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-李利荣,吴宇峰,杨家凤,时庭锐,袁倩,魏恩棋(,300191):建立了固相萃取毛细柱气相色谱-电子捕获检测器定量分析水中硝基苯类化合物的分析方法通过对固相萃取柱的选择固相萃取条件(样品溶液的pH值上样速度上样体积洗脱液选择及配比)的优化,得出了最佳实验条件穿透体积可达115L,回收率在80%~105%,最小检出浓度在0100037~01072LgPL之间,均大大低于GB13194-91的规定相对标准偏差在017%~513%之间该方法准确简单,重现性好回收率高,污染小:固相萃取;硝基苯类化合物;气相色谱;水样分析:X832:A:1002-6002(2007)01-0011-04AnalyticalMethodforaromaticnitrocompoundsinWaterbySPEGC-ECDLILi_rong,etal(TianjinEnvironmentalMonitoringCentre,Tianjin300190,China)Abstract:Amethodforthedeterminationofaromaticnitrocompoundsinwaterhasbeenestablishedbysolid_phaseextraction(SPE),capillarygaschromatographywithelectroncapturedetector.ThroughtheselectionofSPEcolumns,thechosenofSPEconditionswhichincludethepHvalueofwatersample,loadspeed,loadvolume,elutionsolutions,etc,theoptimuminspectionconditionswasgot.Themaxloadvolumescanbe115L.Therecoveriesofeverycompoundswasbetween80%and105%.Therelativestandarddeviationrangedfrom017%to513%,theminimaldetectionconcentrationwasbetween0100037~01072LgPL,lowerthanthoseofGB13194-91.s.Thecorrelationisbetween019993~019999.Keywords:Solid_phaseextraction;Gaschromatographyspectrometry;Aromaticnitrocompounds;Wateranalysis:2006-03-24:(2004DKA10150):(1972-),,,.,,,,[1],GB3838-2002[2],[3][4],[5-7]OasisHLBDB-35MS,,,,1111Agilent6890N();:BF-2000A;:Agilent;:AgilientC18(500mg),WatersOasisHLB(1000mg),AgilentPhenyl(500mg),GDX502(500mg);:1005010Ll;:DB-35ms(30m@0132mm@110Lm)35%;23120072EnvironmentalMonitoringinChinaVol.23No.1Feb.2007:(5g,10ml);:011mg:Fisher:,,-,,-2,4-2,4-,99%:,25ml,,,(1000mgPL):25ml,,115mgPL310mgPL4010LgPL2,4-2,4-5010LgPL:400e4h,,:112GC:DB-35ms(30m@0132mm@110Lm);:100e(0min),5ePmin160e(0min),15ePmin200e(0min),5ePmin220e(0min);:280e;:018mlPmim;LECD:300e113(1):pH,5j,(2):OasisHLB,5ml,5ml,,10ml,(3):(10~1500ml),,,20~25mlPmim,1cm,10ml,10mim(4):,,,10mlP(90B10,VPV),,,40e110ml,110Ll,(5):125102050Ll110ml,,110Ll11y=01934x-13190r=019993-y=01315x-17199r=019999-y=01525x-13192r=019995-y=01377x-17198r=019996-y=3814x+5188r=019998-y=2419x+2315r=019999-y=3413x+4111r=0199992,4-y=3010x+114r=0199992,4-y=4414x+294r=019998(6):,2211FIDNPDECD,ECD,ECD,ECD,ECD2212HP-1HP1701DB-35MSHPINNOWAXDB-FFAP,HPINNOWAX2,4-2,4-,(HPINNOWAX2,4-2,4-),DB-35MSDB_FFAP1212231200722LgPL0125011401021-0120011201051-0124011301040-0133011401072-013501170100061-013001200100076-0128012301000592,4-0162011001000742,4-019301230100037:1L(ECDOasisHLB,NPDFIDC18),DB_35ms,3ECD,ECD1DB-35MS11;21;31;41;51;61;71;812,4;912,42DB_FFAP213015ml100ml10Ll,AgilientODSC18WatersOasisHLBAgilent_Phenyl,GDX502GDX501GDX101GDX103GDX401,20mlPmin,P(90B10,VPV),,5ODS_C18GDX401Agilent_Phenyl60%,80%,ODS_C182,4-2,4-50%,80%ODS-C18,,2,4-2,4-Agilent_PhenylGDX40180%,OasisHLBGDX502GDX502,OasisHLB21421411ECD,OasisHLB,P(100B090B1050B1010B100,VPV),,P(90B10,VPV)33B100%90B10,VPV50B10VPV10B100VPV4616921177185018631791119213561861178916791943116319971278193919521795118017347618941989144822139118831549112,4-10159613851943152,4-7168991395301521412100ml10Ll0015110210510ml,OasisHLB,P(90B10,VPV),,,,,:-133510~1010ml21413100ml10Ll015ml51015202535mlOasisHLB,,,,15~25mlPminSPE21414pH100ml10Ll110mlpH,pH510710910,20%,90%~110%,214151%[8],;,,,,,,015110115210L,,1000mgOasisHLB,,015110115L85%,210L10%,OasisHLB115L215100ml,,44OasisHLB(n=5)(LgPL)(%)(%)(LgPL)(%)(%)(LgPL)(%)(%)144811231514409211118144009516017-279821631727909111219279009712211-278801741327808916219278009316216-309801841930909712310309009813214-31719214414371129511210371129615117-4108315317401094191174009513111-41082145114010911831140094112152,4-517983135135719961331757996183102,4-51128512415511299133105121022131423120072:2006-03-16:(1968-),,,,.216,110L,,(3155LgPL)-(1186LgPL)-(0194LgPL)--(1152LgPL)-(0155LgPL)-(0143LgPL)2,4-2,4-,01005LgPL,80%~105%3-pH,GB13194-91115L,80%:[1].[M].:,389-399.[2]GB3838-2002.[S].[3]GB13194-91.[S].[4]SLPT23711-2001.P.[5],.[J].,2005,24(4):463-466.[6],,.2,4-[J].,1995,23:652-654.[7],,.-[J],,1998,17(1):33-36.[8].[M].:,67-69.GC-MS周雯1,2,王连生1(1.,210093;2.,213001):用固相萃取的方法对样品进行预处理,再进行GC-MS分析测定,对饮用水源水中的痕量半挥发性有机化合物进行了测定,并对结果进行了讨论:饮用水源水;半挥发性;有机物;测定:X832:A:1002-6002(2007)01-0015-03DeterminationofSemi_volatileOrganiccompoundsindrinksourcewaterbyGC-MSZHOUWen1,2,etal(1.StateKeyLaboratoryofPollutionControlandSourcesReuse,DepartmentofEnvironmentalScienceandEngineering,NanjingUniversity,Nanjing210093,China;2.ChangzhouEnvironmentalBureau,Changzhou213001,China)Abstract:Thispaperdescribedthefactthatwepre_processsamplebySPE,thenSemi_volatileOrganiccompoundsindrinksourcewaterwereanalyzedbyGC-MSmethod,theresultwasdiscussed.Keywords:Drinksourcewater;Semi_volatile;Organiccompounds;Determination23120072EnvironmentalMonitoringinChinaVol.23No.1Feb.2007