Department of Chemistry, Aligarh Muslim University, Aligarh, India.
Talanta. 2010 Jun 15;81(4-5):1772-80. doi: 10.1016/j.talanta.2010.03.035. Epub 2010 Mar 25.
A stable extractor of metal ions was synthesized through azo linking of p-hydroxybenzoic acid with Amberlite XAD-4 and was characterized by elemental analyses, infrared spectral and thermal studies. Its water regain value and hydrogen ion capacity were found to be 15.80 and 7.52mmolg(-1), respectively. Both batch and column methods were employed to study the sorption behavior for the metal ions which were subsequently determined by flame atomic absorption spectrophotometry. The optimum pH range for Co(II), Ni(II), Cu(II), Zn(II), and Pb(II) ions were 10.0, 8.0-9.0, 7.0, 7.0-8.0 and 7.0-8.0, respectively. The half-loading time, t(1/2), are 6.0, 8.0, 8.0, 8.0 and 4.0min, respectively. Comparison of breakthrough and overall capacities of the metals ascertains the high degree of column utilization (>75%). The breakthrough capacities for Co(II), Ni(II), Cu(II), Zn(II), and Pb(II) ions were found to be 0.46, 0.43, 0.42, 0.09 and 0.06mmolg(-1) with the corresponding preconcentration factor of 460, 460, 460, 360 and 260, respectively. The limit of preconcentration was in the range of 4.3-7.6microgL(-1). The detection limit for Co(II), Ni(II), Cu(II), Zn(II) and Pb(II) were found to be 0.47, 0.45, 0.50, 0.80, and 1.37microgL(-1), respectively. The Student's t (t-test) values for the analysis of standard reference materials were found to be less than the critical Student's t values at 95% confidence level. The AXAD-4-HBA has been successfully applied for the analysis of natural water, multivitamin formulation, infant milk substitute, hydrogenated oil and fish.
通过对间羟基苯甲酸与 Amberlite XAD-4 的偶氮连接,合成了一种稳定的金属离子萃取剂,并通过元素分析、红外光谱和热研究进行了表征。其回湿值和氢离子容量分别为 15.80 和 7.52mmolg(-1)。分别采用批量和柱法研究了金属离子的吸附行为,随后用火焰原子吸收分光光度法测定。Co(II)、Ni(II)、Cu(II)、Zn(II)和 Pb(II)离子的最佳 pH 范围分别为 10.0、8.0-9.0、7.0、7.0-8.0 和 7.0-8.0。Co(II)、Ni(II)、Cu(II)、Zn(II)和 Pb(II)离子的半加载时间 t(1/2)分别为 6.0、8.0、8.0、8.0 和 4.0min。对金属的穿透和总容量的比较证实了柱利用率很高(>75%)。Co(II)、Ni(II)、Cu(II)、Zn(II)和 Pb(II)离子的穿透容量分别为 0.46、0.43、0.42、0.09 和 0.06mmolg(-1),相应的预浓缩因子分别为 460、460、460、360 和 260。预浓缩的极限范围在 4.3-7.6microgL(-1)之间。Co(II)、Ni(II)、Cu(II)、Zn(II)和 Pb(II)的检测限分别为 0.47、0.45、0.50、0.80 和 1.37microgL(-1)。用标准参考物质分析的学生 t 值(t 检验)小于 95%置信水平下的临界学生 t 值。AXAD-4-HBA 已成功应用于天然水、多种维生素制剂、婴儿代乳品、氢化油和鱼类的分析。