Determination of eighteen trace impurities in high purity tungstencarbide powder by inductively coupled plasma mass spectrometry
ZHANG Ying1,2, LI Lin-yuan1,2, ZHANG Lei1,2
1. Analysis and Testing Center of Zhuzhou Cemented Carbide Group Co., Ltd., Zhuzhou 412000, China; 2. State Key Laboratory of Cemented Carbide, Zhuzhou 412000, China
Abstract：High purity tungsten carbide powder was the raw material for the production of ultrafine cemented carbide. It was of great importance for analysis and control of its impurity elements contents. During the determination of impurity elements in high pure tungsten carbide powder by inductively coupled plasma mass spectrometry (ICP-MS), the carbon in sample should be completely oxidized and removed before determination. Or else the insoluble free carbon would cause the blocking of sampling system, leading to the fluctuation of signal intensity and serious interference of determination. The tungsten carbide powder sample was oxidized in muffle furnace at 600-800℃ to remove free carbon. Then the sample was digested with ammonium hydroxide. After the test isotopes and working parameters of instrument were optimized, the contents of calcium, iron, chromium, magnesium, aluminum, manganese, cobalt, nickel and copper were determined by shield torch cool plasma technology, and the contents of arsenic, bismuth, cadmium, molybdenum, lead, antimony, tin, titanium and vanadium were determined at normal mode to eliminate the mass spectral interference. The calibration curve was plotted by matrix matching method of tungsten to overcome the matrix effect. The matrix mass concentration was controlled at 0.5mg/mL. Consequently, a determination method of these eighteen elements in high-purity tungsten carbide powder by ICP-MS was realized. Under the selected working conditions, the linear correlation coefficients of calibration curves for all elements were higher than 0.9995. The detection limits of method were in range of 0.006-0.330μg/g. The experimental method was applied to the determination of eighteen impurities in high-purity tungsten carbide powder samples. The relative standard deviations (RSDs, n=11) were less than 10% except for tin (24%). The results were basically consistent with those obtained by direct-current arc atomic emission spectrometry (ARC-AES). Since the main composition of high-purity tungsten carbide powder sample after oxidization in muffle furnace was tungsten trioxide, eighteen impurities in certified reference material of tungsten trioxide were determined according to the experimental method to verify the trueness of method. The results showed that the determination results were consistent with the certified values.
李盛意,胡明芳,杨国政,等.ICP-AES法测定碳化钨中的高含量钒、铬、钴[J].中国钨业,2013,28(4):44-47.LI Sheng-yi,HU Ming-fang,YANG Guo-zheng,et al.Determining high contented vanadium, chromium and cobalt in tungsten carbide by ICP-AES[J].China TungstenIndustry,2013,28(4):44-47.
张秀香,梁涛,王旭珍,等.标准加入原子吸收法测定碳化钨中微量Fe,Mg,Ca,K和Na的含量[J].烟台师范学院学报:自然科学版,2001,17(4):266-269.ZHANG Xiu-xiang,LIANG Tao,WANG Xu-zhen,et al.Determination of trace Fe,Mg,Ca,K,Na in tungsten carbide by standard addition FAAS[J].Yantai Teachers University Journal:Natural Science,2001,17(4):266-269.
[7]
葛小鹏.碳化钨及其复合物料中痕量砷的测定[J].现代仪器,1999(5):40-41.GE Xiao-peng.Determination of trace arsenic in tungsten carbide sample[J].Modern Instrument,1999(5):40-41.
[8]
荆淼,陈利琴,陈成祥,等.电感耦合等离子体质谱测定高纯仲钨酸铵中磷及其它微量元素[J].分析化学,2009(3):403-406.JING Miao,CHEN Li-qin,CHEN Cheng-xiang,et al.Determination of trace impurities in high purity ammonium paratungstate by inductively coupled plasma mass spectrometry[J].Chinese Journal of Analytical Chemistry,2009(3):403-406.
[9]
钟道国,潘建忠,刘鸿.纯钨制品中杂质的ICP-MS测定方法研究[J].中国钨业,2009,24(1):43-46.ZHONG Dao-guo,PAN Jian-zhong,LIU Hong.Determination of impurities in tungsten products by inductively coupled plasma-mass spectrometry[J].China Tungsten Industry,2009,24(1):43-46.
[10]
张颖,熊静.电感耦合等离子体质谱法测定高纯钨中26种痕量杂质元素[J].硬质合金,2014,31(5):309-314.ZHANG Ying,XIONG Jing.Determination of 26 trace impurities elements in high purity tungsten by inductively coupled plasma mass spectrometry[J].Cemented Carbide,2014,31(5):309-314.
[11]
刘洁,陈忠颖,刘巍,等.电感耦合等离子体质谱法测定高纯铌中20种痕量杂质元素[J].理化检验:化学分册,2018,54(10):1158-1162.LIU Jie,CHEN Zhong-ying,LIU Wei,et al.Determination of 20 trace impurities elements in high purity niobium by inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(10):1158-1162.
