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首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Elimination of analytical error due to the use of catch weights with loss-eliminated alphas in X-ray fluorescence spectrometric analysis of limestone using borate fusions
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Elimination of analytical error due to the use of catch weights with loss-eliminated alphas in X-ray fluorescence spectrometric analysis of limestone using borate fusions

机译:消除了在硼酸盐熔融法对石灰石进行X射线荧光光谱分析时使用捕获重量和损失消除的α引起的分析误差

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摘要

In X-ray florescence (XRF) spectrometry, the weight of a sample can be partially lost during the high temperature fusion necessary for the casting of borate glass disks. This weight loss is due to the decomposition of compounds such as carbonates and nitrates, and the subsequent loss of loss-on-fusion (LOF) compounds such as CO_2, NO_2 and O_2,etc. Without a prior experimental determination of LOF, its effects on XRF analysis can be eliminated using special matrix correction coefficients called loss-eliminated alphas (LEAs) or alpha_(ije). Using this method, samples are usually analyzed 'as-received' and the difference between 100% and the measured sum of elemental oxides gives the LOF. The LEAs are dependent on the nominal weights of sample and flux specified for the calculation of LEAs. The effect of the use of catch-weights (CWs; weights other than the nominal weights) on the analysis is generally corrected using a simple proportional correction factor. In contrary to the popular belief that CWs can be satisfactorily used for all sample matrices, the results presented here indicate that the error can be significant (> typical precision) and systematic as in the analysis of limestone where the LOF is approximately 40-45%. However, CWs could be used with a modified LEA value to eliminate the error on the analysis of major elements associated with the lost compounds. The results for the analysis of Standard Reference Material, 1C Argillaceous Limestone, are in good agreement with the certified values.
机译:在X射线荧光(XRF)光谱分析中,在浇铸硼酸盐玻璃圆盘所需的高温熔融过程中,样品的重量可能会部分损失。这种重量损失是由于碳酸盐和硝酸盐等化合物的分解,以及随后的CO_2,NO_2和O_2等熔合损失(LOF)化合物的损失造成的。无需事先对LOF进行实验确定,就可以使用称为损耗消除的alphas(LEA)或alpha_(ije)的特殊矩阵校正系数消除其对XRF分析的影响。使用这种方法,通常按“原样”分析样品,并且100%与元素氧化物的测量总和之差即为LOF。 LEA取决于样品的标称重量和为计算LEA而指定的通量。通常使用简单的比例校正因子来校正使用捕捞重量(CW;除标称重量以外的其他重量)对分析的影响。与普遍认为CW可以令人满意地用于所有样品基体的普遍看法相反,此处给出的结果表明,误差可能是显着的(>典型精度),并且像在石灰岩的LOF约为40-45%的分析中一样是系统的。但是,可以将CW与修改后的LEA值一起使用,以消除分析与丢失化合物相关的主要元素时的误差。标准参比物质1C球状石灰石的分析结果与认证值相符。

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