X射线衍射定量相分析新方法

226Vol.22No.6200311FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)Nov.2003X,(,l13001):X,X,,K,JCPDS,,X,,,:X;;:O722:A:1004-4957(2003)06-0080-03XX,,X,[1][2][35],,[6](),,,,11KK,,,K1n,ijIi/Ij=Kji(Xi/Xj)(1)IiIjij;XiXjij;KjiijmnXRD,Yp(2):Yp(2)=ni=1SiPip(2)(i=1,2,3,......,m)(2)Yp(2)p,Sii,Pip(2)ip,2JCPDS(2):Q3=mp=1[Yp(2)-ni=1SiPip(2)]2Q3=Qmin,Si9Q39Si=0(i=1,2,3,......,n):2002-12-07;:2003-09-06:(1952-),,,.6:X81mp=1P1pP1pS1+mp=1P1pP2pS2++mp=1P1pPnpSn=mp=1P1pYpP2pP1pS1+mp=1P2pP2pS2++mp=1P2pPnpSn=mp=1P2pYpPnpP1pS1+mp=1PnpP2pS2++mp=1PnpPnpSn=mp=1PnpYp(3)Siij:Si/Sj=A(Ii/Ij)(4)A,(1)(4):Si/Sj=AKji(Xi/Xj)=kjiXi/Xj(5)(5),Si/SjIi/Ij,X,c,(5):Ii/Ic=(Kc/Ki)(Xi/Xc)(6)(6)Ii/Ic=kci(Xi/Xc)(7)IiIccic,XiXcic,Kci,icKciic11,(7):Xi=(Xc/kci)(Ii/Ic)(8)(8)22.1D/max-RBX,(40kV,50mA):DS=SS=1,RS=0.15mm,,0.25(2)/min;2.2-Al2O3TiO2Mo2O3CaCO3(,99.9%),,-Al2O3(104),TiO2(101),Mo2O3(220),CaCO3(100)310m,4,,12.5g-Al2O3,TiO2,Mo2O3,CaCO33,K2,121,,X,,,mp=1mp=1SamplePhaseX/%X/%Integralintensity,cps3r/%331-Al2O325.0025.002514.670.000.00TiO225.0024.688221.00-0.321.28Mo2O325.0024.461547.33-0.542.16CaCO325.0025.8610777.000.86-3.442-Al2O328.9028.902704.670.000.00TiO227.6026.668297.00-0.943.41Mo2O323.0022.471327.67-0.532.30CaCO320.5021.977684.671.47-7.173-Al2O330.0030.003038.330.000.00TiO230.0029.429908.33-0.58-1.93Mo2O320.0020.911337.330.914.55CaCO320.0019.679285.00-0.33-1.654-Al2O339.4039.404236.330.000.00TiO221.6021.346916.33-0.26-1.23Mo2O328.5029.062000.000.961.96CaCO310.5010.205113.671.302.863,332,,,4X,,KKKKK:[1].X[M].:,1980.97-120.[2].X[J].,1991,49(3):202-206.[3]TORAYAH,TSUSAKAS.Quantitivephaseanalysisthewhole-powder-patterdecompositionmethod.I.solutionfromknowlelgeofchemicalcompositions[J].BJApplCryst,1995,44(28):389-392.[4]CHUG,SUIQ.ExternalstandardmethodforquantitativeX-raydiffractionphaseanalysisofsamplescontainingamorphousmaterial[J].ActaMetallurgicaSinica,1994,47(3):179-182.[5].X[J].,1998,47(7):1143-1145.[6].X[J].,1995,44(1):1679-1683.ANewMethodforQuantitativeX-rayDiffractionPhaseAnalysisSHENChun-yu,CHUGang2Table2Comparisonofanalyticalresultsofthismethod,matrixflashingandexternalstandardmethodSamplePhaseThismethodMatrixflashingExternalstandardmethodX/%X/%r/%X/%r/%X/%r/%1-Al2O339.4039.400.0040.372.4640.412.56TiO221.6021.34-1.2320.18-6.5721.02-2.69Mo2O328.5029.061.9629.965.1229.262.67CaCO310.5010.20-2.869.49-9.619.31-11.32-Al2O328.9028.900.0028.02-3.0429.883.39TiO227.6026.66-3.4129.135.5428.874.60Mo2O323.0022.47-2.3021.28-7.4822.65-1.52CaCO320.5021.977.1721.575.2218.6-9.271Table1Testforrecoverybyaddingcleanoutlotion8222226Vol.22No.6200311FENXICESHIXUEBAO(JournalofInstrumentalAnalysis)Nov.200316Fig.1Thestructureofsixpharmaceuticalracemates(PetrochemicalTechnologyFaculty,LiaoningUniversityofPetroleum&ChemicalTechnology,Fushun113001,China)Abstract:AnewapproachforquantitativeX-raydiffractionphaseanalysisofpowdermixturehasbeendeveloped.Themethodusesallthediffractiondataofthesamplemixture.Beforethedetermination,theflushingagentandallthecomponentstobedeterminedaremixedtogetheranddeterminedatthesamedeterminationcondition.ThustheKvaluesforthesamplecomponentsandthoseforthecorrespondentonesoftheflushingagentareobtained.BycomparingthedatawiththeJCPDSdataandcarryingtheleastsquarecalculation,theneededdatafortheintensityratioofallthephasesareobtainedforthefinalcoefficientswhenthesumofdeviationsistheleast.Theprocedurehasbeentestedbyusingfoursamples,theanalysisresultsagreewellwiththetheory.Keywords:X-raypowderdiffraction;Quantitiesphasecatalyst;Matrixflashingmethod,,,(,300071):,,6;-,6;:;;;;;;;;:O657.72;TQ460.72:A:1004-4957(2003)06-0083-03(atenolol)(celiprolol)(carteolol)-,(nicardipine),(albuterol),(promethazine)6,,(1),(CSP)(HPLC)[15],1994Arm2strong[6],,,,LC[7,8](CE)[9](CEC)[10]CSP3:2002-12-09;:2003-09-13:(1975-),,,;,.