微波消解-电感耦合等离子体发射光谱法测定钽合金中的硅  

Determination of Silicon in Tantalum Alloy by Microwave Digestion with ICP-AES

作　　者：张浩 佡云 马晓卉 ZHANG Hao;NAO Yun;MA Xiao-hui(CNMC Shenyang Research Institute of Nonferrous Metals Co.,Ltd.,Shenyang 110141,China)

机构地区：[1]沈阳有色金属研究院有限公司,辽宁沈阳110141

出　　处：《有色矿冶》2024年第6期63-66,共4页Non-Ferrous Mining and Metallurgy

摘　　要：钽合金中杂质硅的准确检测对钽合金的质量监控有着重要意义。传统水浴法溶解钽合金速度过慢,检测效率低下,不利于指导生产。本工作采用微波消解法以硝酸,氢氟酸处理钽合金,再使用电感耦合等离子体发射光谱仪(ICP-AES)对硅进行检测,建立了微波消解-电感耦合等离子体发射光谱法测定钽合金中硅的方法。实验首先对钽合金样品的微波消解条件进行了优化,探究了氢氟酸和硝酸用量对钽合金样品消解效率的影响,并对两者的用量进行了优化,最佳用量为4 mL氢氟酸和3 mL硝酸;对硅的分析谱线进行了优化,选择251.612 nm作为分析谱线,在最优化的条件下对钽合金标准样品及一般样品进行了检测。其中,校准曲线线性良好,相关系数为0.999 9。按照实验方法对钽合金标准物质中的硅含量进行检测,检测结果与认定值一致,测定结果的相对标准偏差(RSD,n=3)在2.3%~3.5%之间,表明该方法具有良好的准确度和精密度。按照实验方法测定钽合金样品,测定结果的回收率(n=3)在93.3%~105.0%之间,表明该方法可以用于实际钽合金样品中硅含量的快速准确分析。The accurate detection of impurity silicon in tantalum alloy is of great significance to the quality control of tantalum alloy.The speed of dissolving tantalum alloy by traditional water bath method is too slow,and the detection efficiency is low,which is not conducive to guiding production.In this work,tantalum alloy was treated with nitric acid and hydrofluoric acid by microwave digestion,and silicon was detected by inductively coupled plasma atomic emission spectrometry(ICP-AES).A method for the determination of silicon in tantalum alloy by microwave digestion inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The experiment first optimized the microwave digestion conditions of tantalum alloy samples;then investigated the effect of hydrofluoric acid and nitric acid dosage on the digestion efficiency of tantalum alloy samples,and optimized the dosage by adding 4 mL of hydrofluoric acid,3 mL of nitric acid;The analysis spectral line of silicon was optimized,and 251.612 nm was selected as the analysis spectral line;Under optimized conditions,tantalum alloy standard samples and general samples were tested.Among them,the calibration curve has good linearity,with a correlation coefficient of 0.9999;According to the experimental method,silicon in tantalum alloy standard materials was detected,and the detection results were consistent with the recognized values.The relative standard deviation(RSD,n=3)of the measurement results was between 2.3%and 3.5%,indicating that the method has good accuracy and precision;According to the experimental method,tantalum alloy samples were measured,and the recovery(n=3)of the measurement results was between 93.3%and 105.0%,indicating that this method can be used for the rapid and accurate analysis of silicon in actual tantalum alloy samples.

关 键 词：钽合金 微波消解 电感耦合等离子体发射光谱法 硅 

分 类 号：O657[理学—分析化学]