Sample Preparation for X‐Ray Fluorescence Analysis

Marguí, Eva; Queralt, Ignasi

doi:10.1002/9780470027318.a6806m.pub4

Encyclopedia of Analytical Chemistry 2024

DOI: 10.1002/9780470027318.a6806m.pub4

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Sample Preparation for X‐Ray Fluorescence Analysis

Eva Marguí,

Ignasi Queralt

Abstract: The article presents a complete review of different sample preparation methodologies prior to analysis by X‐ray spectrometry ( XRS ) and the basics of classical preparation for X‐ray fluorescence ( XRF ) analysis as well as new methods of preparation, with emphasis on recent applications.

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2024

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Cited by 2 publications

References 152 publications

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Low-Cost and Eco-Friendly Calcium Oxide Prepared via Thermal Decompositions of Calcium Carbonate and Calcium Acetate Precursors Derived from Waste Oyster Shells

Seesanong,

Seangarun,

Boonchom

et al. 2024

Materials

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Waste oyster shells were utilized to produce calcium carbonate (CaCO3) by grinding. This CaCO3 was then reacted with acetic acid to yield calcium acetate monohydrate (Ca(CH3COO)2·H2O). Both CaCO3 and Ca(CH3COO)2·H2O were used as precursors for synthesizing calcium oxide (CaO) through thermal decomposition at 900 °C and 750 °C, respectively. The yields of CaO from both precursors, determined through calcination experiments and thermogravimetric analysis (TGA), exceeded 100% due to the high purity of the raw agents and the formation of calcium hydroxide (Ca(OH)2). X-ray fluorescence (XRF) analysis revealed a CaO content of 87.8% for CaO-CC and 91.5% for CaO-CA, indicating the purity and contamination levels. X-ray diffraction (XRD) patterns confirmed the presence of CaO and minor peaks of Ca(OH)2, attributed to moisture adsorption. Fourier-transform infrared (FTIR) spectroscopy identified the vibrational characteristics of the Ca-O bond. Scanning electron microscopy (SEM) showed similar morphologies for both CaO-CC and CaO-CA, with CaO-CA displaying a significant amount of rod-like crystals. Based on these results, calcium acetate monohydrate (CA) is recommended as the superior precursor for synthesizing high-purity CaO, offering advantages for various applications.

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Low-Cost and Eco-Friendly Calcium Oxide Prepared via Thermal Decompositions of Calcium Carbonate and Calcium Acetate Precursors Derived from Waste Oyster Shells

Seesanong,

Seangarun,

Boonchom

et al. 2024

Materials

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New Strategies in Archaeometric Provenance Analyses of Volcanic Rock Grinding Stones: Examples from Iulia Libica (Spain) and Sidi Zahruni (Tunisia)

Casas,

Di Febo,

Anglisano

et al. 2024

Minerals

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Archaeometry can help archaeologists in many ways, and one of the most common archaeometric objectives is provenance analysis. Volcanic rocks are often found in archaeological sites as materials used to make grinding tools such as millstones and mortars or as building materials. Petrographic characterization is commonly applied to identify their main mineralogical components. However, the provenance study of volcanic stones is usually undertaken by comparing geochemical data from reference outcrops using common descriptive statistical tools such as biplots of chemical elements, and occasionally, unsupervised multivariate data analysis like principal component analysis (PCA) is also used. Recently, the use of supervised classification methods has shown a superior performance in assigning provenance to archaeological samples. However, these methods require the use of reference databases for all the possible provenance classes in order to train the classification models. The existence of comprehensive collections of published geochemical analyses of igneous rocks enables the use of the supervised approach for the provenance determination of volcanic stones. In this paper, the provenance of volcanic grinding tools from two archaeological sites (Iulia Libica, Spain, and Sidi Zahruni, Tunisia) is attempted using data from the GEOROC database through unsupervised and supervised approaches. The materials from Sidi Zahruni have been identified as basalts from Pantelleria (Italy), and the agreement between the different supervised classification models tested is particularly conclusive. In contrast, the provenance of the materials from Iulia Libica remained undetermined. The results illustrate the advantages and limitations of all the examined methods.

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Sample Preparation for X‐Ray Fluorescence Analysis

Cited by 2 publications

References 152 publications

Low-Cost and Eco-Friendly Calcium Oxide Prepared via Thermal Decompositions of Calcium Carbonate and Calcium Acetate Precursors Derived from Waste Oyster Shells

Low-Cost and Eco-Friendly Calcium Oxide Prepared via Thermal Decompositions of Calcium Carbonate and Calcium Acetate Precursors Derived from Waste Oyster Shells

New Strategies in Archaeometric Provenance Analyses of Volcanic Rock Grinding Stones: Examples from Iulia Libica (Spain) and Sidi Zahruni (Tunisia)

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