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Lithium (Li) and Magnesium (Mg) isotopes have been widely used as valuable tracers to study geological processes. In general, several column separation procedures have been used to separate Li and Mg. In this study, we present an optimized protocol for the rapid and simultaneous purification of Li and Mg, which significantly reduces the separation time, required reagent volume, and procedural blanks compared to previous methods. Samples with small amounts of Li (generally 5 ng Li yielding Mg masses of 1 -1200 mu g) were separated, with the corresponding yields of Li and Mg being nearly 100%. Lithium and Mg isotope analyses were performed using an MC-ICP-MS (Thermo Scientific NEPTUNE Plus) and only <0.2 ng Li and <150 ng Mg were consumed for each analysis. Matrix-doping experiments reveal that the matrix effect is negligible for the determination of Li and Mg isotopes from a wide array of geological samples using our protocol. The robustness of the protocol has been validated by replicated analyses of standard solutions and geological standards, which yield long-term external 2 sigma precision better than +/- 0.6 parts per thousand for delta Li-7 and +/- 0.08 parts per thousand for delta Mg-26. Lithium and Mg isotopic ratios of all reference materials measured in this study agreed well with previous data within uncertainties. The method developed in this study allows for the rapid and high-purity separation of Li and Mg and subsequent high-precision isotopic analyses of these elements. (C) 2022 Elsevier B.V. All rights reserved.