压片制样-X射线荧光光谱法测定粗铜吹炼炉渣中12种组分

粗铜吹炼炉渣组分的检测没有相应的国家或行业标准可以借鉴,为此实验采用粉末压片法制样,建立了X射线荧光光谱法(XRF)测定粗铜吹炼炉渣组分的方法。通过试验确定分析条件为:磨样时间60s,粒度180目(84μm);压样压力25t;保压时间25s;工作电压电流60kV、50mA。为克服Pb、Sb、Bi组分的校准曲线线性差的问题,利用理论α系数和经验系数法进行了校正,各组分校准曲线的均方根偏差(RMS)和品质因子(K)均满足要求。对同一闪速粗铜吹炼炉渣压制7个压片以进行精密度试验,结果表明,对于质量分数不小于1%的常量组分,测定结果的相对标准偏差(RSD)小于2%;质量分数小于1%的微量组分,测定结果的RSD小于10%。对粗铜吹炼炉渣试样进行分析,测定值与其他方法的测定值基本一致,尽管Cu分析结果偏差较大,但仍能满足炉前快速分析的要求。

Determination of twelve components in crude copper converting slag by X-ray fluorescence spectrometry with pressed powder pellet

There was no corresponding national standard or industrial standard for determination of components in crude copper converting slag. As a result, a determination method of components in crude copper converting slag was established by X-ray fluorescence spectrometry (XRF) with pressed powder pellet. The analytical conditions were obtained as follows by experiments: the sample grinding time was 60 s; the particle size was 180 mesh (84 μm); the sample pressing pressure was 25 t; the pressing time was 25 s; the working current and voltage was 50 mA and 60 kV, respectively. The problem of poor linearity of calibration curves for Pb, Sb and Bi was solved through correction by theoretical α coefficient and empirical coefficient method. The root mean square deviation (RMS) and quality factor (K) of calibration curves of each component could meet the requirements. Seven specimens of the same flash crude copper converting slag were prepared for precision tests. The relative standard deviations(RSDs) were less than 2% for the major components with mass fraction not less than 1%, while the RSDs were less than 10% for the minor components with mass fraction lower than 1%. The crude copper converting slag sample was analyzed according to the experimental method. The results were consistent with those obtained by other methods. Although the determination deviation of Cu was relatively higher, it could still meet the requirements for rapid ladle analysis.