3
Chemistry
ﻣﺣﺑﺔ رزاق ﻋﻠﻲ: اﺳﺗﺎذ اﻟﻣﺎدة
Lab 5 EXP NO.4
Experiment name / Determination of melting point
PURPOSE
a) Determine the purity of a substance using melting point as physical
property
b) Identify an unknown compound using its melting point
c) Identify an unknown compound using mixture melting point
d) Learn how to obtain an accurate melting point using a Mel-Temp
apparatus
Reasons for determining melting points:
1. The melting point indicates the level of purity of a sample. An impure
compound melts over a wider range of temperatures, usually greater than 2
degrees.
2. The melting point helps to identify unknown samples, narrowing the
number of possibilities, because a pure solid melts reproducibly over a
narrow range of temperatures.
3. The melting point helps to characterize new compounds.
Melting point Definition
When a solid substance is heated, typically it will melt; that is to say, at
some temperature the solid will begin to liquefy and by some slightly higher
temperature all of the solid will have become liquid. The melting point
(actually melting point range) of a compound is then defined as the
temperature at which an observer can first see liquid forming from the solid
to the temperature where the last particle of solid has become liquid. For
example, the melting point of pure sucrose (table sugar) is 185-186C. This
means that as a small sample of sucrose is slowly heated some of the crystals
begin to liquefy at 1850 and all of the crystals have become liquid by 1860C.
3
Chemistry
ﻣﺣﺑﺔ رزاق ﻋﻠﻲ: اﺳﺗﺎذ اﻟﻣﺎدة
Experimental Procedures
A. Preparing the Sample
Place a pea-size mound of one of the listed compounds on a piece of paper
and grind it to a fine powder using a spatula. Use the spatula to push a small
amount of the solid into the open end of a capillary tube. Then drop the
capillary down several times to fill and pack the sample well to cause the
solid to fall to the bottom. Repeat this
step until you have accumulated a sample 2-4 mm (≈ 0.5 cm) high in the
bottom of the tube (see Fig. 1).
B. Taking a Melting Point
1- Fill two capillary tubes each to a depth of 2-4 millimeters with the
compound of interest.
2- Place one of the tubes in the Mel-Tem apparatus and raise the temperature
a relatively fast rate, about 10 °C/minute.
3-Record the range of temperature from the first visible evidence of liquid
(the sample appears moist, or a tiny drop of liquid is observed) to the
complete liquefaction of the sample.
4-Note the temperature at which the compound first begins to melt.
5-Allow the melting point apparatus to cool to about 20 °C below that
temperature, and then insert the second tube. Raise the temperature more
slowly this time, at the rate of about 2 °C/min.
3
Chemistry
ﻣﺣﺑﺔ رزاق ﻋﻠﻲ: اﺳﺗﺎذ اﻟﻣﺎدة
6- Note the temperatures at which: I. the first crystals melt, and; II. at which
the sample has completely melted. This is the melting point range. For
example, a mp range of 164-168 °C average of 166 °C indicates the sample
softened or began to melt at 164 °C and that transition to a liquid was
complete at 168 °C.
Discussion
1- If you were given a known substance for the melting point determination
how could you prove it to be the specific compound and not another
compound with the same melting point ?
2- What is the definition of melting point ?
3- What is the purpose of determining the melting point ?
4- What are the reasons for determining melting point ?
