热抽取法测定钴块中氢含量(论).pdfVIP

第 23 卷 ，第 6 期 化学分析计量 Vol. 23 ，No.6 56 2014 年 11 月 CHEMICAL ANALYSIS AND METERAGE Nov. 2014 doi ：10.3969／j.issn.1008–6145.2014.06.015 热抽取法测定钴块 中氢含量 王艳霞 ( 中核北方核燃料元件有限公司 ，内蒙古包头市 014035) 摘要 研究了钴块中氢含量的测定方法。采用石英坩埚加载样品，热抽取法进行测定。不加任何助熔剂，分析 功率为100% ，匹配的分析时间为110 s ，比较水平设定为0.1%。在选定的参数下，样品能在完全熔融状态下释放出 n 全部氢。方法加标回收率为80% ～119% ，测定结果的相对标准偏差小于15%( =6) ，检出限为0.5 μg ／g。热抽取法 的精密度优于熔融法的精密度，满足微量气体分析的要求。 关键词 热抽取法；钴块；氢；测定 中图分类号 ：O657.9 文献标识码 ：A 文章编号 ：1008–6145(2014)06–0056–03 Determination of Hydrogen Content in Cobalt Pellets by Heat Extractive Method Wang Yanxia (China North Nuclear Fuel Company ，Baotou 014035, China) Abstract The determination of hydrogen content in cobalt pellet was studied. The sample was loaded by quartz crucible ，and detected by heat extractive method. Without aiding any solvent ，the analytical power was 100% ，the suited analytical time was 110 s and the comparative level was 0.1%. Therefore hydrogen in sample could be released completely under the certain conditions. The recovery rate of the method was 80%– 119% ，the relative standard deviation of detection n results was less than 15% ( =6), and the detection limit was 0.5 μg ／g. The precision of heat extractive method was superrior to that of thermal method. The heat extractive method can meet the analysis requirement of trace gas in metals . Keywords heat extractive method; cobalt pellet; hydrogen; determination 自20 世纪 30 年代在重轨钢 中发现 白点以及在 该法未采用助熔剂（主要是金属锡 ），避免 了锡在加 低合金高强度钢 中发现 内部裂纹等 以后 ，氢在