Sánchez Rojas F, Ojeda C Bosch, Pavón J M Cano
Department of Analytical Chemistry, Faculty of Sciences, University of Málaga, Campus Teatinos sn, 29071 Málaga, Spain.
Talanta. 2004 Sep 8;64(1):230-6. doi: 10.1016/j.talanta.2004.02.015.
A method for the determination of rhodium in different samples at trace levels is presented. The investigated metal is preconcentrated on a chelating resin microcolumn (1,5-bis(2-pyridyl)-3-sulphophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)) placed in the autosampler arm. The modification of the autosampler in the tubing line and circuit allowed either the flow of the sample through the column or the operation of the autosampler in the normal mode, where microlitres of 4M HNO(3), which acts as the elution agent, pass through the microcolumn eluting Rh(III), which is directly deposited in the graphite tube as drop of a precisely defined volume. The detection limit is 0.3ngml(-1). Linearity is maintained in the concentration range 0-50ngml(-1) for rhodium, with correlation factor of 0.999 and relative standard deviation of 1.8% for 10ngml(-1) of Rh. The effects of various parameters such as pH, concentration and volume of eluent, sample loading time, sample flow rate and interference of a large number of metal ions and anions on the determination of this metal was studied in detail to optimize the conditions for their determination in various samples. The method is found to be highly selective, fairly sensitive, simple, rapid and economical and may be safely applied to their determination in different complex materials such as environmental samples and catalysts.
本文提出了一种测定不同样品中痕量铑的方法。将被研究的金属预富集在置于自动进样器臂中的螯合树脂微柱上(1,5-双(2-吡啶基)-3-磺苯基亚甲基硫代碳酰肼(PSTH)固定在阴离子交换树脂(Dowex 1x8 - 200)上)。通过对自动进样器在管路和电路方面进行改进,既可以使样品流经柱子,也可以使自动进样器以正常模式运行,即微升的4M硝酸作为洗脱剂流经微柱,洗脱铑(III),铑(III)以精确限定体积的液滴形式直接沉积在石墨管中。检测限为0.3ng/ml⁻¹。铑在0 - 50ng/ml⁻¹浓度范围内保持线性,相关系数为0.999,对于10ng/ml⁻¹的铑,相对标准偏差为1.8%。详细研究了各种参数如pH值、洗脱剂浓度和体积、进样时间、样品流速以及大量金属离子和阴离子的干扰对该金属测定的影响,以优化在各种样品中测定该金属的条件。该方法具有高度选择性、相当灵敏、简单、快速且经济,可安全地应用于测定不同的复杂材料,如环境样品和催化剂中的铑。