Method Colorimetric, Sodium Tetrachloromercurate [IS 5182 (Part II)]

Principle

When sulphur dioxide from the air stream is absorbed in sodium tetrachloromercurate
solution it forms a stable dichlorosulphitomercurate. The amount of sulphur dioxide is then
estimated by the colour produced when p-rosaniline hydrochloride is added to the solution.
The colour is estimated by a reading from an absorption meter or spectrophotometer for
which a calibration curve has already been prepared.

Reagents
1. Absorbing Solution: - Dissolve 27.2 gm (0.1 mole) mercuric chloride and 11.7 gm (0.2
mole) sodium chloride in 1 litre of distilled water. This solution may be stored at room
temperature for several months.
2. P-Rosaniline Hydrochloride: - Dissolve 0.2 gm of p-rosaniline hydrochloride in 100 ml
of distilled water and filter his solution after 48 hours. This solution is stable for at leas 3
month if stored in the dark and kept cool. Pipette 20 ml of this into a 100-ml volumetric
flask. Add 6 ml of concentrated hydrochloric acid. Allow standing for 5 minutes then
dilute to mark with distilled water. It is stable for about 2 weeks if refrigerated.

3. Formaldehyde Solution: - 0.2%, dilute 5 ml of 40% formaldehyde solution to 1 litre with

distilled water. Prepare weekly.
4. Standard Sodium Sulphite Solution: - Dissolve 640 mg of sodium metabishulphite
(assay 65.5% as SO2) in 1 litre of distilled water. This yields solution of approximately
0.40 mg/ml as SO2. The solution should be standardised by titration with standard
0.01N iodine with starch as indicator and should be adjusted to 0.0123 N. then 1 ml is
equivalent to 150 ug of sulphur dioxide. Prepare and standardize freshly.

5. Starch Solution: - Make a thin paste of 1.25 gm of soluble starch in cold water and pour
into 500 ml of boiling water while stirring. Boil for a few minutes. Keep in glass
stoppered bottle.

6. Iodine Solution: - 0.01 N, freshly standardised.

Preparation of Calibration Curve: - Pipette exactly 2 ml of standard sulphite solution into a

100-ml volumetric flask and dilute to make with absorbing reagent. This final solution
contains 3.0 ug of sulphur dioxide per milliliter.

Add accurately 0.5, 1.0, 1.5 and 2.0 ml portion of the dilute standard sulphite solution to a
series of 10 ml volumetric flask and dilute to the marks with absorbing reagent and proceed
as given bellow: Procedure
If mercury precipitate is present, remove by filtration or centrifugation. To the clear sample
adjusted to 10 ml with distilled water for evaporation losses, add 1.0 ml of p-rosaniline
solution and 1.0 ml formaldehyde solution and mix well, take a 10 ml portion of unexposed
sodium tetrachloromercurate solution for use as the blank. After 20 minutes read the
absorbance at 560 nm.
Calculation
SO2 ug/m3 = g/ml x 50 / V

Where,
50

absorbing solution in impinger for collection of sample

Volume of air in m3