镁铝铬质耐火材料的X射线荧光光谱分析  

XRFS ANALYSIS OF Mg-Al-Cr REFRACTORIES

作　　者：宋祖峰[1] 阚斌[1] 陈健[1] 

机构地区：[1]马钢技术中心,马鞍山243000

出　　处：《理化检验（化学分册）》2005年第9期648-650,653,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：将XRFS法应用于Mg-Al-Cr耐火材料中10元素(包括主成分及微量组分)的同时测定。对分解试样的熔剂作了系统研究,发现以1∶1混合的四硼酸锂和偏硼酸锂具有最佳熔融效果,所得熔块光滑透明而均匀。选定的熔融温度和时间为1 150℃和15 min。试样和熔剂的质量比以1∶8为好,所得试样在熔剂中的分散度(浓度)适当,可同时适合试样中高、低含量组分的测定,采用熔融法分解试样的方法有效地消除了试样的粒度效应。对仪器工作条件(包括X-光管的电流及电压、分光晶体的选用等)进行了试验并选定最佳条件,使各元素测定所要求的灵敏度和准确度得到满足。此外,采用理论α系数校正法克服了基体吸收及增强效应。用4个标准样品按所提出的方法进行分析,以考核方法的精密度和准确度。10元素的测定结果与其标准值完全相符。XRFS was applied to the simultaneous determination of 10 components （including major and minor elements and also elements of micro quantities） in Mg-Al-Cr refractories. By a thorough study on the choice of flux, a mixture of lithium tetraborate （Li2 B4 O7 ） and lithium metaborate （LiBO2） in the ratio of 1 to 1 was found to be the best mixed flux for the dissolution of Mg-Al-Cr refractory samples （ 1 g） by giving a smooth, transparent and homogeneous melt. The temperature and time of fusion of sample chosen were 1 150 ℃ and 15 min The mass ratio of sample to flux was chosen as 1 to 8, the concentration of which was proved to be suitable for the XRFS determination of both components of macro and micro amounts. The granularity effect in the analysis was eliminated by the fusion method of sample-dissolution. The working conditions of the instrument （including voltage and current of the X-ray tube, the spectroscopic crystal used and etc） were also studied and optimized to meet with the requirements of sensitivity and accuracy of determination. Furthermore, the effects of matrix absorption and enhancement were overcome by correction with the theoratical α-coefficient. The proposed method was tested for its accuracy and precision by analyzing 4 standard samples, and the results obtained were in good conformity with the standard values.

关 键 词：XRFS Mg—Al-Cr耐火材料 混合熔剂 

分 类 号：O657[理学—分析化学]