工作场所空气中11种烃类有机物的气相色谱同时测定法
|
摘要
目的建立溶剂解吸毛细管气相色谱法同时测定工作场所空气中11种烷烃和卤代烃的测定方法。方法样品经活性炭管采集后,二硫化碳溶剂解吸,经毛细管色谱柱HP-INNOWAX分离,氢火焰离子化检测器检测,保留时间定性,外标法定量。结果 11种烃类化合物线性关系良好,相关系数均大于0.999 0,检出限和定量下限分别为0.14～2.42 mg/L和0.47～8.06mg/L,最低检出浓度和最低定量浓度分别为0.02～8.06 mg/m3和0.08～1.34 mg/m3 (以采集6.0 L空气计);平均解吸效率为85.94%～95.85%,批内、批间精密度分别为0.04%～7.08%和0.09%～8.04%,样品在常温下至少可保存14天。结论该方法准确度高,灵敏快速,检出限低,适合于工作场所空气中11种烃类化合物的同时测定。
[Objective] To establish a method for simultaneous determination of 11 kinds of alkanes and halogenated hydrocarbons in workplace air by solvent desorption-gas chromatography. [Methods] The samples were enriched by activated charcoal tub, and then desorbed with carbon disulfide. The target compounds were separated by HP-INNOWAX capillary column and detected by hydrogen flame ionization detector, qualitatived by retention time and qualified by the matrix-matched external standard method.[Results]Good linearity of the 11 kinds of hydrocarbon compounds was found, and the correlation coefficients were above 0.999 0. The limit of detection and the limit of quantification were 0.14-2.42 mg/L and 0.47-8.06 mg/L respectively.The minimum detectable concentration and the minimum quantification concentration were 0.02-8.06 mg/m3 and 0.08-1.34 mg/m3 respectively(sample volume of 6.0 L). The average desorption efficiency was 85.94%-95.85%. The within-run and between-run precisions were 0.04%-7.08% and 0.09%-8.04%, respectively. The samples could be kept at least 14 days under normal temperature.[Conclusion]This method is highly efficient, accurate and sensitive, with low detection limit. It is suitable for the simultaneous determination of 11 kinds of hydrocarbon organic compounds in workplace air.
[Objective] To establish a method for simultaneous determination of 11 kinds of alkanes and halogenated hydrocarbons in workplace air by solvent desorption-gas chromatography. [Methods] The samples were enriched by activated charcoal tub, and then desorbed with carbon disulfide. The target compounds were separated by HP-INNOWAX capillary column and detected by hydrogen flame ionization detector, qualitatived by retention time and qualified by the matrix-matched external standard method.[Results]Good linearity of the 11 kinds of hydrocarbon compounds was found, and the correlation coefficients were above 0.999 0. The limit of detection and the limit of quantification were 0.14-2.42 mg/L and 0.47-8.06 mg/L respectively.The minimum detectable concentration and the minimum quantification concentration were 0.02-8.06 mg/m3 and 0.08-1.34 mg/m3 respectively(sample volume of 6.0 L). The average desorption efficiency was 85.94%-95.85%. The within-run and between-run precisions were 0.04%-7.08% and 0.09%-8.04%, respectively. The samples could be kept at least 14 days under normal temperature.[Conclusion]This method is highly efficient, accurate and sensitive, with low detection limit. It is suitable for the simultaneous determination of 11 kinds of hydrocarbon organic compounds in workplace air.
引文
[1]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定戊烷、己烷、庚烷、辛烷和壬烷GBZ/T 300.60-2017[S/OL].(2017-11-09)[2018-11-19].http:/www.nhc.gov.cn/zhuz/pyl/20 1712/24d 7917eb51744928ea3cf68b6b1229e.shtml.
[2]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯甲烷、二氯甲烷、三氯甲烷和四氯化碳:GBZ/T 300.73-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/201712/adbb626c7b8e4737a364a4e14ab30e69.shtml.
[3]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯乙烯、二氯乙烯、三氯乙烯和四氯乙烯:GBZ/T 300.78-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/2017 12/dd3c5396b56d49e3bb3b30ffd8041bc9.shtml.
[4]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯丙烯和二氯丙烯GBZ/T 300.80-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/201712/76059140e6734635812838a6602a6755.shtml.
[5]周雯,房超.气相色谱-质谱法测定工作场所空气中的5种卤代烃[J].化学分析计量,2016,25(5):64-67.
[6]余秀娟,那晶晶,曾钰.气相色谱法同时测定空气中五种烷烃类化合物[J].环保科技,2014,20(5):43-46.
[7]张倩,张吉喆.气相色谱法测定室内空气中挥发性卤代烃[J].中国环境管理干部学院学报,2014,24(5):62-64.
[8]梁素丹,陈剑刚.工作场所空气中六种卤代烃类化合物的气相色谱同时测定方法[J].实用预防医学,2013,20(8):1009-1011.
[9]湛社霞,刘钢,王翠桦,等.工作场所空气中13种卤代烃的溶剂解析气相色谱同时测定法[J].职业与健康,2012,28(8):925-927.
[10]湛社霞,臧李纳,孙世宏,等.毛细管气相色谱法测定工作场所空气中8种卤代烃[J].中国卫生检验杂志,2011,21(1):65-67.
[11]蒋凯,丁卯,薛晓康.溶剂解吸气相色谱法测定空气中21种挥发性卤代烃的方法改进[J].化学试剂,2018,40(6):551-554.
[12]王敏,陈振龙.气相色谱法同时测定工作场所空气中的11种卤代烃类化合物[J].现代预防医学,2018,44(18):3297-3300,3308.
[13]赵玉妍,陈伟光.工作场所空气中烷烃类及脂环烃类化合物的气相色谱测定法[J].环境与健康杂志,2015,32(6):516.
[14]季萍,王锡宁,焦燕妮.气相色谱法测定工作场所空气中3种烷烃类化合物[J].中国卫生检验杂志,2012,22(7):1548-1549.
[15]詹铭,奚晔,徐竞良,等.工作场所空气中4种硝基烷烃类化合物的气相色谱测定法[J].环境与健康杂志,2008,25(5):435-437.
[16]中华人民共和国卫生部.工作场所空气中有害物质监测的采样规范:GBZ 159-2004[S].北京:人民卫生出版社,2004:6-8.
[17]中华人民共和国卫生部.职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法:GBZ/T 210.4-2008[S].北京:人民卫生出版社,2008:3-4.
[2]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯甲烷、二氯甲烷、三氯甲烷和四氯化碳:GBZ/T 300.73-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/201712/adbb626c7b8e4737a364a4e14ab30e69.shtml.
[3]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯乙烯、二氯乙烯、三氯乙烯和四氯乙烯:GBZ/T 300.78-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/2017 12/dd3c5396b56d49e3bb3b30ffd8041bc9.shtml.
[4]中华人民共和国卫生与计划生育委员会.工作场所空气有毒物质测定氯丙烯和二氯丙烯GBZ/T 300.80-2017[S/OL].(2017-11-09)[2018-11-19].http://www.nhc.gov.cn/zhuz/pyl/201712/76059140e6734635812838a6602a6755.shtml.
[5]周雯,房超.气相色谱-质谱法测定工作场所空气中的5种卤代烃[J].化学分析计量,2016,25(5):64-67.
[6]余秀娟,那晶晶,曾钰.气相色谱法同时测定空气中五种烷烃类化合物[J].环保科技,2014,20(5):43-46.
[7]张倩,张吉喆.气相色谱法测定室内空气中挥发性卤代烃[J].中国环境管理干部学院学报,2014,24(5):62-64.
[8]梁素丹,陈剑刚.工作场所空气中六种卤代烃类化合物的气相色谱同时测定方法[J].实用预防医学,2013,20(8):1009-1011.
[9]湛社霞,刘钢,王翠桦,等.工作场所空气中13种卤代烃的溶剂解析气相色谱同时测定法[J].职业与健康,2012,28(8):925-927.
[10]湛社霞,臧李纳,孙世宏,等.毛细管气相色谱法测定工作场所空气中8种卤代烃[J].中国卫生检验杂志,2011,21(1):65-67.
[11]蒋凯,丁卯,薛晓康.溶剂解吸气相色谱法测定空气中21种挥发性卤代烃的方法改进[J].化学试剂,2018,40(6):551-554.
[12]王敏,陈振龙.气相色谱法同时测定工作场所空气中的11种卤代烃类化合物[J].现代预防医学,2018,44(18):3297-3300,3308.
[13]赵玉妍,陈伟光.工作场所空气中烷烃类及脂环烃类化合物的气相色谱测定法[J].环境与健康杂志,2015,32(6):516.
[14]季萍,王锡宁,焦燕妮.气相色谱法测定工作场所空气中3种烷烃类化合物[J].中国卫生检验杂志,2012,22(7):1548-1549.
[15]詹铭,奚晔,徐竞良,等.工作场所空气中4种硝基烷烃类化合物的气相色谱测定法[J].环境与健康杂志,2008,25(5):435-437.
[16]中华人民共和国卫生部.工作场所空气中有害物质监测的采样规范:GBZ 159-2004[S].北京:人民卫生出版社,2004:6-8.
[17]中华人民共和国卫生部.职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法:GBZ/T 210.4-2008[S].北京:人民卫生出版社,2008:3-4.