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利用共沉淀法和巯基化表面修饰制备Fe3O4纳米吸附材料,并将其应用于海水中痕量汞检测的富集和分离前处理过程.所制备的巯基化Fe3O4纳米颗粒的粒径小于100 nm,饱和磁化强度达63.64 emu·g-1,巯基含量为3.11 mg·g-1.当巯基化Fe3O4的用量为0.5 mg·m L-1、吸附溶液p H值为7.5—8.0、吸附时间为20min时,吸附剂对汞的富集率可达95%以上,并且在外磁场作用下可快速分离.在优化的吸附条件下并借助原子荧光光谱法测定了实际海水样品中汞离子的含量,加标回收率在89.8%—107.3%之间,11次空白样品测量的检出限(3σ)为5.3 ng·L-1.该方法利用巯基化Fe3O4纳米材料具有高效富集的特点,可应用于海水中痕量汞的快速富集和分离,以实现对海水中痕量汞的准确测量.
Fe3O4 nano-adsorbent was prepared by coprecipitation and thiolated surface modification, and applied to the enrichment and separation pretreatment of trace mercury in seawater.The particle size of the prepared thiolated Fe3O4nanoparticles was less than 100 nm, The saturation magnetization reaches 63.64 emu · g-1 and the content of mercapto group is 3.11 mg · g-1. When the amount of thiolated Fe3O4 is 0.5 mg · m L-1, the pH value of the adsorption solution is 7.5-8.0 and the adsorption time is 20 min , The enrichment rate of mercury adsorbed by adsorbents can reach more than 95%, and can be quickly separated under the action of external magnetic field.The content of mercury ion in the actual seawater samples was determined by atomic fluorescence spectrometry under the optimized adsorption conditions, The recoveries ranged from 89.8% to 107.3%, and the detection limit (3σ) of 11 blank samples was 5.3 ng · L-1.This method utilizes the characteristics of high enrichment of thiolated Fe3O4 nanomaterials and can be applied to seawater Rapid enrichment and separation of trace mercury in the sea to achieve accurate measurement of trace mercury in seawater.