Gowda, H. Sanke

Thimmaiah, K. N.

English

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NOTESZr(IV) with polyvalentinorganicanicns,such asphosphates,tungstates,etc., have useful caticnexchangep~opertiesincluding high uptakes c.fcertainions,reascnablexchangeratesandinterest-ing selectivites8.DPSO seemsto influencethepartitionaffectingtheRf valuesevenonimpregnatedpapers. Paraffincoatedpapersdemonstratesepara-tion of cationsby reversedphasechromatography.The authorsthank the authoritiesof St Joseph's.college,Trichirapallifor the facilitiesprevided.References1. MARKL, P. & JETTMAR, A. A., Microchim.Acta,3 (1974),429.1. SHRINER, STRUCK & JORISON, J. Am. chern.Soc.,52 (1930),2065.3. KRAUS, K. A. & PHILLIPS, H. 0., J. Am. chern.Soc.,78(1956),694.4. MARKINA, N. A., Chern.Abstr., 79 (1973),121563a.5. IMAI, HIROMU, Chern.Abstr., 62 (1965),4590f.6. QURESHI, MOSHIN, AKHTAR, IQBAL & MATHUR,1\:. N.,Analyt. Chern.,39 (1967),1766.7. QURESHI, MOSHIN & SHARMA, S. D., Analyt. Chem.,45(1973),1283.8. KRAUS, K. A. & PHILLIPS, H. 0., J. Am. chern.Soc.,84(1962),2267.SpectrophotometricDetermination ofRu(III) with Promazine HydrochlorideH. SANKE GOWDA & K. N. THIMMAIAHDepartmentof Post-graduateStudiesand ResearchinChemistry,Universityof Mysore,ManasaGangotri,MysoreReceived17July 1976;accepted2 November1976Promazinehydrochloride(PMH) is proposedas anewrea~entfor thespectrophotometricdeterminationof Ru(III) basedon theformationof a red-colouredcomplexin sulphuricacid medium(1·25-2·0M).A"tWenty-nine-foldmolarconcentrationftherea~entisnecessaryfor thefull developmentof thecolourin-tensity.Beer's law is obeyedfor 0·2-11·94ppmofRu(III) withoptimumconcentrationran~e1·3-11·3ppm.Thecomplexhasabsorptionmaximumat515nmwithmolarabsorptivity7·328X 10'litremole-icm-i•~THE reactionbetweenpromazinehydrochloride(PMH) andruthenium(III)doesnot appeartohave beenstudiedso far. We havestudiedthisreactionandproposedPMH as a sensitivereagentfor thespectrophotometricdeterminationof Ru(III).The proposedmethodoffers the advantagesofsimplicity,sensitivityandstabilitywithouttheneedfor extraction.Ruthenium(III) chloride(Mfs JohnsonMatthey;0.989g) was dissolvedin dilute hydrochloricacid(AR) anddilutedto 1 litre to give1M with respectto the acid. It was standardizedgravimetricallyby the thionalidemethod. The stocksolutionwasfurtherdilutedto givea standardsolutioncontain-ing 20 [JogRu(IlI) fml. A knownamountof PMHUohn Wyeth) was dissolvedin doubly distilledwater,solutionstandardizedby theCe(IV)sulphatemethodland storedin an amberbottlein a refri-gerator. Solutions of diverse ions of suitableconcentrationswerepreparedusinganalyticalgradereagents.Procedure- Samplesolutioncontaining5to 298·5[Jogof Ru(IlI) wastransferredto a 25ml volumetricflaskandto this wasadded7·5ml of 5M sulphuricacid (AR) and4·5mlof 0'2%PMH solution. Thesolutionwasdiluted.up to the mark with doublydistilled water,mixedthoroughlyand the absor-bancemeasuredat 515nm after 10min againstareagentblankpreparedin thesameway. Rutheniumconcentrationof thesamplesolutionwascalculatedby meansof a calibrationcurve.PMH formsa red-colouredcomplexwith Ru(III)at roomtempe,.aturein the presenceof sulphuric,hydrochloricor phcsphoricacid. The sensitivityof thereactionandstabilityof theredcolourdependon the natureand strengthof the acid medium.Tile sensitivityin threeacidmediais in the orderof H2S04~HCI>H3P04'The maximum colourdevelopmenttakesplaceafter 10min in l'25-2'OMsulphudcor 2·0-2·70Mphosphoricacid and after50 min in 1·5-3·0M hydrochlo:icacid. The colourof the red complexin H2S04,HCI and H3P04isstablefor 12,3 and12hoursrespectively.Thoughthestabilityof Ru-PMH complexin H3P04is 12hr,the sensitivity(0·0217[Jogfcm2) is very muchlessand hencethe sulphuricacid mediumhas beenselected.Maximumabsorbanceis achievedin 1·25-2·0Msulphuricacidsolution. The complexformationisincompleteat aciditieslower than 1·25M H2S04,The reagentundergoeslow oxidationat aciditieshigherthan 2·0M H2S04, The complexexhibitsmaximumabsorbanceat 510-520nm; the reagentdoesnot absorbaroundthis wavelength.It is foundthat a twenty-nine-foldmolarexcessof the reagentis necessaryin orderto ensurecom-pletecomplexation.The absorbancevaluesremainconstantin the temperaturerangeof 5-70°C.Theorderof additionof reagentsis not critical. Beer'slaw is valid overthe rutheniumconcentration0,2-11·94 ppm. The optimum concentrationrangeevaluatedby Ringbom'smethod2is 1·3-11·3ppm.The molar absorptivityand sensitivityindex are7·328xl03 litre mole-l cm-l and 0·0138[Jogfcm2respectively.The sensitivityof the proposedmethodis morethanthat of prochlorperazinemaleate3,thioridazinehydrochloride4and dithioxamide5whichhavebeenproposedas spectrophotometriceagentsfor ruthe-nium. The sensitivityof the presentmethodisless than that of 4-hydroxy-3-nitroso-5,6-benzo-coumarin6, 2,3-diaminopyridine7 andthiovioluricacid8whichareusedfor the determinationof rutheniumin the samerange.The red Ru-PMH complexis cationicin naturesincethe red colouris retainedon the cationex-changeresin.The followingamounts([Jogfml)of foreignionsarefoundto giveanerrorof ± 1·5%in thedetermina-tion of 4 [Jogof Ru(III) per ml: Palladium(lI) 0'3,Os(VIII) 0·8,Rh(III) 12, Ir(III) 12, Pt(IV) 4'0,Au(III) 0,2, Co(II) 480, Cu(II) 480, Ni(I1) 400,U(VI) 615'8,Fe(III) 1'5,Zr(IV) 1214,Mo(VI) 200,Ce(IV)0,2,chloride4004·7,bromide9365,iodide1'5,477INDIAN J. CHEM., VOL. 15A,MAY 1977:fI.uorie 4088·7,sulphate19624,phosphate3659,nitrat 16,864.acetate7452, citrate 6400, tartrate6233,thiosulphate1·0and EDTA 0,96.Th authorsthankthe CSIR, New Delhi, for theawar of a juniorresearchfellowshipto oneof them(K.N.. ).H. et. ai. (unpublishedwork).4782. RINGBOM, A., Z. analyt. Chem.,115 (1938),332.3. SANKE GOWDA, H. & RAMAPPA, P. G., Anal. chim. Acta,83 (1976),283.4. SANKE GOWDA, H. & RAMAPPA, P. G., Curro Sci., 45(1976),218.5. BEAMISH, F. E., Theanalyticalchemistryof thenoblemetals(PergamonPress, London), 1966.6. NITIN KOHLI & SINGH, R. P., Talanta,21 (1975),638.7. AYRES, G. H. & EASTES, D. T., Anal. chim. Acta, 44(1969),67.8. CHAWLA, R. S. & SINGH. R. P., Mik1'ochim.Acta, (1972),496., I

Spectrophotometric Determination of Ru(III) with Promazine Hydrochloride

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Spectrophotometric Determination of Ru(III) with Promazine Hydrochloride

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