固相萃取-气相色谱法测定水中硝基氯苯类化合物
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摘要
建立固相萃取-气相色谱法测定水中15种硝基氯苯类化合物的方法。选用HLB柱为固相萃取柱,选用环己烷∶丙酮(3∶1,V∶V)混合溶剂作洗脱剂,得到方法检出限为0.011～0.040μg/L。空白水样加标回收率为73.6%～119%,相对标准偏差为6.1%～13.9%,精密度和准确度良好。对成分不复杂的实际水样进行测定,加标回收率为64.1%～118%,相对标准偏差为5.8%～15.6%,该方法能够基本满足成分不复杂的环境水体中痕量硝基氯苯类化合物的测定。
A method was developed for the determination of fifteen kinds of nitrochlorobenzenes in water by gas chromatography with solid-phase extraction.The optimal conditions were discussed in this research,the HLB column was selected as a solid phase extraction column,and a mixed solvent of cyclohexane:acetone(3∶1,V∶V) was used for elution.The detection limits ranged from 0.011 μg/L to 0.040 μg/L.The recoveries of spiked reagent water were 73.6%～119%,and the relative standard deviations were6.1%～13.9%.The recoveries of the spiked actual water sample were 64.1%～118%,and the relative standard deviations were 5.8%～15.6%.The present method meets the requirement of determination of nitrochlorobenzenes in water samples with simple matrix.
A method was developed for the determination of fifteen kinds of nitrochlorobenzenes in water by gas chromatography with solid-phase extraction.The optimal conditions were discussed in this research,the HLB column was selected as a solid phase extraction column,and a mixed solvent of cyclohexane:acetone(3∶1,V∶V) was used for elution.The detection limits ranged from 0.011 μg/L to 0.040 μg/L.The recoveries of spiked reagent water were 73.6%～119%,and the relative standard deviations were6.1%～13.9%.The recoveries of the spiked actual water sample were 64.1%～118%,and the relative standard deviations were 5.8%～15.6%.The present method meets the requirement of determination of nitrochlorobenzenes in water samples with simple matrix.
引文
[1]国家环境保护局有毒化学品管理办公室.化学品毒性法规环境数据手册[M].北京:中国环境科学出版社,1992.
[2]邓权.液液萃取–气相色谱法测定地表水中硝基氯苯[J].化学分析计量,2018,27(1):47-50.
[3]李宪,张凤林,唐维.职业性急性对硝基氯苯中毒特点及诊断分级探讨[J].中国工业医学杂志,2016,29(1):44-46,73.
[4]彭华,李贝,王琪,等.液液萃取-气相色谱法测定水中硝基氯苯类化合物[J].环境监控与预警,2017,9(2):19-22.
[5]赵悠悠,赵临强.土壤中对硝基氯苯的检测[J].山西农业科学,2014,42(3):268-271.
[6]周文敏,傅德黔,孙宗光.水中优先控制污染物黑名单[J].中国环境监测,1990,6(4):1-3.
[7]孙海红,钱叶苗,宋相丽,等.固相萃取技术的应用与研究新进展[J].现代化工,2011(S2):21-24,26.
[8]沈斐,苏晓燕,李睿,等.固相萃取-气相色谱法测定水环境中邻苯二甲酸酯[J].中国环境监测,2014(1):150-153.
[9]李利荣,魏恩棋,王艳丽,等.固相萃取气相色谱法测定水中15种硝基苯类化合物[J].环境监测管理与技术,2012(3):60-63,68.
[10]张蓓蓓,章勇,赵永刚. SPE-GC-ECD法测定水体中五种硝基苯类化合物[J].环境监控与预警,2010(2):18-20.
[11]张欢燕,吴诗剑,刘鸣,等. GC-ECD测定地表水中的硝基苯类和氯苯类化合物[J].环境科学与技术,2013,36(1):84-88.
[2]邓权.液液萃取–气相色谱法测定地表水中硝基氯苯[J].化学分析计量,2018,27(1):47-50.
[3]李宪,张凤林,唐维.职业性急性对硝基氯苯中毒特点及诊断分级探讨[J].中国工业医学杂志,2016,29(1):44-46,73.
[4]彭华,李贝,王琪,等.液液萃取-气相色谱法测定水中硝基氯苯类化合物[J].环境监控与预警,2017,9(2):19-22.
[5]赵悠悠,赵临强.土壤中对硝基氯苯的检测[J].山西农业科学,2014,42(3):268-271.
[6]周文敏,傅德黔,孙宗光.水中优先控制污染物黑名单[J].中国环境监测,1990,6(4):1-3.
[7]孙海红,钱叶苗,宋相丽,等.固相萃取技术的应用与研究新进展[J].现代化工,2011(S2):21-24,26.
[8]沈斐,苏晓燕,李睿,等.固相萃取-气相色谱法测定水环境中邻苯二甲酸酯[J].中国环境监测,2014(1):150-153.
[9]李利荣,魏恩棋,王艳丽,等.固相萃取气相色谱法测定水中15种硝基苯类化合物[J].环境监测管理与技术,2012(3):60-63,68.
[10]张蓓蓓,章勇,赵永刚. SPE-GC-ECD法测定水体中五种硝基苯类化合物[J].环境监控与预警,2010(2):18-20.
[11]张欢燕,吴诗剑,刘鸣,等. GC-ECD测定地表水中的硝基苯类和氯苯类化合物[J].环境科学与技术,2013,36(1):84-88.