EDTA络合滴定法快速测定硫酸锆中氧化锆含量

20093732009373[1]EDTA[2]。、、。EDTAEDTAEDTA[3]。[Zr(SO4)2·4H2O]EDTAEDTA、、。11.1。EDTA0.02mol/L9.03g1mg250mL。150mL1000mL。1.2EDTA[4]43g0.1mg300mL10mL1+1250mL。50mL250mL100mL。GB/T2590.1—19813“31%……”“……900℃”。。0.2%。15mL250mL。HG/T3786-20054“4……”“……”。(1)EDTATg/mL4:EDTA,524048HClEDTAEDTA。。EDTARapidDeterminationofZirconiumOxideContentinZirconiumSulfatewithEDTACompleximetryPANRong-kai,ZHUGui-lian,XUXu-yao,CHENJing(ChemistryScienceandTechnologySchool,ZhanjiangNormalUniversity,GuangdongZhanjiang524048,China)Abstract:TherapiddeterminationofzirconiumoxideinzirconiumsulfateinHClmediumwithEDTAcompleximetricanditstitrationconditionswerestudtied.Amethodwasintroducedwhichcombinedthegravimetricanalysisandvolumetricanalysistogethertodeterminethezirconiumoxidecontentofzirconiumsulfatebygravimetricanalysisatfirst,andusedzir-coniumsulfate(whosezirconiumoxidecontentwasknown)asthecalibrationagenttocalibratetitervalueofstandardEDTAsolution,thenusedtheEDTAtodeterminethezirconiumoxidecontentofzirconiumsulfateproducedwiththesamerawma-terial.Thisanalysiswassimple,rapidthangravimetricanalysisanditsaccuratewassatisfactory.Keywords:EDTAcompleximetry;rapiddetermination;zirconiumoxidecontent(1982-)。E-mail:[e-mail].150··20093732009373T=mW(15/250)V×100=6×10-4mWV(1):mgW%VEDTAmL。1.33g0.1mg1.2250mL。10mL250mL100mL6mol/LHClpH0～0.30.2g2min22g/L0.02mol/LEDTA。。(2)ZrO2(%)=VTm×(10/250)×100=2500VTm(2)TEDTAg/mLVEDTAmLmg。22.1Zr(OH)4。。6mol/LHCl1。2pH0～0.3。pH≥0.4。6mol/LHCl25mL。2.2[ZrO]2+[ZrO]2+2[ZrO]2+→[ZrO]24+。EDTA[ZrO]2+[5]。(25℃)、70℃90℃(2)(25℃)、70℃。90℃、。2.3Al3+、Ca2+、Mg2+、Zn2+、Fe2+Ti4+。Fe3+。Fe3+。2.41.3、EDTA3。3EDTA0.10%。2.5[2]EDTA。、32%～34%。、、。。。101.47-50.77-100.5656.25150.4093.44170.3498.41200.2899.67250.2099.67300.11100.57350.06100.36400.0199.8850--70--6mol/LHCl/mL/pH/%/℃W(ZrO2)/%2512.557026.859033.1423EDTA1#2#3#、。32.9432.9232.8733.0432.9833.0533.0333.1233.1533.0933.1333.1133.1433.2333.17EDTA/%/%/%/%1#2#3#32.9533.320.3733.0933.250.1633.1633.260.10(156)151··200937320093733(1)EDTA。。pH0～0.3。(2)、HG/T3786-2005。[1]、()[S].GB/T2590.1-1981,[2],,.EDTA[J].,2007,39(11):55-57.[3]..:,1986,261.[4][S].HG/T3786-2005.[5],,.EDTA[J].,2001,24(4):39-40.[18]SunL.F.,PeterW.C.,Mixed-moderetentionofpeptidesonphosphate-mod-ifiedpolybutadiene-coatedzirconia.Anal.Chem.,1995,67:2517～2523.[19]ScottT.,Kephart,PurnenduK.,Dasgupta,Hoteluentcapillaryliquidchromatographyusingzirconiaandtitaniabasedstationaryphases.Anal.Chim.Acta,2000,414:71～78.[20]StephanieJ.M.,BrianA.,Affectofhigh-temperatureonhigh-performanceliquidchromatographycolumnstabilityandperformanceundertempera-ture-programmedconditions.J.Chromatogr.A,2004,1030:255～262.[21]HeP.,YangY.,Studiesonthelong-termthermalstabilityofstationaryphasesinsubcriticalwaterchromatography.J.Chromatogr.A,2003,989:55～63.[22]SatoshiY.,ToshiakiI.,TsuneoO.,TomotakaS.,Reversed-phaseliquidchromatographyonamicrosphericalcarboncolumnathightemperature.J.Chromatogr.A,1996,728:189～194.[23]Snyder.L.R,Zhu.P.L,Comnineduseoftemperatureandsolventstrengthinreversed-phasegradientelutionIV.Selectivityforneutral(non-ionized)samplesasafunctionofsampletypeandotherseparationconditions[J].JournalofChromatographyA,1996,756:63.[24]MarsinSanagi.M,See.H.H.Hightemperatureliquidchromatographyoftriazolefungicidesonpolybutadiene-coatedzirconiastationaryphase[J].ChromatographyA,2004,1059:95-101.[25]GreibrokkT,AndersenT,High-temperatureliquidchromatography[J].ChromatographyA,2003,1000(12):743.[26]LiuG.H.,DjordjevicN.M.,ErniF.,High-temperatureopen-tubularcap-illarycolumnliquidchromatography.J.Chromatogr.,1992,592:239～247.[27]CarstenA.B.,ScottT.E.,RobertE.S.,Simultaneousflameionizationandabsorbancedetectionofvolatileandnonvolatilecompoundsbyre-versed-phaseliquidchromatographywithawatermobilephase.Anal.Chem.,1997,69:3465～3470.[28]TronesR.,AndersenT.,HunnesI.,GreibrokkT.,Modifiedlaserlight-scat-teringdetectorforuseinhightemperaturemicroliquidchromatography.J.Chromatogr.A,1998,814:55～61.。[1],,,.[C].2004,76-1790.[2],.[J].,2003,6:33-36.[3]SGeorge,SBalla,VGautam,etal.Effectofdieselsootonlubricantoilviscosity[J].TribologyInternational,2007,40:809-818.[4]SGeorge,SBalla,MGautam,Effectofdieselsootcontaminatedoilonen-ginewear[J],Wear,2007,262:1113-1122.[5],,.[J].,2006,33(3):14-16.[6],,.[J].,2003,3:52-53.[7].[J].,2005,20(2):62-64.[8].()[J].,2004,19(2):38-43.(151)(149)!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!2009《》####156··