C 241 (Experiment No.

___________)

NAME:________________________ BATCH:________

ROLL NO:_____________________ SEM:________

SIGNATURE:__________________ DATE:________

STANDARDIZATION OF SODIUM THIOSULPHATE SOLUTION AND VOLUMETRIC

ESTIMATION OF Cu(II) IODOMETRICALLY

AIM
To determine the amount of Cu(II) in an unknown sample by iodometry.

THEORY
Iodometry refers to the titration of iodine liberated in a quantitative redox reaction by a standard
solution of a reducing agent like sodium thiosulphate. In iodometry, an aqueous solution of
potassium iodide is added to an acidic solution. Oxidants can oxidize iodide quantitatively and
rapidly, liberating an equivalent amount of iodine, which is then determined by titration with
sodium thiosulphate solution, which has been standardized. Oxidants having higher standard
reduction potential than iodine can quantitatvely and rapidly oxidize iodide to iodine usually in acid
medium.

[Note: In iodometry a species is titrated with an iodide solution and then the released iodine is
titrated with thiosulphate whereas in iodimetry, a species is directly titrated with an iodine solution.
Therefore, iodometry is an indirect method and iodimetry is a direct method. Iodometry can be used
to quantify oxidizing agents, whereas iodimetry can be used to quantify reducing agents.]

By using the standard thiosulphate solution copper in a solution of cupric salt has to be determined
iodometrically (eq-1).
2 Cu2+ + 4I‾ 2CuI↓ + I2
As a result of the precipitation of cuprous iodide, the formal potential of the Cu2+/Cu+ rises to about
0.858V [from E0(Cu2+/Cu+) = 0.15 V], consequently Cu2+ oxidizes iodide to iodine [E0(I2/2I‾) =
0.54V] quantitatively and the liberated iodine is then titrated with standard sodium thiosulphate
solution using starch as indicator.

MATERIALS REQUIRED
Sodium thiosulphate, Potassium dichromate (N/10), copper sulfate pentahydrate, Glacial acetic
acid, NH4OH (1:1), Ammonium thiocyanate (2.0%), sodium hydrogen carbonate, Conc. HCl, KI
(20%), starch (1.0%), burette, pipette, conical flask, measuring cylinder, dropper and distilled water
etc.

Step 1: Standardization of Na2S2O5.5H2O (hypo) solution with standard K2Cr2O7 solution

As the thiosulphate is a secondary standard solution, it has to be standardized by titrating against a
primary standard dichromate solution iodometrically using starch indicator.
Procedure:
1. Pipette out 10 mL of standard K2Cr2O7 solution in a 250 mL conical flask.
2. Add 1 mL of 20% KI followed by 2 gm of NaHCO3 and 5 mL of conc. HCl.
3. Swirl the mixture well, cover with watch glass and stand it for 5 min. in dark place to ensure
complete liberation of iodine.
4. Wash down the watch glass and sides of the flask with distilled water and dilute it to ~100 mL.
5. Then immediately titrate the solution against thiosulphate until the brown color fades to straw
yellow.
6. Add 2 mL of 1% freshly prepared starch solution shake the solution to obtain a deep blue color.
7. The titration is continued with continuous shaking until the blue color just disappears leaving a
bright green solution.
8. Note the end point and repeat the process till three concurrent readings are obtained.
9. Calculate the strength of thiosulphate solution (N1V1=N2V2).

S.No. Volume of K2Cr2O7 Burette Readings(mL) Volume of thiosulphate

taken (mL) Initial Final consumed (mL)

Step 2: Estimation of copper in a solution of CuSO4. 5H2O.

1. Pipette out 10 ml of supplied cupric salt solution into a 250 mL conical flask.
2. Add 1:1 NH4OH/H2O drop wise with constant shaking until a greenish white precipitate
appears.
3. Then, add 5 ml of glacial acetic acid to dissolve the precipitate.
4. Cool the solution and add 5 ml of 20% KI.
5. Swirl the mixture well, cover with watch glass and stand it for 5 min. in dark place to ensure
complete liberation of iodine.
6. Wash down the watch glass and sides of the flask with distilled water and dilute it to ~100 mL.
7. Then immediately titrate the solution against thiosulphate until the brown color fades to straw
yellow.
8. Add 2 mL of 1% freshly prepared starch solution shake the solution to obtain a deep blue color.
9. The titration is continued with continuous shaking until the blue color just fades to pale blue.
10. Add 20 ml of 2% aq. solution of NH4CNS and shake the mixture well to deepen the blue color.
11. Add sodium thiosulphate drop by drop with constant shaking until the blue color just disappears
leaving a milky white solution.
12. Note the reading and tabulate the results.
13. Repeat the procedure to get concordant results.

S.No. Volume of cupric Burette Readings(mL) Volume of thiosulphate

solution taken (mL) Initial Final consumed (mL)

OBSERVATIONS AND CALCULATIONS

1. Calculate the strength of thiosulphate and cupric salt solution
2. Estimate the amount of copper in the supplied cupric salt solution.

RESULTS
1. Strength of thiosulphate solution = __________
2. Strength of cupric solution = _______
3. Amount of copper present in the supplied cupric salt solution = ___________