电感耦合等离子体原子发射光谱法测定WC-Co硬质合金中铪元素含量  

Determination of Hafnium Content in WC-Co Cemented Carbide by Inductively Coupled Plasma Atomic Emission Spectroscopy

作　　者：何帅 颜晓华[1,2,3] 彭宇 刘永中[1,2,3] 苏明 He Shuai;Yan Xiaohua;Peng Yu;Liu Yongzhong;Su Ming(State Key Laboratory of Cemented Carbide,Zhuzhou Hunan 412000,China;Laboratory of Industrial Product(Cemented Carbide and Tungsten Products)Quality Control and Technical Evaluation,Zhuzhou Hunan 412000,China;Zhuzhou Cemented Carbide Group Co.,Ltd.,Zhuzhou Hunan 412000,China)

机构地区：[1]硬质合金国家重点实验室,湖南株洲412000 [2]工业(硬质合金及钨制品)产品质量控制及技术评价实验室,湖南株洲412000 [3]株洲硬质合金集团有限公司,湖南株洲412000

出　　处：《硬质合金》2024年第4期331-336,共6页Cemented Carbides

基　　金：2023年湖南省重大科技攻关“揭榜挂帅”制项目(2023GK2091)。

摘　　要：铪在硬质合金生产中,常作为添加剂以提高硬质合金的力学性能,故而硬质合金中铪含量的准确测定具有重要的意义。现存化学容量法测定硬质合金中铪,存在危险性较大、操作复杂、分析效率低等缺点。本文从样品前处理、分析线的选择、基质效应的探究等方面对硬质合金中铪的测定方法进行了探究,建立了电感耦合等离子体原子发射光谱法测定WC-Co硬质合金中铪含量,该方法具有安全、高效、操作简单、低成本等优点。在选定的条件下,选择体积比1∶1的硫酸、硫酸铵混合液结合柠檬酸和双氧水作为前处理溶剂,选择铪谱线264.141 nm作为分析谱线,利用基质匹配法配制标准溶液,方法校正曲线线性大于0.9999,线性范围为0.0~2.0μg/mL,检出限为0.0084μg/g,加标回收率为99.17%~103.63%,相对标准偏差RSD<0.758%。本方法为WC-Co硬质合金中铪含量的检测提供了可行性方法。In the production of cemented carbides,hafnium is often used as an additive to improve the mechanical properties of cemented carbides.Therefore,accurate determination of the hafnium content in cemented carbides is of great significance.The existing chemical volumetric method for determining hafnium in cemented carbides has the disadvantages of high risk,complex operation,and low analysis efficiency.This article explored the determination method of hafnium in cemented carbides from the aspects of sample pre-treatment,selection of analytical lines,and exploration of matrix effects.It established a method for determining the hafnium content in WC-Co cemented carbides by using inductively coupled plasma atomic emission spectrometry,which was safe,efficient,and simple to operate,at a low cost.Under the selected conditions,a mixed solution with sulfuric acid:ammonium sulfate(1:1)was combined with citric acid and hydrogen peroxide to serve as the pretreatment solvent,and the hafnium spectral line 264.141 nm was selected as the analytical spectral line.The standard solution was prepared using the matrix matching method.The linearity of the method calibration curve was greater than 0.9999,and the linear range was 0.0-2.0µg/mL.The detection limit was 0.0084µg/g,and the recovery rate was 99.17%-103.63%.The RSD was less than 0.758%.This method provided a reliable method for detecting the hafnium content in WC-Co cemented carbides.

关 键 词：WC-CO硬质合金 电感耦合等离子体原子发射光谱法 铪 

分 类 号：O657.31[理学—分析化学] TG115.33[理学—化学]