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为了测定镍基高温合金中的痕量有害杂质元素砷、锑、铅、锡和铋,我们用硫代乙酰胺代替硫化氢作沉淀剂,改进了硫化氢化学光谱法。利用合金中含量较高的钼作共沉淀剂,找到了可以同时沉淀分离上述五害元素的化学条件。定量分离出的杂质用碳粉吸收,最后用直流电弧光谱法联合测定。获得的测定下限为砷0.0004%,锑、铅和锡0.0001%,铋0.00002%。通过控制实验和不同方法的对照实验,验证了本方法的准确度。
In order to determine trace arsenic, antimony, lead, tin and bismuth in nickel-base superalloy, we used thioacetamide instead of hydrogen sulphide as precipitating agent, and improved the chemical hydrogen sulphide spectroscopy. Using the higher molybdenum content as the coprecipitator, we found the chemical conditions that can precipitate the above five elements simultaneously. Quantitative separation of impurities with carbon powder absorption, and finally DC arc spectrometry combined determination. The lower limit of determination obtained is 0.0004% of arsenic, 0.0001% of antimony, lead and tin, and 0.00002% of bismuth. The accuracy of this method was verified by the control experiments and the control experiments of different methods.