超声辅助-乳化液液微萃取-气相色谱法测定水体中7种苯系物  

Ultrasound assisted-emulsification liquid liquid microextraction-gas chromatography for determination of seven kinds of benzene series in water samples

作　　者：蓝路梅[1] 朱霞萍[1] 宋坤红 LAN Lumei;ZHU Xiaping;SONG Kunhong(College of Materials and Chemistry 驭Chemical Engineering,Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions,Chengdu University of Technology,Chengdu 610059,China)

机构地区：[1]成都理工大学材料与化学化工学院矿产资源化学四川省高校重点实验室,四川成都610059

出　　处：《中国测试》2017年第2期50-54,共5页China Measurement & Test

基　　金：四川省科技厅科技支撑项目(2015GZ0243);四川省教育厅重点项目(15ZA0071)

摘　　要：采用正己烷为萃取剂,乙腈为乳化剂,建立超声辅助-乳化液液微萃取-气相色谱法(USA-ELLME-GC)检测水中甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯、1,3,5-三甲苯,1,2,4-三甲苯的分析方法。当萃取剂正己烷为150μL,乳化剂乙腈为400μL,超声时间为12 min时,50 m L水溶液中苯系物被成功萃取到正己烷中,富集倍数达到333倍。色谱条件为:DB-5MS(30 m×0.25 mm,0.25μm)毛细管柱,进样口温度220℃,检测器(FID)温度250℃,程序升温(初始45℃保持3 min,3°C/min升温至70℃,再以30℃/min升至200℃保持2 min),氢气流量10m L/min,尾吹气流量30 m L/min,分流比30∶1。在优化的萃取和色谱条件下,7种苯系物在0.08~1.00 mg/L浓度范围内与峰面积呈线性关系,相关系数均>0.9980,方法检出限为0.005~0.01 mg/L,质量浓度均为0.10 mg/L的苯系物的7次前处理及测定结果相对标准偏差RSD为1.5%~4.7%。建立的方法应用于学校内湖水和实验室废水中7种苯系物的测定,平均回收率为86.5%~110.4%,测定结果满足分析化学痕量分析要求。A new method was developed for determination of toluene,ethylbenzene,xylene,m- xylene, o-xylene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene in water samples by GC-FID coupled with ultrasound assisted-emulsification liquid liquid microextraction (USA-ELLME). When the volume of sample was 50 mL, a good extraction efficiency was obtained by using 150 L n- hexane, 400 L acetonitrile under ultrasonic extraction for 12 min, and the enrichment factor reached 333. The chromatographic conditions was as follows: DB-5MS capillary chromatographic column (30mx0.25mm,0.25 m) was used. Injector temperature was 220.FID temperature was 250 益.The initial temperature of column was 45 ,keeping for 3 min, then increased to 70 in 3 /min, and then increased to 200 at 30/min and keeping for 2min. Hydrogen flow rate was 10 mL/min. Make -up gas flow rate was 30 mL/min. Split ratio was 30 1. Under the optimized conditions, the mass concentration of mixed solutions for the seven benzene series in ranges of 0.08-1.00 mg/L had the linear relationships to the peak area with the correlation coefficient >0.9980. The method detection limits were ranged from 0.005 mg/L to 0.01 mg/L. Mixed working solutions of 0.10 mg/L for the seven benzene series were detected by 7 times, RSD were in the range of 1.5%-4.7%. The method had been applied to the school lake water and laboratory wastewater, the ecoveries of seven benzene series ranged from 86.5% to 110.4%. The determination results met the requirements of trace analysis

关 键 词：乳化液液微萃取 超声辅助 气相色谱法 苯系物 废水 

分 类 号：O657.71[理学—分析化学]