固相萃取和高效液相色谱联用测定污水中的五氯苯酚李萍

＊李　萍　管秀娟(,510006)　采用固相萃取和高效液相色谱相结合的方法对污水中五氯苯酚的含量进行定量检测。结果表明,污水的pH值为4,流速控制在4mLL以内,C18固相萃取柱对五氯苯酚有良好的吸附保留性能,以2mL的甲醇洗脱,洗脱效率在85%～95%之间。与传统的液液萃取相比,固相萃取的优势在于操作时间缩短、有机溶剂的使用量减少。　五氯苯酚　固相萃取　液相萃取　　　　　　　　＊(2005B33301007)0　(PCP),,PCP(310℃),,。,。PCP,,(SPE),。-,SPE、、,[1-4]。1　1.1　实验仪器与试剂LC-10AD;SupelcleanLC183mL,;irregular_HC18micron4.6id×25cm;,1～6SupelcleanLC183mL,6。;pH=4;10mgPCP()10mL,。1.2　SPE的操作程序、、0.45μm;5mL100%,10mL,;,;,10min;,HPLC。1.3　HPLC的检测,,HPLCPCP。irregular-HC18micron4.6id×25cm,40℃;,248nm;:8515;20μL;1mLmin。2　2.1　固相萃取条件的优化,pH;;;4,SPE。9:8(ApH3;B90%;C4mL;D4mLmin)PCP,91.3%。4、3PCP1。1R,4PCPApHC;CD;B(80%～100%)PCP,80%。ApHPCP75　　　20076253DOI:10.13205/j.hjgc.2007.03.023　　　1　、(A)pH(B)%(C)mL(D)(mL·min-1)176.182.783.876.9282.481.583.282.0384.879.176.284.4R8.73.67.67.51　PCP　,1,A3(pH3、57),pHPCP。pHPCP,pH4、3、21,8,:4pHPCP。pH=4pH,SPE,pH4。2CD,1,12(4mL2mL),23(2mL1mL),SPE2mL。1,PCP,,SPE4mLmin。2.2　SPE和液-液萃取应用效果的比较、、20μgL200μgLPCP6,SPE-(LLE)2。2。　　2,232,,2PCP。3PCP200μgL,SPELLE2,　　　2　SPELLE2PCP%1,20μgL2,200μgLSPELLESPELLE87.67993.894.7119.588100.4107.8133.6120.3117.698.593.8%～117.6%94.7%～107.8%。PCP20μgL,87.6%～133.6%79%～120.3%。　　LLE,SPE3:①SPE,LLE,,LLE;②SPE,,SPELLE;③SPE1,,,。3　SPEpH4.0、4mLmin、80%、2mL;HPLCC18;,:=85∶15(vv);40℃;248nm。[1]　,,..,2006,24(3):71-73.[2]　CuriniR,GentiliA,MarcheseS.etal.Monitoringofpesticidesinsurfacewater:off_lineSPEfollowwedbyHPLCwithUVdetectionandconfirmatoryanalysisbymassspectrometry.Chromatographia,2001,53:244_250.[3]　DivincenzoJ.P,SparksDL.Sorptionoftheneutralandchargedformsofpentachlorophenolonsoil:evidencefordifferentmechanisms.ArchEnvironmContamToxicol,2001,40:445-450.[4]　DivincenzoJ.P.,SparksDL.Sorptionoftheneutralandchargedformsofpentachlorophenolonsoil:evidencefordifferentmechanisms.ArchEnvironmContamToxicol,2001,43:445-450.　　510006　　　[phone]E-mail　[e-mail]2006-08-1176　　　20076253SYNTHESISOFNANOMETERIRONFROMFLUESLIMEOFBLASTFURNACEXuYing　WangWei　HuBinsheng(64)……………………………………………………………………………………………………………Abstract　TheFeCl2solutionwassynthesizedbyusingflueslimeofblastfurnaceasrawmaterialsongasandsolventextraction.Thenanometerironwassynthesizedinthesystemofethanolandwater.KBH4wasusingasreducer,thesurfaceactivitymaterialexistatthesametime.Theinfluencefactorsofwholeprocesswerestudied.Thesampleofnanometerironwiththeaveragegrainsizeof71nmwaspreparedandcharacterizedbyXRDandSEM.Keywords　flueslimeofblastfurnace,synthesis,extractionandnanometerironmetalDECHLORIDIZATIONMECHANISMANDEXPERIMENTININCINERATIONPROCESSOFMEDICALWASTESQingShan　WangHua　HePingetal(66)…………………………………………………………Abstract　BecausethemedicalwastesincludePVCcontainingchlorineelement,andtheirincinerationwouldproducepollutantHClsoitisnecessarytodechloridizeinmedicalwastesincineration.Firstly,fromthethermodynamicsanalysis,itisknownthatduringthedechloridizationprocesswithadditionofabsorbents,theabsorbentswiththebestdechloridizationeffectareCa(OH)2,CaO,CaCO3,MgCO3,Mg(OH)2,whiletheworstisMgO.Theresultsofexperimentshowthat:thetemperatureplaysimportanteffectsondechloridization,theoptimaltemperatureiscontrolledaroundfrom800℃;Thesmallerthegranuleofabsorbentis,thehighertheutilizingefficiencyofabsorbentsurfaceis,andthehigherthedechloridizationefficiencyis;withtheCaClincreases,thedechloridizationefficiencyincreases,buttheincreasingratetendstoslow,andtheoptimalCaClis2.5～3.Keywords　medicalwaste,dechloridization,mechanismandexperimentANALYSISOFENVIRONMENTALPROTECTIONFORELECTRONICPRODUCTION&CIRCULARECONOMYPROJECTYuJun　QiuWanhua(71)………………………………………………………Abstract　Itisanalyzedtheproblemsofe-wasterecyclinginChina,andsomesolutionsarealsoproposed.Throughtheanalysisofenvironmentalprotectionforelectronicproduction&circulareconomyprojectinHaidianDistrict,Beijing,theimportantroleofgovernmentpushingcombiningwithmarketpullinginimprovinge-wasterecyclingchainisstressed.Theirpracticescanbepopularized.Keywords　e-wasterecycling,treatment,technologyandcirculareconomyDETERMINATIONOFPCPFROMSEWAGEBYSPEANDHPLCLiPing　GuanXiujuan(75)………Abstract　ThemethodofdeterminationPCPfromsewagebysolid-phaseextraction(SPE)andhigh-performanceliquidchromatography(HPLC)wasstudied.Resultsshowthat:samplepH=4,elutingsolventwas100%methanol,elutingsolventvolumewas2mL,flowrateofwatersamplewas4mLL.TherecoveriesofPCPwerebetween85%～95%.ImportantadvantagesoftheSPEmethodcomparedtotheliquid-liquidextractionmethodweretheshortextractiontime,andreducedconsumptionoforganicsolvents.Keywords　pentachlorophenol(PCP),solid-phaseextractionandliquid-liquidextrationDETERMINATIONOFMICROANALYSISMETHODOFMINIMPHTHALATEESTERSINWATERChengAihua　WangLei　ZhangRuietal(77)…………………………………………………………………………………Abstract　Thephthalateesters(PAEs)areakindofpersistentharmfulpollutantwhosecontentistinyandmeasurementisdifficult.Throughcomparisonoftheliquid-liquidextraction,thesolidphaseextraction,thehighperformanceliquidchromatographyandthegaschromatographymassspectrometryanalyticalmethoddeterminingPAEsinwater,theSPE-GC-MSanalyticalmethodforthesimultaneousseparationanddeterminationofPAEsfromwatersampleswasconsideredthebestmethodinlaboratory.Keywords　phtha