惰气熔融-红外吸收/热导法测定高纯金属铼中氧、氮元素的含量  

Determination of Oxygen and Nitrogen Elements in High-Purity Metal Rhenium by Infrared Absorption/Thermal Conductivity Method with Inert Gas Fusion

作　　者：杨峥 王子豪 梁钪 郑松波 王桂军 YANG Zheng;WANG Zihao;LIANG Kang;ZHENG Songbo;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 Science and Technology on Aeronautical Materials Testing and Evaluation,Aero Engine Corporation of China,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

出　　处：《理化检验(化学分册)》2025年第1期93-97,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：提出了惰气熔融-红外吸收/热导法测定高纯金属铼中氧、氮元素含量的方法。使用机械装置磨碎高纯金属铼样品,用丙酮进行超声波清洗,晾干,取0.10~0.30 g样品置于镍篮-镍囊中并封口,装入试样孔中进行测定,通过单点校准法建立校准曲线。结果表明,氧、氮元素的质量分数在一定范围内与积分强度呈线性关系,检出限(3s)分别为0.0005%,0.00005%。实际样品测定值的相对标准偏差(n=8)均小于7.0%,按照标准加入法进行回收试验,回收率为83.3%~128%。本方法的测定值和惰气熔融-气相色谱法的基本一致。A method for determination of oxygen and nitrogen elements in high-purity metal rhenium by infrared absorption/thermal conductivity method with inert gas fusion was proposed.The high-purity metal rhenium sample was taken and ground by a mechanical device.The sample was cleaned with acetone by ultrasonic waves and dried.0.10-0.30 g of the sample was taken and placed in a nickel basket with nickel bag.The mixture was sealed and put in the sample hole for determination.The calibration curve was established by the single point calibration method.As shown by the results,linear relationships between the corresponding integral intensities and mass fractions of oxygen and nitrogen elements were kept in definite ranges,with detection limits(3s)of 0.0005%and 0.00005%,respectively.RSDs(n=8)of the determined values of actual samples were less than 7.0%.Test for recovery was made by the standard addition method,giving results in the range of 83.3%-128%.The determined values of this method were basically consistent with those of the inert gas fusion-gas chromatography method.

关 键 词：惰气熔融 红外吸收/热导法 高纯金属铼 氧元素 氮元素 

分 类 号：O657.33[理学—分析化学]