电感耦合等离子体原子发射光谱法测定铌铁中硅磷铝

DETERMINATION OF Si,P AND Al IN FERRIC NIOBIUM BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

铌铁因可以增强钢的强度、韧性,改善焊接性能等而在炼钢生产中被广范应用。已有的铌铁中元素成分检测方法常需要化学分离各元素,操作繁琐,难以满足检测需求。该研究在温度低于60℃的条件下,以铌铁标准样品为研究对象,通过加入纯水和硝酸,并逐滴滴加氢氟酸,同时摇匀的方法将样品消解,对样品的溶解方法、酸的用量进行了选择。通过将标准样品溶解完全,配制成系列标准溶液,绘制工作曲线,选用自动匹配法进行谱线校正,对分析谱线进行了优选,建立了电感耦合等离子体原子发射光谱法(ICP-OES)测定铌铁中硅磷铝含量的方法。实验结果表明,该方法简便、快速,采用该方法检测,标准样品的测定值与标准值相符。各待测元素校准曲线的线性相关系数均大于0.9994。该方法应用于铌铁标准样品的测定,结果的相对标准偏差RSD(n=6)不大于1.91%,加标回收率在96%~105%范围内,结果满意。

Ferric niobium is widely used in steelmaking because it can enhance the strength and toughness of steel and improve the weldability.The existing methods for the detection of elements in ferric niobium often require chemical separation of each element,which is difficult to meet the detection requirements.Under the condition of temperature below 60℃,the standard sample of ferric niobium was taken as the research object,and the sample was dissolved by adding pure water and nitric acid,adding hydrofluoric acid one by one,and shaking well at the same time.The dissolution method and the amount of acid were selected.A new method for the determination of Si,P and Al in ferric niobium by inductively coupled plasma atomic emission spectrometry(ICP-OES)was established by dissolving the standard sample into a series of standard solution,drawing the working curve,selecting the automatic matching method for spectral line correction and optimizing the analytical spectral line.The experimental results show that the method is simple and rapid,and the measured values of the standard samples are in agreement with the standard values.The linear correlation coefficient of calibration curve of each element to be measured is greater than 0.9994.The method was applied to the determination of ferric niobium standard samples.The RSD(n=6)of the results was less than 1.91%,and the recovery rate was in the range of 96%~105%.