X射线荧光光谱法测定不锈钢中多种元素

采用铣床制样,建立了X射线荧光光谱法(XRF)测定不锈钢中硅、锰、磷、硫、铬、镍、铜、钼、钒、钛、铌、钴元素的分析方法。通过对铣床和磨样机处理样品表面的分析,确定了铣床制备样品表面的最佳参数。对X射线荧光分析仪基本分析条件优化后,绘制了不锈钢样品中碳、硅、锰、磷、硫、铬、镍、铜、铝、钼、钒、钛、铌、钴、钨、钙、砷、锡、铅、锑和铁21个元素的回归曲线,对其中磷、硫、铬、镍、铜和钴元素进行干扰校正后,得到了较为理想的结果。比较了实验方法与火花源原子发射光谱法分析不锈钢中铬和镍元素的精密度,结果表明,实验方法的分析精密度较好。对精密度进行了验证,硅、锰、磷、硫、铬、镍、铜、钼、钒、钴元素的相对标准偏差(n=11)在0.08%~3.8%之间;对不锈钢标准样品进行分析,实验方法的分析结果与湿法或火花源原子发射光谱的测定值吻合较好。

Determination of multi-element in stainless steel by X-ray fluorescence spectrometry

A method for the determination of Si,Mn,P,S,Cr,Ni,Cu,Mo,V,Ti,Nb,Co was established by X-ray fluorescence spectrometry (XRF) with milling machine preparation. The optimal parameters for sample surface preparation by milling machine were determined through analysis of sample surface treatment by miling machine and grinding machine. After the basic analytical conditions of X-ray fluorescence spectrometer were optimized, the regression curves of twenty-one elements in stainless steel sample such as C,Si,Mn,P,S,Cr,Ni,Cu,Al,Mo,V,Ti,Nb,Co,W,Ca,As,Sn,Pb,Sb and Fe were established. After the interference correction for P,S,Cr,Ni,Cu and Co was done, relatively satisfactory results were obtained. The precision of the determination of Cr and Ni in stainless steel by the proposed method and spark source atomic emission spectrometry were compared. It was found that the precision of the proposed method was higher. After precision was validated, the relative standard deviation (RSD,n=11) of Si,Mn,P,S,Cr,Ni,Cu,Mo,V and Co were between 0.08%-3.8%. The stainless steel standard sample was analyzed. The analytical results of the proposed method were consistent with those by wet method or spark source atomic emission spectrometry