全谱直流电弧发射光谱法同时测定钼样品中17种杂质元素

为了解决现有测定方法中样品前处理复杂、测定过程繁琐的问题,研究了直流电弧发射光谱法测定钼样品中Al、Bi、Ca、Cd、Co、Cr、Cu、Fe、Mg、Mn、Ni、Pb、Sb、Si、Sn、Ti、V等17种元素的方法。用石墨粉(98%)、碳酸钠(1%)和氟化钠(1%)作为光谱缓冲剂抑制基体元素蒸发、稳定弧焰、促进杂质元素的蒸发;采用样品装满电极后下压2 mm和滴加蔗糖乙醇水溶液(2%)的方式,防止喷溅的发生,稳定激发过程,减小基体干扰;对挥发难易程度不同的元素采用信号分段采集的方式,提高各元素信噪比。方法灵敏度高、分析速度快、操作简便,加标回收率为85%~120%,各元素分析精密度均小于15%。

Simultaneous Determination of 17 Impurity Elements in Molybdenum Sample by Full Spectrum DC Arc Emission Spectrometry

In order to solve the problems of complex sample pretreatment and complicated determination process in existing determination methods, a method for the determination of 17 elements such as Al, Bi, Ca, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sb, Si, Sn, Ti, V in molybdenum sample by DC arc emission spectrometry was studied. 98% graphite powder, 1% sodium carbonate and 1% sodium fluoride were used as spectral buffers to inhibit the evaporation of matrix elements, stabilize arc flame and promote the evaporation of impurity elements. Samples filled with electrodes were pressed down for 2 mm and 2% sucrose ethanol aqueous solution was added to prevent splashing, stabilize the excitation process and reduce matrix interference. The signal-to-noise ratio of elements was improved by means of segmented signal acquisition for different volatilization difficulty. The method had high sensitivity, fast analysis speed and simple operation. The recovery of standard addition was 85%~120%, and the precision of each element was less than 15%.