Determination of hydrogen in tungsten alloy by inert gas pulse fusion infrared absorption method
MA Qi1, ZHU Xiu-hui2, WANG Bo2, HE Xia2, WANG Wan-ying2
1. Ordnance Industry Northwestern Physical and Chemistry Testing Center, Xi′an 710043, China; 2. Northwest Industrial Group Metrology Physical and Chemistry First Center, Xi′an 710043, China
Abstract:The introduction of trace hydrogen in the sintering process of tungsten alloy was harmful to the properties of materials. The determination of hydrogen in tungsten alloy by inert gas pulse fusion infrared absorption was studied. By optimizing the analytical power, sample mass, flux and its addition mode, the following conditions were obtained: the U-shaped thick graphite crucible was selected; the analytical power was 4.0kW; the sampling mass was in range of 0.20-0.50g; the nickel flux was directly added into the crucible; after degassing (lower bath material), the tested tungsten alloy sample was put into the crucible. This addition mode could effectively reduce the interference caused by carrier gas, graphite crucible, furnace blank and especially flux. The calibration curve of hydrogen was established with iron and steel reference material. The linear correlation coefficient was 0.9990, and the limit of detection was 0.15μg/g. The precision test of hydrogen in tungsten alloy was carried out, and the relative standard deviations (RSD, n=6) of analysis results were not more than 8.4%. The spiked recovery test was conducted using the mixed powder based on three kinds of tungsten alloy with high hydrogen content. The recoveries were between 94.4% and 105.6%.
马琪, 朱秀慧, 王博, 何侠, 王婉英. 惰气脉冲熔融红外吸收法测定钨合金中氢[J]. 冶金分析, 2020, 40(9): 53-56.
MA Qi, ZHU Xiu-hui, WANG Bo, HE Xia, WANG Wan-ying. Determination of hydrogen in tungsten alloy by inert gas pulse fusion infrared absorption method. , 2020, 40(9): 53-56.
黄劲松,周继承,黄伯云.元素及其化合物对钨基高密度合金性能的影响[J].稀有金属材料与工程,2004,33(5):454-458.HUANG Jin-song,ZHOU Ji-cheng,HUANG Bai-yun.Effects of elements and their compunds on properties of high density alloy[J].Rare Metal Materials and Engineering,2004,33(5):454-458.
[2]
张存信,秦丽柏,米文宇,等.我国穿甲弹用钨合金研究的最新进展与展望[J].粉末冶金材料科学与工程,2006,11(3):127-132.ZHANG Cun-xin,QIN Li-bai,MI Wen-yu,et al.Recent research progress and prospect of armour-piercing projectile in China[J].Materials Science and Engineering of Powder Metallurgy,2006,11(3):127-132.
[3]
王蓬,王海舟.金属中氢的分析技术进展[J].冶金分析,2007,27(3):37-44.WANG Peng,WANG Hai-zhou.Recent progress in analytical technologies of hydrogen in metal[J].Metallurgical Analysis,2007,27(3):37-44.
[4]
杨倩倩,吴振宁,陈雨,等.惰气熔融-热导法测定钕铁硼永磁材料中的氢[J].化学分析计量,2014,23(3):21-24.YANG Qian-qian,WU Zhen-ning,CHEN Yu,et al.Determination of hydrogen in Nd-Fe-B permanent magnet mater by inert gas fusion-thermal conductivity method[J].Chemical Analysis and Meterage,2014,23(3):21-24.
[5]
邹乐西,李英秋,刘钧,等.影响铀铌合金中微量氢测定的因素研究[J].核化学与放射化学,2002,24(1):26-29.ZOU Le-xi,LI Ying-qiu,LIU Jun,et al.Studies of effects on determination of trace hydrogen in U-Nb alloy[J].Journal of Nuclear and Radiochemistry,2002,24(1):26-29.
[6]
马琪,郭增强,蒙娟娟.惰气脉冲熔融-红外吸收法测定钛合金中氢含量的不确定度评定[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2012,48(增刊):403-405.