Scaccia Silvera, Goszczynska Barbara
IDROCOMB, Hydrogen Project and Fuel Cells, ENEA, C.R. Casaccia, via Anguillarese 301, I-00060 Rome, Italy.
Talanta. 2004 Jun 17;63(3):791-6. doi: 10.1016/j.talanta.2003.12.014.
A simple accurate and precise analytical method for the determination of platinum, ruthenium, and molybdenum in Pt, PtRu, and PtMo nanoparticles catalysts deposited on high-surface area carbon by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) is described. The complete digestion of samples (0.010-0.020g), which contain noble metals (NMs) in the range between 0 and 30% in combination among them or with other non-NMs, is obtained under mild conditions using both concentrated HCl and HCl+HNO(3) (1+1 (v/v)) mixture to boiling for 30min in an open vessel. Carbon is separated from the solution by filtering it. Under optimized conditions of the flame, the poor sensitivity of platinum is enhanced 50-fold in presence of 1% (mV(-1)) ascorbic acid, whereas the analytical signal of ruthenium increased by the presence of co-existing platinum. Any kind of interference is observed on the analytical signal of molybdenum. Recovery test obtained by analyzing commercial powder catalysts ranged from 99 to 101%. The precision, expressed as relative standard deviation of five measurements, is better than 1%. Electrode catalysts, made by using the carbon-supported platinum-based powder catalysts, have been analyzed for the metal loadings onto the electrode by GFAAS after dissolution under the same conditions used for the powder catalysts. The precision, expressed as relative standard deviation of three measurements, is better than 2%.
介绍了一种通过火焰原子吸收光谱法（FAAS）和石墨炉原子吸收光谱法（GFAAS）测定负载在高比表面积碳上的Pt、PtRu和PtMo纳米颗粒催化剂中铂、钌和钼的简单、准确且精密的分析方法。使用浓盐酸和HCl+HNO₃（1+1（v/v））混合物在敞口容器中煮沸30分钟，在温和条件下可实现对样品（0.010 - 0.020g）的完全消解，这些样品中贵金属（NMs）的含量在0%至30%之间，它们之间或与其他非贵金属组合存在。通过过滤将碳从溶液中分离出来。在火焰的优化条件下，在1%（mV⁻¹）抗坏血酸存在下，铂的低灵敏度提高了50倍，而共存的铂会使钌的分析信号增加。未观察到对钼分析信号的任何干扰。分析商业粉末催化剂获得的回收率测试范围为99%至101%。以五次测量的相对标准偏差表示的精密度优于1%。使用碳载铂基粉末催化剂制成的电极催化剂，在与粉末催化剂相同的条件下溶解后，通过GFAAS分析电极上的金属负载量。以三次测量的相对标准偏差表示的精密度优于2%。
