磁性氮掺杂石墨烯固相萃取环境水样中的4种有机氯污染物

发布时间：2018-09-05 08:04

【摘要】：采用化学共沉淀法成功合成了磁性氮掺杂石墨烯纳米材料,对其吸附性能进行了初步探讨。此磁性纳米材料对对氯间二甲苯酚的吸附不局限于均匀的单分子层吸附,吸附动力学符合准二级动力学模型。将其作为磁性固相吸附剂,通过对吸附剂用量、超声萃取时间、水样pH值、上样体积等条件的优化,建立了超声辅助磁性固相萃取-气相色谱/串联质谱同时测定环境水样中的三氯生(TCS)、对氯间二甲苯酚(PCMX)、六氯苯(HCB)和2,2',4,4',5,5'-六氯联苯(PCB-153)4种有机氯污染物的方法。在优化条件下,将6.0 mg Fe_3O_4/N-G分散于100 mL水样中,调节水样至pH 5,超声萃取15 s,磁性分离,3 mL乙醇和2 mL二氯甲烷分步洗脱,洗脱液氮吹定容,进行气相色谱-质谱联用分析。4种有机污染物在0.1~10μg/L范围内与峰面积呈良好的线性关系,相关系数为0.9983~0.9999,检出限(S/N=3)和定量限(S/N=10)分别为0.05~0.6 ng/L和0.4~2.4 ng/L,3个加标浓度水平的回收率为68.3%~103.4%,日内、日间测定的相对标准偏差分别为3.3%~6.9%和3.4%~9.4%(n=6)。本方法简单方便,易于操作,适用于环境水样中有机氯污染物的检测。
[Abstract]:The magnetic nitrogen-doped graphene nanomaterials were successfully synthesized by chemical coprecipitation and their adsorption properties were preliminarily discussed. The adsorption of p-chloro-m-xylenol by the magnetic nanomaterials is not limited to the homogeneous monolayer adsorption, and the adsorption kinetics is in accordance with the quasi-second-order kinetic model. It was used as magnetic solid phase adsorbent. The optimum conditions such as the amount of adsorbent, ultrasonic extraction time, pH value of water sample and sample volume were optimized. An ultrasonic assisted magnetic solid phase extraction-gas chromatography-tandem mass spectrometry (GC-MS) method for the simultaneous determination of four organochlorine pollutants, trichlorobenzene p-chlorobenzene (PCMX), hexachlorobenzene (HCB) and trichloro-m-xylenol (PCMX), and four organochlorinated pollutants (PCB-153), was developed. Under the optimized conditions, 6.0 mg Fe_3O_4/N-G was dispersed in 100 mL water sample, water sample was adjusted to pH 5, ultrasonic extraction was performed for 15 s, magnetic separation of 3 mL ethanol and 2 mL dichloromethane were separated step by step, and liquid nitrogen was eluted by blowing constant volume. Gas chromatography-mass spectrometry (GC-MS) was used to analyze the linear relationship between the peak area of 4 organic pollutants in the range of 0.1 渭 g / L and 10 渭 g / L, the correlation coefficient was 0.9983 卤0.9999, the recoveries of detection limit (S/N=3) and quantitative limit (S/N=10) were 0.050.60 ng/L and 0.4 渭 g / L, respectively, and the recoveries of the three standard concentration levels were 68.3% and 103.44 渭 g 路L ~ (-1), respectively, in the range of 0.1 渭 g / L and 0.9983 渭 g / L, respectively. The relative standard deviations were 3.3% and 9.4%, respectively. The method is simple and easy to operate, and is suitable for the detection of organochlorine pollutants in environmental water samples.
【作者单位】：浙江工业大学化学工程学院;浙江工业大学分析测试中心;
【基金】：浙江省科技厅公益技术应用研究项目(Nos.2017C33014,2014C03026)资助
【分类号】：X832;O658.2

【相似文献】