60 Project – K 7. Double Titration 7.1 Acid - base double titration 7.2 Oxidation Reduction titration 7.3 Calculation of double titration 61 7.1 Acid-Base Double Titration Double Titration : Titration is performed between the two solutions of opposite nature. If A and B are the two Solutions of same nature and normality or concentration of one solution (suppose A ) is known the concentration of solution B cannot be determined directly after titration. In such cases a solution having opposite nature is used is called intermediate solution of both solutions is performed by this. For example to determine the concentration of unknown oxalic acid or hydrochloric acid by standard solution of oxalic acid. In such a case a solution having opposite nature is used in called intermediate solution & the titration. is N/10 & prepare its 25 qubic cm. Solution. Then according to the equation of normality : Standard solution = Intermediate solution At first the titration is performed between A (standard solution) and C (intermediate solution). So that the concentration of solution C is determined. Now the titration is performed between C and B and the concentration of B is determined by calculation. This kind of titration is called ‘Double Titration’. Now find the normality of unknown solution with the help of intermediate solution. According to the equation of normality More pure result are obtaind by the double titration then the single (simple) titration choice of indicator is the double titration – In double titration the choice of indicator depends on the nature of the solution of titration flask. Add that indicator into the solution of titration flask which does not change the colour with the solution of titration flask & produces the pink colour when the solution of burrete is added at the last drop. Formula used in the calculation of double titration : First find the normality of the intermediate solution with the help of standard solution. Suppose that normality of standard solution N1 × V1 = N ′ × V2 1 10 ∵ N1 = ∴ 1 × 25 = N ′ × V2 10 or N′ = ∴ V = 25 & 25 10 × V2 Normality of intermediate solution ( N ′) = 1 25 × 10 V2 ..................... (a) N ′V3 = H 2V4 N′ = Normality of intermediate solution = 25 10 V1 according to the equation (a) = The Volume of intermediate solution which has titration with 25 cubic cm. Solution of unknown solution = 25 ml. Put the above values into the equation of normality Intermediate solution = Unknown solution. V3 25 × V3 = N 2 × 25 10 × V2 25 V3 1 × × = N2 10 V2 25 ∴ , 1 V3 × = N2 10 V2 Normality of unknown solution = N V3 × 10 V2 / 62 were V2 = The volume of intermediate solution which is used with the titration of 25 cubic cm standard solution with the help. of standard solution of sodium carbonate. After that find the normality of unknown solution by performing titration of sulphuric acid with unknown solution of sodium carbonate. Method : (i) To prepare a standard solution of Na2CO3 Required quantity of V3 = The volume of intermediate solution which is used of the titration of 25 cubic cm of solution of unknown concentration. Now, ∵ the concentration of standard solution = ∴ Na2CO3 = 4 ×W × N E for N/10 solution = 53 × 1/ 10 × 1000 gm the concentration in the normality of unknown solution = Equivalent weight × Normality × volume 1000 = 54/4 = 1.325 gm 4 × W × N V3 × E V2 1.325 gm Na2CO3 is required to prepare a 250 qubic cm. Solution of N/10 concentration of Na2CO3 . Concentration of 4 × N × measure × V3 × Value of unknown solution = intermedia te solution which is used with unknown solution The volume of intermedia te E × V2 solution which is used with the known solution of Weight of of subtance Concentration = volume of intermedia t solution which is used with unknown solution The volume of intermedia te V2 solution which is used with the known solution weight of × V3 4 × N × substance Note : The above equation follows only when the standard solution and unknown solution are having same nature & same Volume. Experiment No 1 Object : To prepare a standard solution of sodium carbonate of N/10 concentration and to find the concentration of sodium carbonate of given concentration solution. Principle : In this experiment the normality of surface acid (intermediate solution) is determined Take 1.325 gm Na2CO3 into the clean and dry weighing tube and pour it into a flask of 250 cubic cm. capacity in which distilled water is already present. Some crystals of the substances are left on the wall of the funnel. To pour these crystals into the funnel pour some distilled water in it so that the all substance of funnel goes to the flask, Remove the funnel and stir the flask, that the substance will completely dissolve. Pour that much of water into the flask, which reaches to the marked point of the flask. Titration : Clean the burette with distilled water and wash it with the given sulfuric acid, note the reading. Wash the pipette 2 times with the standard solution of Na2CO3 and fill 25 ml. Na2CO3 solution into the titration flask by the measuring flask. Add 2 drops of Methyl orange so that the solution becomes yellow colour. Place the titration flask on the burette stand after putting it an the white paper and gradually open the cork to allow the H 2SO4 to fall in it, fix the titration flask and stirr it. At first the colour of the solution is pink after sometime it will be disappeared. Now allow to fall the solution drop by drop. 63 The drop at which the light read colour is not disappeared & it becomes permanent. stop to add the solution at that point & note the reading of burette. This is the end point. Throw the solution of the titration flask, clean it to repeat the experiment upto the two same readings of sulfuric acid is obtained. After that perform the titration of sulfuric acid (intermediate solution) with the solution of Na2CO3 of unknown concentration according to the above method. Observation : solution – (B) Weight of weighing tube + oxalic acid = 8.5776 gm. (C) Weighing tube + left oxalic and = 7.2532 gm. ∴ The weight of Na2CO3 pour into the flask = 8.5776 – 7.2532 = 1.3244 gm. Normality of solution of Na2CO3 4 ×W × N E = = = The titration between intermediate solution (H 2SO4 ) and solution of (Na2CO3 ) of unknown concentration S. No. Volume of 1. Burette Volume Na2CO3 Start End 25.0 ml 0.0 ml 26.8 ml 2. 25.0 ml 0.0 ml 26.4 ml 3. 25.0 ml 0.0 ml 26.4 ml Formula : (1) N1 × V1 4 × 1.3244 × N 53 = (ii) Titration : Table – 1 Standard solution ( Na2CO3 ) and intermediate solution Solution Solution (Na2CO3 ) (H 2SO4 ) (2) Intermediate Solution concentration Solution of unknown (H 2SO4 ) (Na2CO3 ) N2 V2 = Volume of Reading 1. 2. 3. 2.0 ml 25.0 ml 25.0 ml Na2CO3 0.0 ml 0.0 ml 0.0 ml Burette of Start Volume End of acid 25.8 ml 25.6 ml 25.6 ml 25.6 ml N2 V2 Calculation : To calculate normality of standard solution ∵ Normality of Na2CO3 solution = 4 ×W × N E = 5.2976 53 = 4 × 1.3244 × N 53 Standard Solution Solution Intermeditate H 2SO4 S. No. 26.4 ml N2 V2 (2) To calculate the normality of intermediate solution (H 2SO4 ) N1V1 N 2 V2 = 5.2976 53 of acid Standard Intermediate (i) To prepare a standard (A) Weight of the weighing tube = 7.240 gm. ∵ Table – 2 (Na2CO3 ) (H 2SO4 ) 5.2976 × 25 = N 2 × 25.6 53 or N2 = 5.2976 × 25 53 × 25.6 64 (3) To calculate the normality of solution of unknown concentration (Na2CO3 ) – N 2 × V2 or (4) N3 × V3 = Intermediate Solution Solution of unknown concentration (H 2SO4 ) (Na2CO3 ) 5.2975 × 25 26.4 N3 = × 53 × 25.6 25 6. It each titration use some (less) indicator both equal sides. It is difficult to see the change in colour if you use less or more indicator. 7. The intensity of colour which is represented by the indicator at the end point in pair titration is same in both titration. = 0.103 N To determine the concentration of solution of unknown concentration – Concentration (strength) – Normality ×Equivalent weight Concentration of Na2CO3 solution 0.103 × 53 = 5.46 gm / litre Result : (1) Normality of solution of Na2CO3 = 0.103 N (2) Concentration of solution of Na2CO3 = 5.46 gm / litre Indication for titration : 1. Wash the pipette and burette with the given solution. 2. titration. It does not matter if the distilled water is attached with the wall of the titration flask. It is not necessary to dry it because the certain amount of volume is only pour into the flask by pipette. So it don’t effect the result. Note the reading for waiting few seconds after stirring the solution when the end point is found. 3. Note the reading only when the changes in color is appeared at end point, Do not think about the intensity of colour. 4. Do not take the mean of the different volumes obtained in titration. But take that Volume which is at least two times same. 5. It is necessary to wash the titration flask with the distilled water after each Experiment No – 2 Objective : You have a standard solution of NaOH. Which is prepared by dissolving 0.8 gm subtance in 200 ml water. With its help find the concentration of B solution of Na2CO3 solution is normality solution of 500 ml. C solution of HCl in a standard solution and phenolphthalein indicator. Apparatus : As per the experiment no. 1 Equations of reaction : In Ist titration (Standard solution NaOH and intermediate. solution HCl) NaOH = Na + + OH − HCl = H + + Cl − NaOH + HCl = Na + + Cl − + H 2O In IInd titration intermediate solution is HCl & Solution of unknown concentrations is Na2CO3 . Result : phenolphthalein (indicator), solution of NaOH, solution of Na2CO3 and intermediate solution of acid. Method : As per the titration in the experiment no 1. 65 (I) S. No. 1. 2. 3. N1 × V1 Table – 3 Standard solution (NaOH) ‘A’ and intermediate solution (HCl) ‘C’ Volume of base 25.0 ml 25.0 ml 25.0 ml Reading of Burette Start End 0.0 ml 27.7 ml 0.0 ml 22.3 ml 0.0 ml 22.3 ml Volume of acid (II) S. No. Volume of base Reading of Burette Start End 1. 2. 3. 25.0 ml 25.0 ml 25.0 ml 0.0 ml 25.8 ml 0.0 ml 25.4 ml 0.0 ml 25.4 ml N 2 V2 = Intermediate Solution of unknown concentration 3. 0.08 × 1000 0.8 × 10 = 200 2 25 N 25.4 25.5 × = = 0.114 N 22.3 25 2230 or Normality of ‘B’ solution of Na2CO3 = 0.114 N 4. ∴ To calculate the concentration – Concentration = Normality × gm equivalent weight = 0.114 × 53 = 6.042 gm / litre when 6.042 gm Na2CO3 is dissolved in the 1000 ml solution . The quantity of Na2CO3 dissolved in the 500 ml solution. = 6.042 × 500 1000 Therfore concentration of NaOH solution = 4 gm / litre. = 6.042 2 Concentrat ion Equivalent weight To calculate the normality of intermediate solution : N 2 × 0.25 N2 = = 0.8 × 4 gm Normality = 2. = or To calculate the normality of standard solution when 0.8 gm NaOH is dissolved in 200 ml water = To calculate the normality of solution of unknown concentration : = N 3 × V3 N 2 × V2 Standard Solution of solution unknown concentration 25 N × 25.4 22.3 Calculation : 1. Acid (HCl) Normality of intermediate solution = 0.112 N 25.4 ml N3 V3 N2 × V2 N × 25 = N 2 × 22.3 10 N 25 25N N2 = × = 10 22.3 22.3 N 2 = 0.112 or Volume of acid Formula : (1) N1 V1 = N 2 V2 Standard Intermediate Solution Solution (2) Base (NaOH) 22.3 ml Table – 4 Intermediate solution ‘C’ (HCl) and solution of Na2CO3 ’B’ = gm. Result : (1) Normality of Na2CO3 solution – 0.114 N (2) Concentration into 500ml – 3.021 gm Precaution : As per the experiment no. 1. 66 Experiment No – 3 Object : Add 12.6 gm oxalic acid into 250 gm of water and add more water in it to prepare a solution of Volume 2 litre. Determine the normality of oxalic acid and its concentration into the 500 ml solution. With the help of standard solution, the solution of phenolphthalein indicator and caustic potash is intermediate solution. S. No. Volume of base 1. 2. 3. 25.0 ml 25.0 ml 25.0 ml Reagents : Phenolphthalein indicator, Standard solution oxilic acid, solution of oxilic acid of unknown concentration and solution of caustic potash. = N 2 × V2 Standard solution Intermediate solution (H 2C 2O4 ) (KOH) 2. N 2 × V2 = N 3 × V3 Intermediate Solution of unknown concentration 2KOH + H 2C 2O4 = 2K + + C 2O4 − − + 2H 2O Intermediate solution, solution of unknown concentration. Volume of acid Start End 0.0 ml 25.8 ml 0.0 ml 25.4 ml 25.4 ml 0.0 ml 25.4 ml Formula : 1. N1 × V1 Equation of Reaction : A. H 2C2O4 + 2KOH = 2K + + C2O4 −− + 2H 2O Standard solution, intermediate solution. B. Reading of Burette (KOH) (H 2C 2O4 ) Calculation : 1. To calculate the normality of standard solution When 12.06 gm oxalic acid is dissolved into the litre solution. Method : Phenolphthalein indicator is used in the titration therefore the solution of acid and base is taken into the burette by pipette 1. Then follow the above procedure. 12.5 = 6.3 2 gm / litre Equivalent weight of oxalic acid = 63 Concentrat ion Normality = Equivalent Weight Table – 5 Standard solution (oxalic acid) and standard solution (KOH) S. No. Volume of base Reading of Burette Start End 1. 2. 20.0 ml 20.0 ml 0.0 ml 23.9 ml 0.0 ml 23.7 ml 3. 20.0 ml 0.0 ml 23.7 ml Volume of acid 23.7 ml Table – 6 Standard solution (KOH) and Titration between standard solution (KOH) and solution of unknown concentration (H 2O2O4 ) = 2. 6.3 1 N = = 6.3 10 10 To calculate the normality of intermediate solution N 2 × V2 N3 × V3 = Standard Solution Intermediate Solution (H 2C 2O4 ) (KOH) N × 20 = N 2 × 23.7 10 67 or N2 = 20.0 × N 2.37 × 10 N2 = N = 0.084 N 237 N3 = Concentration = Normality × gram equivalent weight Normality of intermediate solution (KOH) = 0.084 N 3. To calculate the normality of solution of unknown concentration : N 2 × V2 = Acid 27.3 = 0.115 N 273 N 3 × V3 = 0.115N × 63 = 7.245 = 7.245 gm / litre When 6.049 gm of Na2CO3 is dissolved in 1000 ml solution ∴ Base Concentration is 500 ml = 7.245 × 500 1000 = 3.62 gm. 20 × 27.3 = N 3 × 20 237 N3 = 20 27.3 × 273 20 N3 = 27.3 273 Result : (1) Normality of solution of oxalic acid = 0.115 N (2) Concentration of solution of oxalic acid is 500 ml = 3.62 gm. 7.2 Redox – Titration KMNO 4 1. – Oxilic acid titration : heat upto the 60° – 70°C, Now titrate this solution with the KMnO4 solution of In acid medium ( is presence of H 2SO4 ) KMNO 4 acts as a burette. The end point is indicated by light according to pink colour. following reactions – Experiment No. – 1 2KMnO 4 +3H 2SO4 → K 2SO4 + 2MnSO 4 + 2H 2O + 5O 2. The above produced oxygen oxidised the oxalic acid. acid and to find the concentration of given solution of KMnO4 by titration. Chemical Reaction : According to the above principle Indicator : KMnO4 is a self indicator. COOH 5| Object : To prepare a standard solution of oxalic + 5O → 5H 2O + 10CO2 COOH Add dilute H 2SO 4 in oxalic acid and (i) To prepare a standard solution : The required weight of oxalic acid to prepare a 250ml, N/10 solution of oxalic acid. 68 63 = 6.3 10 ∴ gm gm/litre Base of acid in 250 ml. = 6.3 × 250 1000 = ∴ weight of oxalic acid in 1000 ml = 1.564 × 4 gm 1.575 gm Take 1.575 gm oxalic acid in the weighing tube and measure it. Now pour it into measuring flask carefully with the help of funnel. Now again measure the weighing tube. Pour the distilled water on the funnel and put the substance in flask, and dissolve it into water. in the flask upto the mark & stirr the solution to make it homogeneous. Note these observations into your practical note book. Titration : Rinre the burette with given KMnO4 and fill it with KMnO4 . Now fix the burette to the stand. Take 20 ml solution of oxilic acid is the conical flask with help of pipette. Add 5 ml, H 2SO4 in it and heat it upto 70.80°C. The solution should not boil. Pour the solution of KMnO4 from the burette into the hot so heated solution gradually and stirres the solution. At the time of starting colour of KMnO4 is displaced but at the last point by adding one drop of KMnO4 the light pink colour is obtained permanently. Write the observations of titration in form of table. Observation : 1. Oxilic acid + weight of weighing tube = 7.5642 gm weight of empty weighing tube = 6.0002 gm weight of oxilic acid in 250 ml = 1.5640 gm. Normality of oxalic acid : weight of oxalic acid in 250 ml = 1.564 ∴ Therefore normality = 2. 6.256 N N= 63 10.07 Titration of oxalic acid and KMnO4 Table – 1 S. No. Volume of base Reading of Burrete Start End 1. 2. 3 20.0 ml 20.0 ml 20.0 ml 0.0 ml 18.2 ml 0.0 ml 18.0 ml 0.0 ml 18.0 ml Volume of acid 18.0 ml Calculation : N1 × V1 N 2 × V2 = Oxalic acid KMnO4 N N1 = , 10.07 N2 = ? V1 = 20 ml V2 = 18 ml or ∴ N1 × 20 = N 2 × 18 10.07 20 N N2 = × = N / 9.063 18 10.07 ∴ The normality of KMnO4 solution = N / 9.063 Equivalent weight of KMnO 4 = 31.6 Thus concentration in gram / litre = 31.6 = 3.48 = gm / litre 9.063 Result : (1) Normality of KMnO4 solution = N 9.063 (2) Concentration = 3.48 gm / litre Precautions : 1. The titration should be performed in the hot oxalic acid solution. 69 2. 3. 4. Do not add H 2SO 4 in less quantity. It should be added in more quantity otherwise the brown colour of MnO2 is produced. Read the up side surface of KMnO4 while taking the reading of burette Place a glased tile or white paper below the conical flask to see clearly last point gradually. KMnO4 Ferrous Ammonium Sulphate Titration Experiment – 2 Object : A standard solution of N/2 feerrous ammonium sulphate is given. To find the normality of given KMnO4 solution by the titration Principle : burette the solution taken in to the conical flask by KMnO4 N/10 ferrous sulphate. Rinre the burette with KMnO4 solution and fill it that. Take 25 ml ferrous sulphate solution in conical flask or beaker with the help of pipette and pour 5ml. H 2SO4 in it. Now titrate with KMnO4 . First the colour of KMnO4 . is disappeared, but at the last point light pink colour will appcar. Repeat the titration and obtain the 2 same readings of value of KMnO4 Observation Table – 2 Volume of ferrous Sulphate Reading of Burette 1. 25.0 ml 0.0 ml 21.9 ml 2 KMnO 4 + 3H 2SO4 → 2. 25.0 ml 0.0 ml 21.8 ml K 2SO4 + 2MnSO 4 + 2H 2O + 50 3. 25.0 ml 0.0 ml 21.8 ml It oxidises ferrous sulphate of ferrous ammonium in ferrous sulphate. (NH 4 )2 SO 4 do not take parts in this reaction Acid sulphate reacts with acidic KMnO4 in following way : S. No. = N 2 V2 Ferrous Sulphate KMnO4 N1 = or O4 + 8H 2SO4 + 10FeSO4 (NH 4 )2 SO4 → 2KMnO 4 + 10F2SO4 + 8H 2SO4 → K 2SO4 + 2MnSO 4 + 5Fe Ionization Equation : 2KMnO 4− + + 16H + 10F2 2Mn ++ Titration method : The solution taken into the V2 = 21.8 ml N × 25 = N 2 × 21.8 20 N 25 N2 = × 20 21 .8 Concentration = Normality × Equivalent weight = 0.0573 ×31.6 = 1.812 gm/litre (Equivalent weight of KMnO4 = 316) Result : (ous ) → + 10F2+ + + (i c ) + 8H 2O N , N 2 = 1 V1 25 ml , 20 = 0.0573 N (Normality of KMnO4 ) 1. ++ 21.8 ml N1V2 10F2SO4 (NH 4 )2 SO4 + 5H 2SO4 → Because (NH 4 )2 SO 4 does not take part into this reaction Therefore it can be written in following way. KMnO4 Calculation : K 2SO4 + 2MnSO 4 + 2H 2O + 50 K 2SO4 + 2MnSO 4 End Therefore 25 ml, N/20 ferrous sulphate = 21.8 ml KMnO4 2KMnO 4 + 3H 2SO4 → 5F2 (SO4 )3 + 5H 2O + 10(NH 4 )2 Start Volume of 2. Normality of KMnO4 solution = 0.0573 N Concentration of KMnO4 solution = 1.812 gm/litre 70 Precaution : 1. H 2SO4 should be added into more quantity otherwise the brown ppt of MnO2 is produced. 2. Do not heat the ferrous sulphate solution at time of titration. Perform the titration at the room temperature. KMnO4 is coloured solution. Therefore 3. see the upper surface at the time of taking the reading of burette. 4. Obtain the two same readings in titration. 5. Do not use HCl or HNO3 in place of H 2SO4 because the HCl is oxidised itself and HNO3 is a oxidization Substance. 6. Place a glave tile or white paper below the conical flask for observing the end point gradually. Oxidation Reduction Double Titration Experiment No - 3 Object : The N/30 focus ammonia sulphate is given. The normality and concentration of ferrous sulphate is determined with its help. Potassium permanganate is a intermediate solution. Principle: As per experiment no -2 Indicator - Self indicator Method (i) The titration of ferrous ammonium sulphate is performed by the potassium permagnate solution. as per the experiment no-2. (ii) Titration of ferrous ammonium sulphate of unknown concentration from intermediate solution of KMnO4 : Fill the burette with KMnO4 and note its reading. Clean the pipette by distilled water, wash it with ferrous ammonium sulphate table then 25ml solution and pour it into the titration flask. Pour dilute H 2SO4 to fill the titration to half, then gradually drop the solution of KMnO4 from the burette. Note the reading when the permanent light pink colour appears in the solution at the end point Repeat the titration for equal volume of KMnO4 Observation : 1. The titration in standard solution of ferrous ammonium sulpate and intermediate solution of KMnO4 . Table – 3 S. Solution of Reading Burette Used No. foous of End KMnO4 ammonium start (ml) solution sulphate (ml) (ml) 1. 2. 3. (ii) 25.0 ml 25.0 ml 25.0 ml 0.0 ml 0.0 ml 0.0 ml 24.8 ml 23.5 ml 23.5 ml 24.8 23.5 23.5 Proper Used KMnO4 (ml) 23.5 Titration in the solution of unknown ferrous ammonium sulphate and Intermediate KMnO4 Table – 4 S. Solution of No. foous ammonium sulphate Reading Burette Used KMnO4 of End start (ml) solution (ml) (ml) 1. 25.0 ml 0.0 ml 24.0 ml 24.8 2. 25.0 ml 0.0 ml 23.9 ml 23.9 3. 25.0 ml 0.0 ml 23.9 ml 23.9 Proper Used KMnO4 (ml) 23.9 Calculation 1. Standared solution (Ferrous Ammonium Sulpate of normality N = 30) 2. To calculate the noramality of intermediate solution [KMnO4 ] 71 N1 × V1 = Standard Solution N 2 × V2 Intermediate Solution N × 25 = N 2 × 23.5 30 25 N × N2 = 30 23.5 Normality of intermediate solution (N 2 ) = 3. 25 N 23.5 × 30 To calculate the normality of ferrous ammonium sulphate of unknown concentration : – = N 3 × V3 N 2 × V2 Standard Solution of unknown Solution concentration (F2SO4 (NH 4 )2 SO4 .6H 2O ) 250 N × 23.9 = N 2 × 25 23.5 × 3 250 N 23.5 N3 = × 23.5 × 30 25 N3 = N 23.9 23.9 N × = 30 23.5 30 × 23.5 Normality N/20 oxalic acid. The solution of potassium permanganate is intermediate solution. Principle : As per the experiment no. 1 Indication : Self indicator [ KMnO4 solution] Method : Take KMnO4 solution in burette and measure oxalic acid by pipette. Its titration method is according to the experiment no. 1. Observation : (i) Titration of standard ferrous ammonium sulphate solution and intermediate solution of KMnO4 . Table – 5 S. Solution of Reading Burette Used KMnO4 No. of oxalic of End acid start (ml) solution (ml) (ml) (ml) 1. 2. 3. (ii) solution F2SO4 (NH 4 )2 SO4 ⋅ 6H 2O having unknown concentration = 4. of 23.9 N 30 × 23.5 Concentration of solution having unknown concentration (Ferrous ammonium sulphate) Concentration = Normality × Equivalent weight = 23.9 N × 392 30 × 23.5 = 12.77 gm/litre Result : The concentration of given ferrous ammonium sulphate is 12.77 gm / litre Precautions : As per the experiment no - 2 Experiment – 4 Objectivet : To find the concentration of oxalic acid having unknown concentration with the help 25.0 ml 25.0 ml 25.0 ml 0.0 ml 0.0 ml 0.0 ml 25.1 ml 24.8 ml 24.8 ml 25.1 24.8 24.8 Properly Used KMnO4 solution v2 (ml) 24.8 Titration between the solutions of unknown ferrous ammonium sulphate and Intermediate KMnO4 Table – 6 S. Solution of Reading Burette Used KMnO4 No. of oxalic of End acid start (ml) solution (ml) (ml) (ml) 1. 2. 3. 25.0 ml 25.0 ml 25.0 ml 0.0 ml 0.0 ml 0.0 ml 23.4 ml 23.2 ml 23.2 ml 25.1 23.2 23.2 Properly Used KMnO4 solution v2 (ml) 23.2 Calculation 1. Normality of standard solution (oxalic acid). N / 20 2. To calculate Normality of intermediate solution : = N 2 × V2 N1 × V1 Standard Intermediate Solution Solution [C2H 2O4 ] [KMnO4 ] 72 N × 25 = N 2 × 24.8 20 25 N N2 = 20 × 24.8 3. N3 = To calculate the normality of solution of unknown concentration : N 2 × V2 N3 × V3 = Intermediate concentration [KMnO4 ] [C2 H 2 O4 ] 4. To calculate the concentration of oxalic acid of unknown concentration : Concentration = Normality × Equivalent weight = 0.0467 × 63 = 2.946 gm/litre 25 N × 23.2 = N3 × 25 20 × 24.8 N3 = Normality of oxalic acid of unknown concentration = 0.0467 N Solution of unknown solution 23.2 N 20 × 24.8 Result : The concentration of given oxalic acid in 2.946 gm/litre 25 N × 23.2 20 × 24 .8 × 25 Precaution : As per the experiment no. 1. 7.3 Calculations of double Titration Example : In the experiment of titration to neutralise 23.7 ml. deci normal solution of H 2SO 4 you require 26.6 ml HCl acid to neutrilize the 25 ml. NaOH and 25 ml NaOH of its base. Calculate normality of, by calculation 1. To calculate the normality of intermediate solution : Standard solution (H 2SO4 ) = Deci Normal solution = Normality of intermediate solution 2. To calculate the normality of solution of unknown concentration. N2 × N 2 Intermediate solution Solution of unknown concentration [NaOH ] [HCl ] 23.7 × 25 = N 3 × 26.6 250 N 10 N3 = 23.7 × 25 250 × 26.6 Standard Solution Intermediate Solution N3 = 23.7 266 H 2SO4 NaOH = N × 23.7 = N 2 × 25 10 N2 = N 23.7 × 10 25 N3 × N 3 = N 2 × V2 N1 × V1 23.7 250 = 0.884 N Concentration = Normality × Equivalent weight = 0.088 × 36.5 = 3.22 = 3.22 gm/litre Result : 1. Normality of HCl is 0.884 N 73 2. Concentration is 3.22 gm/ litre Example 2 : To perform the titration of 25 ml. NaOH of 2.09 N concentration from the intermediate solution of HCl you require 20.8 ml. To neutralize 25 ml of KOH solution of unknown concentration 21.5 ml, HCl solution is required To calculate the normality of KOH solution and find the quantity of KOH dissolved in 3 litre solution. Calculation : 1. Normality of standard solution = (NaOH ) . 09 N 2. Calculation of Normality of intermediate solution N1 × V1 N 2 × V2 Base Acid 0.09 × 25 N 2 × 20.8 N2 = II. = Normality of KOH = 0.93 N Concentration = Normality ×Equivalent weight = 0.093N × 56 = Concentration of 5.209 KOH is 5.20 gm /litre The 5.20 gm of solution is present in KOH solution Solution present in 3 litre solution is 5.20 × 3 = 15.60 gm Result : 1. Normality of KOH = 0.093 N 2. The quantity of solution 3 litre solution of KOH. Example 3: The standard solution 23.9 ml of HCl solution 25 ml of standard NaOH Solution when 22.7 ml HCl is require to neutralize 25% of 25 ml Na2CO3 . Calculate the equivalent weight of Na2CO3 I. 0.09 × 25 20.8 = 9 × 25 2080 = 225 2080 = 45 416 N1 × V1 = [HCl] 43 × 9 4160 = 387 4160 Intermediate Solution Solution N2 = [KOH] 45 × 21.5 416 × 25 = N 2 × V2 Standard = 0.093 N II. HCl N1 × V1 V2 = N 25 × 20 23.9 = 25N 478 N 3 × V3 45 = 21.5 = N3 × 25 416 N3 = = NaOH = 0.108 N To calculate the normality of solution of unknown concentration = N 2 × V2 Calculate the normality of intermediate solution (HCl): To calculate the normality of Na2CO3 solution : N 2 × V2 = N 3 × V3 Intermediate Na2CO3 Solution Solution 25N × 22.7 = N 3 × 25 478 74 N3 = 25N 22.7 × 478 25 Solution Potassium Permanganate Normality of solution of Na2CO3 = 0.047 N 1 0.25% Concentration of Na2CO3 = 25 gm/litre 14.2 x 28.4 concentration Ferrous Ammonium sulphate = N3 x 10 = 2.5 gm/litre Concentration = Normality × Equivalent weight or N3 Equivalent weight = Concentrat ion = Example 4: 14.2 ml of solution KMnO4 is Sulphate is required for the titeration of 28.4 ml solution of that KMnO4 solution then find the quantity of ferrous ammonium sulphate in one litre solution of ferrous ammonium sulphate To calculate the normality of intermediate solution:N1 x V1 = N2 x V2 Oxalic acid Potassium permanganate 0.1 x 10 = N2 x 14.2 N2 = = 1.5 X 10.0 14.2 permanganate - 14.2 There fore normality of KMnO4 = N 14.2 II. Calculation of normality of unknown concentrated solution N2 x V2 Intermediate = 10 = 0.2N 250 ml. of solution have 4.9 gm. of ferrous ammonium sulphate. weight of ferrous ammonium sulphate in 1000 ml. of solution = 4.9 x 1000 250 normality N3 x V3 Solution of unknown 1 10 = 78.4 gm/ltr. Result Concentration of ferrous ammonium sulphate = 78.4 gm/ltr. Example 5 4.9 gm of ferrous ammonium sulphate is added to 250 ml of water to make a initial solution. To neutralize 25 ml. of this solution, 22.4 ml. of KMnO4 solution is required. We required 27.2 ml. of KMnO4 solution to neutralize, a solution of ferrous ammonium sulphate of unknown concentration. Find the concentration of ferrous ammonium sulphate solution. - 1 x = 0.2N x 392 Concentration of ferrous ammonium sulphate Result : Equivalent of Na2CO3 is 53.19 acid solution. If 10ml of ferrous ammonium. 14.2 Concentration=normality x equivalent weight. 2.5 = 53.19 0.047 required for the titration of 10 ml, 0.1 N oxalic 28.4 2 Normality = 1. = = 19.6 392 = = 19.6 gm. Concentration Equivalent Weight 75 (Equivalent weight of ferrous ammonium Sulphate = 392) = N/20 I. To calculate the normality of mitermediate solution = N2 N2 N1 V1 Ferrous Potassium ammonium permagnate Sulphate N × 25 20 N2 = II. N 2 × 22.4 25N 20 × 22.4 Normality of KMnO4 Potassium Permagnet ferrous ammonium sulphate 25N × 27.2 20 × 22.4 = N3 = 25N × 27.2 20 × 22 .4 × 25 27.2N 20 × 22.4 = = N3 × 25 27.2 = 0.0607 N 4480 To calculate the normality of solution unknown concentration Normality ferrous ammonium sulphate = 0.06.7 N Concentration of ferrous ammonium sulphate = N 2 × V2 N 3 × V3 = Normality × Equivalent weight Intermediate Solution of = 0.0607 × 392 Solution unknown concentration = 29.79 gm/litre = Result : 23.79 gm/litre Exercise Question Q.1 Give one example of self indication. How does it work ? Q.2 What is a double titration ? Q.3 What is Oxidation reduction Titration ? Q.4 Describe the reaction between oxalic acid and potasium permaganate during titration ? Q.5 Why ferrous ammonium sulphate is used in place of ferrous sulphate during titration ? Q.6 What is the function of KMnO4 in Oxidation-Reduction titration ? Q.7 Why the heated solution of oxalic acid in used in Oxidation-Reduction Titration ? Q.8 Why HNO3 acid is not used in place of HCl in Oxidation-Reduction Titration ? Q.9 Why the solution of potassium permaganate is taken into the burette during the titration between ferrous ammonium sulphate and potassium permanganate ? Q.10 Describe the reactions of the potassium permanganate during titration ? Q.11 Sodium Carbonate is a salt, then why it is used as a base during titration ? Q.12 Which solution should be take titration in the flask while using phinalptheiline indicator and why ? Q.13 The burrete and pipetle are rinsed during titration, flask and beaker are not rinsed, why it is so ? Q.14 Why standard solution of sulphuric acid and sodium. Hydroxide. Can’t be prepared by measuring it ? 75 76 Q.15 What quantity of substance is required to prepare 250 ml, N/10 oxalic acid ? Q.16 Prepare 250 ml. solution by dissolving 2.45 gm ferrous ammonium sulphate in acidic water. Find its normality ? Q.17 What quantity of substance is required to dissolve in 250 ml distilled water to prepare 0.2 ml ferrous ammonium solution ? Q.18 What quantity of substance is required to dissolve in 250 ml distilled water to prepare N/30 ferrous ammonium sulphate solution ? Q.19 14.0 gm solvent is dissolved in 2.5 litre of caustic potash solution, 24.6 ml acid is spent for the titration of 25ml intermediate solution of acilic acid. 19.7 ml acid of unknown concentration was cansumed for the titration of 25ml solution of Caustic Soda. Find the normality of Causitc Soda. Find the normality of Caustic Soda and it concentration in 1.5 ml solution. Q.20 1.4175 gm acid is dissolved in 250 ml of any acid. Its atomic weight is 126 and basisity is 2. To neutrilize the 22.5 ml of its solution 25.00 ml is consumed. 25 ml of this is completely neutralised by 20ml. Find the concentration is gm/litre Answers N 40 (15) 1.575 (16) (19) 1.080, 4.8 gm/1.5 litre (20) 4.96 gm / litre (17) 19.6 gm (18) 3.2667 gm