[LOBJECTIVE / To prepare 250 mL solution of x oxalic acid. 1 THEORY Crystalline oxalic acid is a primary standard, its standard solution can be prepared by taking a given weight of the salt. COOH Molecular mass of oxalic acid | | -2H,0 | = 126 g. COOH ‘Amount of oxalic acid for 1000 mL of x solution = % =63¢. Amount of oxalic acid for 250 mL of x solution = LaTERIALS REQUIRED A. Apparatus: 250 mL measuring flask, weighing bottle or watch glass, beaker, wash bottle, pipette. B. Chemical: Oxalic acid (crystalline pure). PROCEDURE 1 Take a dry weighing bottle. Weigh it accurately. Let it be w g. 2. Add approximately 1.5 g pure oxalic acid in the already weighted weighing bottle and place it on left pan of the balance. 3. Keep a weight of (x, + 1.575)g on the right pan of the balance. Take the weight.4. Add a little more of oxalic acid in the weighing bottle so that the two sides get by, ul lance If necessary take out some of oxalic acid. Always use spatula ‘Adding last drops to make | up the volume © @ Fig, 10.13. Preparation of standard solution 5. Take out weighing bottle and pour the acid in a clean beaker. Wash the weighing bottle with about 20 ml, of distilled water from wash bottle into the beaker. Again wash with — another 20-25 mL water so that all the weighed oxalic acid goes into the beaker. 6. Shake the beaker gently to get a clear solution. 7. Transfer this solution into the measuring flask through a funnel. 8. Wash the funnel into the measuring flask (250 mL) with distilled water with the help of 10. wash bottle 2-3 times using 20-25 mL each time. ‘Take out the funnel. Make water in the measuring flask below the mark. Finally use pipette to make water up to the mark. Stopper the measuring flask tightly and shake to get a uniform g solution of oxalic acidEXPERIMENT 2 ‘ CTIVE posvecte To prepare 250 mL of Mohr’s sat [1HE0R Ferrous iron is available as primary standard as Mohr’s salt. So standard solution of Mohr’s salt can be prepared. Molecular mass of Mohr’s salt = 392 grams. “20 “1000 containing 10 mL dil. sulphuric acid and make up the solution to 250 mL. In redox reaction ferrous of Mohr’s salt is oxidised to ferric iron and thus one electron per molecule is used. Thus its equivalent weight is equal to the molecular weight. Therefore, 4.9 g of the salt will be required to prepare © solutions of Mohr’s salt. . M For preparing 250 ml. of =~ Moh’s salt solution, take 49 ¢ (= 250, ) of the salt in waterpeRoceDURE a. Preparation of Standard Solution of Mohr's Salt 1. Weigh a clean dry weighing bottle ions 2. Add approx 1.9 g Mohr’s salt to the weighing bottle 3. Keep adding Mohr’s salt to the weighing bottle with the help of a clean spatula, a little at 2 a till the weight in the pan is balanced with the weight of the weighing bottle + Mohr’s (Note: It is difficult to take a exact calculated weight and so take exact weight of the bottle + salt when the amount of Mohr’s salt is near the calculated value.) Let it be w, g 4, Remove the weighing bottle from the pan. 5. Transfer the salt to the standard measuring flask through the funnel. 6. Weigh the weighing bottle again. Let it be w, g. 7. Wash the salt into the measuring flask with distilled water with the help of wash bottle Add a little dil. H,SO,. 8 Take out the funnel and add more distilled water till it is a little lower than the etched mark. 9. Stopper the flask and swirl to mix up the solution. 10. Finally add water with the help of a pipette till the level of solution reaches the etched mark.EXPERIMENT 3 [LOBJECTIVE es ity and strengtp i is ind out the molarii ath of Prepare ~~ solution of Mohr’s salt. Using this solution fi ‘ rep 0 given KMnO, solution. [LtHEorY The reaction between KMn0, (MnO;) and Mohr’s salt Cea by a — eee ae eins hrs salt (Fe** ——+ Fe“) in the acidic as well as in alkaline medium n re fais pa is not used for titration purpose because brown MnO, formed during the reaction interferes with the determination of end point. Conc. HNO, cannot be used as it itself also OXidises Mohr’s salt. HCI can also be not used as it itself gets oxidised by KMn0O,,. Therefore for the Purpose of volumetric titration dil. SO, provides the best acidic medium). 2KMnO, + 8H,SO, + 10FeSO, - (NH), SO, - 6H,0 Tay 7 M280, + 2MnSO, + 5Fey(S0,), + 100VH,), SO, + 68H,0 Tonic equation may be written as: MnO; + 8H*+ Se” Mn? + 41,0 Fe? Fe ge] x 5 Amount of Mohr’s Salt for Standard Solution Suppose itis required to prepare 100 mL of x Mohr’s salt, Molarity (= Weight of salt x 100 Molecular weight * Vol. of solution Required weight for 100 mi. of M solution 20 ~ Mol. wt.xM xv -_ aie 3 1000" ap * 100= 1.96 gthe strength of KMnO, is determine From the overall balanced equation, o's sat ‘d by law of equivalence which is given as. it is clear that 2 moles of KMn0, react with 10 moles of Miao, X Visio, 2 To, Myohrssat % Vain 10 WATERIALS REQUIRED A. Apparatus: Standard measuring flask (100 mL), weighing bottle, funnel, burette, pipette, wash bottle, conical flask, weight boxes, weighing bottle, ; B. Chemicals: Solid Mobr’s salt, given KMnO, solution, distilled water C. Indicator : KMn0, is a self indicator.[LOBSERVATIONS AND CALCULATIONS =u Weight of weighing bottle + Mohr’s salt 1 . Weight of weighing bottle + Remaining Mohr’s salt = 2 & oe Weight of Mohr’s salt actually dissolved - 2 =w Volume of solution prepared = 100 mL. w , 1000 Molarity of Mobr's salt, Myaues sit = 399 “392 Titration Table Volume of Mohr’s salt solution taken for each titration = 25mL jume of KMn0O, | SNo. Initial reading of the Final reading of the — ae burette (0,) mL burette (v,) mL used (0, - %y 1 © me 1B) me Wepme 2 Ome 13-0 mL \S-o mL | s One 125 me 12S me | a ome Jas me 1S me Volume of KMnO, (concordant reading) = Vigo; 2 Muonrssat * Viren (2) > 2X 00S KQS_ Myatao, = <2 x Meneses * Mote mit 19) = O-0em ~~ Vega, fox 12-5 Strength (g/L) of KMn0,= Myauo, x Molecular mass = Mra, X18 = OVOT KISH > 316 gle [LREsuLtT Molarity of KMnO, solution = 0..02M Strength of KMnO, solution o/h [LPRECAUTIONS + Always use freshly prepared solutions. + Ensure accuracy while taking readings of * Do not use rubber KMn0,. Burette and pipette should bé cleaned immediately after use. Always use distilled water. Before use, rinse the burette and the pipette with the respective solutions, Always use rider if it is required to use a weight of less than .001 g. Weights should be handled with foreep only. pipette and burette by avoiding parallax error. Pinch cock burette. Rubber being an organic matter, is attacked byEXPERIMENT oBJECTIVE M on ME solution ee Prepare “56 of oxalic acid. With the help of this solution find out molarity and strength of se given KMnO, solution. [LtHEORY KMn0, oxidises oxalic acid in acidic medium. Thus reaction between KMnO, and oxalic acid is redox reaction. The titration is done in acidic medium using dil. H,SO,. Since this reaction is slow at room temperature, the titration is done at 60-70°C. For this purpose the mixture of oxalic acid and dilute H,SO, is heated before starting the titration. However, the mixture should not be overheated as it will lead to decomposition of oxalic acid to CO, and volumetric titration will not give correct result. (COOH), HEP CO, + CO + H,0 The molecular reaction between KMnO, and oxalic acid is 2KMn0, + 5C,H,0, + 3H,S0, —> K,SO, + 2MnSO, + 1000, + 8H,0 Corresponding ionic equation is MnO, + 8H* + 5e°——> Mn + 4H,0 ] x2 —— 2€0, + 261 x Ee 2MnO; + 16H* + 5C,0,,—> 2Mn*? + 8H,O + 10CO, Amount of oxalic acid for standard solution in / Suppose it is required to prepare 100 mL of M/20 oxalic acid solution. ~ Weight of oxalic acid a 1000 Now molarity (M) = s¢[ceular weight of oxalic acid Vol of solution ". Required weight of oxalic acid for 100 mL of x solution (H,C,0, - 2H,0) Mol. weight , 1 y 100 700020 - x = 0.63.8 strength of KMnO, is determined by law of equivalence which is given as: i a 0, is devs lear that 2 moles of KMnO, react with 5 moles of snag Et the overall balanced equation it is cl ic acid. Magno, Vivo, 2 _ Mao, “600 — = Morale acid * Wonatc act[LWATERIALS REQUIRED A. Apparatus: Standard measuring flask, weighing bottle, funnel, burette, pipette, wash bottle, conical flask, weight box, burner, tripod-stand, wire gauze. B. Chemicals: Oxalic acid crystals, KMnO, solution, distilled water. C. Indicator: KMnO, is a self indicator.l OBSERVATIONS AND CALCULATIONS Weight of weighing bottle + Oxalic acid =u, Weight of weighing bottle + Remaining oxalic acid = w, & Weight of oxalic acid actually dissolved w,- Wye =wg Volume of solution = 100 mL . aad __w 1000 Molarity of oxalic acid (Myratie acia) “500% Titration Table Volume of oxalic acid solution taken for each titration = 25mL S.No. | Initial reading of the Final reading of the Volume of KMnO, burette (v,) burette (o,) used (v, ~ v,) mL 1 © mnt 24-0 me 24-8 me 2 Oo mL 24-5 m& 24 $ me a Ome AS+p me | AS1p me 4 oml 2s) me Aft meVolume of KMnO, (concordant reading) = Viyyo Meee Mowiicnia XVonaienia %2 - 0-05 X2USKZ Viatno, *5 Strength of KMn0, = Mygio, 158 g/l. = O0lgxisge 714 FL 281X5 _ y.019m RESULT Molarity of given KMn0, solution = 0:019 M Strength of given KMnO, solution = 2:19. g/L[LPRECAUTIONS Always use freshly prepared solutions. 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