Dakova Ivanka, Karadjova Irina, Georgieva Ventsislava, Georgiev George
Department of Chemistry, Sofia University, Sofia, Bulgaria.
Talanta. 2009 Apr 30;78(2):523-9. doi: 10.1016/j.talanta.2008.12.005. Epub 2008 Dec 7.
Metal ion-imprinted polymer particles have been prepared by copolymerization of methacrylic acid as monomer, trimethylolpropane trimethacrylate as cross-linking agent and 2,2'-azobisisobutyronitrile as initiator, in the presence of Hg(II)-1-(2-thiazolylazo)-2-naphthol complex. The separation and preconcentration characteristics of the Hg-ion-imprinted microbeads for inorganic mercury have been investigated by batch procedure. The optimal pH value for the quantitative sorption is 7. The adsorbed inorganic mercury is easily eluted by 2 mL 4M HNO(3). The adsorption capacity of the newly synthesized Hg ion-imprinted microbeads is 32.0 micromol g(-1) for dry copolymer. The selectivity of the copolymer toward inorganic mercury (Hg(II)) ion is confirmed through the comparison of the competitive adsorptions of Cd(II), Co(II), Cu(II), Ni(II), Pb(II), Zn(II)) and high values of the selectivity and distribution coefficients have been calculated. Experiments performed for selective determination of inorganic mercury in mineral and sea waters showed that the interfering matrix does not influence the extraction efficiency of Hg ion-imprinted microbeads. The detection limit for inorganic mercury is 0.006 microg L(-1) (3 sigma), determined by cold vapor atomic adsorption spectrometry. The relative standard deviation varied in the range 5-9 % at 0.02-1 microg L(-1) Hg levels. The new Hg-ion-imprinted microbeads have been tested and applied for the speciation of Hg in river and mineral waters: inorganic mercury has been determined selectively in nondigested sample, while total mercury e.g. sum of inorganic and methylmercury, has been determined in digested sample.
以甲基丙烯酸为单体、三羟甲基丙烷三甲基丙烯酸酯为交联剂、2,2'-偶氮二异丁腈为引发剂，在Hg(II)-1-(2-噻唑基偶氮)-2-萘酚配合物存在下，通过共聚反应制备了金属离子印迹聚合物颗粒。采用分批法研究了汞离子印迹微球对无机汞的分离和预富集特性。定量吸附的最佳pH值为7。吸附的无机汞很容易用2 mL 4M HNO₃洗脱。新合成的汞离子印迹微球对干共聚物的吸附容量为32.0 μmol g⁻¹。通过比较Cd(II)、Co(II)、Cu(II)、Ni(II)、Pb(II)、Zn(II)的竞争吸附，证实了该共聚物对无机汞(Hg(II))离子的选择性，并计算出了较高的选择性和分配系数值。对矿物和海水中无机汞进行选择性测定的实验表明，干扰基质不影响汞离子印迹微球的萃取效率。无机汞的检测限为0.006 μg L⁻¹(3σ)，采用冷蒸气原子吸收光谱法测定。在0.02 - 1 μg L⁻¹汞水平下，相对标准偏差在5 - 9%范围内。新型汞离子印迹微球已进行测试并应用于河流和矿泉水中汞的形态分析：在未消化的样品中选择性测定无机汞，而在消化的样品中测定总汞，即无机汞和甲基汞的总和。
