Abstract：Silver-nickel graphite (AgNiC) is an electrical contact material for medium-load switchgears, and carbon is its main constituent element. It is of great significance to determine carbon content in AgNiC for the performance research and quality control of AgNiC products. After 0.10 g of sample was fused with the flux composed of 0.4 g of pure iron and 1.5 g of multi-component flux, the determination of carbon content in AgNiC was realized by high frequency combustion infrared absorption method. According to the determination range of silver and carbon in standard in progress as well as the content composition of silver, nickel and carbon in two grades of AgNiC electrical contact materials, the synthetic samples of AgNiC with carbon content of 2.00% and 3.00% were prepared with high purity silver, high purity nickel and high purity graphite powder, respectively. The effects of matrix of silver and nickel on the determination of carbon were investigated. The results showed that the determination values of carbon were consistent with the theoretical values, indicating that silver and nickel in the sample almost had no influence on the determination of carbon. The calibration curve of carbon was drawn with the certified reference materials of steel, cast iron, pig iron and calibration samples prepared by cast iron certified reference material and high purity graphite powder. The linear range was 0.81%-8.67% with correlation coefficient of 0.999 8. The limit of detection of method was 0.001 1%, and the limit of quantification was 0.003 3%. The carbon contents in three AgNiC samples were determined according to the proposed method, and the relative standard deviations (RSD,n=9) of determination results were between 0.37% and 0.75%. The determination values of the proposed method were basically consistent with those obtained by gas volumetric method in the industry standard of JB/T 4107.3—2014. The recovery test was carried out by adding the certified reference material for pig iron composition analysis, and the recoveries were between 97% and 103%.
[1] 石平,熊二涛.新型银镍石墨电触头材料的制备及性能[J].机械工程材料,2011,35(10):73-75. SHI Ping,XIONG Ertao.Preparation and properties of a new-style AgNiC electrical contact material[J].Materials for Mechanical Engineering,2011,35(10):73-75. [2] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 27751—2011 银镍石墨电触头技术条件[S].北京:中国标准出版社,2011. [3] 中华人民共和国机械行业标准,中华人民共和国工业和信息化部.JB/T 4107.3—2014 电触头材料化学分析方法 第3部分:银石墨中碳含量的测定[S].北京:机械工业出版社,2014. [4] 殷艺丹,李晖,张健康,等.高频燃烧红外吸收光谱法测定高纯铝粉中碳含量[J].中国无机分析化学,2021,11(1):68-72. YIN Yidan,LI Hui,ZHANG Jiankang,et al.Determination of carbon in high purity aluminum powder by high-frequency combustion infrared absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(1):68-72. [5] 王涛,黄少荣,张庆桂,等.高频燃烧红外吸收光谱法测定铀金属中的碳、硫[J].化学分析计量,2019,28(2):106-110. WANG Tao,HUANG Shaorong,ZHANG Qinggui,et al.Determination of carbon and sulfur in uranium metals by high frequency combustion infrared absorption spectrometry[J].Chemical Analysis and Meterage,2019,28(2):106-110. [6] Tetsuya Ashino,Kunio Takada,Yukitoshi Morinoto,et al.Determination of trace amounts of carbon in high-purity iron by infrared absorption after combustion:pretreatment of reaction accelerator and ceramic crucible[J].Materials Transactions,2000,41(1):47-52. [7] 陈彩霞,李涛,付鹏飞.高频感应燃烧红外吸收法测定硅碳复合负极材料中的碳[J].化学分析计量,2019,28(2):65-67. CHEN Caixia,LI Tao,FU Pengfei.Determination of carbon in silicon-carbon composite anode material by high frequency induction combustion infrared absorption spectrometry[J].Chemical Analysis and Meterage,2019,28(2):65-67. [8] 杨晓倩,谭胜楠,戚振南,等.高频燃烧红外吸收法测定镍基耐蚀合金中碳和硫[J].冶金分析,2020,40(2):46-52. YANG Xiaoqian,TAN Shengnan,QI Zhennan,et al.Determination of carbon and sulfur in nickel-based corrosion resistant alloy by high frequency combustion infrared absorption method[J].Metallurgical Analysis,2020,40(2):46-52. [9] 汪磊,韦建环,蒙益林,等.高频燃烧-红外吸收法测定高纯净度GH4169 高温合金中碳[J].化学分析计量,2021,30(6):39-43. WANG Lei,WEI Jianhuan,MENG Yilin,et al.Determination of carbon in high purity GH4169 superalloy by high frequency combustion infrared absorption method[J].Chemical Analysis and Meterage,2021,30(6):39-43. [10] WEI Jianhuan,YANG Chunsheng,LI Yanchang.Improve carbon-sulfur detection level to adapt to the development of aero-engine[C]//Proceedings of 2019 2nd International Conference on Sustainable Energy,Environment and Information Engineering(SEEIE 2019).Paris:Atlantis Press,2019:58-65. [11] 齐东子,陈东平,沈文杰.高频燃烧-红外分析仪测定海洋沉积物的总碳含量[J].理化检验(化学分册),2019,55(7):791-795. QI Dongzi,CHEN Dongping,SHEN Wenjie.Determination of total carbon in marine sediments by high frequency combustion-infrared analyze[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2019,55(7):791-795. [12] Shigeru Terashima.Determination of total carbon and sulfur in fifty-two geochemical reference samples by combustion and infrared absorption spectrometry[J].Geostandards Newsletter,1988,12(2):249-252. [13] 郑伟,梁清华,魏宏楠,等.高频燃烧红外吸收光谱法测定铪合金中碳[J].中国无机分析化学,2019,9(3):45-47. ZHENG Wei,LIANG Qinghua,WEI Hongnan,et al.Determination of carbon in hafnium alloy by high-frequency combustion infrared absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2019,9(3):45-47. [14] 常国梁,刘攀,张毅.高频感应燃烧-红外吸收光谱法测定蒙乃尔镍铜合金中碳[J].冶金分析,2020,40(7):16-21. CHANG Guoliang,LIU Pan,ZHANG Yi.Determination of carbonin Monel nickel-copper alloy by high frequency induction combustion infrared absorption spectroscopy[J].Metallurgical Analysis,2020,40(7):16-21. [15] 廖思远,甘启达,杜俐颖.高频红外碳硫仪法测银石墨合金中的C含量[J].电工材料,2017(4):20-22. LIAO Siyuan,GAN Qida,DU Liying.C content of silver graphite alloy measured by high frequency infrared carbon sulfur analyzer[J].Electrical Materal,2017(4):20-22. [16] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 27417—2017 合格评定 化学分析方法确认和验证指南[S].北京:中国标准出版社,2017.
