融熔制样-X射线荧光光谱分析测定硅锰中硅、锰、磷

Determination of Si, Mn, P elements in silicomanganese samples by fused bead-x ray fluorescence spectrometry

首先将样品与LiCO3和Li2B4O7熔剂（m（LiCO3）：m（Li2B4O）=1：2）、硝酸锶混合，置于石墨坩埚中，于500℃将包裹试样的滤纸灰化后，逐步升温至850℃熔融制备成融珠，然后以Li：B。O，为熔剂，将融珠置于黄铂金坩埚中，于1100℃熔融制成玻璃熔片，用X-射线荧光光谱分析仪对熔片中Si、Mn、P元素进行同时测定。由于样品进行了预处理，减小了融样对黄铂金坩埚的腐蚀，较好的保护了黄铂金坩埚；同时采用大的熔剂稀释比（1：30）进行高温熔融减小了复杂结构效应，降低共存元素间基体效应影响，并采用理论a系数对的元素间基体效应影响进行校正。本测定方法用于硅锰标样检测，各组分的测定值与认定值相符。

First, the sample was mixed with LiCO3 and Li2B4O7 flux （m （LiCO3）： m （Li2B40） = 1： 2）, strontium nitrate in a graphite crucible, ashed the filters at 500℃ and then fused turning to melt ball at 850 ℃.The melt was mixed with Li2B4O7 flux in a platinum crucible and fused at 1100℃ to formed sample glass pieces after which was used for XRFS determination of Si, Mn, P elements. For the pre-treatment, corrosion to the crucible were reduced. Meanwhile complex structure effect were reduced because of the application of solvent with high dilution ratio, the matrix-effect were reduced among the coexist elements, matrix effect were eliminated by applying the theoratical a coefficient method. This method were utilized in silicomanganese-steel sample analysis, giving results of each group in consistency with the certified values.