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1、離子色譜-脈沖安培法測定卷煙主流煙氣中的硫化氫劉獻(xiàn)軍作者簡介:劉獻(xiàn)軍(1972-),男,碩士,工程師。研究方向:卷煙煙氣化學(xué)及煙氣分析,E-mail:njliuxianjun@sina.com。沈曉晨莊亞東張映(江蘇中煙工業(yè)有限責(zé)任公司技術(shù)研發(fā)中心,南京210010)摘要:提出了卷煙主流煙氣中硫化氫的離子交換色譜-脈沖安培測定方法。硫化氫經(jīng)100mmol/L氫氧化鈉、400mmol/L乙酸鈉、0.5%乙二胺、20mmol/L抗壞血酸組成的捕集液捕集后,使用100mmol/L氫氧化鈉、400mmol/L
2、乙酸鈉、0.5%乙二胺組成的淋洗液(流量為1.0mL/min)在IonPacAS7陰離子交換色譜柱(250mm×4mm)上分離,以銀電極、脈沖安培檢測器檢測。結(jié)果表明:硫離子檢出限(IDL)為1.52μg/L(t(α=0.01,n-1=7)=2.998),硫化氫檢出限(MDL)為20.14ng/支;平均加標(biāo)回收率在92.38%~96.38%之間,相對(duì)標(biāo)準(zhǔn)偏差在2.03%~3.26%之間。關(guān)鍵詞:硫化氫;陰離子交換色譜;脈沖安培檢測器;卷煙主流煙氣中圖分類號(hào):657.7文獻(xiàn)標(biāo)識(shí)碼:A文章編號(hào):Deter
3、minationofHydrogenSulfideinMain-streamSmokeofCigarettebyAnionExchangeChromatographywithPulsedAmperometricDetectorLIUXian-jun,SHENXiao-chen,ZHUANGYa-dongandZHANGYing(R&DCenter,ChinaTobaccoJiangsuIndustrialCo.,Ltd.,Nanjing210019,China)Abstract:Anovelmetho
4、dforthedeterminationofhydrogensulfide(H2S)inmain-streamsmokeofcigarettebyanionexchangechromatographywithpulsedamperometricdetector(AEC-PAD)wasdeveloped.ThetrappingconditionsofH2Sinmainstreamsmokewereinvestigated.Itwasfoundthattheabsorptionsolutioncompos
5、edof100mmol/LNaOH,400mmol/Lsodiumacetate,0.5%2-ethanediamineand20mmol/LascorbicacidcouldtrapH2Sinmain-streamsmokeinthewhole.S2-inabsorptionsolutionwasseparatedonananionexchangecolumnIonPacAS7(250mm×4mm),withtheuseofamobilephasecomposedof100mmol/LNaOHand
6、400mmol/Lsodiumacetateand0.5%2-ethanediamineataflowrateof1.0mL/minandwasdetectedbypulsedamperometricdetectorwithAg/AgClelectrode.Undertheaboveoptimalconditions,thecalibrationcurvewaslinearintheconcentrationrangeof0.1mg/L~5.0mg/LS2-withacorrelationcoeffi
7、cientof0.99950.ThespikedrecoveriesofS2-wereintherangeof92.38%~96.38%withrelativestandarddeviations(RSDs)of2.03%~3.26%.Instrumentdetectionlimit(IDL)ofS2-was1.52μg/L(EPA,t(α=0.01,n-1=7)=2.998).Methoddetectionlimit(MDL)ofH2Sinmain-streamsmokeofcigarettewas
8、20.14ng/cig..Themethodwassimple,rapidandaccurate,andcouldbeappliedforthedeterminationofH2Sinmain-streamsmokeofcigarette.Keywords:H2S;anionexchangechromatography;pulsedamperometricdetector;main-streamsmokeofcigarette煙草中有含硫蛋白質(zhì)及含硫氨基