Assessment of the accuracy of the method of fundamental parameters for XRF analysis of soil samples using an ARL Quant’X energy dispersive spectrometer with the UniQuant software

E. I. Denisov, V. S. Semenishchev, M. V. Voitenko, D. V. Ryansky
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Abstract

X-ray fluorescent (XRF) analysis is one of the most widely used methods for analytical control of soil and rock samples, which allows determining a wide range of elements using a single sample with minimum costs. This work is aimed to expand the XRF capabilities in terms of obtaining calibration dependences for various types of samples. The work presents the results of the experimental assessment of the accuracy of the method of fundamental parameters for analysis of soil samples on a Quant’X energy dispersive spectrometer with the UniQuant software using artificial samples. The suggested methodical approach has shown the potentiality of using a Quant’X energy dispersive spectrometer with the UniQuant software for analysis of soil samples prepared by different methods (fused, pressed and bulk). The systematic deviation from the target value and a random error were estimated. For fused soil samples, deviations from the target value for most of the major components were (1.01) with a random error of 0.01 – 0.06. A Quant’X spectrometer with the UniQuant software allows determining light elements in fused samples with an error of up to 0.06. For the majority of impurity elements, a significant deviation was found, more than one (an underestimation of the determination results by an average of 1.18 times). This requires correction of the results obtained and the analysis error will be determined by values?? ranging from 0.01 to 0.1. In most cases, the deviation from the target value and the error of the element determination decreased as the sample preparation became more complex. After adjustment, bulk soil samples showed the highest error of the analysis results (from 0.1 to 0.2 for the major elements and 0.05 – 0.10 for impurity elements). The detection limits of some elements in fused soil samples were estimated. When the component content in the soil is more than 0.1%, the best option is to analyze fused samples. To determine concentration levels of about 50 ppm, it is proposed to measure pressed samples and take into account the increased error.
评估使用 ARL Quant'X 能量色散光谱仪和 UniQuant 软件对土壤样品进行 XRF 分析的基本参数方法的准确性
X 射线荧光(XRF)分析是土壤和岩石样本分析控制中使用最广泛的方法之一,它允许使用单一样本以最低成本测定多种元素。这项工作旨在扩展 XRF 的能力,以获得各类样品的校准相关性。该工作介绍了利用人工样品,在 Quant'X 能量色散光谱仪上使用 UniQuant 软件分析土壤样品的基本参数方法的准确性实验评估结果。建议的方法显示了使用带有 UniQuant 软件的 Quant'X 能量色散光谱仪分析不同方法制备的土壤样品(熔融、压制和散装)的潜力。对目标值的系统偏差和随机误差进行了估算。对于熔融土壤样品,大多数主要成分与目标值的偏差为(1.01),随机误差为 0.01 - 0.06。使用 Quant'X 光谱仪和 UniQuant 软件可以测定熔融样品中的轻元素,误差不超过 0.06。对于大多数杂质元素来说,偏差都很大,超过了 1(测定结果平均低估了 1.18 倍)。这就需要对所得结果进行修正,分析误差将根据 0.01 至 0.1 之间的数值来确定。在大多数情况下,随着样品制备的复杂化,与目标值的偏差和元素测定的误差都会减小。经过调整后,块状土壤样品的分析结果误差最大(主要元素的误差在 0.1 至 0.2 之间,杂质元素的误差在 0.05 至 0.10 之间)。对熔融土壤样品中某些元素的检测限进行了估算。当土壤中的成分含量超过 0.1%时,最佳选择是分析熔融样品。若要确定约 50 ppm 的浓度水平,建议测量压制样品,并考虑增加的误差。
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