ePrints@IIScePrints@IISc Home | About | Browse | Latest Additions | Advanced Search | Contact | Help

Determination of Trace Elemental Composition of CaCO3: Application to Mass Limited Abiogenic and Biogenic Carbonates

Satya Chanakya, IV and Misra, S (2024) Determination of Trace Elemental Composition of CaCO3: Application to Mass Limited Abiogenic and Biogenic Carbonates. In: Geochemistry, Geophysics, Geosystems, 25 (2).

Geo_geo_geo_25_2_2024.pdf - Published Version

Download (2MB) | Preview
Official URL: https://doi.org/10.1029/2023GC011202


An improved method for accurate and precise determination of metal to calcium ratio in mass limited calcium carbonate samples has been developed. We used an Agilent®5800 ICP-OES for major element (Na/Mg/Sr to Ca) and an Agilent®8900 ICP-QQQ-MS for minor and trace element (Li/B/Na/Mg/Al/Mn/Fe/Zn/Sr/Cd/Ba/U to Ca) ratio determination. We report a long-term precision of �1 (1�) by repeat analysis, spread over �6 analytical sessions, of multiple external standards that spanned a large range of concentration. We quasi-quantitatively eliminated potential matrix effect from high Ca by concentration matching samples and standards (�Ca � ±5%) during both ICP-OES and ICP-QQQ-MS sessions. The ICP-OES analyses were done on 200 μl of sample at 60 ppm Ca, consuming �30 μg of CaCO3 per analysis. Whereas trace element analyses by ICP-QQQ-MS required �150 μl of sample at 20 ppm Ca, consuming �7.5 µg of CaCO3 per analysis. Thus, the present method allows for high precision determination of TE/Ca in <40 μg of CaCO3. We present a comprehensive approach for optimization of ICP-OES sensitivity and stability to select elemental (Ca/Na/Mg/Sr) wavelengths with minimal interferences, high sensitivity and linearity. For choice of Ca lines, we focused on the minimization of self-matrix effect. For the ICP-MS method, we improved reproducibility and precision by lowering Ca of analyte and preconditioning of cones. Furthermore, the present method allows for precise B/Ca determination sans the use of HF matrix. In summary, we present an easily adoptable method based on readily available instrumentation for determining element-to-calcium ratios that is suitable for analyzing mass-limited carbonate samples. © 2024 The Authors. Geochemistry, Geophysics, Geosystems published by Wiley Periodicals LLC on behalf of American Geophysical Union.

Item Type: Journal Article
Publication: Geochemistry, Geophysics, Geosystems
Publisher: John Wiley and Sons Inc
Additional Information: The copyright for this article belongs to authors.
Keywords: Aluminum; Barium; Calcite; Calcium; Inductively coupled plasma mass spectrometry; Iron; Magnesium; Manganese; Mass spectrometers; Sodium; Strontium; Trace analysis; Trace elements; Zinc, Abiogenic; Agilent; B/ca; Element/calcium; Elemental compositions; ICP-OES; Mass-limited; Matrices effect; Mg/ca; QQQ-ICP-MS, Calcium carbonate, calcium; calcium carbonate; magnesium; mass spectrometry; optimization; trace element; wavelength
Department/Centre: Division of Mechanical Sciences > Centre for Earth Sciences
Date Deposited: 01 Mar 2024 10:27
Last Modified: 01 Mar 2024 10:27
URI: https://eprints.iisc.ac.in/id/eprint/84155

Actions (login required)

View Item View Item