Evaluation of the use of polyvinyl alcohol in the manufacture of pressed samples for X-ray fluorescence analysis

A. S. Segrenev, M. E. Prots
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Abstract

The reliability of the results of X-ray fluorescence analysis (XRF), which is widely used in determination of the elemental composition of various materials, largely depends on the quality of sample preparation. When producing pressed tablets for X-ray fluorescence analysis of trace elements, a binder is often used in a powder form, which requires significant time for thorough homogenization. We present the results of applicating a polyvinyl alcohol solution as a binder in the manufacture of pressed samples without using a substrate in determination of microelements by XRF. The parameters for obtaining a durable tablet with a homogeneous composition that matches the condition of minimum impact on the intensity of the analytical lines of the elements being determined are presented. It is shown that the optimal sample weight for the proposed method of producing pressed tablets is 7 g with the addition of polyvinyl alcohol in a ratio of 7:1, the optimal drying time for the tablet after pressing is 1 hour. The calculated variation coefficients of the analytical signal (<2%) indicate the homogeneity of the produced tablets. The maximum values of standard deviations of pressed tablets for the selected ranges of elements are much less than acceptable, which confirms the validity of the proposed method of sample preparation. It is also shown that during long-term storage and repeated measurements, pressed tablets with the polyvinyl alcohol solution retain their original structure and intensity of analytical lines of elements. The accuracy of measurements in the subsequent determination of rock-forming elements is consistent with their certified contents. The results obtained can be used to reduce the time spent on getting a representative pressed sample when using polyvinyl alcohol, determining elements without additional support (coating films), microelement and silicate analyzes from one sample.
评估在制造用于 X 射线荧光分析的压制样品时使用聚乙烯醇的情况
X 射线荧光分析(XRF)广泛用于测定各种材料的元素组成,其结果的可靠性在很大程度上取决于样品制备的质量。在生产用于痕量元素 X 射线荧光分析的压制片剂时,通常使用粉末状的粘合剂,这需要大量时间进行彻底均质。我们介绍了将聚乙烯醇溶液作为粘合剂用于制造压制样品的结果,这种方法在利用 XRF 测定微量元素时无需使用基质。我们提出了获得具有均匀成分的耐用片剂的参数,这些成分应符合对所测定元素的分析线强度影响最小的条件。结果表明,采用所建议的方法生产压制片剂的最佳样品重量为 7 克,添加聚乙烯醇的比例为 7:1,压制后片剂的最佳干燥时间为 1 小时。计算得出的分析信号变异系数(小于 2%)表明所生产的片剂是均匀的。压制片剂在选定元素范围内的最大标准偏差值远远小于可接受值,这证实了所建议的样品制备方法的有效性。实验还表明,在长期储存和重复测量过程中,含有聚乙烯醇溶液的压片仍能保持其原有结构和元素分析线的强度。在随后的成岩元素测定中,测量结果的准确性与其认证含量一致。在使用聚乙烯醇、测定无附加支持物(涂膜)的元素、从一个样品进行微量元素和硅酸盐分析时,所获得的结果可用于减少获得具有代表性的压制样品所花费的时间。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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CiteScore
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