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利用原子发射光谱原理,运用载体分馏效应,在载体存在的条件下利用基体与杂质元素的蒸发特性,电极中实现杂质元素与基体分馏,用直流电弧阳极激发,仪器在激发过程同时进行信号采集和背景校正,完成所有光谱数据的采集。通过大量的试验,选择碳粉、碳酸钠、氧化镓、氟化钠、氧化锗、氧化锌按一定比例混合做载体,采用12A作为工作电流,根据时序分析、扫描峰等确定各元素积分时间、50 s总曝光时间、分析线波长,建立了直流电弧直读光谱仪同时测定钼粉及其化合物中铁、硅等17种杂质元素的分析方法,分析范围为0.5~350μg/g,加标回收率94%~107%,RSD小于17%,满足光谱分析要求。方法快速简便,适用于生产分析。
Using the principle of atomic emission spectrometry, using the carrier fractionation effect, using the evaporation characteristics of the substrate and the impurity elements in the presence of the carrier, the impurity elements and the matrix are fractionated in the electrode, excited by a DC arc anode, and the signal acquisition and Background correction, complete collection of all spectral data. Through a large number of tests, choose carbon powder, sodium carbonate, gallium oxide, sodium fluoride, germanium oxide, zinc oxide as a carrier mixed in a certain proportion, using 12A as the working current, according to time series analysis and scanning peak to determine the integral time of each element, 50 s total exposure time and analysis of line wavelength, a direct current arc direct reading spectrometer was established for the simultaneous determination of 17 impurity elements such as iron and silicon in molybdenum powder and its compounds. The analytical range was 0.5-350 μg / g and the recovery was 94 % ~ 107%, RSD less than 17%, to meet the spectral analysis requirements. The method is quick and easy for production analysis.