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投稿时间:2025-02-25 修订日期:2025-02-25
投稿时间:2025-02-25 修订日期:2025-02-25
中文摘要: 针对高纯钽测试过程基体对被测杂质元素干扰的问题,通过将样品湿法消解后经基体分离,消除钽基体对杂质的质谱干扰,建立基体分离-电感耦合等离子体质谱法,测定高纯钽中杂质元素含量。考察基体干扰0~1 000 ng/mL、仪器功率0.8~1.4 kW、采样深度5~9 mm、等离子体气流量7.5~12 L/min、雾化气流量0.6~1.1 L/min等影响因素的干扰情况,确定了最佳分析条件。结果表明,在基体分离,RF功率1.36 kW、采样深度5 mm、等离子气流量9.0 L/min、雾化气流量0.88 L/min条件下,仪器处于最佳分析测试状态,在此条件下Ni、B的校准曲线方程相关系数均大于0.999,检出限(LOD)分别为0.3、1.2 ng/g,加标回收率在96.0%~105%,样品测试相对标准偏差(RSD)<3%(n = 10)。方法检出限低,准确性高,适用于高纯钽中Ni、B杂质元素含量的快速定量测试。
中文关键词: 电感耦合等离子体质谱法 高纯钽 基体分离
Abstract:In view of the interference problem caused by the matrix in the determination of impurity elements during the testing process of high-purity tantalum, a Matrix Separation-Inductively Coupled Plasma Mass Spectrometry (MS) method was developed to measure the content of impurity elements in high-purity tantalum. After wet digestion, the samples were subjected to matrix separation, which effectively eliminated the mass spectrometric interference of the tantalum matrix on impurities. This method examined the interference scenarios of several influencing factors, including matrix interference ranging from 0 to 1000 ng/mL, instrument power from 0.8 to 1.4 kW, sampling depth from 5 to 9 mm, plasma gas flow rate from 7.5 to 12 L/min, and nebulizer gas flow rate from 0.6 to 1.1 L/min, and subsequently determined the optimal analytical conditions. The results demonstrated that under the conditions of matrix separation, with an RF power of 1.36 kW, a sampling depth of 5 mm, a plasma gas flow rate of 9.0 L/min, and a nebulizer gas flow rate of 0.88 L/min, the instrument achieved its optimal analytical and testing state. In this state, the correlation coefficients of the calibration curve equations for both Ni and B exceeded 0.999. The Limits of Detection (LOD) were calculated to be 0.3 ng/g and 1.2 ng/g for Ni and B, respectively. The spiked recoveries ranged from 96% to 105%, and the relative standard deviations (RSD) of sample testing were less than 3% (n = 10). This method features a low limit of detection, and high accuracy, making it highly suitable for the rapid quantitative determination of Ni and B impurity elements in high-purity tantalum.
文章编号: 中图分类号:O657.63; TH843 文献标志码:
基金项目:国防科工局技术基础科研项目
作者 | 单位 | |
巩 琛 | 山东非金属材料研究所 | 919333720@qq.com |
黄辉* | 山东非金属材料研究所 | huanghuicc@sina.com |
张嘉祺 | 山东非金属材料研究所 | 1@QQ.com |
苗世海 | 山东非金属材料研究所,济南 250031 | 1@QQ.com |
李 颖 | 山东非金属材料研究所 | 1@QQ.com |
李本涛 | 山东非金属材料研究所 | 1@QQ.com |
引用文本:
巩 琛,黄辉,张嘉祺,苗世海,李 颖,李本涛.基体分离-电感耦合等离子体质谱法测定高纯钽中Ni、B含量[J].中国无机分析化学,2025,15(3):398-405.
gong chen,huang hui,ZHANG Jiaqi,MIAO Shihai,LI Ying,LI Bentao.Determination of Ni and B Contents in High-purity Tantalum by Inductively Coupled Plasma Mass Spectrometry with Matrix Separation[J].Chinese Journal of Inorganic Analytical Chemistry,2025,15(3):398-405.
巩 琛,黄辉,张嘉祺,苗世海,李 颖,李本涛.基体分离-电感耦合等离子体质谱法测定高纯钽中Ni、B含量[J].中国无机分析化学,2025,15(3):398-405.
gong chen,huang hui,ZHANG Jiaqi,MIAO Shihai,LI Ying,LI Bentao.Determination of Ni and B Contents in High-purity Tantalum by Inductively Coupled Plasma Mass Spectrometry with Matrix Separation[J].Chinese Journal of Inorganic Analytical Chemistry,2025,15(3):398-405.