Multielement analysis of continental and lacustrine ferromanganese nodules by WDXRF, TXRF, and ICP-MS methods. Intercomparison study and accuracy assessment

Чубаров, В. М.; Pashkova, Galina V.; Panteeva, Svetlana V.; Amosova, Alena A.

doi:10.1016/j.apradiso.2021.109981

Cited by 4 publications

(3 citation statements)

References 49 publications

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“…Calibration curves were constructed, and accuracy testing was carried out using the geological reference materials of sedimentary, ultramafic, and mafic rocks. This technique was previously successfully applied for the elemental analysis of rocks and sediments [33,34];…”

Section: Description and Preliminary Preparation Of Ceramic Samples F...mentioning

confidence: 99%

A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

et al. 2023

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In this study, the assessment of uncertainties introduced at different stages of the elemental analysis of archaeological ceramics has been described using the example of the Neolithic pottery sherds from Popovsky Lug (eastern Siberia). To evaluate the uncertainty introduced by sampling due to ceramic heterogeneity, three original sherds were cut into small subsamples. Powdered subsamples (250–350 mg) were analyzed using wavelength-dispersive X-ray fluorescence and inductively coupled plasma mass spectrometry methods, and the variations between analytical results for independent subsamples were compared with the variations introduced during the analytical process (measurement and sample preparation). It was shown that 250–350 mg of ceramic is sufficient to obtain good reproducibility (2–15%) between separate subsamples for most major and trace elements, even for the heterogeneous Neolithic ceramics included in this study. The differing behavior of concentration variations in some elements was explained by measuring the ceramic cross-sections by scanning electron microscopy and micro-X-ray fluorescence spectrometry, as well as by the theoretic modeling of the sampling error. The described workflow can be useful in finding uncertainties in elemental analysis results, which may affect the interpretation of bulk chemical composition in ceramic provenance studies.

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Section: Description and Preliminary Preparation Of Ceramic Samples F...mentioning

confidence: 99%

A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

et al. 2023

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“…TXRF can be applied for direct analysis of iron, manganese, ferromanganese, nickel-copper sulfide ores, oceanic and lacustrine nodules [Pashkova et al, 2020;Akhmetzhanov et al, 2021;Chubarov et al, 2021]. The suspension preparation (5 mL of 1 % Triton X-100 solution and 20 mg of fine powder with a size <10 μm and internal standard of Ga) gives a possibility for fast reliable determination of major and minor elements by the internal standard method with the recovery values 75-125 %.…”

Section: Application Of Txrf To Geological Objectsmentioning

confidence: 99%

“…One of the problems of TXRF analysis is strong peaks overlapping due to poor spectral resolution of the energy-dispersive spectrum. For instance, the differences between the TXRF results and the certified values in CRMs may be more than 30 % for As, Pb, V, Cr, Ba in the nodules due to PbLα/AsKα, BaLα/TiKα, CrKα/VKβ, VKα/TiKβ lines overlapping [Pashkova et al, 2020;Chubarov et al, 2021]. Chemometric approaches may be used to solve this problem [Akhmetzhanov et al, 2021].…”

Section: Application Of Txrf To Geological Objectsmentioning

confidence: 99%

Application of Total-Reflection X-Ray Fluorescence Spectrometry (Txrf) to Geological Objects: Experience of the TXRF Laboratory, Center for Geodynamics and Geochronology

Maltsev

Pashkova

2022

Geodin. tektonofiz.

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Unlike conventional X-ray fluorescence spectrometry, the total-reflection X-ray fluorescence spectrometry is not a widespread and routine method for analyzing solid samples with mineral matrix, but it has a great potential for geochemical, geological, and archaeological studies. Rapid multi-elemental analysis of very small sample amounts can be performed by the internal standard method which does not require the matrix-matched reference materials. This is an undoubted advantage of the TXRF method over the conventional X-ray fluorescence method, especially if there is a limited available sample amount and a lack of well-characterized reference materials. This paper presents our experience with the application of TXRF spectrometry in the elemental analysis of apatite, ceramics, sediments, ores, and nodules. Special attention has been paid to the sample preparation procedure because it is one of the main sources of errors in the analysis. Preparing thin homogeneous specimen from the solid sample with a complex mineral matrix is not easy. Sample preparation strategy should be chosen considering the features of an analytical object, the content of the elements to be determined, and the accuracy required for a reliable interpretation. Consideration is being given to the examples of the preparation of a suspension for rapid analysis of ores and sediments, and to the original techniques of chemical decomposition for apatite and ceramics.

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Preparación de muestras sólidas para el análisis por fluorescencia de rayos X: una revisión

Pérez Diaz,

Serna Saiz,

Torres Quezada

2024

Rev. Colomb. Quim.

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La fluorescencia de rayos X (XRF, por sus siglas en inglés) permite realizar análisis multielementales en diversas matrices sólidas, incluidos polvos y granos. Para obtener resultados confiables, la muestra preparada debe cumplir con ciertos criterios relacionados con su espesor, la planitud de su superficie, su homogeneidad y el tamaño de sus partículas. Las muestras sólidas heterogéneas que se deseen medir deben pulverizarse, homogeneizarse y prepararse como polvo suelto, polvos prensados (pellets) o perlas fundidas, si se buscan mediciones precisas y reproducibles. Las condiciones de medición están definidas por la profundidad analítica de los rayos X fluorescentes de los analitos, y se pueden estimar a partir de la relación que existe entre la absorción de cada rayo y su respectiva energía, y la composición y densidad de la muestra. Así mismo, con el propósito de asegurar la validez de los resultados, se debe validar el método de medición, para confirmar que cumple con el propósito para el cual fue desarrollado. Esta revisión está enfocada en la preparación de muestras sólidas, en el análisis cuantitativo, el cual incluye la validación de los métodos involucrados en las mediciones por espectrometría de XRF, y en las principales aplicaciones de la técnica.

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Multielement analysis of continental and lacustrine ferromanganese nodules by WDXRF, TXRF, and ICP-MS methods. Intercomparison study and accuracy assessment

Cited by 4 publications

References 49 publications

A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

A Workflow for Uncertainty Assessment in Elemental Analysis of Archaeological Ceramics: A Case Study of Neolithic Coarse Pottery from Eastern Siberia

Application of Total-Reflection X-Ray Fluorescence Spectrometry (Txrf) to Geological Objects: Experience of the TXRF Laboratory, Center for Geodynamics and Geochronology

Preparación de muestras sólidas para el análisis por fluorescencia de rayos X: una revisión

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