脉冲热导法测定铝中氢的探讨

发布时间：2018-03-19 11:40

  本文选题：脉冲热导法　切入点：铝　出处：《冶金分析》2016年12期 　论文类型：期刊论文

【摘要】：探讨了样品前处理方法、空白和分析功率对脉冲热导法测定铝中氢的影响,并探索了实验中遇到的表面氢问题、热抽取氢失败的问题及二次样仍能测出氢的问题。实验表明:铝中氢分析要求现车新鲜表面样品,最好在气体分析实验室备有车床现车现分析,且增加超声波清洗程序,以有效清除样品制备过程中可能存在的微量污染,确保样品足够清洁;坩埚空白差值为0.01~0.04μg/g,对于0.10μg/g附近的超低含量氢的分析,需要单个扣除空白,对于0.19μg/g以上较高含量氢的分析,用平均值扣空白亦可;为使每单个样品的分析功率落在最佳微小区域,每次取出坩埚时,均需使样品熔融后为亮球状态最佳,一般分析功率控制在1 100~1 300kW之间。按照实验方法对铝合金标准样品进行测定,8次平行测定结果的相对标准偏差(RSD)为4.1%,测定值为(0.19±0.029)μg/g,比该标样证书给出的(0.19±0.04)μg/g更好,且每个点均不超差。方法可以准确测定低至0.09μg/g铝中总氢或全氢。
[Abstract]:The influence of sample pretreatment method, blank and analytical power on the determination of hydrogen in aluminum by pulsed thermal conductivity method was discussed, and the surface hydrogen problems encountered in the experiment were explored. The failure of hot extraction of hydrogen and the problem that hydrogen can still be measured by secondary samples. The experiment shows that hydrogen analysis in aluminum requires fresh surface samples, it is better to have lathe present analysis in gas analysis laboratory, and to add ultrasonic cleaning procedure. The crucible blank difference is 0.01g / g, 0.04 渭 g / g for the analysis of ultra-low hydrogen content near 0.10 渭 g / g, which requires a single deduction blank, and for the analysis of higher hydrogen content above 0.19 渭 g / g, it is necessary to remove the trace contamination that may exist during the preparation of the sample, and to ensure that the sample is clean enough, and the crucible blank value is 0.04 渭 g / g. In order to make the analysis power of each single sample fall in the best small area, the sample should be melted and the bright sphere should be optimized when the crucible is taken out. The general analytical power is controlled between 1 100 and 1 300 kW. The relative standard deviation (RSDs) for 8 parallel measurements of aluminium alloy standard samples is 4. 1 and the measured value is 0. 19 卤0. 029 渭 g / g, which is better than that given by the standard sample certificate of 0. 19 卤0. 04 渭 g / g. The method can accurately determine total hydrogen or total hydrogen in aluminum as low as 0.09 渭 g / g.
【作者单位】： 中国科学院金属研究所;沈阳铸造研究所;
【分类号】：TG115.25
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本文编号：1634104