分析硅偶联剂合成产生的废催化剂中铂的样品预处理研究  

Study on the sample pretreatment for analyzing platinum in waste catalyst generated during silicon coupling agent synthesis

作　　者：谢芳琴[1,2] 董占能[2] 吴立生[3] 李秋果[1] 李华[2] 

机构地区：[1]长江大学化学与环境工程学院,湖北荆州434100 [2]昆明理工大学环境科学与工程学院,云南昆明650093 [3]云南大学分析测试中心,云南昆明650090

出　　处：《冶金分析》2009年第5期69-72,共4页Metallurgical Analysis

摘　　要：有机硅偶联剂合成中产生的废催化剂,含有微量的铂和大量有机硅高聚物,铂的分离、分析难度较大。本文采用王水与氢氟酸共同溶解硅和铂的方法,达到铂分析的全溶制样目的。研究了预处理制样过程中各种因素对铂分析的影响。实验结果表明,溶解1.000 g废催化剂样品,优化的操作因素如下:氢氟酸量为5 mL,除氟用硫酸量为2 mL,溶铂用的王水量为5mL,除硝酸用的盐酸量为1 mL,定容溶液盐酸浓度为3 mol/L以及先加王水后加氢氟酸的试剂加入顺序。硅偶联剂合成中废催化剂样品用本方法处理后以氯化亚锡分光光度法测定铂含量,分析值重现性好。The waste catalyst produced during the synthesis of silicon coupling agent contained trace platinum and a great deal of organic silicon polymers. The separation and analysis of platinum were difficult. In this study, the silicon and platinum in catalyst sample were both dissolved with aqua regia and hydrofluoric acid to dissolve the sample completely for platinum analysis. The factors affecting platinum analysis in pretreatment process were investigated. The results indicated that the optimal conditions for dissolving 1. 000 g of waste catalyst sulfuric acid for removing fluorine, 5 mL of aqua acid, and 3 mol/L hydrochloric acid for constant were as follows： 5 mL of hydrofluoric acid, 2 mL of regia, 1 mL of hydrochloric acid for removing nitric volume, with the adding sequence of aqua regia to hydrofluoric acid. After the waste catalyst sample during silicon coupling agent synthesis was pretreated with this method, theplatinum in sample was determined by tin dichloride spectrophotometry. The sample solution was stable and the repeatability of analytical values was good.

关 键 词：有机硅偶联剂 铂 废催化剂 预处理 

分 类 号：X705[环境科学与工程—环境工程]