固相萃取-气相色谱法测定水中四乙基铅含量
GC Determination of Tetraethyl Lead in Water with Solid Phase Extraction
摘 要
水样经Supelco C18固相萃取柱富集样品中四乙基铅,用正己烷淋洗,洗脱液于40 ℃水浴氮吹浓缩至0.5 mL,供气相色谱仪测定。用HP-5色谱柱分离,用电子捕获检测器测定。四乙基铅的峰面积与其质量浓度在0.05~5.0 μg·L-1范围内呈线性,方法检出限(3S/N)为0.02 μg·L-1。在3种不同浓度水平条件下对方法的回收率和精密度进行了试验,测得回收率在89.0%~92.4%之间,测定值的相对标准偏差(n=7)在3.5%~5.0%之间。
气相色谱法
四乙基铅
Solid phase extraction
GC
Tetraethyl lead
Abstract
Tetraethyl lead in water sample was enriched by passing through Supelco C18 SPE column, and was eluted from the column with n-hexane, and concentrated to 0.5 mL by N2-blowing in a water bath at 40 ℃, which was used for GC determination. HP-5 chromatographic column was used for separation and ECD was used in the determination. Linear relationship between values of peak area and mass concentration of tetraethyl lead was obtained in the range of 0.05-5.0 μg·L-1, with detection limit (3S/N) of 0.02 μg·L-1. Recovery and precision of the method were tested at 3 concentration levels, giving results of recovery in the range of 89.0%-92.4%, and RSD′s (n=7) in the range of 3.5%-5.0%.
中图分类号 O657.7
所属栏目 工作简报
基金项目
收稿日期 2011/11/9
修改稿日期
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备注曹志斌(1983-),男,江苏苏州人,硕士,主要从事水质检测工作。
引用该论文: CAO Zhi-bin,WANG Jin-yu,LU Wen-juan,GUO Zhi-yu,CHEN Ling-hu. GC Determination of Tetraethyl Lead in Water with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(12): 1421～1423
曹志斌,王晋宇,陆文娟,郭志宇,陈玲瑚. 固相萃取-气相色谱法测定水中四乙基铅含量[J]. 理化检验－化学分册, 2012, 48(12): 1421～1423
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参考文献
【1】ANDREOTTOLA G, DALLAGO I, FERRARESE E. Feasibility study for the remediation of groundwater contaminated by organolead compounds［J］. Hazardous materials, 2008,156:488-498.
【2】GB 3838-2002地表水环境质量标准［S］.
【3】GB/T 5750.6-2006生活饮用水标准检验方法 金属指标［S］.
【4】ANMESTER Z, LORD H, PAWLISZYN J. Speciation of trimethyllead and triethyllead by in-tube solid phase microextraction high-performance liquid chromatography electrospray ionization mass spectrometry［J］. Journal of Analytical Atomic Spectrometry, 2000,15:595-660.
【5】YU Xiao-mei, PAWLISZYN J. Speciation of alkyllead and inorganic lead by derivatization with deuterium-labeled sodium tetraethylborate and SPME-GC/MS［J］. Anal Chem, 2000,72(8):1788-1792.
【6】刘劲松,马荻荻,叶伟红,等.地表水中四乙基铅吹扫捕集-气相色谱/质谱分析方法研究及其应用［J］.中国环境监测, 2010,26(4):20-22.
【7】程滢,杨文武,张宗祥.石墨炉原子吸收光谱法测定水中四乙基铅［J］.环境监测管理与技术, 2009,21(2):40-41.
【8】李明,李爱荣,帅琴,等.双气路校正-固相微萃取电感耦合等离子体质谱法测定四乙基铅［J］.分析试验室, 2007,26(6):107-110.
【9】李世荣,吕鹂,娄涛,等.液液萃取-高效液相色谱法测定水中四乙基铅［J］.环境监测管理与技术, 2011,23(2):45-47.
【10】王晋宇,彭亮,陈玲瑚,等.液液萃取处理样品-毛细管气相色谱法测定水中四乙基铅［J］.理化检验-化学分册, 2011,47(7):972-973.
【11】江桂斌.环境样品前处理技术［M］.北京:化学工业出版社, 2004:67-69.
【2】GB 3838-2002地表水环境质量标准［S］.
【3】GB/T 5750.6-2006生活饮用水标准检验方法 金属指标［S］.
【4】ANMESTER Z, LORD H, PAWLISZYN J. Speciation of trimethyllead and triethyllead by in-tube solid phase microextraction high-performance liquid chromatography electrospray ionization mass spectrometry［J］. Journal of Analytical Atomic Spectrometry, 2000,15:595-660.
【5】YU Xiao-mei, PAWLISZYN J. Speciation of alkyllead and inorganic lead by derivatization with deuterium-labeled sodium tetraethylborate and SPME-GC/MS［J］. Anal Chem, 2000,72(8):1788-1792.
【6】刘劲松,马荻荻,叶伟红,等.地表水中四乙基铅吹扫捕集-气相色谱/质谱分析方法研究及其应用［J］.中国环境监测, 2010,26(4):20-22.
【7】程滢,杨文武,张宗祥.石墨炉原子吸收光谱法测定水中四乙基铅［J］.环境监测管理与技术, 2009,21(2):40-41.
【8】李明,李爱荣,帅琴,等.双气路校正-固相微萃取电感耦合等离子体质谱法测定四乙基铅［J］.分析试验室, 2007,26(6):107-110.
【9】李世荣,吕鹂,娄涛,等.液液萃取-高效液相色谱法测定水中四乙基铅［J］.环境监测管理与技术, 2011,23(2):45-47.
【10】王晋宇,彭亮,陈玲瑚,等.液液萃取处理样品-毛细管气相色谱法测定水中四乙基铅［J］.理化检验-化学分册, 2011,47(7):972-973.
【11】江桂斌.环境样品前处理技术［M］.北京:化学工业出版社, 2004:67-69.
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