脉冲加热惰气熔融-红外吸收法测定高纯金属铬中氢  

Determination of hydrogen in high purity metal chromium by pulse heating inert gas fusion-infrared absorption method

作　　者：杨峥 李蓓 梁钪 陈靖 王桂军 YANG Zheng;LI Bei;LIANG Kang;CHEN Jing;WANG Guijun(AECC Beijing Institute of Aeronautical Materials,Beijing 100095,China;Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Beijing 100095,China;Key Laboratory of Material Testing and Evaluation of China Aviation Engine Group,Beijing 100095,China;Key Laboratory of Materials Testing and Evaluation Aerospace Science and Technology,Beijing 100095,China)

机构地区：[1]中国航发北京航空材料研究院,北京100095 [2]航空材料检测与评价北京市重点实验室,北京100095 [3]中国航空发动机集团材料检测与评价重点实验室,北京100095 [4]材料检测与评价航空科技重点实验室,北京100095

出　　处：《冶金分析》2023年第8期74-78,共5页Metallurgical Analysis

摘　　要：高纯金属铬中氢会导致金属发生点蚀,因此需要严格控制其含量。称取0.05~0.20 g试样,以锡囊为助熔剂,控制分析功率为4500 W,实现了脉冲加热惰气熔融-红外吸收法对块状和碎屑状两种形态高纯金属铬中氢含量的测定,方法可用于分析氢含量小于10μg/g的样品。采用单点校准法,以氢含量尽量接近或略高于未知试样中氢含量为原则,选用钢标准样品502-855绘制氢的校准曲线,并用其他钢标准样品502-416和501-529对校准曲线进行验证,结果表明,测定结果处于标准值的允许范围之内。方法的检出限为0.025μg/g,定量限为0.081μg/g。应用实验方法对块状和碎屑状高纯金属铬试样中的氢含量进行测定,测定结果与脉冲加热惰气熔融-热导法的结果一致,相对标准偏差(RSD,n=8)分别为1.2%和2.5%。在块状和碎屑状高纯金属铬试样中分别加入钢中氢标准样品进行加标回收试验,回收率为97%~106%。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 4500 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 10μg/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 0.025μg/g and 0.081μg/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%.

关 键 词：脉冲加热 惰气熔融 红外吸收法 高纯金属铬 氢 

分 类 号：O659.21[理学—分析化学] O657.33[理学—化学] TF791[冶金工程—钢铁冶金]