电感耦合等离子体质谱法测定车用金属催化剂中铂钯铑  

Determination of platinum,palladium,rhodium in motor metal catalyst by inductively coupled plasma mass spectrometry

作　　者：姚慧[1] 张仲荣[1] 高俊华[1] 张云霞[1] 

机构地区：[1]中国汽车技术研究中心,天津300300

出　　处：《冶金分析》2013年第12期8-12,共5页Metallurgical Analysis

摘　　要：车用金属催化剂经盐酸溶解,过滤滤渣经灰化研磨为试验样品.将样品碱熔融后采用碲共沉淀分离富集其中的Pt、Pd和Rh,建立了电感耦合等离子体质谱法（ICP-MS）测定样品中Pt、Pd和Rh的方法.设计正交试验L9 （34）对过氧化钠用量、熔融温度、盐酸体积、碲沉淀时间等溶解条件进行了研究.通过选择合适的测定同位素消除了可能存在的质谱干扰;选用In作为Pd和Rh的内标,Tl作为Pt的内标消除了信号漂移的影响.方法应用于车用金属载体催化剂企业标准样品KTA038中Pt、Pd和Rh的测定,测定值与参考值一致,相对标准偏差在3.1％～4.9％之间,回收率在98％～102％之间.After motor metal catalyst was dissolved with hydrochloric acid and filtered, the residue was treated by ashing and grinding. The sample was fused by alkali, and co-precipitated with tellurium for separation and enrichment of Pt, Pd and Rh, Consequently, a determination method Qf Pt, Pd and Rh by inductively coupled plasma mass spectrometry （!CP-MS） wa~ established, The dissolution condi- tions, including sodium peronide dosage, fusion temperature, hydrochloric acid volume, and tellurium co-precipitation time, were investigated by Qrthogona! test L9 （34）, The possible mass spectral inter- ference was eliminated hy selecting the appropriate determination isotope; and the influence of signal drift was canceled with In as internal standard element for Pd and Rh and T1 as internal standard ele- ment for Pt. Tile method was applied to the determination of Pt, Pd and Rh in the industrial reference material KTAQ38 of motor metal catalyst. The results were consistent with the certified values, and the relative standard deviations were between 3.1%-4. 9 %. The recoveries were in the range of 98%- 102%.

关 键 词：车用金属载体催化剂 铂 钯 铑 电感耦合等离子体质谱法 

分 类 号：O657.63[理学—分析化学] TQ426.8[理学—化学]