胺功能化聚丙烯腈固相萃取法在线分离富集环境水体中铜和铅  

Amine-functionalized Polyacrylonitrile Solid Phase Extraction Method for On-line Separation and Enrichment of Copper and Lead in Environmental Water

作　　者：赵峻谊 王佳妮[1] 任红云 吴坤 张子兴[1] 贾晓宇 ZHAO Jun-Yi;WANG Jia-Ni;REN Hong-Yun;WU Kun;ZHANG Zi-Xing;JIA Xiao-Yu(CAS Key Lab of Urban Environment and Health,Institute of Urban Environment,Chinese Academy of Sciences,Xiamen 361021,China;Zhejiang Key Laboratory of Urban Environmental Processes and Pollution Control,Ningbo Urban Environment Observation and Research Station,Chinese Academy of Sciences,Ningbo 315830,China)

机构地区：[1]中国科学院城市环境研究所,中国科学院城市环境与健康重点实验室,厦门361021 [2]中国科学院宁波城市环境观测研究站,浙江省城市环境过程与污染控制重点实验室,宁波315830

出　　处：《分析化学》2021年第12期2126-2133,共8页Chinese Journal of Analytical Chemistry

基　　金：宁波市科技计划项目(No.202002N3107);国家自然科学基金项目(No.21806161)资助。

摘　　要：采用聚丙烯腈为原料,以三乙烯四胺(TETA)为修饰基团,制备了一种新型胺功能化聚合物吸附材料。利用扫描电子显微镜(SEM)及傅里叶变换红外光谱仪(FT-IR)对聚合物材料的形貌结构进行表征。自制固相萃取小柱与电感耦合等离子体质谱技术相结合,建立了集分离、富集和测定于一体的在线快速分析方法。考察了溶液pH值、流速、体积及共存干扰离子对铜和铅分离富集效果的影响。结果表明,目标物在溶液pH=7、流速为5 mL/min、样品量为50 mL的条件下,仅需10 min即可实现高达95%的吸附率,并且不受环境水体中干扰离子的影响,铜和铅的动态吸附饱和容量分别为15.1和22.5 mg/g。在1 mL/min流速下,采用1%HNO 3溶液定量洗脱目标物,获得了较高的富集倍数。本方法对水中铜和铅的检出限(LOD)分别为1.7和2.5μg/L,相对标准偏差(RSD)小于3.5%。通过环境标准参考物质GSB07-3186-2014(水质铅和铜、镉、镍)验证了本方法的可行性和准确性。所制备的胺功能化聚丙烯腈材料具有价格低廉、环境友好、吸附效率高及可重复利用等优势,在线一体化方法操作简单、分析速度快且稳定性好,可用于实际环境水体中痕量铜和铅的分离分析。A new type of amine functionalized polymer adsorption material was synthesized by using polyacrylonitrile as the raw material and triethylenetetramine(TETA)as the modified group.The morphology and structure of polymer materials were characterized by scanning electron microscope(SEM)and Fourier transform infrared spectrometer(FT-IR).A fast on-line analysis method integrating separation,enrichment and determination was established by combining with a home-made solid phase extraction column and inductively coupled plasma mass spectrometry technology.The effects of pH,flow rate,volume and coexisting interfering ions on the separation and preconcentration of copper and lead were investigated.Under the conditions of pH 7,flow rate of 5 mL/min and sample volume of 50 mL,the adsorption efficiency of the metal ions could reach 95%within 10 min,and the interfering ions in real environmental water could be ignored.The dynamic adsorption saturation capacities of copper and lead were 15.1 and 22.5 mg/g,respectively.At a flow rate of 1 mL/min,1%HNO 3 solution was adopted to quantitatively elute the trace elements,and high enrichment factors were obtained.The limits of detection(LODs)of the method for copper and lead were 1.7 and 2.5μg/L,respectively,and the relative standard deviation(RSD%)was less than 3.5%.Finally,the environmental Certified Reference Material GSB07-3186-2014(CRM)was selected to verify the feasibility and accuracy of the on-line method.The prepared amine functionalized polyacrylonitrile had many advantages such as low cost,environmental friendliness,high adsorption efficiency and reusability.The online integrated method had the merits of easy to operate,fast,stable,and was suitable for the analysis of trace copper and lead in real environmental water samples.

关 键 词：胺功能化聚丙烯腈 分离富集 电感耦合等离子体质谱仪 环境水体 痕量金属 铜 铅 

分 类 号：X832[环境科学与工程—环境工程] O657[理学—分析化学]