performed in thin glass
capillary tubes with an internal diameter of 1 mm and a wall
thickness of 0.1 – 0.2 mm. A finely-ground sample is placed in the
capillary tube to a filling level of 2 – 3 mm and introduced in a
heated stand (liquid bath or metal block) in close proximity to a
high accuracy thermometer. The temperature in the heating stand
is ramped at a user-programmable fixed rate. The melting process
is visually inspected to determine the melting point of the sample.
Modern instruments, like the Melting Point Excellence
instruments, enable automated detection of the melting point and
melting range and visual inspection by a video camera. The
capillary method is required in many local pharmacopeias as the
standard technique for melting point determination.
3
Techniques for refractory materials:
For refractory materials (e.g. platinum, tungsten, tantalum, some
carbides and nitrides, etc.) the extremely high melting point
(typically considered to be above, say, 1,800 °C) may be
determined by heating the material in a black body furnace and
measuring the black-body temperature with an optical pyrometer.
For the highest melting materials, this may require extrapolation
by several hundred degrees. The spectral radiance from an
incandescent body is known to be a function of its temperature.
An optical pyrometer matches the radiance of a body under study
to the radiance of a source that has been previously calibrated as
a function of temperature. In this way, the measurement of the
absolute magnitude of the intensity of radiation is unnecessary.
However, known temperatures must be used to determine the
calibration of the pyrometer. For temperatures above the
calibration range of the source, an extrapolation technique must
be employed. This extrapolation is accomplished by using Planck's
law of radiation. The constants in this equation are not known
with sufficient accuracy, causing errors in the extrapolation to
become larger at higher temperatures. However, standard
techniques have been developed to perform this extrapolation.

4
Sample Preparation:
Firstly, you must ensure that the sample is fully dry and in
powdered form. Then with your capillary tube, use the open end
of the tube to press down gently on the sample several times. You
then need to get the powder all the way to the bottom of the
capillary tube by tapping the closed-end multiple times on a hard
surface so that the sample is compacted down at the closed end
of the tube (you could also use a method where you drop the tube
multiple times through a glass tube approx. 1m in length). For
further accuracy, you can use a packing wire to further compact
the sample. Note that the sample height should be between 2 and
3mm to ensure best results.

References:
 Byjus
 Slideshare
 ScienceDirect
 pharmacopeia