作者：蓝路梅, 朱霞萍, 宋坤红

作者单位：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

关键词：乳化液液微萃取;超声辅助;气相色谱法;苯系物;废水

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150 L，乳化剂乙腈为400 L，超声时间为12 min时，50 mL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 m0.25 mm，0.25 m）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，3C/min升温至70℃，再以30℃/min升至200℃保持2 min），氢气流量10mL/min，尾吹气流量30 mL/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。

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

LAN Lumei, ZHU Xiaping, SONG Kunhong

College of Materials and Chemistry & Chemical Engineering, Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, Chengdu University of Technology, Chengdu 610059, China

Abstract: 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 μL n-hexane, 400 μL acetonitrile under ultrasonic extraction for 12 min, and the enrichment factor reached 333. The chromatographic conditions was as follows: DB-5MS capillary chromatographic column (30 m×0.25 mm,0.25 μm) was used. Injector temperature was 220℃. FID temperature was 250℃. 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 2 min. 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 recoveries of seven benzene series ranged from 86.5% to 110.4%. The determination results met the requirements of trace analysis.

Keywords: emulsification liquid liquid microextraction;ultrasound assisted;GC;benzene series;wastewater

2017, 43(2): 50-54  收稿日期: 2016-07-14;收到修改稿日期: 2016-09-23

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

作者简介: 蓝路梅(1991-),女,广东英德市人,硕士研究生,专业方向为分析化学。

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