Experiment (1: Etermination of Elting Oints Purpose

Download as pdf or txt
Download as pdf or txt
You are on page 1of 4

EXPERIMENT (1)

DETERMINATION OF MELTING POINTS


Purpose:
The purpose of this experiment is to determine the melting points of organic
compounds and check the purity of compound.
Theory:
The melting point (m.p)0C of a compound is the temperature at which it changes
from a solid to a liquid. Since this requires that the intermolecular forces that hold the
solid together have to be overcome . The melting point is a physical property
(melting point, boiling point, density, solubility ,etc.) often used to identify
compounds . Usually, chemists can only obtain a melting range of a 2 - 3oC accuracy.

A pure, nonionic, crystalline organic compound usually has a sharp and


characteristic melting point (usually 0.5-1.0 0C range). A mixture of very small
amounts of miscible impurities will produce a depression of the melting point and an
increase in the melting point range .
Melting point range: The interval between the temperature at which a solid sample
just begins to turn to liquid and the temperature at which the entire sample becomes
liquid. or range of temperatures in which the first crystal starts to melt until the
temperature at which the last crystal just disappears.

What are the factors that affect the melting point?

1- Molecular weight
Melting points are higher for higher molecular weight compounds. The reason the
melting point increases with the weight is that it takes more energy to separate larger
molecules from a crystalline structure than it takes to separate smaller ones.

2- The nature of the organic compound s


Ionic compounds, often form crystal lattices in which each ion is surrounded by
ions of the opposite charge ,because of the strength of this electrostatic attraction,.
Breaking up an ionic crystal lattice requires considerable energy as a result, ionic
compounds have high melting points, While the Covalent compounds consist of
molecules rather than ions. Since the attraction between molecules is weaker than is
the attraction between ions, covalent compounds usually have a lower melting point
than ionic compounds. Moreover, some covalent compounds have polar molecules in
which one end is more electronegative than the other, such polar compounds have a
higher melting point than nonpolar molecules .
3-Impurities
Impurities decrease the melting point. ice-salt mixtures. contaminants normally lower
the melting point and broaden the melting point range Pure samples usually have sharp
melting points, for example( 149.5-150)0C, impure samples of the same compounds
melt at lower temperatures and over a wider range, for example 145-1480C .
4-Shape of Molecules
Molecular shape influences the melting point of a substance. If the shape of the
molecules allows them to be packed together in a compact fashion, For example,
symmetrical molecules give compound ( 4- n –propyl benzoic acid ) a higher melting
point than that of ( 4- iso –propyl benzoic acid ) , the molecules of which do not pack
well,

Types of measuring apparatus of melting point:

Fig1:Melting point apparats (old fashion model)


Fig 2: Melting point digital apparatus (new fashion model)

Properties of oil bath


1 )It has a high Boiling point 3000C rather than water (1000C)
2) It does not emit toxic gases
3) It is transparence and you can see the M.P tube through it. It stays pretty clear on
heating.
4) It has high density rather than water
5) It does not decompose
apparatus / Materials:
oil bath( beaker contain oil ) capillary tubes
Thermometer solid organic compounds
Bunsen burner Rubber bands(ring)

Procedure:
1- Take a capillary tube and sealed an open end of capillary tube by inserting the tip
into a Bunsen flame near the base of the flame and turning the tube in your fingers
using benzen burner
2- Place a small amount of the compound (Benzoic acid) in a clean surface. Push the
open end of the capillary tube into the compound as shown in Fig: 3a .
3- Move the powder to the closed end of the capillary tube by tapping it on the
tables . Repeat until the compound occupies 1-2 mm of the capillary tube end Fig:3a.
5- Attach the capillary tube to a thermometer using a thread. And align the bulb of
the thermometer with the closed end of the capillary tube as illustrated in Fig: 3b.
6- put an oil in a beaker and place it over a piece of wire gauze placed over a tripod
stand.
7-. Heat the beaker slowly while constantly stirring the contents using a stirrer to
insure a uniform temperature throughout. Fig: 3c .
8- Note the temperature at which the compound melts and Record the temperature at
which the solid in the capillary tube melts

3a 3b 3c
Figure 3. The set-up for the procedure

Discussion
The amount of sample that you use and the heating rate through the melting range
are critical. If you use too much sample or heat too rapidly you will not get accurate
results. Be patient and do it right the first time.
Once the sample in the capillary melts, don't use it again. If you have to repeat a
measurement for any reason, you must start with a fresh sample in a new capillary.
Questions:

1. Why the content of the beaker (oil bath) is stirring ?


2. Why this method not used for finding the melting points of inorganic compounds?
3. Why could the rate of heating influence the melting point?

You might also like