TITRATION OF IODINE WITH STANDARD THISULPHATE SOLUTION GENERAL DISCUSSION: Oxidation and reduction titration involving Iodine is known

as Iodometric titration .The indirect iodometric titration method deals with the titration of iodine liberated in chemical reactions .In this experiment iodide ions are oxidized into iodine .The liberated iodide (I2) ,when titrated with standard sodium thiosulphate oxidizes the latter while itself gets reduced to iodide ions. 2Cu2+ + 4II2 + 2S2O32 2I2CuI2 (unstable) + S4O62Cu2I2 + I2

The latter reaction can be used to determine the amount of iodine librated in chemical reaction. In iodide-thiosulphate titration thiosulphate solution is run from burette. In these circumstances, the colour changes from intense yellow or brown (colour I 2) to a colorless (colour of I-) at the end point. The end point is made visible by the use of a solution of starch as indicator. Starch reacts with iodide in the presence of iodide ions to form an intensely blue-colored complex. At the end point i.e .when there is no iodine (I 2) starch gives colorless solution. Though starch is inexpensive its main disadvantage is that it adsorbs iodine and gives a water-insoluble complex and titration becomes less accurate. For this reason, in titration of iodine the starch should not be added until just before the end point when the colour beings to fade i.e. the solution becomes light yellow. Another point to remember is that evolved iodine is lost due to its appreciable volatility. Therefore titration should not be prolonged unnecessarily. Titration should be performed in cold solution in conical flasks and not in open beakers. Mouth of the conical flasks containing iodine should be covered with watch glass to check the loss of iodine by evaporation and at the beginning of the titration evaporated iodine should be transferred back to conical flask by rinsing the watch glass with water and collecting the water in the conical flask. Another important source of error in this titration is the oxidation of acid solution of iodide by oxygen from the air: 4I- + O2 +4H+ 2I2 + 2H2O

This reaction is catalyzed by certain metal ions of variable valency (particularly copper) by NO2- and also by strong sunlight. Therefore, iodine solution should be kept in dark and titration should not be performed in excess light.

EXPERIMENT: TO ESTIMATE THE AMOUNT OF COPPER IN A GIVEN SAMPLE OF COPPER (II) SULPHATE BY IODOMETRIC TITRATION. APPARATUS: Burette, Pipette, Conical flask, Watch glass THEORY: A known weight of supplied cupper (II) sulplate crystals is dissolved in water and certain volume of this solution is treated with excess potassium iodine solution. The unstable copper (II) iodide (CuI2) formed decomposes to give copper (I) iodide (Cu 2I2) and free iodine. The liberated iodine is titrated with standard sodium thiosulphate solution. 2Cu2+ + 4II2 + 2S2O322CuI2 S4O62Cu2I2 + I2 + 2I-

From above reactions it follows that: 2 moles of Cu2+ 1 mole of I2 i.e

2 moles of S2O32-

1 moles of Cu2+ 1 mole of S2O32-

By calculating the number of moles of thiosulphate ions consumed in the titration the number of moles of copper and the amount of copper also can be determined. (Relative atomic mass of Cu=63.546) PROCEDURE: 1. Fill up the burette with standard (0.1 M) Na2S2O3 solution. 2. Weigh out accurately 6.24g of CuSO4 crystals and dissolve it in water in 250cm3volumetric flask. Add about 2 cm3 of dil. Sulfuric acid to the solution (to remove turbidity due to hydrolysis of the salt) and add more water to make up the volume upto the mark. Shake the solution well to make it homogeneous. 3. Take 10cm3 of copper (II) sulphate solution in a conical flask; add ammonia solution drop by drop until little turbidity is seen. Add acetic acid dropwise to redissolve the turbidity .This is done to remove mineral acid (H2SO4) present in the solution otherwise in the presence of mineral acid iodide ions are oxalised into iodine. 4. Add 5.0cm3 of (1.0 M) KI solution to the flask, cover its mouth with watch glass and keep the flask in dark for at least 5 minutes .Liberated iodine is volatile .Therefore, it condenses on the watch glass surface. Transfer this iodine into the flask by washing it with water and collecting the water in the flask. 5. Now run the standard thiosulphate solution from the burette until the deep brown colour of iodine turns into pale yellow colour.Then add about 1cm 3 of starch solution (as an indicator )to obtain blue colour. Again run the thiosulphate solution dropwise until the blue colour of the solution just disappears.

6. Repeat the process (procedure no.3 to 5) to obtain at least two concurrent reading. OBSERVATION: Concentration of sodium thiosulphate (Na2S2O3) solution=

No. Volume of CuSo4 solution taken Initial final

Burette Reading difference Concurrent reading

Titration summary: Iodine liberated from ____________ cm 3 copper (II) sulphate solution consumed _______________ cm3 of 0.1M sodium thiosulphate (Na2S2 O3) solution.

RESULT: amount of copper in _____ g of Copper (II) sulphate crystals is__________ g.

Percentage Amount of copper (by weight) in copper (II) sulphate is ____________

SPACE FOR CALCULATION: