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我們采用硫化氫分离、深孔电极直流电弧粉末法进行了含有Ni、Cr、Ti、Al等元素的鎳基合金中微量有害杂质(Pb、Sn、Bi、Sb、As)的分析。由于操作手續较长,試剂用量亦較大,因而即使采用分析純級試剂,实驗空白(主要是Pb、Sn、As)也很高。我們系統地分析了空白的来源,并寻找了降低的办法;最后使Pb、Sn的空白降低至1～2v,滿足了分析的要求。在实际試样中,As的蒸发不完全。我們加入了P_2O_5,使As的蒸发大大加速。由于有效地利用了样品,因而使As的灵敏度提高了4～5倍。实驗中发現,在As 2349(?)处有碳电极在空气中燃弧所产生的带状光譜。系統实驗的結果說明,可以用經过H_2S沉淀后的純溶液来配制标准样品。避免了采用一般增量法制訂定标曲綫,保証了結果的准确度。通过系統实驗,确定了操作条件。对于三个实际試样进行了多次分析。结果表明,本法的分析下限分別为:Pb～0.0001%,Sn、Sb～0.0002%,As～0.0003%,Bi～0.00002%。
We use hydrogen sulfide separation, deep-hole electrode DC arc powder method for the analysis of trace harmful impurities (Pb, Sn, Bi, Sb, As) in Ni-based alloys containing Ni, Cr, Ti, Al and other elements. Due to the long operating procedures and the large amount of reagents, experimental blank (mainly Pb, Sn, As) is high even with analytical grade reagents. We systematically analyzed the source of the blank and looked for ways to reduce it. Finally, the blank of Pb and Sn was reduced to 1-2v to meet the requirements of the analysis. In the actual sample, As evaporation incomplete. We added P_2O_5 to accelerate the As evaporation greatly. As the effective use of the sample, thus increasing the sensitivity of As 4 to 5 times. It was found in the experiment that there is a banded spectrum produced by arcing carbon electrodes in air at As 2349 (?). The results of the system experiment show that the standard sample can be prepared with pure solution after H 2 S precipitation. Avoid using the general incremental method to formulate the calibration curve, to ensure the accuracy of the results. Through systematic experiments, the operating conditions were determined. Multiple analyzes were performed on three actual specimens. The results show that the lower limits of this method are: Pb ~ 0.0001%, Sn, Sb ~ 0.0002%, As ~ 0.0003%, Bi ~ 0.00002%.