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Comparison of the fluctuations of the signals measured by ICP-MS after laser ablation of powdered geological materials prepared by four methods

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Abstract

Sample preparation is a crucial point for quantitative multi-elemental analses by LA-ICP-MS of powdered geological materials. Four different methods are compared in this study with respect to signal stability and intensity as follows: the preparation of glass beads (GlassB) by alkaline fusion method and three grinding and pelletizing methods relying on the use of an organic binder (VanBind, vanillic acid), an adhesive binder (MixGlue, methyl methacrylate) and a sol–gel process for glass formation (SolGel, chemical reaction of tetraethoxysilane), respectively. Sixty elements were analyzed by means of a ns-UV (213 nm) laser ablation system coupled to a single collector sector field ICP-MS with a low or medium mass resolution. Signal stability was found to strongly depend on the sample homogeneity provided by the preparation method. These methods were applied to three geological standard materials (CRM). The following criteria were used to evaluate and compare the methods: (1) proportion of the measurement cycles which are above a given signal intensity threshold (defined here as signal average ± 3 times the standard deviation), (2) signal stability of the analyzed nuclides (internal precision estimated by the relative standard deviations on raw count rates), (3) signal stability of the internal standards added to the samples, (4) external precision estimated by the relative standard deviation over five preparations for each geological CRM. For the majority of the analyzed elements, signals measured for samples prepared with the four methods are reproducible. Specific contamination in one or several elements (Cr, Fe, Co, Ni, Cu, Mo, W, Au and Bi) was observed depending on the sample preparation method. In addition, compared to grinding made with PTFE material, grinding performed with tungsten carbide material was found to produce better homogeneity, especially for the sol–gel and mixing with glue protocols, although some metallic contamination (W and Co) was observed. Thanks to the suppression of grain effects by alkaline melting, the glass bead method systematically provided signal stability and percentage of “over the threshold” close to those of the NIST glasses. This may be explained by the preparation of more homogeneous samples by alkaline melting. Finally, the described methods were found to be reproducible for the majority of the analyzed elements.

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The data presented in this study are available on request from the corresponding author.

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Acknowledgements

This work was performed with financial backing of a PhD thesis from Orano Mining and the CEA/DAM/DIF. The authors would like to express their gratitude to Valérie Granger, Mike Maury and Magali Celier (Orano Mining, CIME) for the main lines of the alkaline fusion protocol, the formation on the Katanax X-Fluxer X-600 and of their reception during the preparation of the glass beads. Authors would thank Olivier Marie (CEA, DAM/DIF) for the MEB imaging. Authors would also thank Aurélie Diacre (CEA, DAM/DIF and LSCE) for the laser granulometry measurements. Finally, authors express their gratitude to the two anonymous reviewers for their time and their helpful comments.

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Authors and Affiliations

  1. CEA, DAM, DIF, 91297, Arpajon, France

    Michaël Susset, Axelle Leduc--Gauthier, Anne-Claire Humbert & Fabien Pointurier

  2. Universite de Pau et des Pays de l’Adour, E2S UPPA, CNRS, IPREM, Avenue de l’Université, 64012, PAU Cedex, France

    Christophe Pécheyran

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  1. Michaël Susset
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MS: writing—original draft, data curation, formal analysis, software, investigation. AL–G: data curation, formal analysis, investigation. A-CH: methodology, writing review and editing, supervision. FP: methodology, writing review and editing, supervision. CP: methodology, writing review and editing, supervision.

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Susset, M., Leduc--Gauthier, A., Humbert, AC. et al. Comparison of the fluctuations of the signals measured by ICP-MS after laser ablation of powdered geological materials prepared by four methods. ANAL. SCI. 39, 999–1014 (2023). https://doi.org/10.1007/s44211-023-00309-5

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