高压消解流动注射光度法同时测定水中总氮与总磷

/1,1,2(1.,214073;2.,210098):,,0.0010.0mg/L0.001.00mg/L,,5%,1%3%,2.27g/L2.11g/L,,97.2%108%,100%106%,:;;;:X703.1:C:1000-4602(2009)22-0093-05DeterminationofTotalNitrogenandPhosphorusinWaterbyAutomaticHighPressureDigestion/FlowInjectionAnalyzerZOULin1,ZHOUSheng2dong1,CHENWei2(1.WuxiWaterSupplyGeneralCompany,Wuxi214073,China;2.CollegeofEnvironmentalScienceandEngineering,HohaiUniversity,Nanjing210098,China)Abstract:Theflowinjectionanalyzerwasusedfordeterminationoftotalnitrogenandphosphorusinwater.Theresultsshowthatthereisagoodlinearrelationshipwhenthetotalnitrogenandphosphorusareintherangeof0.00to10.0mg/Land0.00to1.00mg/Lrespectively.Therelativeerrorsarealllessthan5%.Therelativestandarddeviationsareallintherangeof1%to3%.Theminimumdetectionlimitsare2.27g/Land2.11g/Lrespectively,beinglowerthanthosebythenationalmethod.Therecoveriesoftotalnitrogenandphosphorusare97.2%to108%and100%to106%respectively.Themethodissuitabletoautomaticallyanalyzetotalnitrogenandphosphorusinwateratthesametime.Keywords:flowinjectionanalyzer;totalnitrogen;totalphosphorus;highpressuredigestion,[13],,,(,;;;[4];;[25]),[5]20087AA3/,,,,,,1111(110392522200911CHINAWATER&WASTEWATERVol.25No.22Nov.2009),:,,,N-(NEDD)(45),550nm:,,75,800nm112,,,[6]2211Bran+LuebbeAutoAnalyzer3Bran+Luebbe,XY(110)212AA3,,,,,,,,,,,[7]21321311,1000mg/L,(100mg/L)(10mg/L),21312:4,24h,,[12]:;,,,21313,550nm800nm,,,110,,,,,,(1),,,,1Tab.1Determinationparametersoftotalnitrogenandtotalphosphorus/(min-1)3.753.75/(min-1)330.810.81/%1010/%858500/110110/kPa8080/kPa50/45753311,121Fig.1Standardcurveoftotalnitrogen492522(n=4)Tab.2Experimentaldataofaccuracyandprecision(n=4)/(mgL-1)0.0500.5002.005.000.0200.0500.2000.500/(mgL-1)0.0490.0480.0460.0470.4970.5000.4960.5001.972.052.072.005.005.145.145.120.0200.0210.0200.0200.0480.0510.0490.0490.2020.2060.2000.1980.5060.4970.5060.506/(mgL-1)0.0480.4982.025.090.0200.0490.2020.504/%-4.0-0.41.01.91.2-1.50.80.8/%2.70.42.21.32.52.61.70.93134,,33Tab.3Recoveryofstandardaddition/(mgL-1)/(mgL-1)/(mgL-1)/%/(mgL-1)/(mgL-1)/(mgL-1)/%0.9262.002.8797.20.0480.2000.2481001.762.003.791010.0790.2000.2821020.4432.002.4399.20.0190.2000.21910024.310.035.11081.401.002.461063,/97.2%108%,100%106%314EPA,(MDL),,,MDL15,MDL:MDL=St(S,t,1-a=0.99n=7,t=3.143)Bran+Luebbe9g/L,2g/L,,050g/L20.0g/L10.0g/L,7,4,2.27g/L,,20;2.11g/L,,4Tab.4CalculationtableofMDLgL-1SMDL20.020.27,19.47,20.49,21.35,20.71,21.58,21.130.722.2710.010.71,10.50,9.94,10.56,11.25,11.90,10.130.672.11315/(G-394-08Rev.0),[(GB1189489)(GB1189389)],5,,59:/25225Tab.5Experimentalresultsofdifferentmethods/(mgL-1)/(mgL-1)/%/(mgL-1)/(mgL-1)/%0.500mg/L0.5080.4933.00.050mg/L0.0500.0484.21.211.182.50.0310.0297.52.032.15-5.60.0680.075-9.8()13.814.0-1.4()0.1600.1590.6()27.033.6-11.8()1.801.601210.9120.9060.710.0100.0100.021.041.05-1.020.0330.036-8.3316,,6,/6Tab.6Oxidationrateofonlinehighpressuredigestion/(mgL-1)/(mgL-1)/%/(mgL-1)/(mgL-1)/%2.002.001000.2000.2001002.001.9999.50.2000.2101052.002.111060.2000.19597.52.001.9899.00.2000.19095.02.002.021010.2000.2011003177,,7Tab.7ComparisonbetweencontinousflowanalyzerandGBstandards/mL0.5100.525200300mL200300mL,,,,,,,,4575,,,/30/h4h/30/h4h//(gL-1)50.02.2710.02.11692522[7](80kPa),,,,,,-,,,NaOH,NaClO,,,,,200h:[1]GB1189489,[S].[2]GB1189389,[S].[3].(4)[M].:,2002.[4],,.[J].,2007,23(22):82-84.[5],,.[J].,2008,(3):51-54.[6],,,.()[M].:,1997.[7],.[J].,2008,36(2):57-59.E-mail:[e-mail]:2009-06-08(92),,MC-RRMC-LRMC-YR94.0%94.9%95.8%,,MC-YR,MC-LR,MC-LR:[1],.[J].,2001,29(5):522-525.[2],.[J].,2008,10:87-88.[3]HideakiMurata,HirokoShoji,MotojiOshikata,etal.High2performanceliquidchromatographywithchemilumi2nescencedetectionofderivatizedmicrocystins[J].JChromatogrA,1995,693(2):263-270.[4],.RRLR[J].,2006,22(3):12-13.[5]IkawaM,PhillipsN,HaneyJF,etal.InterferencebyplasticsadditivesintheHPLCdeterminationofmicrocys2tin-LRand-YR[J].Toxicon,1999,37(6):923-929.[6],,,.[J].,2005,35(3):446-451.[7],,,.[J].,2007,31(4):604-605.[8],,,.[J].,2005,33(11):1578-1579.:[phone]E-mail:[e-mail]::2009-05-3179:/2522