微波消解和精密电流滴定法测定铂类化合物中的铂含量  

Determination of Platinum Content in Platinum Compounds Using Microwave Digestion and Micro Electricity Titration Method

作　　者：朱利亚[1] 陈云江[1] 赵辉[1] 赵忆宁 黄章杰[3] 杨光宇[3] 朱武勋[1] 

机构地区：[1]昆明贵金属研究所,云南昆明650106 [2]云南省标准化研究院,云南昆明650228 [3]云南大学化学系,云南昆明650091

出　　处：《贵金属》2007年第3期51-55,共5页Precious Metals

基　　金：国家标准化技术委员会行业标准制订基金项目(No.2006080-72);贵金属研究所创新基金项目(No.2002BY-1)资助

摘　　要：提出了微波密闭快速消解Pt(NH3)2(NO2)2、Pt(NH3)2Cl2、Pt(NH3)4Cl2、(NH4)2PtCl6、K2PtCl4难分解化合物的新方法;优化了KMnO4电流滴定法测定Pt(Ⅳ)的条件;比较了本法与氯铂酸铵重量法、水合肼还原重量法、烘箱罐消解电流滴定法;同时,将精密电流滴定法应用于PtCl4、Na2PtCl6、K2PtCl6、H2PtCl4化合物中Pt(Ⅳ)含量的测定。结果表明:测定37%~65%的Pt(Ⅳ)含量,本法、氯铂酸氨重量法、水合肼还原重量法的相对平均误差分别为-0.14%^+0.13%、-0.21%^+0.21%、-0.13%^+0.14%,相对标准偏差分别为0.05%~0.08%、0.11%~0.14%、0.08%~0.09%,故本法的准确度和精密度与水合肼还原重量法的基本一致,较氯铂酸氨重量法的略好;但本法消解快速、节能、安全,操作简便,对环境污染程度小,适宜推广运用。A microwave-assisted sealing digestion method for determination of platinum in difficultly decomposed compounds of Pt（NH3）2（NO2）2, Pt（NH3）2Cl2, Pt（NH3）4Cl2, （NH4）2PtCl6 and K2PtCl4 is proposed. The condition for determination of platinum （Ⅳ） with KMnO4 micro electricity titration was optimized. The proposed method was compared with traditional gravimetric analysis and oven-heating analysis. At the same time, the platinum （Ⅳ） in compounds of PtCl4, Na2PtCl6, K2PtCl6 and H2PtCl4 was also determined under optimal conditions. Experimental results showed that the relative average error of the proposed method, the hydrazine hydrate gravimetry and the ammonium chloroplatinate gravimetry is -0.14%-40.13%, -0.21%-＋0.21% and -0.13%-＋0.14%, respectively, and the relative standard deviation of three methods is 0.05%-0.08%, 0.11%-0.14% and 0.08%-0.09%, respectively, for Pt content from 37% to 65%. Therefore, the accuracy and precision of the proposed method are almost the same with hydrazine hydrate gravimetry, and are a little better than ammonium chloroplatinate gravimetry. But it is rapid, economic, secure, easy to operate and environmental friendly.

关 键 词：分析化学 微波消解 KMnO4精密电流滴定法 铂类化合物 铂 

分 类 号：O655.2[理学—分析化学]