Pre-column Derivatization-GC Determination of Trace Amounts of Phenol in Water After Separation by Micro-wave Heated Extraction
摘 要
含痕量苯酚的水样与丙酮和环己烷(1+1)的混合溶剂混合,置于控温在60 ℃的微波炉中加热30 s,使苯酚萃取进入有机相,分取部分萃取液在pH 8~9的条件下与衍生试剂乙酸酐反应15 min,所生成的苯酚衍生物用石油醚萃取,分取部分经脱水后的有机相进样作气相色谱分析.色谱测定中采用DB-17毛细管色谱柱(30 m×0.53 mm,1.0 μm)及氢火焰离子化检测器,在优化的条件下测得方法的检出限(3S/N)为0.01 mg·L-1.按所提出方法分析了8个模拟水样,根据测得苯酚的含量值算得其相对标准偏差为4.2%,并按标准加入法求得其平均回收率为94.0%.
Abstract
Water sample containing phenol was extracted with mixed solvent of acetone and cyclohexane(1+1),heated at 60 ℃ in a microwave oven for 30 s.An aliquot of the extract was reacted with the derivatizing reagent,acetic anhydride for 15 min at pH 8~9.The derivatized product of phenol was then extracted with petroleum ether.An aliquot of the organic phase,after dehydration,was used for GC determination.DB-17 capillary chromatographic column (30 m×0.53 mm,1.0 μm) and hydogen flame ionization detector were used in the gas chromatography.Detection limit (3S/N) found under the optimum condition was 0.01 mg·L-1.Precision and recovery were tested by analyzing 8 simulated water samples with addition of standard phenol,giving values of RSD′s and average recovery of 4.2% and 94.0% respectively.
中图分类号 O657.7
所属栏目 工作简报
基金项目 湖南省科技厅项目(2007FJ4156)
收稿日期 2008/8/2
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备注谭晓燕(1974-),女,湖南郴州人,讲师,博士研究生,主要研究方向为精细有机中间体的合成.
引用该论文: TAN Xiao-yan,LI Guo-lan,LI Song,ZHAO Ying,WANG Juan. Pre-column Derivatization-GC Determination of Trace Amounts of Phenol in Water After Separation by Micro-wave Heated Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(1): 32~34
谭晓燕,黎国兰,李松,赵莹,王娟. 微波萃取-柱前衍生-气相色谱法测定水中痕量苯酚[J]. 理化检验-化学分册, 2009, 45(1): 32~34
被引情况:
【1】张伟亚,李红丽,刘丽华,徐烨,韩彦龙, "分散液相微萃取-高效液相色谱法同时测定尿样中2,5-己二酮、苯酚及邻甲酚",理化检验-化学分册 51, 1274-1277(2015)
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参考文献
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【2】Serban C Moldoveanu,Melissa Kiser.Gas chromatography/mass spectrometry versus liquid chromatography/ fluorescence detection in the analysis of phenols in mainstream cigarette smoke[J].J Chromatography A,2007,1141(1/2):90-97.
【3】Wennrich L,Efer J,Engewald W.Programmed temperature vaporisers-based large volume ingection in capillary gas chromatography[J].J Chromatographia A,1999,842:143-161.
【4】EPA Method 604-Phenols:Methods for Organic Chemical Analysis of Municipal and Industrial Wastewater[S].
【5】Goren Bengttsson.A gas chromatographic micromethod for Trace determination of phenols[J].J Chromatograph Science,1985,23(9):397-401.
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