Abstract
A new X-ray fluorescence (XRF) method is proposed for sample preparation and impurity quantification for elements heavier than sodium in carbon materials. The analysis is suitable for various materials including amorphous ones, such as petroleum cokes, with an impurity content higher than 0.01%. We compared a new method with the regular additive method to measure impurities in electrode graphite and petroleum coke. The XRF-based method provides the same sensitivity and accuracy and much greater reproducibility of the analysis results for variations in the sample mass, its density, and coverage by exciting X-ray radiation. The method does not require changes in the instrument software and is easily implemented on commercial analytical equipment.
Highlights
It is often necessary to quantitatively determine the impurities of heavy metals and rock-forming elements in materials of various nature, without directly destructing them.[1−5] A certain approach is required when working with carbon-based materials.[6−8] Most often, in this case, one has to deal with soot,[9] graphite,[10−12] nanotubes, petroleum cokes, and coals.[13−15] Typical values of the content of trace elements in carbon materials of various types are in limits 10−1500 ppm.[16]
It is highly resistant to variations in sample preparation and allows us to find the absolute content of all detected elements by adding one of them
Let us assume that we have a common X-ray fluorescence (XRF) analysis data of a certain carbon material for the content of elements heavier than sodium in the fundamental parameter mode (FPM1)
Summary
It is often necessary to quantitatively determine the impurities of heavy metals and rock-forming elements in materials of various nature, without directly destructing them.[1−5] A certain approach is required when working with carbon-based materials.[6−8] Most often, in this case, one has to deal with soot,[9] graphite,[10−12] nanotubes, petroleum cokes, and coals.[13−15] Typical values of the content of trace elements in carbon materials of various types are in limits 10−1500 ppm.[16]. The classic approach to solve this problem is to preburn the sample, dissolve the residue in a mixture of concentrated acids, and determine the elements using one of the conventional analysis.[17−19] This method has two disadvantages. Sample preparation requires a specially equipped workplace.[20−22] Second, many elements (mercury, lead, or sulfur) partially volatilize during combustion.[23−25] These problems limit the use of the methods for educational purposes in educational and scientific laboratories.[26] The only method for the rapid and direct detection of elements heavier than sodium without prior destruction of the material is X-ray fluorescence (XRF). This article is devoted to the practical application of the said method and its comparison with the classical variants
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