X射线荧光光谱法测定钒铁合金中钒铝硅锰

Determination of vanadium,aluminum,silicon and manganese in ferrovanadium alloy by X-ray fluorescence spectrometry

采用铂金坩埚直接熔融钒铁合金,存在腐蚀铂金坩埚的危险。实验采用HNO3(1+1)和H2SO4(1+1)先消解钒铁合金,再用熔融制样法将样品浓缩物在铂金坩埚中与四硼酸锂和碳酸锂进行熔融,熔体在铂金坩埚中成型,避免了试样对铂金钳锅的腐蚀。然后以钒铁合金标准样品建立校准曲线,采用OXSAS软件提供的数学模型对谱线重叠效应进行校正,可实现X射线荧光光谱法(XRF)对钒铁合金中V、Al、Si和Mn元素含量的准确测定。精密度试验表明,待测元素的相对标准偏差均低于0.7%(RSD,n=9),能满足钒铁合金中各元素的检测要求。采用实验方法分析钒铁合金标准样品,测定值与认定值吻合良好。

If the ferrovanadium alloy was directly melted in platinum-gold crucible,there were the dangerous for corrosion of platinum-gold crucible.The ferrovanadium sample was firstly digested with HNO_3（1＋1）and H_2SO_4（1＋1）.Then sample concentrates was fused in platinum-gold crucible with lithium tetraborate and lithium carbonate by fusion sample preparation method,and the melt was molded in platinum-gold crucible avoiding the corrosion of platinum-gold crucible by sample.After the calibration curve was established with certified reference material of ferrovanadium alloy and the spectral overlapping effect was corrected by the mathematical model in OXSAS software,the accurate determination of V,Al,Si and Mn in ferrovanadium alloy was realized by X-ray fluorescence spectrometry（XRF）.The precision test results indicated that the relative standard deviations（RSD,n=9）of testing elements were all lower than 0.7%,which could meet the detection requirements for each element in ferrovanadium alloy.Three certified reference materials of ferrovanadium alloy were analyzed according to the experimental method,and the results were well consistent with the certified values.