电感耦合等离子体发射光谱测定钼铝合金中硅含量的方法研究  

Determination of Silicon Content in Molybdenum Aluminum Alloy by Inductively Coupled Plasma Optical Emission Spectrometry

作　　者：罗策[1] 李剑[1] 颜燕[2] 刘婷[1] 康琼 赵武丽 卢凡 LUO Ce;LI Jian;YAN Yan;LIU Ting;KANG Qiong;ZHAO Wuli;LU Fan(BaoTi Group Co.,Ltd.,Baoji 721014;Baoji Education Institute of Shaanxi,Baoji 721000)

机构地区：[1]宝钛集团有限公司,陕西宝鸡721014 [2]陕西省宝鸡教育学院,陕西宝鸡721000

出　　处：《分析科学学报》2021年第5期711-715,共5页Journal of Analytical Science

摘　　要：采用王水、氢氟酸在180℃加热条件下溶解试样,全面分析了硅元素的212.412、221.667、251.611、252.851、288.158 nm五条分析谱线的受干扰情况,最终选择了灵敏度和信噪比较高、受钼基体干扰程度较小的Si 288.158 nm为分析谱线。使用多谱线拟合(MSF)技术建立了Si 288.158 nm的光谱校正模型,通过校正模型对样品检测信号峰进行了校正,消除了基体钼(Mo 288.137 nm)的光谱干扰,建立了电感耦合等离子体发射光谱法(ICP-OES)测定钼铝合金中硅含量的方法。该方法在0.10~5.00 mg/L范围内(对应固体样品中硅的质量分数范围为0.010%~0.50%),硅的工作曲线线性关系良好,相关系数为0.9995;方法检出限和定量限分别为23μg/g和76μg/g;对3个不同含量的钼铝样品中的硅含量进行了测定,测定结果的相对标准偏差(RSD)在0.76%~1.36%之间,加标回收率在98.0%~106%范围,与标准(YS/T 1075.3-2015)中钼蓝分光光度法的测定结果一致。Samples were dissolved by aqua regia and hydrofluoric acid under heating condition of 180℃and the sensitivity,signal-to-noise ratio and interference status of five analytical spectral lines of silicon elements at 212.412 nm,221.667 nm,251.611 nm,252.851 nm and 288.158 nm were analyzed comprehensively.It was found that all spectral lines were interfered by molybdenum matrix.Finally,Si 288.158 nm with higher sensitivity,higher signal-to-noise ratio and lower interference from molybdenum matrix was selected as the analysis spectral line.The spectral correction model of Si 288.158 nm was established by using the multi-spectral line fitting(MSF)technique.The peak of the detected signal was corrected by the correction model,and the spectral interference formed by the matrix molybdenum(Mo 288.137 nm)was eliminated.Then,a method of determination of silicon content in molybdenum aluminum alloy by ICP-OES was established.Within the concentration range of 0.10-5.00 mg/L(the mass fraction of silicon in the corresponding solid sample ranges from 0.010%to 0.50%),the working curve has a good linear relationship and the correlation coefficient is 0.9995.The detection limit and quantitative limit of this method are 23μg/g and 76μg/g,respectively.The silicon content in three molybdenum aluminum alloy samples with different contents was determined and the results were consistent with those of YS/T 1075.3-2015 molybdenum blue spectrophotometry.The relative standard deviation(RSD)of determination results ranged from 0.76%to 1.36%,and the standard recovery was from 98.0%to 106.0%.

关 键 词：电感耦合等离子体发射光谱法 光谱干扰 多谱线拟合 钼铝合金 硅 

分 类 号：O657.31[理学—分析化学]