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    烧失量修正的粉末压片-波长色散X射线荧光光谱法快速测定高烧失量锰矿石中主、次量元素

    Rapid Determination of Major and Minor Elements in High Loss-on-Ignition Manganese Ore by Wavelength Dispersive X-Ray Fluorescence Spectrometry with Pressed Powder after Correction with Loss-on-Ignition

    • 摘要: 为解决粉末压片-波长色散X射线荧光光谱法测定高烧失量锰矿石中元素含量时准确度较低的问题,进行了题示研究。样品于105 ℃预干燥2 h,再于1 000 ℃灼烧至恒重,利用灼烧前后样品量差值计算烧失量。冷却后,将样品研磨成粒径不大于74 μm的粉末,分取约10 g,压成直径34 mm的样片,采用波长色散X射线荧光光谱仪测定,基本参数法消除谱线重叠干扰和基体干扰,烧失量修正测定结果。结果显示,系列锰矿石国家有证标准物质中11种主、次量元素氧化物的荧光强度和烧失量修正后的认定值在一定范围内呈线性关系,检出限为0.001 5%~0.008 4%。方法用于不同浓度梯度样品和标准物质的分析,MnO、SiO2、Fe2O3、CaO、BaO、TiO2、K2O测定值的相对标准偏差(RSD,n=7)在10%以内,Al2O3、MgO、Na2O、P2O5测定值的RSD (n=7)在20%内;11种目标元素氧化物的测定值和GB/T 24519—2009中熔融制样-波长色散X射线荧光光谱法的一致。

       

      Abstract: A study mentioned by the title was conducted to address the issue of low accuracy in the determination of element content in high loss-on-ignition manganese ore using wavelength dispersive X-ray fluorescence spectrometry. The sample was pre-dried at 105 ℃ for 2 h, and then burned at 1 000 ℃ to a constant weight. The loss-on-ignition was calculated based on the difference in sample mass before and after burning. After cooling, the sample was ground to the powder with particle size of no more than 74 μm, and 10 g of the powder was taken, and pressed into sample pieces with diameter of 34 mm for determination by wavelength dispersive X-ray fluorescence spectrometer, eliminating spectral line overlap interference and matrix interference with basic parameter method, and correcting the determination results with loss-on-ignition. As found by results, linear relationships between values of the fluorescence intensity of the 11 major and minor element oxides in a series of national certified reference materials for manganese ore and certified values corrected by ignition-on-loss were kept in definite ranges, with detection limits in the range of 0.001 5%-0.008 4%. The proposed method was used for the analysis of samples and reference materials with different concentration gradients, and RSDs (n=7) of determined values of MnO, SiO2, Fe2O3, CaO, BaO, TiO2, and K2O were within 10%, while RSDs (n=7) of determined values of Al2O3, MgO, Na2O, and P2O5 were within 20%. The determined values of 11 target element oxides were consistent with those given by the wavelength dispersive X-ray fluorescence spectrometry with fusion sampling in GB/T 24519—2009.

       

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