GC-MS Determination of Aroclors in Soil with Rapid Solvent Extraction
摘 要
采用气相色谱-质谱法在选择离子方式下测定土壤中多氯联苯Aroclor系列Aroclor 1016、Aroclor 1221、Aroclor 1232、Aroclor 1242、Aroclor 1248、Aroclor 1254、Aroclor 1260.样品经正己烷-丙酮(体积比1比1)混合溶剂进行快速溶剂萃取仪提取后,经浓硫酸液-液分配,再经氟罗里硅土柱净化浓缩,洗脱液浓缩并定容至1 mL后,供气相色谱-质谱仪测定,外标法定量.回收率在76%~108%之间,相对标准偏差(n=7)小于13%.应用提出的方法分析了一个土壤标样物质,测定结果(2.19 mg·kg-1)与证书值(2.14 mg·kg-1)之间的相对误差为2.3%.以土壤样品为基体,加入十氯联苯替代物的标准溶液做回收试验,测得回收率在70%~120%之间.
Abstract
7 Aroclors,namely Aroclor 1016,Aroclor 1221,Aroclor 1232,Aroclor 1242,Aroclor 1248,Aroclor 1254 and Aroclor 1260,in soil were determined by GC-MS under selective ion monitoring mode.The sample was extracted with n-hexane and acetone mixed in the ratio of 1 to 1 by rapid solvent extractor,and then partitioned with conc.H2SO4.The extract was purified by passing through florisil column.The eluate was concentrated and made up to 1 mL,which was used for GC-MS determination,with external standard method.Values of recovery were found in the range of 76%-108% with RSD′s (n=7) less than 13%.In application of the proposed method to the analysis of a CRM of soil,the relative error between the result obtained (2.19 mg·kg-1) and the certified value (2.14 mg·kg-1) was found to be 2.3%.Tests for recovery and precision were made by addition of standard solution of the substitute decachlorobiphenyl to a soil sample as matrix which was then analyzed by the proposed method.Values of recovery obtained were in the range of 70%-120%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2008/11/25
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备注俞是聃(1967-),女,福建福清人,高级工程师,研究方向为仪器分析(有机物及重金属).
引用该论文: YU Shi-dan. GC-MS Determination of Aroclors in Soil with Rapid Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(3): 288~292
俞是聃. 快速溶剂萃取-气相色谱-质谱联用法测定土壤中多氯联苯Aroclor系列[J]. 理化检验-化学分册, 2009, 45(3): 288~292
被引情况:
【1】唐磊,应剑波, "快速溶剂萃取-气相色谱-串联质谱法测定血中巴比妥类药物",理化检验-化学分册 48, 845-847(2012)
【2】范磊,黄素华,田霆,何日安,周华俏,黄可尊, "气相色谱-串联质谱法测定水中多氯联苯",理化检验-化学分册 49, 1479-1482(2013)
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【2】国家环境保护总局.水和废水监测分析方法[M].北京:中国环境科学出版社,2006:638.
【3】国家环境保护总局.水和废水监测分析方法[M].北京:中国环境科学出版社,2006:29.
【4】EPA method 8082: Analysis and testing of PCB congeners and aroclors[S].
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