Determination of hydrogen in high purity metal chromium by pulse heating inert gas fusion-infrared absorption method
YANG Zheng1,2,3,4, LI Bei1,2,3,4, LIANG Kang*1,2,3,4, CHEN Jing1,2,3,4, WANG Guijun1,2,3,4
1. AECC Beijing Institute of Aeronautical Materials,Beijing 100095, China; 2. Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Beijing 100095, China; 3. Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation,Beijing 100095, China; 4. Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation, Beijing 100095, China
Abstract：The hydrogen in high purity metal chromium will cause pitting corrosion of the metal, so its content should be controlled strictly. In experiments, 0.05-0.20 g of sample was fused using tin capsules as the flux. The analysis power was controlled at 4 500 W. The determination of hydrogen content in massive and detrital high purity metal chromium by pulse heating inert gas fusion-infrared absorption method was realized. This method was applicable for the analysis of samples with hydrogen content less than 10 μg/g. A single point calibration method was used to draw the calibration curve of hydrogen with steel standard sample 502-855 (the principle is that the hydrogen content should be close to or slightly higher than that in the unknown sample), and other steel standard samples 502-416 and 501-529 were used to verify the calibration curve. The results showed that the measured results were within the allowable range of standard values. The limit of detection and limit of quantification was 0.025 μg/g and 0.081 μg/g, respectively. The proposed method was applied for the determination of hydrogen content in massive and clastic in high purity metal chromium samples, and the found results were consistent with those obtained by pulse heating inert gas fusion-thermal conductivity method. The relative standard deviation (RSDs, n=8) was 1.2% and 2.5%, respectively. The hydrogen standard samples in steel were added to the massive and detrital high purity metal chromium samples for the standard addition recovery tests. The spiked recoveries were between 97% and 106%.
杨峥, 李蓓, 梁钪, 陈靖, 王桂军. 脉冲加热惰气熔融-红外吸收法测定高纯金属铬中氢[J]. 冶金分析, 2023, 43(8): 74-78.
YANG Zheng, LI Bei, LIANG Kang, CHEN Jing, WANG Guijun. Determination of hydrogen in high purity metal chromium by pulse heating inert gas fusion-infrared absorption method. , 2023, 43(8): 74-78.
[1] 刘质彬,赖灿伟,农彬艺,等.铬含量对Ni-10Al-xCr-0.6Y2O3合金高温抗氧化性能及室温力学性能的影响[J].机械工程材料,2018,42(3):67-73. LIU Zhibin,LAI Canwei,NONG Binyi,et al.Effect of chromium content on high temperature oxidation resistance and room temperature mechanical properties of Ni-10Al-xCr-0.6Y2O3 alloy[J].Materials for Mechanical Engineering,2018,42(3):67-73. [2] Daniel S N,Ding W C,Jacques P T,et al.Effect of Cr additions on a γ-γ' microstructure and creep behavior of a Co-based superalloy with low W content[J].Materials Science and Engineering,2020,778:139108. [3] 魏国华.氢对金属氧化膜的影响[D].武汉:华中科技大学,2013. [4] 陈长风,于浩波,郑树启.氢在Cr2O3中扩散机制的第一性原理研究[J].中国科学,2011,41(1):25-31. CHEN Changfeng,YU Haobo,ZHENG Shuqi.First principles study of hydrogen diffusion mechanism in Cr2O3[J].Science China Technological Sciences,2011,41(1):25-31. [5] 第一重型机器厂中心试验室.真空加热微压法定氢仪钢——氢的测定[J].机械工程师(Mechanical Engineer),1974(1):49-53. [6] 宋忠训.脉冲色谱法测定金属铬中的氢[J].分析试验室,1996(2):83-85. SONG Zhongxun.Determination of hydrogen contents in chromium by impulse heating gas chromatography[J].Chinese Journal of Analysis Laboratory,1996(2):83-85. [7] 刘攀,张毅,张健豪,等.脉冲加热-惰气熔融-热导法测定B30铜镍合金中氢[J].冶金分析,2022,42(11):37-43. LIU Pan,ZHANG Yi,ZHANG Jianhao,et al.Determination of hydrogen in B30 cupronickel alloy by pulse heating-inert gas fusion-thermal conductivity method[J].Metallurgical Analysis,2022,42(11):37-43. [8] 赵飞,杨军红,翟通德,等.惰气脉冲熔融热导法测定铌钛合金中氢含量[J].中国无机分析化学,2017,7(2):15-17. ZHAO Fei,YANG Junhong,ZHAI Tongde,et al.Determination of hydrogen content in niobium-titanium alloy by inert gas impulse fusion heat conductivity method[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):15-17. [9] 钟华.脉冲加热-红外吸收光谱法测定钒铝合金中氢[J].中国无机分析化学,2013,3(2):56-59. ZHONG Hua.Determination of hydrogen in vanadium-aluminum alloy by pulse heating-infrared absorption method[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(2):56-59. [10] 王宽,高东旭,王芳,等.惰气熔融-红外吸收法测定钽钨合金中氢[J].冶金分析,2022,42(4):34-37. WANG Kuan,GAO Dongxu,WANG Fang,et al.Determination of hydrogen in tantalum-tungsten alloy by inert gas fusion-infrared absorption method[J].Metallurgical Analysis,2022,42(4):34-37. [11] 马琪,朱秀慧,王博,等.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 Xiuhui,WANG Bo,et al.Determination of hydrogen in tungsten alloy by inert gas pulse fusion infrared absorption method[J].Metallurgical Analysis,2020,40(9):53-56.
