Class-12 Chemistry practical file A-Salt analysis 1-NH4C03 2-Pb(CH3C00)2 3-CuS04 4-AICI3 5-ZnCl2 6-CaSO4 7-MgCl2 B- To determine the molarity of KMnO4 solution by titrating it against M/ 20solution of oxalic acid. To determine the molarity of KMnO4 solution by titrating it against 250 ml ofM/20 solution of ferrous Ammonium Sulphate. Group test -C6HSOHAim :- 3 To Determine the Molarity of KMnO, solution by titrating it against M/20 solution of Oxalic acid Apparatus and Chemicals Required :- ¥ Measuring flask (250 mL) : One Y Oxalic acid : As per need ¥ Burette (50 mL) : One Y Potassium permanganate solution : As per need Y Burette stand : One ¥ 1.0 M Sulphuric acid : As per need Y Pipette : One ¥ Conical flask : One ¥ Funnel : One Y Weighing bottle : One ¥ Glazed tile(white) : One ¥ Burner : One ¥ Wire gauze : One ¥ Chemical balance : OneTheory :- ( 4 ) In the present experiment, potassium permanganate acts as a powerful oxidizing agent. Although KMn0O, acts as an oxidizing agent in alkaline medium also, for quantitative analysis mostly acidic medium is used. The oxidizing action of KMnO, in the acidic medium can be represented by the following equation : MnO, ~ + 8H* + Se~ > Mn?* + 4H,0 The acid used in this titration is dilute Sulphuric acid. Nitric acid is not used as it is itself an oxidizing agent and hydrochloric acid is usually avoided because it reacts with KMnO, according to the equation given below to produce chlorine and chlorine which is also an oxidizing agent in the aqueous solution. 2KMn0O, + 16HCI > 2KCl + 2MnCl, + SCI, + 8H,0 Since, oxalic acid acts as a reducing agent, it can be titrated against potassium permanganate in the acidic medium according to the following equation —Reactions of Oxalic acid ( 5 A. Chemical Equations Reduction half reaction : 2KMnO, + 3H,SO, > K,SO, + 2MnSO, + 3H,0 + 5[O] Oxidation half reaction : H,C,04 + [O] > 2CO, + H,0] x 5 2KMn0O, + 3H,SO, + 5H,C,O, > K,SO, + 2MnSO, + 8H,O + 10CO, B. lonic Equations Reduction half Reaction : MnO, + 5e + 8H* > Mn**+ 4H,O]x 2 Oxidation half Rection : C,0,2 > 2CO, + 2e]x 5 2MnO, + 5C,0,7 + 16H* > 2Mn**+ 10CO, + 8H,0In these equations, MnO, ~ is reduced to Mn?* and C,0,?" is oxidized to CO,. The oxidat! number of carbon in C,0,?- changes from +3 to +4. In these titrations, potassium permanganate acts as a self indicator. Initially color of potassium permanganate is discharged due to its reduction by oxalic acid. After complete consumption of oxalate ions, the end point is indicated by the appearance of a light pink color produced by the addition of a little excess of unreacted potassium permanganate. Further, during the titration of oxalic acid against potassium permanganate, warming of oxalic acid solution (50°-60°C) along with dilute H,SO, is required. This is essential because the reaction takes place at higher temperature. During the titration, first manganous sulphate is formed which acts as a catalyst for the reduction of KMnO, by oxalic acid. Therefore, in the beginning the reaction rate is slow and as the reaction proceeds, the rate of the reaction increases.Procedure ( 7 ) A. Preparation of 0.1 M standard solution of oxalic acid Prepare 0.05M oxalic acid solution. 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 of the burette by releasing some solution through it. The burette used in the permanganate titration must have a glass stop cock as rubber is attacked by permanganate ions. (ii) Take 10 mL of 0.05 M oxalic acid solution in a conical flask and add half of the test tube full (= 5 mL) of 1.0 M H,SO, 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°— 60°C before titrating it with potassium permanganate solution taken in the burette. To increase the visibility of the color change, place the conical flask containing the solution to be titrated over a white glazed tile kept below the nozzle of the vertically fitted burette. (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 violet color of permanganate solution is discharged on reaction with oxalic acid.The end point is indicated by the appearance of permanent light pink color due to a s 8 excess of permanganate solution. (v) Repeat the titration till three concordant readings are obtained. Since the solution of KMnO, is of dark color, the upper meniscus should be considered for noting the burette readings. (vi) Record the readings and calculate the strength of potassium permanganate solution in mols/litre.Observations :- (9) PMO Leconte cy Oe eee ss aed Final Reading of Burette (y) (v-x) 1. 0 8.2 8.2 2. 8.2 13.4 5.2 a 13.4 18.2 48 8.24+5.2+ 48 _ 18.2 3 3 = 6.06 ml Concordant value =Calculations :- Calculation of amount of oxalic acid to be weighed to prepare 100 ml M/20 solution : Molecular Mass of Oxalic Acid = 126 g/mol 1000 cm? of 1M oxalic acid require 126 g oxalic acid 1000 cm? of M/20 oxalic acid require = 126/20g = 6.3 g Using formula- N,M,V, = N,M,V, Where N, = 5 (for KMnO,), V,= 6.06 , M, =? N, = 2 (for oxalic acid), V, = 10 ml, M, = 1/20 mu, = NaMaV2 ON,Strength of KmnO, = Molarity x Molar mass ay = 0.033 X 158 = 5.214 gm/mlResult :- The molarity and strength of KMnO, solution is 0.033M and 5.214 gm/ml.(a) (b) (c) (d) (e) (f) (8) (h) (i) (i) (k) Precautions :- (a3) Always rinse the burette and the pipette with the solutions to be taken in them. Never rinse the conical flask with the experimental solutions. Remove the air gaps if any, from the burette. Never forget to remove the funnel from the burette before noting the initial reading of the burette. No drop of the liquid should hang at the tip of the burette at the end point and while noting reading. Always read the upper meniscus for recording the burette reading in the case of all coloured solutions. Never use pipette and burette with a broken nozzle. Lower end of the pipette should always remain dipped in the liquid while sucking the liquid. Do not blow out the last drop of the solution from the jet end of the pipette. The strength of the solution must be calculated up to the fourth decimal place. Do not forget to heat the mixture of oxalic acid and HSO, solutions between 50°-60° C while titrating it against potassium permanganate.Aim :- To determine the concentration/molarity of KMnO, solution by titrating it against 250 ml of M/20 solution of ferrous ammonium sulphate (FAS). Apparatus and Chemicals Required :- ¥ Mohr's salt ¥ Beakers VY weighing bottle ¥ conical flask Y weight box Y Funnel ¥ volumetric flask oe pipette v Funnel ¥ clamp stand ¥ distilled water ¥ chemical balance ¥ dilute H,SO, vTile ¥KMn0O, solution.Theory :- as) Mohr's salt having the formula FeSO,.(NH,)2SO,.6H,0 has molar mass gm/mol. It is a primary standard. It's equivalent mass is 392/1 = 392 as its n factor is 1 as per the following reaction- Fe?* > Fe +e 1. The reaction between KMnO, and Mohr's salt is a redox reaction and the titration is therefore called a redox titration. 2. Mohr's salt is the reducing agent and KMnQ, is the oxidizing agent. 3. KMnoO, acts as an oxidizing agent in all the mediums: i.e. acidic, basic and neutral medium. 4. KMnO, acts as the strongest oxidizing agent in the acidic medium and therefore diluted H,SO, is added to the conical flask before starting the titration.Theory :- Qs) Mohr's salt having the formula FeSO,.(NH,)2SO,.6H,0 has molar mass gm/mol. It is a primary standard. It's equivalent mass is 392/1 = 392 as its n factor is 1 as per the following reaction- Fe > Fe +e 1. The reaction between KMnO, and Mohr's salt is a redox reaction and the titration is therefore called a redox titration. 2. Mohr's salt is the reducing agent and KMn0O, is the oxidizing agent. 3. KMnO, acts as an oxidizing agent in all the mediums: i.e. acidic, basic and neutral medium. 4. KMnO, acts as the strongest oxidizing agent in the acidic medium and therefore diluted H,SO, is added to the conical flask before starting the titration.Procedure :- SPN OM PSP SP ree eB eB > YN PS Weigh a clean dry bottle using a chemical balance. Add 4.9 g more weights to the pan containing the weights for the weighing bottle. Add Mohr's salt in small amounts to the weighing bottle, so that the pans are balanced. Remove the weighing bottle from the pan. Using a funnel, transfer the Mohr's salt to the volumetric flask. Add about 5ml. of dilute HSO, to the flask followed by distilled water and dissolve the Mohr's salt. Make up the volume to the required level using distilled water. The standard solution is prepared. Fill the burette with KMnO, solution. Pipette out 10ml. of Mohr's salt solution into the conical flask. . Add half a test tube of diluted H,SO,. Keep a glazed tile under the burette and place the conical flask on it. Note down the initial reading of the burette. Run down the KMn0, solution into the conical flask drop wise withlonic Reactions Involved :- Reduction Half :- MnO, + 8H* + 5e > Mn**+4H,O Oxidation Half :- 5Fe?* > SFe**+ + 5e Overall Equation :- MnO, + 8H* + 5Fe** > Mn**+ 5Fe?* + 4H,0 Indicator :- KMn0O, acts as a self-indicator. End Point :- Colorless to light pink (KMnO, in the burette)Observations :- NWR unr | Co ea scabs POC eats isc 09) ee ae 0 10.2 10.2 2. 10.2 16.5 63 Je 16.5 19.1 2.6 10.246.3+2.6 _ 19.1 3 Concordant value = = 6.36 mlCalculations :- Calculation of amount of Mohr’s Salt to be weighed to prepare 100 ml M/20 solution : Molecular Mass of Mohr’s salt = 392 g/mole 1000 cm? of 1M KMn0O, require 392 g Mohr’s salt 250 cm? of M/40 KMn0O, require = 392/20g = 4.9 g Using formula- N,M,V, = N,M,V, Where N, = 5 (for KMn0O,), V,= 6.36 , M, =? N, = 1 (for Mohr’s salt), V, = 10 ml, M, = 1/20 m,= MMe V4 M, = 2x1x10___20 _gasyy ~1x20x636 127.2Strength of KmnO, = Molarity x Molar mass =0.15 X 158 = 23.7 gm/mlResult :- The molarity and strength of KMnO, solution is 0.15 M and 23.7 gm/ml.