极谱法直接连测物料中铂和铑

Direct simultaneous determination of platinum and rhodium in materials by polarography method

建立了不经分离富集,极谱法直接连测物料（矿样、矿渣及催化剂）中铂和铑的方法。在H_2SO_4-NH_4Cl-六次甲基四胺-硫酸肼体系中,铂和铑有高灵敏度及高选择性的催化极谱波,峰电位分别为-0.99V和-1.16V（vs.SCE）,二阶导数峰峰电流与质量浓度在0.001-0.008μg/m L和0.0001-0.0008μg/m L范围内呈良好的线性关系（r_（Pt）=0.9994,r_（Rh）=0.9999）,检出限分别为0.0002和0.00002μg/m L。物料经碱熔酸化后连测铂和铑,回收率在98%-106%之间,相对标准偏差（RSD）≤9.6%。与其它经典方法比较,分析结果基本吻合。

A polarography method for the determination of platinum and rhodium in materials（ mineral sample,slag and catalyst） without separation and enrichment was established. In the solution of H2SO4- NH4Cl-（ CH2）6N4-NH2NH2· H2SO4,the platinum and rhodium showed catalytic polarography waves with high sensitivity and selectivity at- 0. 99 V and- 1. 16 V（ vs. SCE） respectively. The second derivative peak current of the waves was linearly proportional to the concentration in the range of 0. 001 - 0. 008 μg / m L（ r（Pt）= 0. 9994）and 0. 0001 - 0. 0008 μg / m L（ r（Rh）= 0. 9999）. The detection limits were 0. 0002 μg / m L and 0. 00002 μg / m L.Platinum and rhodium in materials were determined after alkaline fusion and acidification of the samples. The recoveries were between 98% and 106%,and relative standard deviation（ RSD） was less than 9. 6%. The results were basically consistent with other classical methods.