文章摘要
钯和铂中痕量杂质元素锭状固体标准样品制备的研究
Study on Preparation of Solid Ingot Calibration Standards for Trace Impurities in Palladium and Platinum
  
DOI:
中文关键词: 标准样品  仪器分析  痕量杂质  污染
英文关键词: calibration standards  instrumental analysis  trace impurities  contamination
基金项目:
作者单位
NAUJOKAS Algis 赛本金属公司斯科茨维尔 14546纽约美国 
VESA Brent 赛本金属公司斯科茨维尔 14546纽约美国 
PETISHNOK David 赛本金属公司斯科茨维尔 14546纽约美国 
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中文摘要:
      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。
英文摘要:
      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.
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