DEON MUNASHE KUMUKWAYA

20BBT1312

Aim: Chloride &Sulfate Estimation

Introduction

Suspended dust is collected from the air using an air mover like that on a vacuum cleaner. The
dust samples are collected on a flat sheet of filter paper. Initially glass fiber filter paper was
used as the collecting medium. These papers are made using a resin binder and then flash fired
to remove the binder. The batch of papers we first received was free from soluble chlorides,
sulphates, and nitrates. Later batches of paper were found to be extremely high in water
soluble chloride. The quantities of these materials initially present on paper were larger than
the amount of material which would be found in a typical air

sample. The variation in amounts of chloride between different s h e e t s within the same batch
was also high. The manufacturer explained the change as resulting from the use of a different
grade of glass fiber. Subsequent glass fiber papers sent us were represented as being low in
chloride content, however, the values were high enough to make these

papers unacceptable for our use.

Sulphate

The water-soluble sulphates are determined using a modified turbidimetric procedure. Some
difficulty was encountered because of a yellow coloration of water extracts which led to high
values in the turbidimetric determination. The resin treatment of the extract effectively
removed this color. The color may have been the result of ferrous chlorides present as

such or formed from ferrous sulphide. The initial water extracts did show a large amount of
ferrous ion present. On standing, a solution of ferrous sulphide and sodium chloride develops

the same color as was found in our samples due to the dissociation of FeS to form FeCl2. The
color in extracts of air samples became similarly more intense on standing.

In the sulphate determination 10 ml (about 0.34 oz). of sample extract are added to 10ml
(about 0.34 oz). of water in a 1U0 ml (about 0 oz). Erlenmeyer flask. To this is added 1 ml (about
0.03 oz). of 10 N HC1 and 1 ml. of a 1 to 2 glycerin

alcohol mixture. The solutions are mixed and the flask placed on a rotary agitator.
Approximately 0.25 g. of barium chloride is then measured into the flask with an appropriately
sized scoop and the flask shaken for 1 min. About 12 samples may be conveniently handled at
one time. After 40 min. the optical density is determined at 500 /x. A Spectronic20 colorimeter
and 1 in. cuvettes were used. A calibration curve from known amounts of sulphate is
determined in a similar manner in the range of 100- 1000mmg. in 10 ml. of solution. If total
Sulphur as sulphates is desired the sample may be first treated with

some bromine water, the solution heated to expel excess bromine and the sulphate
determination made as above. The uniform shaking with a mechanical agitator was found
necessary to obtain reproducible results.

Chloride Determination

The use of a silver turbidimetric procedure <6) for estimation of chloride resulted in values high
as compared with a mercurimetrictitration(7). Since the presence of sulphide in our samples
was indicated, it was felt the high results could be explained by the formation of silver sulphide.
The Mercuri metric procedure (7> was adopted since there appeared to be less interferences
and the procedure is more convenient and rapid. In this procedure 50 ml. of

The water extract was treated with 3 drops of 30% hydrogen peroxide and the solution then
titrated with mercuric nitrate using a diphenyl carbazone indicator. The peroxide treatment is
necessary to oxidize any sulphites present in the sample. Ferric ions will interfere in this
procedure but are removed by the preliminary treatment of the extract with ion exchange
resin.