高频燃烧红外吸收法测定银镍石墨中碳  

Determination of carbon in silver-nickel graphite by high frequency combustion infrared absorption method

作　　者：徐华 吕长宽 田松 唐碧玉 施意华 XU Hua;Lü Changkuan;TIAN Song;TANG Biyu;SHI Yihua(China Nonferrous Metal(Guilin)Geology and Mining Co.,Ltd.,Guilin 541004,China)

机构地区：[1]中国有色桂林矿产地质研究院有限公司,广西桂林541004

出　　处：《冶金分析》2023年第3期45-51,共7页Metallurgical Analysis

基　　金：广西科学研究与技术开发计划项目(桂科AD20325011)。

摘　　要：银镍石墨(AgNiC)是中等负荷开关电器的电接触材料,碳是其主要构成元素,测定银镍石墨中碳对其产品性能研究和质量控制具有重要意义。选取称样量为0.10 g,以0.4 g纯铁-1.5 g多元助熔剂进行助熔,实现了高频燃烧红外吸收法对银镍石墨中碳的测定。根据在研标准中银、碳的测定范围和两个牌号的银镍石墨电触头材料中银、镍、碳的含量组成,用高纯银、高纯镍和高纯石墨粉配制碳质量分数分别为2.00%和3.00%的银镍石墨合成样品,考察了基体银和镍对碳测定的影响。结果表明,碳测定值和理论值一致,说明样品中银和镍对碳的测定几乎没有影响。采用钢铁、生铸铁、生铁标准物质及由生铸铁标准物质与高纯石墨粉配制的校准样品绘制校准曲线,线性范围为0.81%~8.67%,相关系数为0.9998。方法检出限为0.0011%,定量限为0.0033%。按照实验方法测定3个银镍石墨样品中碳,结果的相对标准偏差(RSD,n=9)为0.37%~0.75%,测定值与行业标准JB/T 4107.3—2014中的气体容量法相符,加入生铁成分分析标准物质进行加标回收试验,回收率为97%~103%。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 0.9998.The limit of detection of method was 0.0011%,and the limit of quantification was 0.0033%.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%.

关 键 词：高频燃烧 红外吸收法 银镍石墨 碳 

分 类 号：O659.2[理学—分析化学] TB33[理学—化学] TF122[一般工业技术—材料科学与工程]