GC Determination of Short-Chain Chlorinated Paraffin in Rubber Products
摘 要
提出了气相色谱法测定橡胶制品中短链氯化石蜡(C10~C13)含量的方法。样品经正己烷-丙酮(1+1)混合溶液超声提取,采用HP-5石英毛细管色谱柱(30 m×0.35 mm,0.25 μm)分离,电子捕获检测器检测。短链氯化石蜡的质量浓度在100 mg·L-1以内与其峰面积呈线性关系,测定下限为20 mg·kg-1。方法的回收率在92.4%~100.4%之间,相对标准偏差(n=6)在1.8%~4.5%之间。
Abstract
The contents of short-chain chlorinated paraffin (C10-C13) in rubber products were determined by GC with electron capture detector. The sample was extracted ultrasonically with a mixture of n-hexane and acetone (1+1) and separated on HP-5 quartz capillary column (30 m×0.35 mm, 0.25 μm). Linear relationship between values of peak area and mass concentration of short-chain chlorinated paraffin was obtained in the range within 100 mg·L-1, with lower limits of determination of 20 mg·kg-1. Values of recovery found were in range of 92.4%-100.4%, and values of RSD′s (n=6) found were in range of 1.8%-4.5%.
中图分类号 O657.7
所属栏目 工作简报
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收稿日期 2011/7/1
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备注袁丽凤(1978-),女,湖南资兴人,硕士,工程师,主要从事石油化工产品分析检测。
引用该论文: YUAN Li-feng,WU Bei-lei,LUO Chuan,XU Shan-hao,HUA Zheng-jiang,WANG Hao. GC Determination of Short-Chain Chlorinated Paraffin in Rubber Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(8): 920~922
袁丽凤,邬蓓蕾,罗川,徐善浩,华正江,王豪. 气相色谱法测定橡胶制品中短链氯化石蜡含量[J]. 理化检验-化学分册, 2012, 48(8): 920~922
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参考文献
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【2】COELHAN M. Determination of short-chain polychlorinated paraffins in fish samples by short-column GC/ECNI-MS[J]. Anal Chem, 1999,71(20):4498-4505.
【3】KOH I, ROTARD W, THIEMANN W H P. Analysis of chlorinated paraffins in cutting fluids and sealing materials by carbon skeleton reaction gas chromatography[J]. Chemosphere, 2002,47:219-227.
【4】CASTELLS P, SANTOS F J, GALCERAN M T. Evaluation of three ionisation modes for the analysis of chlorinated paraffins by gas chromatography/ion-trap mass spectrometry[J]. Rapid Commun Mass Spectrom, 2004,18:529-536.
【5】CASTELLS P, SANTOS F J, GALCERAN M T. Solid-phase extraction versus solid-phase micro-extraction for the determination of chlorinated paraffins in water using gas chromatography-negative chemical ionisation mass spectrometry[J]. J Chromatog A, 2004,1025:157-162.
【6】RETH M, ZENCAK Z, OEHME M. New quantification procedure for the analysis of chlorinated paraffins using electron capture negative ionization mass spectrometry[J]. J Chromatog A, 2005,1081:225-231.
【7】TEJNAROV P, COELHANB M, KOSTRHOU-NOVA R, et al. Analysis of short chain chlorinated paraffins in sedment sample from the Czech Republic by short-column GC/ECNI-MS[J]. Chemosphere, 2005,5:253-262.
【8】PARERA J. Micarowave-assisted extration versus Soxhlet extration for the analysis of short-chain chlorinated alkanes in sediment[J]. J Chromatog A, 2004,1046:19-26.
【9】马玲玲,徐殿斗,陈扬,等.短链氯化石蜡分析方法[J].化学进展, 2010,22(4):720-726.
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