摘要
采用气相色谱法测定了污水中苯胺、N,N-二甲基苯胺、邻甲苯胺、间甲苯胺和邻氯苯胺5种化合物的含量。采用气相色谱法-氢火焰离子化检测器(GC-FID),OV-17毛细管色谱柱(30 m×0.32 mm×0.5μm),对色谱条件、液液萃取的pH、盐用量等实验条件进行了优化,使得各组分得到完全分离。实验结果表明,5种苯胺类化合物在质量浓度0.5～50.0 mg/L内均与峰面积呈良好的线性关系,相关系数大于0.999;最佳液液萃取条件为:在水样中加入9 g NaCl,用1 mol/L NaOH溶液调节水样pH=11,采用二氯甲烷萃取3次。在最佳分析条件下,方法的检出限为0.056～0.093 mg/L,重复性实验的相对标准偏差为0.8%～4.5%,加标回收率为82%～103%(n=3)。该分析方法快速、准确,适合污水中苯胺类化合物的检测。
A method including liquid-liquid extraction and gas chromatography was developed for determination of aniline, N, N-dimethylaniline, o-toluidine, m-toluidine and o-chloroaniline in sewage water. The effects of chromatographic conditions, pH and salinity of the sewage water samples on the determination were investigated. Aniline and its substituted derivatives were completely separated on an OV-17 capillary column （30 m × 0.32 mm × 0.5 pμm） and determined by GC equipped with FID. The results indicated good linear correlations between the oeak areas and the mass concentrations of aniline and its substituted derivatives in the linearity range of 0.5-50.0 mg/L. All the correlation coefficients were more than 0.999. The optimal conditions for the liquid-liquid extraction were NaC1 dosage 9 g, adjusting sewage water sample pH with NaOH solution（1 mol/L） to 11 and extraction with dichloromethane for 3 times. Under the optimal determination conditions, the detection limits were in therange of 0.056-0.093 mg/L, RSD of the reproducibility was 0.8%-4.5%, and the recoveries were in the range of 82%-103%. It is showed that the method is rapid and accurate.
出处
《石油化工》
CAS
CSCD
北大核心
2012年第3期342-346,共5页
Petrochemical Technology
关键词
液液萃取
气相色谱法
污水
苯胺
N
N-二甲基苯胺
邻甲苯胺
间甲苯胺
邻氯苯胺
liquid-liquid extraction
gas chromatography
sewage water
aniline
N, N-dimethylaniline
o-toluidine
m-toluidine
o-chloroaniline
