惰气熔融红外吸收法测定锆及锆合金中痕量氢
Determination of Trace Hydrogen in Zirconium and Zirconium Alloys by Inert Gas Fusion Infrared Absorption Method

锆及锆合金中的氢含量是影响材料性能的关键因素，通过对助熔剂、称样量、分析功率、脱气功率以及仪器校准实验的探讨，建立了锆及锆合金中痕量氢的测定方法。实验使用LECO NH836氮氢分析仪进行分析，在实验过程中，采用气体分析专用石墨套坩埚，并加入0.10~0.20 g分析纯锡粒作为助熔剂。实验优化参数如下：称取0.10~0.20 g的试样、分析功率4000 W、积分时间60 s、脱气功率4500 W。经空白实验计算方法测定下限0.0000356%。根据实验方法对锆合金样品进行分析，氢含量测定结果相对标准偏差(RSD)为7.31%，进行加标回收实验回收率为95%~105%。
^*第一作者。^#通讯作者。Hydrogen content in zirconium and zirconium alloys is a key factor affecting the material properties. A method for the determination of trace hydrogen in zirconium and zirconium alloys was established by exploring flux, weighing volume, analytical power, degassing power and instrument calibration experiments. The experiments were carried out using LECO NH836 nitrogen-hydrogen analyzer, in which a special graphite jacket crucible for gas analysis was used and 0.10~0.20 g of analytically pure tin grains were added as flux. The optimized parameters were as follows: weighing 0.10~0.20 g of specimen, analytical power of 4000 W, integration time of 60 s, degassing power of 4500 W. The lower limit of method determination was calculated as 0.0000356% after blank experiment. The zirconium alloy samples were analyzed according to the experimental method, and the relative standard deviation (RSD) of the hydrogen content was 7.31%, and the recoveries were 95%~105% in the spiked recovery experiments.