摘要
为了开发一种用于环境水样中痕量氯酚类化合物样品预处理及灵敏检测的方法,以钛丝表面原位阳极氧化生成的二氧化钛纳米颗粒为基体,在石英管式炉内高温退火后,通过电聚合吡咯组装得到新型聚吡咯复合二氧化钛纳米颗粒纤维(PPy@TiO_(2)NPs/Ti),用于固相微萃取(SPME)氯酚类污染物。讨论了吡咯单体浓度、聚合电压、聚合时间对吡咯电化学聚合的影响。利用场发射扫描电子显微镜(SEM)和能量色散X射线光谱(EDS)进行纤维表面形貌和成分分析。PPy@TiO_(2)NPs/Ti纤维涂层兼具二氧化钛和聚吡咯纤维的优点,与单独的聚吡咯和二氧化钛涂层相比,具有萃取效率高、机械稳定性好和使用寿命长等优点。将PPy@TiO_(2)NPs/Ti纤维与带紫外检测器的高效液相色谱联用测定实际水样中的多氯酚(CPs),结果表明所制备的纤维对一些CPs具有良好的萃取能力。试验对影响该纤维SPME酚类化合物的影响因素进行了优化。在最佳的萃取条件下,该纤维对CPs萃取分析的特征数据如下:回归方程线性相关性(R^(2))大于0.9965,检出限(LOD,信噪比为3)和定量限(LOQ,信噪比为10)的范围分别为0.008~0.026μg/L和0.03~0.09μg/L,单个纤维测定5次和3个纤维平行测定得到的相对标准差(RSD)数值范围分别在3.5%~5.8%和4.6%~7.2%。对实际水样黄河水、废水和自来水中的酚类化合物测定并加标分析,平均回收率在89.7%~112%。与商品纤维相比,该纤维萃取效率高,操作性强,可灵敏测定复杂环境样品中的CPs。这种新型纤维具有化学稳定性和制备复制性好的特点。
The purpose of this test is to develop an effective sample pretreatment and sensitive detection method for the determination of trace chlorophenols in environmental water samples.A novel polypyrrole composite titanium dioxide nanoparticle fiber(PPy@TiO_(2)NPs/Ti)was fabricated by direct electropolymerization of pyrrole on annealed TiO_(2)nanoparticles,which was used for solid-phase microextraction(SPME)of chlorophenols.The effects of pyrrole monomer concentration,polymerization voltage,and polymerization time on the surface morphology of the fiber were discussed.The surface morphology and composition of PPy@TiO_(2)NPs coating were analyzed by field emission scanning electron microscope(SEM)and energydispersive X-ray spectroscopy(EDS).This PPy@TiO_(2)NPs coating combined the merits of both PPy and TiO_(2),and thereby has several advantages over that of individual PPy and TiO_(2)coatings such as improved extraction efficiency,enhanced mechanical stability,and prolonged service life.The asfabricated fiber exhibited good extraction capability for some chlorophenols(CPs)and was employed to determine the CPs in combination with high-performance liquid chromatography-UV detection.The factors affecting the fiber solid-phase microextraction(SPME)of CPs were examined and optimized.At the optimum SPME conditions,the calibration curves were linear(R^(2)≥0.9965).The limits of detection(LOD,signal noise ration is 3)and limits of quantitation(LOQ,signal noise ration is 10)ranged from 0.008 to 0.026μg/L and from 0.03 to 0.09μg/L for CPs,respectively.Relative standard deviations(RSDs)for single fiber repeatability ranged from 3.5%to 5.8%(n=5)and RSDs for fiber-to-fiber reproducibility(n=3)varied from 4.6%to 7.2%.The proposed method was employed for selective concentration and determination of CPs in real environmental water samples,including Yellow River water,wastewater,and tap water.To evaluate accuracy and precision,water samples were fortified by spiking CPs standards into the real water samples and the recovery rate was
作者
马明广
魏云霞
魏慧娟
叶鹤琳
刘芳
周敏
MA Ming-guang;WEI Yun-xia;WEI Hui-juan;YE He-lin;LIU Fang;ZHOU Min(College of Chemical Engineering,Lanzhou City University,Lanzhou 730070,China;College of Chemistry and Chemical Engineering,Northwest Normal University,Lanzhou 730070,China)
出处
《安全与环境学报》
CAS
CSCD
北大核心
2022年第6期3508-3517,共10页
Journal of Safety and Environment
基金
国家自然科学基金项目(22166032)
2021甘肃省重点人才项目
环境友好能源材料国家重点实验室开放项目(KF-20-0217)。
关键词
环境工程学
固相微萃取
高效液相色谱
多氯酚
三氯生
二氧化钛
聚吡咯
environmental engineering
solid phase microextraction
high performance liquid chromatography
chlorophenols
triclosan
titanium dioxide
polypyrrole
