Chromatographic purification of Ca and Mg from biological and geological samples for isotope analysis by MC-ICP-MS

Abstract

This study presented a chemical protocol for purification of calcium and magnesium from a single aliquot of biological and geological samples. The separation protocol was based on a two-step cation exchange chromatography using DGA resin and AG50W-X12 (200–400 mesh) resin. Calcium fraction was first collected using 0.25 mL of DGA resin, and Mg fraction was then collected using 0.5 mL of AG50W-X12 cation exchange resin. For Ca isotope analysis, the effect of acidity and concentration mismatch as well as the matrix effect were rigorously evaluated using the Neptune Plus MC-ICP-MS with a wet-plasma mode. Based on repeated measurements on BHVO-2 and NIST SRM 1400, the long-term reproducibility was evaluated at 0.08‰ (2SD) for δ44/42Ca915a. The δ26Mg ratios of the analyzed reference materials varied from −1.22‰ to 0.03‰ with the external precision better than 0.11‰ (2SD). The robustness of the protocol has been validated by replicated analyses of biological and geological standards. Calcium and magnesium isotopic ratios of all reference materials measured in this study agreed well with previous data within uncertainties. Therefore, the proposed method can be used for simultaneous determination of Ca and Mg isotopic ratios from a single aliquot of biological and geological samples.