波长色散X射线荧光光谱法测定硫精矿中铁、硫、砷、铅、锌

Determination of Iron,Sulfur,Arsenic,Lead and Zinc in Sulfur Concentrate by Wavelength Dispersive X-ray Fluorescence Spectrometry

硫精矿作为硫铁矿烧渣的主要原料,铁、硫、铅、锌、砷等元素含量直接影响产品硫铁矿烧渣的质量。在对硫精矿多种元素进行同时分析过程中,传统化学分析存在一定滞后性,对指导生产存在一定的限制。为快速取得可靠结果,实验采用粉末压样,波长色散X射线荧光光谱法(WD-XRF)同时测定硫精矿中铁、硫、砷、铅、锌,根据样品中硫元素含量的差距建立三条工作曲线,采用经验系数法对各曲线进行基体效应校正,同时启用X荧光仪条件选择程序(APS),样品初测后,仪器根据硫的计数率自动选择适宜的工作曲线再测一次出具最终结果。实验发现,粒度74μm的样品在压力为40t、保压25s条件下制备的样片能有效改善粒度效应对荧光强度的影响。方法用于实际样品分析,铁、硫、砷、铅、锌的相对标准偏差(RSD,n=11)分别为0.18%~0.20%、0.24%~0.26%、2.0%~3.9%、4.3%~4.5%、1.8%~2.0%,分析结果和传统化学分析方法结果一致。

Sulfur concentrate is the main raw material for pyrite cinder,the content of iron,sulfur,lead,zinc,arsenic and other elements directly affects the quality of the product pyrite cinder.In the process of simultaneous analysis of multiple elements in sulfur concentrate,there is a certain lag in traditional chemical analysis,which has certain limitations in guiding production.To quickly obtain reliable results,the experiment used powder tablet preparation and wavelength dispersive X-ray fluorescence spectroscopy(WD-XRF) to simultaneously determine iron,sulfur,arsenic,lead,and zinc in sulfur concentrate.Three working curves were established based on the difference in sulfur element content in the sample,and the matrix effect correction was performed on each curve using the empirical coefficient method.At the same time,the X-ray fluorescence instrument condition selection program(APS) was used.After the initial sample testing,the instrument automatically selects a suitable working curve based on the sulfur counting rate and conducts another measurement to produce the final result.The experiment found that the sample with a particle size of 74 μm,prepared under pressure of 40 t and holding for 25 s,can effectively improve the influence of particle size effect on fluorescence intensity.The method is used for actual sample analysis,and the relative standard deviations(RSD,n=11) of iron,sulfur,arsenic,lead,and zinc are 0.18%-0.20%,0.24%-0.26%,2.0%-3.9%,4.3%-4.5%,and 1.8%-2.0%,respectively.The analysis results are consistent with those of traditional chemical analysis methods.