本文選題：脈沖熱導法　切入點：鋁　出處：《冶金分析》2016年12期 　論文類型：期刊論文

【摘要】：探討了樣品前處理方法、空白和分析功率對脈沖熱導法測定鋁中氫的影響,并探索了實驗中遇到的表面氫問題、熱抽取氫失敗的問題及二次樣仍能測出氫的問題。實驗表明:鋁中氫分析要求現(xiàn)車新鮮表面樣品,最好在氣體分析實驗室備有車床現(xiàn)車現(xiàn)分析,且增加超聲波清洗程序,以有效清除樣品制備過程中可能存在的微量污染,確保樣品足夠清潔;坩堝空白差值為0.01~0.04μg/g,對于0.10μg/g附近的超低含量氫的分析,需要單個扣除空白,對于0.19μg/g以上較高含量氫的分析,用平均值扣空白亦可;為使每單個樣品的分析功率落在最佳微小區(qū)域,每次取出坩堝時,均需使樣品熔融后為亮球狀態(tài)最佳,一般分析功率控制在1 100~1 300kW之間。按照實驗方法對鋁合金標準樣品進行測定,8次平行測定結果的相對標準偏差(RSD)為4.1%,測定值為(0.19±0.029)μg/g,比該標樣證書給出的(0.19±0.04)μg/g更好,且每個點均不超差。方法可以準確測定低至0.09μg/g鋁中總氫或全氫。
[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 鹵0. 029 渭 g / g, which is better than that given by the standard sample certificate of 0. 19 鹵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.
【作者單位】： 中國科學院金屬研究所;沈陽鑄造研究所;
【分類號】：TG115.25
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本文編號：1634104