摘要
按DD 2008-01规定采集浅层地下水样品并于4℃保温箱中保存。取水样1.000 0L置于分液漏斗中,依次加入氯化钠20.0g,1.0mg·L^(-1)替代物混合标准溶液100μL和正己烷-二氯甲烷(1+1)混合萃取液60mL,萃取10min,分层后,取有机相并保留,再用正己烷萃取2次,每次用30mL。合并3次萃取液,旋转蒸发至体积约为2～3mL,随即改用吹氮蒸发至约剩0.8mL,加入2.0mg·L^(-1)内标混合标准溶液100μL,用正己烷定容至1.0mL。用Rxi-5Sil MS毛细管色谱柱选择初始温度为65℃,按程序升温条件进行气相色谱分离;质谱分析采用电子轰击离子源,全扫描模式定性和选择离子模式定量。结果表明:36种多环芳烃及其衍生物的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)在1.3～8.8ng·L^(-1)之间。以空白水样为基体进行加标回收试验,回收率在71.1%～120%之间,测定值的相对标准偏差(n=5)在1.2%～9.7%之间。
Samples of shallow groundwater were collected and stored at 4 ℃in a refrigerator according to DD 2008-01.1.000 0 Lof the water sample was taken,and extracted for 10 min with 60 mL of a mixed extracting solvent of n-hexane and dichloromethane(1+1),after successive addition of 20.0 g of NaCl and 100μL of 1.0 mg·L^-1 standard solution of mixed substitutes.After the 2 phases were separated,the organic phase was separated and preserved,and the water phase was extracted twice further with 30 mL of n-hexane for each extraction.The 3 extracts were combined and evaporated under swirling until its volume was concentrated to 2-3 mL,the evaporation was continued by N2-blowing to concentrate the solution to a volume ca.0.8 mL.100μL of the2.0 mg·L^-1 mixed internal standard solution was added and the volume of the solution was made up to 1.0 mL with n-hexane.Rxi-5 Sil MS capillary chromatographic column was selected for GC separation,under temperature elevation program by choosing 65℃ as the initial temperature.In MS analysis,EI ionization source was used,and mode of full-scanning was adopted for qualification while the mode of SIM for quantification.As shown by the results,linear relationships between values of peak area and mass concentration of the 36 polycyclic aromatic hydrocarbons and their derivatives were found in definite ranges,with detection limits(3 S/N)in the range of 1.3-8.8 ng·L^-1.Test for recovery by standard addition method was made on the base of blank water sample,giving results in the range of 71.1%-120%,and RSDs(n=5)ranged from 1.2%to 9.7%.
作者
许丹丹
饶竹
梁汉东
XU Dandan;RAO Zhu;LIANG Handong(College of Geoseience and Surveying Engineering,China University of Mining and Technology (Beijing),Beijing 100083,China;State Key Laboratory of Coal Resources and Safe Mining,China University of Mining and Technology (Beijing),Beijing 100083,China;Key Laboratory of Ecological Geochemistry Sponsored by the Ministry of Land and Resources, National Geological Experimental Testing Center,Beijing 100037,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第1期31-38,共8页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
中国地质调查项目(DD20160312
DD20160323
1212011120283
12120123500016000902)
关键词
气相色谱-质谱法
多环芳烃及其衍生物
地下水
gas chromatography-mass spectrometry
polycyclic aromatic hydrocarbon and their derivative
groundwater
