DICHROMATOMETRY .s dichromatometry. In acid medi oxidant are known ai Cea int; however, itis a Weake, (Sado it acts asa powerful oxida ana reduction potential B= 13V E sy table fusion, soluble in water and aque ca in aS ne gt iota y Col di HC, SoKsC0, is used as an excellent primary standard, and in this respect it is superior to KMnOg. It is very helpful for the estimation offerou and fei ion Inacid medium orange ia0 reduces to green C with the increase in pH the standard reduction potential Consequently Cr* is oxidised to yellow chromate in alkaline medium. ‘Redox titrations with Potassium dichromat C10) has higher standard reduction potential ‘uidant than KMn04 for its comparatively lower st (C07 + 14H + 6¢ <> 2Cr*? + 7H2O MnOj + 8H* + Se <== Mat? + 4H;0 #3 — the rate of reduction is reasonable below pH=2, | falls; above pH=7, reductant becomes powerful reparation of 250 ml (7) Standard Potassium Dichromate Solution : Gram-equivalent of KC.) 220394 2452 TIO 294 Frag ORB Weight ofKCr0y required to prepare 250 ml N 49 x 250 (By) sstwion = fr oSS 91.225 8 About 1.2 g of AR. grade KyCt20; is accurately weighed out by a chemical balance by method of ase os! elo he kof 250ml measuring sk. Te slid is washed down complet sing led water fom 8 wih bot, ‘The asks shaken unt all KpCr0 dissolve; distilled watt : lume comes very near tothe mark; finally the volume matk by Gisilled water drop by crop from the jt of he wash bot, The sk ieee aie lution uniform taking care thatthe liquid does no leak out a apeaseeny mule Weight ofthe botle with KCr20; = Wg ‘Weight of the bottle after transfer = W, g. 4 Skee, = ¥1=W2 (S (XN Has (8) (8 10. Redox Indicators Suitable for Titration with Potas __Sodium or Barium diphenylamine su Diphenylamine may also be used as indesee Se Babs 5 oxidation and can be stored fora long time, BaDS gives s ’, ) f = factor ‘sium Dichromate : Weal Used asthe indicator. Freshly prepa) ae rs ter as its solution can resist acrid! ave ‘colour change from colourless throul* al t ons wit inion OF FERRO c poussit m dichromate 1 do not inte joride ion +; Because of tte q ITATIVE INORGANIC ANALYSIS (PART I) ey quanraTE jor to the start of the titration to lower the reduction potential of Fe'/Fe*? system (See Page B sndieator and inthe these cases addition of HPO, or Fis not necessary. Preparation of Indicator Solution ; (@) Barium diphenylamine sulphonate (CeHs—NH—CgHSO3), Ba :0,15% solution in cone, 1,50, () Sodium diphenylamine sulphonate : 0.2% aqueous solution (© Diphenylamine : 1.0% solution in conc. HSO, (@ Diphenyl benzidine : 1.0% solution in conc. HySO, (© N-phenylanthranilic acid : 0.25 g is dissolved in 12 ml of(X) sodium hydroxide solution and then diluted to 250 ml with distilled water. Titrations with Standard Potassium Dichromate Solution : —— ESTIMATION OF FERROUS IRON IN MOHR’S SALT Potassium dichromate is superior to Potassium permanganate in estimating Fe*? and Fe*? iron because chloride ions do not interfere in titration with the former. Theory : Because of the higher standard reduction potential than that of Fe? Potassium dichromate quantitatively oxidises ferrous iron of Mohn's sat to ferric iron in acid medium, Cr,07? + 14H* + 6¢ === 2Cr+ + 71,0 = 133V Fe +e == Fet? FE = 077 Cr,07 + 6Fe*? + 14H* => 2Cr!3 + 6Fe} + 7H,0 EP = 056V Indicator : Fe*? is estimated by using Barium or Sodium diphenylamine sulphonate or Diphenylamine indicator in presence of HPO, or F-, which reduces the standard reduction potential of Fe"/Fe*? system and makes the indicator suitable for the titration.. Work to be done : Preparation of Solutions Required : 1. 250ml of (3) K,Cr20; solution (See Page No. 138) 2. Mohr's salt solution : About 9.8 g of A.R. grade salt is weighed out by a rough balance into a 250 ml measuring flask, the solid is dissolved in 200 ml 2(N) HSO,, the volume is made up to the mark with the same acid and finally made uniform by shaking. 3. 0.15% solution of BaDS in conc. HSO4. Titration Procedure : 25 ml of the stock solution is pipetted out into a 250 ml conical flask, diluted to 150 mi with distilled water, 5 ml of conc. HpSOq, 5 ml of syrupy phosphoric acid are added followed by 5 é ops of BaDS indicator and then the mixture is titrated with standard KCr207 solution running from & as burette with constant shaking until the first prominent red-violet colouration. The experiment is repeated to et burettc readings not differing by more than 0.05 ml. Results : Table Caleulation : 2S mlofMonr's sat = Vil of (2) KC, = vxtmiot (%) Kicr0,WCED COURSE IN PRACTICAL CHE gy | ANADVA or N ) Mohr's salt N) fet? + iwontar(*) 5585 gm of Fe 10. N 7 0.005585 g of Fe mlot(~}k:cn0) = eo (5) - S = Vx fx 0.005585 g of Fe Veet a 0.005585 g Fe 25 ml of Mohr’ salt solution contain V x £x 0.0 : any x 00ss85 x10 of Fo ESTIMATION OF FERRIC IRON IN FERRIC ALUM 25 mi 250 See ma ces Fet3 +4/Snt2 system, SnCly reduces Fe*? in Ho) ory : Because of lower standard reduction potential of S/S n uces afin io Fes as dichromate, having a higher standard reduction potential quantitatively oxidis, Fe to Fe", also in acid medium. . Snt4 4.2¢ ead Sot? Ee = 015V Fet34¢ ea Fei? E = O77V precautions Determination of Preparation of So! 2Fet3 + Sn? = 2Fet? + Sn4 0.62 V tion E 3 @ Titration of Boones a Bs E Cra07? + 4H + 60> 2Cr947HO BP = 133. ae Naion: Indicator : The estimation of Fe*? is done by using Barium or Sodium diphenylamine sulphonate or iphenylamipe indicator in presence of HsPO, or F~. HsPO, or reduces the standard reduction potential of Fet/ Fe*? system to about 0.61V and makes the Preparation of Solutions Required ; 1 santas (%) rac soon (©) Titration of ‘mount of ferrous iro © Volume of volume required in (a — SSIMATION OF BAR Jenny Bat? ions ie, 4. whic 207 produced 4 011% solution of BaDS in cone. 1350, teece Mohs salt Titration Procedure : "SO. For estima ati a ir iat boxed! 500 ml conical flask, 20 mio! ao '€ solution is then reduced bf the 2 colOut OF the solution jus « ‘olution is rapidly cooled unde! indienoh*K€M and allowed to stand fo reduction of Fe™ ionate india Tee ML of syrupy HsPOs dev the fae pee ten a i se i x