微波消解-电感耦合等离子体原子发射光谱法测定钴铬钨系合金粉末中钨

doi:10.13228/j.boyuan.issn1000-7571.011496

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摘要钴铬钨系合金常温常压下酸溶分解较为困难。实验利用微波消解提高溶样时的温度和压力,在盐酸、硝酸和氢氟酸介质中使样品充分消解。样品溶解后,定容分取,加入酒石酸溶液,在稀盐酸介质中,以W 207.912 nm为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定钴铬钨系合金中钨的方法。结果表明:共存元素对测定结果基本没有影响。在选定的操作条件下,校准曲线的线性相关系数为0.999 9;钨的检出限为0.002 3%(质量分数)。按照实验方法测定钴铬钨系合金粉末中钨,结果的相对标准偏差(RSD,n=11)小于3%,加标回收率为97.4%～102.3%。

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	罗海霞
	王强

关键词 ：钴铬钨系合金, 钨, 微波消解, 电感耦合等离子体原子发射光谱法(ICP-AES)

Abstract：It is difficult to decompose the cobalt-chromium-tungsten alloy in acid solution under normal temperature and pressure. The microwave digestion was used to increase the temperature and pressure for sample dissolution. The sample was fully digested in the medium of hydrochloric acid, nitric acid and hydrofluoric acid. After dissolution and dilution, tartaric acid solution was added. A method for the determination of tungsten in cobalt-chromium-tungsten alloy powder by inductively coupled plasma atomic emission spectrometry (ICP-AES) in the medium of dilute hydrochloric acid was established using W 207.912 nm as the analytical line. The experimental results showed that the coexisting elements almost had no influence on the determination results. Under the selected operating conditions, the linear correlation coefficient of calibration curve was 0.999 9.Limit of detection of tungsten was 0.002 3% (mass fraction). The proposed method was applied for the determination of tungsten in cobalt-chromium-tungsten alloy powder, and the relative standard deviation (RSD, n=11) of determination results was less than 3%. The spiked recoveries were between 97.4% and 102.3%.

Key words： cobalt-chromium-tungsten alloy tungsten microwave digestion inductively coupled plasma atomic emission spectrometry (ICP-AES)

收稿日期: 2021-04-22

ZTFLH:	O657.31
	TF125.2+12

基金资助:“十四五”国家重点研发计划国家质量基础设施体系专项(2021YFF0602602)

作者简介: 罗海霞(1982—),女,高级工程师,硕士,主要从事地矿及冶金产品的无机元素的分析检测研究;E-mail:haixia0813@126.com

引用本文:

罗海霞, 王强. 微波消解-电感耦合等离子体原子发射光谱法测定钴铬钨系合金粉末中钨[J]. 冶金分析, 2022, 42(2): 40-46. LUO Haixia, WANG Qiang. Determination of tungsten in cobalt-chromium-tungsten alloy powder by inductively coupled plasma atomic emission spectrometry with microwave digestion. , 2022, 42(2): 40-46.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.011496 或 http://yjfx.chinamet.cn/CN/Y2022/V42/I2/40

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