Expt No.

1 Titrimetric Analysis (Redox Reactions) Determination of concentration/molarity of KMnO4 Aim: To determine the concentration/molarity of KMnO4 solution by titrating it against a 0.1 M standard solution of oxalic acid. Theory: Potassium permanganate acts as a powerful oxidising agent. The oxidising action of KMnO4 in the acidic medium can be represented by the following equation. MnO4- + 8H+ + 5eMn2+ + 4H2O The acid used in the titration is dilute sulphuric acid. Nitric acid is not used as it is itself an oxidising agent and hydrochloric acid is usually avoided because it reacts with KMnO4 according to produce chlorine which is also an oxidising agent in the aqueous solution. Since oxalic acid acts as a reducing agent, it can be titrated against KMnO4 in the acidic medium according to the equation on the left hand side. Chemical equation: 2 KMnO4 + 3H2SO4 + 5H2C2O4 Ionic equation: MnO4- + 5C2O42- + 16H+ K2SO4 + 2MnSO4 + 8H2O + 10CO2 2Mn2+ + 10CO2 + 8H2O

In these equations MnO4- is reduced to Mn2+ and C2O42- is oxidised to CO2. The oxidation number of carbon changes from +3 to +4. Procedure: A. Preparation of 0.1 M standard solution of oxalic acid. Weigh exactly 3.15 g of oxalic acid in a weighing bottle using a digital balanceand transfer in to a 250 mL standard measuring flask using a funnel and a glass rod. Wash the funnel many times and dissolve the oxalic acid by swirling the measuring flask. Make up the solution to the mark with the help of a pipette or dropper. B. Titration of oxalic acid solution against potassium permanganate solution (i) Rinse and fill a clean burette with potassium permanganate solution. Remove the air bubble if any, from the nozzle. (ii) Take 10ml of 0.1 M oxalic acid solution in a conical flask and add half of the test tube full of 1.0 M H2SO4 to it to prevent the formation of any precipitate of manganese dioxide during the course of the titration. (iii) Heat the oxalic acid solution upto 50 to 60 before titrating it with potassium permanganate solution. (iv) Note the initial reading of the volume of permanganate solution in the burette and add it in small volumes to the hot oxalic acid solution while swirling the contents of the flask gently. The end point is indicated by the appearance of permanent pale pink colour due to a slight excess of potassium permanganate solution. (v) Repeat the titration for concordant values are obtained. Record the readings and calculate the strength of potassium permanganate solution in mols/litre. Observation and calculations: Sl.No. Volume of oxalic acid in mL Burette readings Initial (x) 1. 2. 3. final (y) Volume of KMnO4 used V= (y-x) mL

The strength of the unknown solution in terms of molarity may be determined by the following equation a1M1V1 = a2M2V2 For oxalic acid vs potassium permanganate titration: a1 = 2; a2 = 5; M1 and M2 are the molarities of oxalic acid and potassium permanganate solutions; V1 and V2 are the volumes of oxalic acid and potassium permanganate solutions. a1M1V1 = a2M2V2 2M1V1 = 5M2V2 M2 = 2M1V1 5V2 Strength = Molarity X Molar mass Result: Molarity of KMnO4 solution is Strength of KMnO4 solution is Expt No.2 Determination of concentration and molarity of KMnO4 solution Aim: To determine the concentration and molarity of KMnO4 solution by titrating it against standard solution of ferrous ammonium sulphate. Theory: FAS acts as a reducing agent in the titration against KMnO4. The reaction is as given in the left hand side. 2 KMnO4 + 8H2SO4 + 10FeSO4(NH4)2SO4.6H2O K2SO4 + 2MnSO4 + 5Fe2(SO4)3 + 10(NH4)2SO4 +68H2O

The oxidation number of iron in Mohrs salt is +2. Iron is oxidised during the reaction and its oxidation number changes from +2 to +3. In this titration heating of FAS is not required because the reaction rate is very high even at room temperature. Procedure: A. Preparation of 0.05 M standard solution of FAS (Molar mass of FeSO4(NH4)2SO4.6H2O = 392g mol-1) (i) Weigh 4.9000 g of FAS and transfer it into a 250 mL measuring flask through a funnel. (ii) Transfer the solid sticking to the funnel with the help of distilled water into the flask and add dilute sulphuric acid into the flask dropwise to get the clear solution. (iii) Shake the flask till the substance dissolves and make the solution up to the mark. B. Titration of FAS against potassium permanganate solution. (i) Rinse and fill the clean burette with potassium permanganate solution. Remove air bubbles if any from the burette tip. (ii) Take 10 mL of 0.05 M FAS in a conical flask and add half test tube full of sulphuric acid to it. (iii) Titrate the above solution with KMnO4 solution till the colour of the solution changes to permanent pale pink colour. Swirl the contents of the flask during the titration. (iv) Repeat the titration till the concordant value is obtained. (v) Record the readings and calculate the strength of KMnO4 solution in mols/litre. Observation and Calculations: Sl.No. Volume of FAS in mL Burette readings Initial (x) 1. 2. 3. final (y) Volume of KMnO4 used V= (y-x) mL

The strength of the unknown solution in terms of molarity may be determined by the following equation a1M1V1 = a2M2V2 For FAS vs potassium permanganate titration: a1 = 1; a2 = 5; M1 and M2 are the molarities of FAS and potassium permanganate solutions; V1 and V2 are the volumes of FAS and potassium permanganate solutions. a1M1V1 = a2M2V2 1M1V1 = 5M2V2 M2 = 1M1V1 5V2 Strength = Molarity X Molar mass Result: Molarity of KMnO4 solution is _________ Strength of KMnO4 solution is __________

Expt No.3 Preparation of Ferrous Ammonium Sulphate (Mohrs salt) Aim: To prepare double salt ferrous ammonium sulphate Theory: When a mixture containing equimolar proportions of ferrous sulphate and ammonium sulphate is crystallised from its solution, a double salt is formed. FeSO4 + (NH4)2SO4 + 6H2O FeSO4.(NH4)2SO4.6H2O

Fe2+ ions undergo hydrolysis, therefore while preparing aqueous solutions of ferrous sulphate in water 2 3 mL dilute sulphuric acid is added to prevent the hydrolysis of the salt. Procedure: (i) Dissolve 3.5 g of ferrous sulphate and 1.7 g of ammonium sulphate in 5 ml of distilled water contained in a 50 ml conical flask by heating. Add about 0.5 ml of dilute sulphuric acid to the flask and concentrate the solution by heating till the crystallization point is reached. (ii) Allow the mixture to cool to the room temperature slowly. (iii) On cooling, light green crystals of ferrous ammonium sulphate separate out. (iv) Decant the mother liquor and wash the crystals by shaking with very small amounts of 1:1 cold water and alcohol mixture to remove sticking mother liquor. (v) Separate the crystals by filtration wash with alcohol, dry between the folds of filter paper and record the yield. Result: Yield of Mohrs salt is ______g Expt No. 4 Preparation of Potash Alum Aim: To prepare Potassium Aluminium Sulphate (Potash Alum) Theory: When a mixture containing equimolar proportions of potassium sulphate and aluminium sulphate is crystallized from its solution, a double salt is formed. K2SO4 + Al2(SO4)3 + 24 H2O K2SO4.Al2(SO4)3.24H2O

Procedure: (i) Take 10 mL of distilled water in a 50 mL beaker and heat it to about 40C. Dissolve 6.6 g of aluminium sulphate in it and add about 0.4 mL of dilute sulphuric acid. (ii) Weigh 2.4 g of powdered potassium sulphate and transfer it to the above solution. (iii) Heat the solution with constant stirring till potassium sulphate dissolves completely. (iv) Allow the solution to cool to room temperature slowly. (v) On cooling, white crystals of potash alum separate out. (vi) Decant the mother liquor and wash the crystals by gently shaking with 1:1 cold water and alcohol mixture. (vii) Filter the crystals, dry these between the folds of filter paper and note the yield. Result: Yield of potash alum is _______ g.