Bruzzoniti M C, Mucchino C, Tarasco E, Sarzanini C
Department of Analytical Chemistry, University of Turin, Via P. Giuria 5, 10125 Turin, Italy.
J Chromatogr A. 2003 Jul 25;1007(1-2):93-100. doi: 10.1016/s0021-9673(03)00931-2.
A new method for the determination of Pd by ion chromatography and spectrophotometric detection has been developed. The technique is based on the separation of palladium as PdCl4(2-) by anion exchange and on the detection, at a wavelength of 407 nm, of metal as PdI4(2-) after a post-column reaction with KI. The column used was an IonPac AS4 with HCl and HClO4 eluents. The eluent concentration and composition of post-column reagent were optimised in order to obtain the best separation and sensitivity for Pd. In order to reduce the detection limit, an on-line preconcentration step, has been optimised. The method, as developed, was suitable for palladium determination within a 300 ng/l D.L. value. The method applied to a BCR reference material (CRM 277, estuarine sediment) gave satisfactory results in agreement with the certified value within a D.L. value of 1.3 microg/l for the real sample.
已开发出一种通过离子色谱和分光光度检测法测定钯的新方法。该技术基于通过阴离子交换将钯分离为PdCl4(2-)，以及在与KI进行柱后反应后，于407 nm波长处检测作为PdI4(2-)的金属。所使用的色谱柱为配备HCl和HClO4洗脱液的IonPac AS4。对洗脱液浓度和柱后试剂组成进行了优化，以获得钯的最佳分离效果和灵敏度。为降低检测限，对在线预浓缩步骤进行了优化。所开发的方法适用于在300 ng/l的检测限内测定钯。将该方法应用于BCR标准物质（CRM 277，河口沉积物），对于实际样品，在1.3 μg/l的检测限内得到了与认证值相符的满意结果。
