本文通过乳液聚合法制备磁性离子印迹材料Fe3O4@SiO2@IIM,并运用多种技术手段对其进行了表征。所制备的Fe3O4@SiO2@IIM磁材料颗粒较均一,粒径约为20nm,单分散性好,具有超顺磁性(饱和磁化强度为8.66emu·g^-1)。基于此,建立了离子印迹磁固相萃取(IIMSPE)-石墨炉原子吸收光谱法(GFAAS)联用技术分析环境水样中Ni(Ⅱ)的新方法。对影响MSPE的因素进行了详细的考察。在最优实验条件下,方法对Ni(Ⅱ)的检出限为0.015ng·mL^-1,相对标准偏差(RSDs)为7.3%(n=7,c=0.1ng·mL^-1),富集倍数为24.8,所制备的磁性离子印迹材料不同批次间RSDs为10.9%(n=5,c=0.1ng·mL^-1),所合成的材料可以重复使用5次以上。采用该方法分析了标准水样(GSBZ50009-88)中的Ni(Ⅱ)含量,验证方法的准确性,测定值和标准值吻合良好。将该方法应用于东湖水和长江水中Ni(Ⅱ)的测定,加标回收率为90.6%-107.2%。
Magnetic ion imprinted materials(Fe3O4@SiO2@IIM)were synthesized by emulsion polymerization along with magnetic non-ion imprinted materials(Fe3O4@SiO2@NIIM),followed by characterization via various analytical techniques.The prepared Fe3O4@SiO2@IIM are well uniform and monodispersed,with the particle size of about 20 nm,featuring with super-paramagnetism.Based on the as-prepared Fe3O4@SiO2@IIM,a novel method of ion imprinted magnetic solid phase extraction(IIMSPE)combined with graphite furnace atomic absorption spectrometry(GFAAS)detection was developed for the determination of trace Ni(Ⅱ)in environmental water samples.The factors affecting the extraction,such as pH of sample solution,concentration of elution,elution volume,elution time,sample volume,extraction time were investigated in detail.Under the optimized conditions,the limit of detection was 0.015ng·mL^-1,with relative standard deviation of 7.3%(c=0.1,ng·mL^-1)and enrichment factor of 24.8.The prepared Fe3O4@SiO2@IIM could be used more than 5times.For the validation of the proposed method,certified reference material GSBZ50009-88(environmental water)was analyzed and the determined value was in good agreement with the certified value.The developed method was applied to the analysis of Ni(Ⅱ)in Yangtze River water and East Lake water,and the recoveries for the spiked samples were in the range of 90.6%-107.2%,indicating agood application potential of the proposed method for the quantification of trace Ni(Ⅱ)in environmental water samples.