直接进样-气相色谱法测定废水中5种含氮化合物
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摘要
采用直接进样-气相色谱法测定废水中丙烯腈、乙腈、吡啶、N,N-二甲基甲酰胺和N,N-二甲基乙酰胺等5种含氮化合物的含量。5种含氮化合物用DB-FFAP色谱柱(30 m×0.53mm,1.5μm)分离,氮磷检测器检测。5种含氮化合物的质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限为0.004～0.005mg·L~(-1)。以空白样品为基体进行加标回收试验,所得回收率为92.9%～110%,回收量的相对标准偏差(n=7)为1.0%～6.2%。
GC was applied to the determination of 5 nitrogenous compounds,i.e.acrylonitrile,acetonitrile,pyridine,N,N-dimethylformamide and N,N-dimethylacetamide in wastewater with direct injection.The 5 nitrogenous compounds were separated on DB-FFAP chromatographic column(30 m×0.53 mm,1.5μm) and detected by NPD.Linear relationships between values of peak area and mass concentration of the 5 nitrogenous compounds were kept in definite ranges,with detection limits in the range of 0.004-0.005 mg·L~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 92.9%-110%,with RSDs(n=7) of recovery amounts in the range of 1.0%-6.2%.
GC was applied to the determination of 5 nitrogenous compounds,i.e.acrylonitrile,acetonitrile,pyridine,N,N-dimethylformamide and N,N-dimethylacetamide in wastewater with direct injection.The 5 nitrogenous compounds were separated on DB-FFAP chromatographic column(30 m×0.53 mm,1.5μm) and detected by NPD.Linear relationships between values of peak area and mass concentration of the 5 nitrogenous compounds were kept in definite ranges,with detection limits in the range of 0.004-0.005 mg·L~(-1).On the base of blank sample,test for recovery was made by standard addition method;values of recovery found were in the range of 92.9%-110%,with RSDs(n=7) of recovery amounts in the range of 1.0%-6.2%.
引文
[1]王箴.化工辞典[M].4版.北京:化学工业出版社,2000.
[2]江泉观,纪云晶,常元勋.环境化学毒物防治手册[M].北京:化学工业出版社,2004.
[3]唐访良,许皖菁,冯宁.气相色谱法测定环境空气中的微量丙烯腈[J].色谱,2000,18(5):473-474.
[4] GB/T 5750.8-2006生活饮用水标准检验方法有机物指标[S].
[5] HJ 788-2016水质乙腈的测定吹扫捕集/气相色谱法[S].
[6] HJ 789-2016水质乙腈的测定直接进样/气相色谱法[S].
[7] GB/T 14672-1993水质吡啶的测定气相色谱法[S].
[8] GBZ/T 160.62-2004工作场所空气中有毒物质测定酰胺类化合物[S].
[9]陈小辉,黄剑明,徐廷国,等.顶空进样-大口径毛细柱-NPD气相色谱法测定水中吡啶[J].工业水处理,2006,26(1):61-62.
[10]唐访良,朱文.气相色谱法测定水和废水中N,N-二甲基甲酰胺和N,N-二甲基乙酰胺[J].理化检验-化学分册,2006,42(11):941-942.
[11]梁坚.顶空-气相色谱法测定水中苯系物、乙腈和丙烯腈[J].理化检验-化学分册,2010,46(4):393-395.
[12]李海燕.顶空-毛细管气相色谱法同步测定水中吡啶丙酮乙腈[J].中国环境监测,2011,27(2):56-58.
[13]赖永忠.顶空进样-固相微萃取测定饮用水源水中吡啶[J].岩矿测试,2011,30(5):596-600.
[14]陆文娟,王晋宇,陈玲瑚,等.吹扫捕集-气相色谱法测定水中乙醛、丙烯醛、丙烯腈[J].理化检验-化学分册,2011,47(10):1214-1215.
[15]张明,唐访良,范晓开,等.固相萃取-亲水相互作用液相色谱法同时测定环境水样中3种酰胺类化合物[J].分析化学,2012,40(10):1555-1560.
[16]孙睿华.动态顶空气相色谱法测定水中极性水溶性有机物[J].环境监测管理与技术,2014,26(5):43-45.
[17]张明,唐访良,徐建芬,等.N,N-二甲基甲酰胺及其降解产物分析方法研究进展[J].化学分析计量,2014,23(3):102-104.
[18]徐建芬,唐访良,张明,等.气相色谱法测定水中4种酰胺类化合物含量[J].理化检验-化学分册,2015,51(8):1191-1193.
[19]郑锦辉,李津津.顶空气相色谱法测定水中乙醛、丙烯醛、丙烯腈和吡啶[J].贵州师范大学学报(自然科学版),2016,34(3):85-88.
[20]陆国永,吴悦,赖永忠.顶空固相微萃取法同时分析源水中5种极性挥发性有机物[J].中国给水排水,2017,33(12):123-129.
[21] HJ 168-2010环境监测分析方法标准制订技术导则[S].
[2]江泉观,纪云晶,常元勋.环境化学毒物防治手册[M].北京:化学工业出版社,2004.
[3]唐访良,许皖菁,冯宁.气相色谱法测定环境空气中的微量丙烯腈[J].色谱,2000,18(5):473-474.
[4] GB/T 5750.8-2006生活饮用水标准检验方法有机物指标[S].
[5] HJ 788-2016水质乙腈的测定吹扫捕集/气相色谱法[S].
[6] HJ 789-2016水质乙腈的测定直接进样/气相色谱法[S].
[7] GB/T 14672-1993水质吡啶的测定气相色谱法[S].
[8] GBZ/T 160.62-2004工作场所空气中有毒物质测定酰胺类化合物[S].
[9]陈小辉,黄剑明,徐廷国,等.顶空进样-大口径毛细柱-NPD气相色谱法测定水中吡啶[J].工业水处理,2006,26(1):61-62.
[10]唐访良,朱文.气相色谱法测定水和废水中N,N-二甲基甲酰胺和N,N-二甲基乙酰胺[J].理化检验-化学分册,2006,42(11):941-942.
[11]梁坚.顶空-气相色谱法测定水中苯系物、乙腈和丙烯腈[J].理化检验-化学分册,2010,46(4):393-395.
[12]李海燕.顶空-毛细管气相色谱法同步测定水中吡啶丙酮乙腈[J].中国环境监测,2011,27(2):56-58.
[13]赖永忠.顶空进样-固相微萃取测定饮用水源水中吡啶[J].岩矿测试,2011,30(5):596-600.
[14]陆文娟,王晋宇,陈玲瑚,等.吹扫捕集-气相色谱法测定水中乙醛、丙烯醛、丙烯腈[J].理化检验-化学分册,2011,47(10):1214-1215.
[15]张明,唐访良,范晓开,等.固相萃取-亲水相互作用液相色谱法同时测定环境水样中3种酰胺类化合物[J].分析化学,2012,40(10):1555-1560.
[16]孙睿华.动态顶空气相色谱法测定水中极性水溶性有机物[J].环境监测管理与技术,2014,26(5):43-45.
[17]张明,唐访良,徐建芬,等.N,N-二甲基甲酰胺及其降解产物分析方法研究进展[J].化学分析计量,2014,23(3):102-104.
[18]徐建芬,唐访良,张明,等.气相色谱法测定水中4种酰胺类化合物含量[J].理化检验-化学分册,2015,51(8):1191-1193.
[19]郑锦辉,李津津.顶空气相色谱法测定水中乙醛、丙烯醛、丙烯腈和吡啶[J].贵州师范大学学报(自然科学版),2016,34(3):85-88.
[20]陆国永,吴悦,赖永忠.顶空固相微萃取法同时分析源水中5种极性挥发性有机物[J].中国给水排水,2017,33(12):123-129.
[21] HJ 168-2010环境监测分析方法标准制订技术导则[S].