催化裂化催化剂中镍钒锑的测定严方

1，21.2665552.257061：XNi、V、SbNi、V、Sb。Ni0.10%～1.20%V0.05%～0.30%Sb0.02%～0.20%0.99992%。。：X：TH744.16；TG146.1+5：A：1674-5124（2010）01-0046-03DeterminationofNi、V、SbonFCCcatalystsYANFang1XIEYong-jie21.CollegeofChemistryandChemicalEngineeringChinaUniversityofPetroleumQingdao266555China2.ShandongShtarScience&TechnologyCo.LtdDongying257061ChinaAbstract:Incatalystsheavymetalpollutionisaseriousproblem.TheXRFmethodwasintroducedinthispaperfordeterminingNiVSbinFCCcatalysts.Bytheestablishmentofanalyticalmethodthecauseandeffectofcontentdeterminationhasbeendiscussed.Thematrixeffectcanbeovercomebyusingcalibrationstandardswithfreshcatalystasmatrix.Linearitywindowis0.10%~1.20%forNi0.05%~0.30%forV0.02%~0.20%forSbthecorrelativecoefficientsarelargerthan0.9999forthreemetalsandmeasurementRSDsarelessthan2%.Resultsshowthatthemethodisfastaccurateandconvenient.TheresultsaregenerallyconsistentwiththosefromAAS.Keywords:ChemicalanalysisX-rayfluorescencespectrometryCatalystNiVSb：2009-04-07；：2009-06-15：1970-。1、。Ni、V[1-4]。、、。、。、。。Ni、V、Sb、[5-9]。。XXRFNi、V、Sb、。22.1、X3063p99.5%V2O5Sb2O3A2.0%B0.6%。1。36120101CHINAMEASUREMENT&TESTVol.36No.1January2010361NiVSb/%RSD/%/%RSD/%/%RSD/%1#1.211.30.311.00.200.982#0.721.20.450.890.241.015（n=20）2.22.2.1、V2O5Sb2O31+1Ni、V、Sb5g/L、3g/L、3g/L。2.2.2Ni、V、Sb、850℃1h1.5g25mm。2.2.3、850℃1h。1.5g25mm。。33.1Ni、V、Sb。。2.0%0.6%。3.2Ni、V、Sb2。Ni、V、Sb。Ic3。3.3Ni、V、SbKα。30tNi、V、Sb。Ni、V、Sb1.2gNi、V、Sb1.4g。1.4～1.6g。3.4112nσ34。X。3.5Ni、V、Sb1%Ni;1%Ni、V、Sb。/kV/mA2θ/（°）2θ/（°）/sNiKαW5040LiF（200）SC48.6449.5020VKαW5040LiF（200）SC76.9275.0020SbKαW5040LiF（200）SC13.4611.50201NiVSbABABAB1#0.820.820.050.050.020.022#1.221.220.100.100.080.083#1.021.020.150.150.120.124#0.120.120.200.200.160.165#0.420.420.300.300.200.202/%Ni0.10～1.20I=12.195c-0.390.9999V0.05～0.30I=30.303c-0.3330.9999Sb0.02～0.20I=55.58c-0.1130.99993/（μg·g-1）Ni20V30Sb23447201012.0%0.5%1%1%。3.6。1。2.0%1#0.6%2#1.5g2020Ni、V、Sb。5。2%。2。20Ni、V、Sb。2%。。3.710Ni、V、Sb6。6Ni、V、Sb。3.8AAS。XXRF207。7。4XNi、V、Sb、。。[1].[M].2000.[2].FCC[J].2006141126-30.[3].FCC[J].199181-3.[4].[J].200935181-83.[5].[M].1998.[6].X[M].2005.[7].-ICP-AES、、、、、、[J].200834266-68.[8].ICP-AES[J].19887237.[9].[J].200710142-45.NiVSbXRFAASXRFAASXRFAAS10.790.780.440.430.170.1620.760.760.650.640.150.1530.730.740.820.830.200.1841.011.000.430.450.020.0250.530.550.360.370.020.0260.330.350.560.580.020.0170.450.440.780.760.230.2080.080.090.320.330.020.0290.610.620.550.560.020.02100.690.680.570.570.160.15110.870.880.640.630.070.07120.560.560.550.540.150.15130.530.540.420.430.200.19141.111.130.230.250.120.12150.830.850.260.270.050.06160.730.750.160.180.030.03170.350.340.180.160.130.12180.180.190.120.130.070.08190.910.920.250.260.120.12200.290.280.270.270.130.1476/%/%/%/%Ni0.500.49Ni0.280.29N-1V0.200.21N-6V0.200.21Sb0.050.048Sb0.150.14Ni0.320.31Ni0.500.49N-2V0.480.47N-7V0.200.21Sb0.170.16Sb0.050.047Ni0.630.65Ni0.750.78N-3V0.250.24N-8V0.300.27Sb0.150.14Sb0.100.11Ni0.780.79Ni0.600.59N-4V0.300.28N-9V0.100.11Sb0.080.07Sb0.150.14Ni0.900.92Ni0.800.79N-5V0.300.31N-10V0.260.24Sb0.020.018Sb0.100.00948