Assay of copper sulphate by Iodometry

BACKGROUND

An assay is an investigation of an analyte with a proper procedure in medicines,

pharmacology, environmental and molecular biology for qualitative and quantitative
measurement of the presence of the amount, or functional activity of the targeted entity.

The assay is done on the basis of the oxidation-reduction reaction of iodine/thiosulphate. A

solution of copper sulphate is first treated with potassium iodide and acetic acid. Cuprous
iodide (CuI) is formed with iodine and the liberated iodine is titrated with 0.1 N sodium
thiosulphate. copper sulphate is assayed by iodometric method. Reducing agent KI is added
in presence of Acetic Acid to form cupric iodide. Acetic acid is added to form a weakly acidic
solution.
Cupric iodide is unstable and decomposes into cuprous iodide and Iodine. The liberated
iodine is titrated with sodium thiosulphate in the solution becomes yellow. Most of the
liberated iodine is reacted with sodium thiosulphate, little amount is left (indicated by yellow
colour).

Starch mucilage is added towards the end because it forms a stable Complex with excess of
Iodine. The decomposition of cupric iodide in to cuprous iodide and Iodine is reversible,
hence to make quantitative, Potassium thiocyanate is added which reacts with the reaction
product, cuprous iodide, to form cuprous thiocyanate. Potassium thiocyanate is added to
water the end of the titration to avoid errors due to absorption of iodine by cuprous
thiocyanate.

Each ml of 0.1 normal Na2S2O3 is equivalent to 0.02497 gm of CuSO4.5H2O

Reaction:

Eq. wt. of sodium thio-sulphate (Na2S2O3. 5H2O): 248.18

Eq. wt. of copper sulphate (CuSO4. 5H2O): 249.68

i.e. Each ml of 0.1 N sodium thiosulfate is equivalent to 24.968 mg of CuSO4 · 5H2O.

Preparations:

1. Standard 0.1 N sodium thiosulphate solution-

2.48 g sodium thiosulfate pentahydrate (Na2S2O3.5H2O) or 15.8 g anhydrous sodium

thiosulfate (Na2S2O3) is dissolved in 100 ml water. 0.01 g anhydrous sodium carbonate and
0.4 ml chloroform are added to stabilize the solution. It is mixed thoroughly by shaking or by
aerating with nitrogen for about 15 min, and stored in a glass-stoppered, reagent bottle.
2. Starch Indicator Solution-

1 g of corn or potato starch is added into 10 ml of distilled water, well-shaken and poured
into 100 ml of boiling distilled water. The solution is stirred thoroughly and boiled for 1
minute. Then it is left in air to cool down. If the precipitate forms, the supernatant is
decanted and used as the indicator solution.

REQUIREMENTS
Chemicals: Copper sulphate, Potassium iodide, Acetic acid, Sodium thiosulphate, Starch
solution, Sodium thiocyanate.

Apparatus: Volumetric flask, Iodine flask

PROCEDURE
Weigh accurately 1 gm of copper sulphate and dissolve in water (50 ml), add
potassium iodide (3 gm) and acetic acid (5 ml) and titrate the liberated iodine with 0.1
normal sodium thiosulphate light yellow colour is obtained. At this stage starch mucilage
and potassium thiocyanate (2 gm) are added at the titration is continued until blue colour
disappears. A blank determination is noted following the similar procedure and taking
distilled water in place of test solution, to minimise the error.