González García M M, Sánchez Rojas F, Bosch Ojeda C, García de Torres A, Cano Pavón J M
Department of Analytical Chemistry, Faculty of Sciences, University of Málaga, 29071, Málaga, Spain.
Anal Bioanal Chem. 2003 Apr;375(8):1229-33. doi: 10.1007/s00216-002-1679-y. Epub 2003 Jan 8.
A method to determine trace amounts of platinum in different samples based on electrothermal atomic absorption spectrometry is described. The preconcentration step is performed on a chelating resin microcolumn [1,5-bis(2-pyridyl)-3-sulfophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)] placed in the autosampler arm. The combination of a peristaltic pump for sample loading and the atomic absorption spectrometer pumps for elution through a selection valve simplifies the hardware. The peristaltic pump and the selection valve are easily controlled electronically with two switches placed in the autosampler, which are activated when the autosampler arm is down. Thus, the process is fully automated without any modification of the software of the atomic absorption spectrometer. Under the optimum conditions with a 60-s preconcentration time, a sample flow rate of 2.4 mL min(-1), and an injection volume of eluent of 40 microL, a linear calibration graph was obtained in the range 0-100 ng mL(-1). The enrichment factor was 14. The detection limit under these conditions is 1 ng mL(-1), and the relative standard deviation (RSD) is 1.6% for 10 ng mL(-1) of Pt. The method has been applied to the determination of platinum in catalyst, vegetation, soil, and natural water samples. The results showed good agreement with the certified value and the recoveries of Pt added to samples were 98-105%.
描述了一种基于电热原子吸收光谱法测定不同样品中痕量铂的方法。预富集步骤在置于自动进样器臂上的螯合树脂微柱[固定在阴离子交换树脂(Dowex 1x8 - 200)上的1,5 - 双(2 - 吡啶基)- 3 - 磺苯基亚甲基硫代碳酰肼(PSTH)]上进行。用于样品加载的蠕动泵与用于通过选择阀进行洗脱的原子吸收光谱仪泵相结合,简化了硬件。蠕动泵和选择阀通过置于自动进样器中的两个开关很容易地进行电子控制,当自动进样器臂下降时启动。因此,该过程完全自动化,无需对原子吸收光谱仪的软件进行任何修改。在最佳条件下,预富集时间为60秒,样品流速为2.4 mL min⁻¹,洗脱剂进样体积为40 μL,在0 - 100 ng mL⁻¹范围内获得了线性校准曲线。富集因子为14。在这些条件下,检测限为1 ng mL⁻¹,对于10 ng mL⁻¹的铂,相对标准偏差(RSD)为1.6%。该方法已应用于催化剂、植被、土壤和天然水样中铂的测定。结果与认证值显示出良好的一致性