能量色散X射线荧光光谱仪在镁砂成分测定中的应用

Application of energy dispersive X-ray fluorescence spectrometer in determination of magnesia composition

能量色散X射线荧光光谱仪(X射线能谱仪)具有体积小、价格低、分析速度快等优点而被广泛应用于高分子、陶瓷、混凝土、生物等材料的成分和形态分析,但是在耐火材料行业没有相关方法标准的规定。为了实现X射线能谱仪对镁砂中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO含量的快速分析,通过优化仪器参数,优选样片制备方法,进行精密度和准确度试验,能谱法和波谱法比对试验。结果表明:以熔铸玻璃片法制取样片,采用X射线能谱仪,可以快速测试镁砂样品中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO的含量,其相对标准偏差为0.09%~1.85%,具有满意的精密度和准确度。能谱法与波谱法的检测差值满足现用标准GB/T 21114—2019规定的允许差要求,数据可靠。

Owning to the advantages of small size,low price,and fast analysis speed,energy dispersive X-ray fluorescence(EDXRF)spectrometers are widely used in the composition and morphology analyses of materials such as polymers,ceramics,concrete,and biomaterials.However,there are no relevant standards in the refractory material industry.To realize the rapid analysis of SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),TiO_(2),CaO and MgO contents in magnesia by the EDXRF spectrometer,the instrument parameters and the sample preparation methods were optimized,and the precision and accuracy tests,as well as the comparison tests by EDXRF and wave length dispersive X-ray fluorescence(WDXRF)spectrometry were conducted.The results show that the contents of SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),TiO_(2),CaO and MgO can be quickly tested by the EDXRF spectrometer through sampling with the fused cast-bead method,with a relative standard deviation of 0.09%-1.85%,showing satisfactory precision and accuracy.The detection difference by EDXRF and WDXRF meets the requirements of the allowable deviation in the current standard GB/T 21114—2019,so the data are reliable.