惰气熔融-红外吸收法测定铜及铜合金中氢  

Determination of hydrogen in copper and copper alloy by inert gas fusion infrared absorption method

作　　者：李绍文 刘攀[2,3,4] 陈倩倩 孟秋达 LI Shaowen;LIU Pan;CHEN Qianqian;MENG Qiuda(Chinalco Luoyang Copper Co.,Ltd.,Luoyang 471039,China;Luoyang Ship Material Research Institute,Luoyang 471023,China;National Key Laboratory for Marine Corrosion and Protection,Luoyang 471023,China;Xiamen Sunrui Material Research Institute Co.,Ltd.,Xiamen 361100,China)

机构地区：[1]中铝洛阳铜加工有限公司,河南洛阳471039 [2]洛阳船舶材料研究所,河南洛阳471023 [3]海洋腐蚀与防护全国重点实验室,河南洛阳471023 [4]厦门双瑞材料研究院有限公司,福建厦门361100

出　　处：《冶金分析》2024年第7期49-54,共6页Metallurgical Analysis

基　　金：国标委2022年第二批推荐性国家标准计划(国标委发[2022]22号20220713-T-610,W20222369)。

摘　　要：氢是铜及铜合金的有害元素,对其进行准确定量分析有助于提升产品质量。针对国内外普遍缺乏铜及铜合金中氢含量的分析方法标准这一问题,在GB/T 5121.8的修订过程中增加了氢元素的分析方法,开展了惰气熔融-红外吸收法测定铜及铜合金中氢含量的分析方法研究和参数优化,确定的分析条件如下:分析功率为2.75 kW,样品量为1~2 g,推荐1 g锡做助熔剂,采用标准型坩埚或套坩埚进行测试,并使用钢铁标准样品建立仪器校准系数。所建立方法的检出限为0.1μg/g,定量限为0.4μg/g。按照实验方法进行测定,并分别加入邻苯二甲酸氢钾和氯化铵标准物质进行加标回收试验,回收率为90%~115%。测定氢含量在2~6μg/g范围内的铜及铜合金样品,测得结果的标准偏差不大于0.5μg/g,相对标准偏差(RSD,n=7)为5.2%~9.1%,测定值与实验室间协同验证数值或热导法相符。Hydrogen is a harmful element in copper and copper alloys.The accurate and quantitative analysis of hydrogen is helpful to improve the product quality.In view of the lack of analytical method standard for hydrogen content in copper and copper alloys in China and abroad,the analysis method of hydrogen was added during the revision of GB/T 5121.8.The analysis method and parameter optimization for the determination of hydrogen in copper and copper alloys by inert gas fusion infrared absorption method were studied.The optimal operating conditions were obtained as below:the analysis power was 2.75 kW;the sample mass was 1-2 g;the flux was 1 g of tin;the standard crucible or duplex crucible was used for testing.The certified reference materials of steel were used to establish the calibration coefficients of the instrument.The limit of detection was 0.1μg/g,and the limit of quantification was 0.4μg/g,respectively.The recovery tests were carried out by adding certified reference material of potassium hydrogen phthalate and ammonium chloride separately according to the experimental method.The recoveries were between 90%and 115%.The proposed method was applied for the analysis of copper and copper alloy samples with hydrogen in range of 2-6μg/g.The standard deviations of determination results were not higher than 0.5μg/g,and the relative standard deviations(RSD,n=7)were between 5.2%and 9.1%.The analysis results were consistent with those verified by inter laboratory study or obtained by thermal conductivity method.

关 键 词：惰气熔融 红外吸收法 光谱 铜 铜合金 氢 锡 

分 类 号：O659.2[理学—分析化学] TF125.211[理学—化学]