New Analysis Protocol for Stable Isotopes by a Standard Doping Method─An Example of Antimony

The current analytical methods of stable antimony isotopes are cumbersome and not suitable for rock samples with low antimony content (<1 μg/g). In this study, we propose a new protocol for antimony isotopic analysis with a single column of AG50W-X8 resin and antimony standard doping. This method separates antimony effectively from matrices and then mixes it with the Sb standard. As Te does not affect the accuracy of antimony measurement when the Te/Sb ratio is low, we can obtain an accurate Sb isotope composition of the mixture. Then, we can calculate the antimony isotope composition of natural samples. The error propagation of the mixing and calculation processes was evaluated by the Monte Carlo method, and no significant error was found. The antimony isotope compositions were measured using a Thermo Fisher Scientific Neptune Plus multicollector-inductively coupled-mass spectrometry instrument. The instrumental mass bias of Sb isotopes was corrected with a standard-sample bracketing combined with a Sn internal normalization technique. Using the standard doping method, the measured δ123Sb values of standard solutions (Alfa, SPEX, GSB, and SCP) relative to NIST SRM 3102a were 0.02 ± 0.03‰ (2SD, N = 50), 0.29 ± 0.03‰ (2SD, N = 15), 0.24 ± 0.03‰ (2SD, N = 56), and 0.30 ± 0.03‰ (2SD, N = 15), respectively. The reproducibility for δ123Sb was better than 0.03‰ (2SD) throughout one year. This methodology has been testified by geological samples, yielding δ123Sb identical to the previously reported values. The actual Sb consumption for each sample test is as low as 5 ng. This standard doping method provides new insights into the analytical strategy of stable isotopes.