Determination of major, minor and trace elements in rock samples by laser ablation inductively coupled plasma mass spectrometry: Progress in the utilization of borate glasses as targets |
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Authors: | Tá cito Dantas F. Leite,Rainé rio Escalfoni Jr.,Teresa Cristina O. da FonsecaNorbert Miekeley |
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Affiliation: | a Departmento de Química da Pontifícia Universidade Católica do Rio de Janeiro, Rua Marques de São Vicente 225, 22451-900 Rio de Janeiro, Brazilb Universidade Estadual de Goiás (UEG), Brazilc Instituto Federal de Educação, Ciência e Tecnologia de Brasília (IFB), Brazild Centro de Pesquisas Leopoldo A. Miguez de Mello da Petrobras (CENPES), Brazil |
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Abstract: | The present work is a continuation of a research study performed at our laboratory aiming at the multielement analysis of rock samples (basalts and shale) by inductively coupled plasma mass spectrometry in combination with laser ablation using borate glasses as analytical targets. Argon, nitrogen-argon mixtures and helium were evaluated as cell gases, the latter confirming its better performance. Different operational parameters of the laser, such as gas flow, energy, focus, scanning speed and sampling frequency were optimized. External calibration was made with standards prepared by fusion of geological reference materials (basalts 688 and BCR-2, obsidian SRM 278, and shale SGR-1) of different mass fractions in the meta-tetra borate matrix. Coefficients of determination (R2) were > 0.99 for 30 elements from o total of 40 determined. Method validation was then performed using additional certified reference materials (BHVO-2, BIR-1, SCo-1) produced as borate targets in a similar way. Accuracies were better than 10% for most of the elements studied and analytical precisions, calculated from the residual standard deviations of calibration curves were, typically, between 6% and 10%. Additionally, the semiquantitative TotalQuant® technique was applied, which gave, within the expected uncertainty for this calibration technique, concordant results when compared to the quantitative external calibration procedure. Both methods were then used for the analysis of marine shale samples, which are of great geological interest in petroleum prospecting. |
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Keywords: | Laser ablation ICP-MS Borate glasses calibration techniques Rock analysis |
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