酸分解-容量法测定四(三苯基膦)钯中的钯含量  

Volumetric Determination of Palladium Content in Tetrakis (triphenylphosphine) Palladium Decomposed by Acid

作　　者：鲁瑞智 金娅秋[1] 杨晓滔[1] 曾荷峰 付仕梅 马媛[1] 甘建壮[1] LU Ruizhi;JIN Yaqiu;YANG Xiaotao;ZENG Hefeng;FU Shimei;MA Yuan;GAN Jianzhuang(Kunming Institute of Precious Metals,State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino-Platinum Metals Co.Ltd.,Kunming 650106,China)

机构地区：[1]昆明贵金属研究所,贵研铂业股份有限公司稀贵金属综合利用新技术国家重点实验室,昆明650106

出　　处：《贵金属》2018年第A01期215-218,共4页Precious Metals

摘　　要：采用硝酸溶解四(三苯基膦)钯样品,高氯酸发烟分解有机物,以络合滴定法测定钯含量。对样品发烟分解条件进行了详细考察,结果表明,高氯酸残留量在1.0 mL以内,经3次发烟可完全分解有机物。采用丁二肟析出-EDTA络合滴定法测定钯,所得结果相对标准偏差(RSD)为0.28%,加标回收率为99.66%～100.04%,满足样品中钯含量测定的要求。Samples were digestion by HNO3-HClO4,then dissolved with HNO3-HCl.Using EDTA complexometric,ZnNO3 back titration by dioxime precipitation determinated palladium content in samples.The method discussed conditions of digestion by HNO3-HClO4.The results showed that the residual amount of HClO4 was within 1.0 mL,and the organic matter was decomposed completely by 3 times of smoke.The standard recovery rate was 99.66%~100.04%,and the relative standard deviation(RSD)was 0.28%.These results meet the requirements of determination palladium.

关 键 词：分析化学 四(三苯基膦)钯 钯 硝酸-高氯酸 发烟分解 容量法 

分 类 号：O655.25[理学—分析化学] O652.4[理学—化学]