铬黑T 形成树脂分离富集极谱测试地质样品中贵金属Pt、Rh、Ru 研究

合成并研究了铬黑T 形成树脂分离富集地质标准样品中的钌、铂、铑，获得了最佳实验条件。结果表明: pH = 2. 00 的盐酸溶液作为介质、温度为293 K、流速v≤1. 0 mL·min － 1、柱高h≥10. 0 cm，铂、铑、钌吸附率均在95%以上; 在293 K，使用40 mL 的pH 2. 00 盐酸－ 3%硫脲溶液静态洗脱或以1. 0 mL·min － 1的流速进行动态洗脱，洗脱率均在95%以上。树脂对铂、铑、钌的吸附过程符合拟二级动力学模型。实验条件下的标准回收实验，回收率均＞ 95%。对地质标准样品进行了分析测定，相对误差均＜ 7%。铂、铑、钌的相对标准偏差分别是铂: 0. 852 0%和0. 325 0%; 铑: 4. 20%和 4. 89%; 钌: 1. 24%和1. 79%。铂、铑、钌的检出限分别为3. 55 × 10 － 6 μg·mL － 1、6. 23 × 10 － 7 μg· mL － 1、1. 92 × 10 － 5μg·mL － 1。该方法的准确度和精密度较高。

Determination of Pt,Rh and Ru in geological samples with oscillolarography after separation and enrichment by EBT forming resin

The resin modified with EBT was synthesized and the optimum experiment parameter was identified． The Pt，Rh and Ru in geological standard samples were separated and enriched by EBT forming resin． When the pH ( HCl) in 2. 00，the temperature is 293 K． The flow rates of sample solution is lower than or equal to 1. 0 mL /min． Column is longer than 10. 0 cm． The adsorption rates of Pt，Rh and Ru are greater than 95%． When the temperature is 293 K，elution with pH 2. 00 hydrochloric acid － 3% thiourea ( 40 mL) by batch method or elution with the velocity of fiow at 1. 0 mL per minute by dynamic method，the elution rates of Pt，Rh and Ru are greater than 95%． The adsorption kinetics follow a pseudo-second － order model for the adsorption of Pt，Rh and Ru by EBT forming resin． In the standard recovery experiment，the recoveries of Pt，Rh and Ru are greater than 95%． Being determined by oscillolarography，relative errors are less than 7%． The relative standard deviations are 0. 852 0% and 0. 325 0% for Pt，4. 20 % and 4. 89 % for Rh，and 1. 24% and 1. 79% for Ru． The detection limits: Pt: 3. 55 × 10 － 6 μg·mL － 1 ; Rh: 6. 23 × 10 － 7 μg·mL － 1 ; Ru: 1. 92 × 10 － 5μg·mL － 1 ． It is proved that this method is higher in accuracy and precision．