Abstract：Rhenium is widely used as an additive in the production of cemented carbide to improve its toughness. 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 relationship 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 analytical line. The results were consistent with those obtained by GB/T 14352.18-2010. The relative standard deviations (RSD, n=11) of determination results were all less than 1%.
[1] 唐彦渊,钟志强,羊求民,等.碳含量对WC-10Co硬质合金微观组织及力学性能的影响[J].稀有金属与硬质合金,2021,49(6):73-78,93. TANG Yanyuan,ZHONG Zhiqiang,YANG Qiumin,et al.Effect of carbon content on microstructure and mechanical properties of WC-10Co cemented carbides[J].Rare Metals and Cemented Carbides,2021,49(6):73-78,93. [2] TANG Y Y,CHEN L Y,YANG Q M,et al.Effect of a slight change in carbon content near the upper/lower limit on the microstructure and mechanical properties of WC-10Co cemented carbides[J].International Journal of Refractory Metals and Hard Materials,2021,96:105465. [3] TANG Y Y,WANG S N,XU F Y,et al.Effect of carbon content on the properties of inhomogeneous cemented carbides with fine-grained structures produced via one-step transformation[J].Journal of Alloys and Compounds,2021,882:160638. [4] 俞学节.铼、铈对硬质合金性能和组织的影响[J].上海钢研(Shanghai Steel & Iron Research),1991(2):24-27,11. [5] Lisovskii A F.Cemented carbides alloyed with ruthenium,osmium and rhenium[J].Powder Metallurgy and Metal Ceramics,2000,39(9):428-433. [6] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 20225.4—2006硬质合金化学分析方法 钴、铁、镍、锰、钛和钒量的测定 火焰原子吸收光谱法[S].北京:中国标准出版社,2006. [7] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 20225.1—2006 硬质合金化学分析方法 钙、钾、镁和钠量的测定 火焰原子吸收光谱法[S].北京:中国标准出版社,2006. [8] 国家市场监督管理总局,国家标准化管理委员会.GB/T 40347—2021硬质合金化学分析方法 铅量和镉量的测定 火焰原子吸收光谱法和电感耦合等离子体原子发射光谱法[S].北京:中国标准出版社,2021. [9] 国家标准局.YS/T 502—2006钨铼合金中铼的测定 丁二酮肟比色法[S].北京:中国标准出版社,2006. [10] 中华人民共和国信息产业部.SJ 20963—2006钨铼合金中铼含量的测定方法[S].北京:中国标准出版社,2006. [11] 中华人民共和国国家发展和改革委员会.YS/T 372.17—2006贵金属合金素分析方法 钨量和铼量的测定 钨酸重量法和硫脲分光光度法[S].北京:中国标准出版社,2006. [12] 那勃,王伟,崔建军,等.电感耦合等离子体发射光谱法测定金饰品中铼元素[J].贵金属,2022,43(S1):152-156. NA Bo,WANG Wei,CUI Jianjun,et al.Determination of rhenium in gold adornaments by inductively coupled plasma optical emission spectrometry[J].Precious Metals,2022,43(S1):152-156. [13] 朱天一,冯典英,李本涛,等.电感耦合等离子体原子发射光谱法测定镍基单晶高温合金中钨钽铪铼[J].冶金分析,2020,40(4):29-35. ZHU Tianyi,FENG Dianying,LI Bentao,et al.Determination of tungsten, tantalum, hafnium and rhenium in nickel-based single crystal high temperature alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2020,40(4):29-35. [14] 宋祖峰,陆向东,荚江霞,等.电感耦合等离子体原子发射光谱法测定低碳低钛硅铁中痕量铌钒锆[J].冶金分析,2018,38(5):35-40. SONG Zufeng,LU Xiangdong,JIA Jiangxia,et al.Determination of trace niobium, vanadium and zirconium in low carbon and low titanium ferrosilicon by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(5):35-40.
