Hang Chaozhang, Hu Bin, Jiang Zucheng, Zhang Nan
Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
Talanta. 2007 Feb 28;71(3):1239-45. doi: 10.1016/j.talanta.2006.06.033. Epub 2006 Aug 4.
A novel organic reagent 3-(8-quinolinylazo)-4-hydroxybenzoic acid (QAHBA) was synthesized for chemically modified nanometer-sized alumina, and it was characterized with infrared spectrum and (1)H NMR spectra. By using modified nanometer-sized alumina as micro-column packing material, a new method of flow injection (FI) on-line preconcentration coupled to ICP-OES was developed for simultaneous determination of trace metals (Ag, Pd, Au, Ga, In and Nb) in geological and environmental samples. The effects of pH, sample flow rate, sample volume, elution and interfering ions on the recovery of the analytes have been investigated. Under the optimized operating conditions, the adsorption capacity of the modified nanometer-sized alumina for Ag, Pd, Au, Ga, In and Nb were found to be 5.1, 7.6, 17.7, 15.6, 8.1 and 12.3mgg(-1), respectively. With 4min preconcentration time and 24s elution time, the enrichment factor was 10 and the sample frequency was 10h(-1). The detection limits of this method for Ag, Pd, Au, Ga, In and Nb were 0.12, 0.44, 0.27, 0.19, 0.54 and 0.18mugl(-1), respectively, while the R.S.D.s were 1.6, 2.3, 4.5, 1.6, 1.9 and 1.7% (n=7, c=50ngml(-1)), respectively. The proposed method has been applied to the determination of these trace metals in geological-certified reference materials and natural water samples with satisfactory results.
合成了一种新型有机试剂3-(8-喹啉基偶氮)-4-羟基苯甲酸(QAHBA)用于化学修饰纳米氧化铝，并通过红外光谱和核磁共振氢谱对其进行了表征。以修饰后的纳米氧化铝为微柱填充材料，建立了一种流动注射在线预富集与电感耦合等离子体发射光谱联用的新方法，用于同时测定地质和环境样品中的痕量金属(银、钯、金、镓、铟和铌)。研究了pH值、样品流速、样品体积、洗脱和干扰离子对分析物回收率的影响。在优化的操作条件下，修饰后的纳米氧化铝对银、钯、金、镓、铟和铌的吸附容量分别为5.1、7.6、17.7、15.6、8.1和12.3mg g(-1)。在4min预富集时间和24s洗脱时间下，富集因子为10，进样频率为10h(-1)。该方法对银、钯、金、镓、铟和铌的检出限分别为0.12、0.44、0.27、0.19、0.54和0.18μg l(-1)，相对标准偏差分别为1.6%、2.3%、4.5%、1.6%、1.9%和1.7%(n = 7，c = 50ng ml(-1))。该方法已应用于地质标准参考物质和天然水样中这些痕量金属的测定，结果令人满意。
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