EXPERIMENT 4

DETERMINATION OF THE PURITY OF A SODIUM SULPHATE SAMPLE BY

GRAVIMETRIC ANALYSIS

Objective
To determine the purity of sodium sulphate in a sample.

Introduction
Sulphate ion can be determined gravimetrically by precipitating it in aqueous solution by barium
ion.

Ba2+(aq) + SO42-(aq)  BaSO4(s)

Sulphates are precipitated in acidic solution for two reasons. First, the presence of acid results
in the formation of larger crystals of barium sulphate. Secondly, acidic solution prevents the
precipitation of other anions, such as carbonates. These anions might present as impurities in
real samples.

In this experiment, the sulphate ions in a sodium sulphate sample will be precipitated as barium
sulphate. The mass of the barium sulphate obtained will be used to calculate the purity of the
sample.

Apparatus
400 mL beaker
Burette
Filter funnel
Conical flask
Rubber policeman
Filter paper

Chemicals
Sodium sulphate
0.25 M Barium chloride solution
Concentrated HCl
Silver nitrate solution
Procedure

(a) Precipitating stage

1. Weigh accurately about 0.6 g of sodium sulphate given and dissolve it in 20 mL

distilled water in a 400 mL beaker.
2. Heat the solution until all the sodium sulphate dissolves. Acidify the solution with 0.5
mL concentrated HCl.
3. Dilute the solution to 250 mL. Continue heating the dilute solution to 80oC.
4. Slowly, add to the hot solution, 20 mL of 0.25 M BaCl2 from the burette whilst stirring
the solution.
5. Cover the beaker with a watch glass and place it in a water bath for one hour.

(b) Filtration and washing the precipitate

1. Weigh a filter paper. Record its mass.

2. Without stirring the solution in the beaker, pour the supernatant onto the filter paper,
leaving behind as much precipitate as possible.
3. Wash the precipitate in the beaker with 100 mL warm distilled water. Pour the
supernatant again onto the filter paper. Repeat these steps once and then transfer
the precipitate quantitatively onto the filter paper. This can be done with the help of a
rubber policeman and a wash bottle.
4. Wash the precipitate in the funnel with warm distilled water until there is no more
chloride ion detected in the filtrate. Use silver nitrate solution to test the presence of
chloride ion.

(c) Drying and weighing the product

1. Allow the filter paper and the precipitate to dry.

2. Weigh the filter paper with its content and get the constant mass of the precipitate.
Record the mass of the product and perform the calculation as shown in the Results
section of this experiment.
RESULTS

Data

Mass of the sodium sulphate sample = ………………

Mass of the filter paper = …………………

Mass of filter paper + precipitate = …………………

Calculations

1. Calculate the mass of the BaSO4 precipitate obtained.

2. Calculate the actual mass of sodium sulphate in the sample.

3. Calculate the purity of the sodium sulphate sample.

QUESTION

Assuming that the sodium sulphate sample is 100% pure, calculate the volume of 0.25 M BaCl2
required to precipitate all the sulphate in it. (as in step 4 in the precipitation stage in the
experiment)