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电感耦合等离子体原子发射光谱法测定WC-Co硬质合金中铼

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在硬质合金生产中,铼元素被广泛应用于提高硬质合金韧性的添加剂.铼元素因价格高昂且添加量要求精准,为此,准确测定硬质合金中的铼含量具有重要意义.实验利用氟离子可与钨结合形成络合物的特性,采用硝酸-氢氟酸体系消解样品从而避免了钨酸的析出,以基体匹配法绘制校准曲线克服基体效应,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定WC-Co硬质合金中铼含量的方法.在选定的实验条件下,分别选择Re 221.426 nm和Re 227.525 nm为分析谱线,铼质量浓度与其对应的发射强度呈良好的线性关系,线性范围为1.0~20.0 μg/mL,线性相关系数分别为0.999 98和0.999 93;方法检出限分别为0.000 048%和0.000 054%;定量限分别为0.000 16%和0.000 18%.按照实验方法选用Re 221.426 nm为分析谱线测定5个WC-Co硬质合金样品中铼的含量,测定结果与国标法GB/T 14352.18-2010相吻合,测定结果的相对标准偏差(RSD,n=11)均小于1%.
Determination of rhenium in WC-Co cemented carbide by inductively coupled plasma atomic emission spectrometry
Rhenium is widely used as an additive in the production of cemented carbide to improve its tough-ness.Due to the high price of rhenium and the requirement of precision addition,it is of great significance to determine accurately rhenium content in cemented carbide.Based on the characteristic that fluorine ion could combine with tungsten to form a complex,the sample was digested by nitric acid and hydrofluoric acid system to avoid the precipitation of tungstic acid.The calibration curve was drawn by matrix matching method to eliminate matrix effect.Consequently,a method for determination of rhenium content in WC-Co cemented carbide was established by inductively coupled plasma atomic emission spectrometry(ICP-AES).Under the selected experimental conditions,the mass concentration of rhenium showed good linear rela-tionship with its corresponding emission intensity with Re 221.426 nm and Re 227.525 nm as the analytical lines,respectively.The linear range was 1.0-20.0 μg/mL,and the linear correlation coefficients were 0.999 98 and 0.999 93,respectively.The limit of detection were 0.000 048%and 0.000 054%,and the limit of quantification were 0.000 16%and 0.000 18%,respectively.The contents of rhenium in 5 WC-Co cemented carbide samples were determined according to the proposed method with Re 221.426 nm as ana-lytical line.The results were consistent with those obtained by GB/T 14352.18-2010.The relative stand-ard deviations(RSD,n=11)of determination results were all less than 1%.

WC-Co cemented carbideinductively coupled plasma atomic emission spectrometry(ICP-AES)rhenium

唐彦渊、何红梅、刘香、钟志强

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崇义章源钨业股份有限公司,江西赣州 341000

WC-Co硬质合金 电感耦合等离子体原子发射光谱法(ICP-AES)

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(3)
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