GC Determination of Total PCBs in Water with Automatic Solid Phase Extraction
摘 要
应用全自动固相萃取-气相色谱法测定水中多氯联苯6个Aroclor系列的总量。以特征“指纹峰”为定性依据,用外标法定量。优化的固相萃取条件为:① 固相萃取柱为Bond Elut C18柱;② 水样体积1.0 L;③ 水样流量10 mL·min-1;④ 洗脱剂为15 mL二氯甲烷和15 mL乙酸乙酯。用DB-5MS柱分离,电子捕获检测器检测。各多氯联苯的线性范围均为7.0~140.0 μg·L-1,检出限均为0.7 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率在70.1%~90.0%之间,测定值的相对标准偏差(n=6)在4.3%~6.6%之间。
Abstract
GC was applied to the determination of total PCBs in water with automatic solid phase extraction. Characterized “fingerprint peaks” were used for qualitative anaylsis while the external standard was used for quantitative analysis. The optimized conditions of solid phase extraction found were as follows: ① column of solid phase extraction: Bond Elut C18 column; ② volume of water sample: 1.0 L; ③ flow of water sample: 10 mL·min-1; ④ elution solvents: 15 mL methylene chloride and 15 mL of ethyl acetate. The analytes were separated on DB-5MS column and detected by ECD. Linearity ranges of PCBs were found same between 7.0 μg·L-1 and 140.0 μg·L-1 with detection limits of 0.7 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 70.1%-90.0%, with RSD′s (n=6) in the range of 4.3%-6.6%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2013/8/31
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联系人作者何娟(jstzhqhj@163.com)
备注何娟(1983-),女,江苏泰州人,工程师,硕士,主要从事环境监测有机化学分析与研究工作。
引用该论文: HE Juan,ZHANG Zong-xiang,YANG Wen-wu,DING Jin-mei. GC Determination of Total PCBs in Water with Automatic Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(9): 1135~1138
何娟,张宗祥,杨文武,丁金美. 全自动固相萃取-气相色谱法测定水中多氯联苯总量[J]. 理化检验-化学分册, 2014, 50(9): 1135~1138
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【8】王玲玲,申剑.固相萃取/GC-MS法测定水中半挥发性有机物[J].现代科学仪器, 2003(3):53-55.
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