钯和铂中痕量杂质元素锭状固体标准样品制备的研究

摘要

This work details, on a laboratory scale, a method to prepare small solid ingot calibration standards of palladium and platinum for use in solid sampling instrumentation such as arc/spark OES, spark ablation OES and GD-MS. Standards were prepared by first precipitating and co-precipitating spiked solutions of palladium and platinum along with the desired analytes then melting the "stock" powder with a bulk amount of 99.999% pure metal to attempt to achieve a final concentration in the metal of (5~10) ×10-6 for 33 elements. Losses occurred in both the precipitation step and the thermal step with a final of 25 elements for Pd being quantitatively incorporated into the final ingot and 26 elements in Pt. Several contamination issues arose with Au, B, Fe, and Si.%详细介绍了制备钯和铂锭状固体标准样品的实验方法。该固体标样可用于测定固体样品的电弧/火花发射光谱、火花烧蚀发射光谱和辉光放电质谱(GD-MS)等仪器分析方法。在标准样品的制备过程中，首先将含有33种待测杂质元素的钯或铂溶液进行沉淀和共沉淀得到“贮备”粉末，然后将粉末与99.999%纯金属钯或铂进行熔炼，从而获得杂质元素含量在(5~10)×10-6的固体标准样品。部分杂质元素在沉淀和共沉淀过程、热处理环节会发生损失，在最终得到的锭中，钯标准样品有25个元素、铂标准样品有26个元素得到定量回收，发生污染的元素主要包括金、硼、铁和硅。