A single-stage anion exchange separation method for Cd isotopic analysis in geological and environmental samples by MC-ICP-MS

Abstract

AG-MP-1M anion exchange resin is commonly used to separate and purify Cd from geological and environmental samples. However, a second column using anion exchange, TRU Spec, or BPHA extraction resins is also required to further purify Cd from the residual Sn for high-precision Cd isotope ratio measurements. In this study, a new and efficient single-stage separation method using AG-MP-1M (100–200 mesh) anion exchange resin was developed to separate Cd from geological and environmental samples for high-precision Cd isotope ratio measurements. Most of the Sn (>99%) is effectively stripped from the resin using a 2 M HCl + 4 M HF mixed eluent, unlike commonly used separation protocols with AG-MP-1M anion exchange resin, which only removes ∼65% of the Sn using HCl eluent. Furthermore, potential residual Sn is retained on the resin by elution of 0.04 M HCl + 2 M HF and 0.005 M HCl + 2 M HF, which allows quantitative collection of the Cd fraction (∼99.5%) without Sn tailing. The single-stage purification procedure takes advantage of the different affinities of Sn on AG-MP-1M anion exchange resin at different HCl and HF concentrations in mixed HCl + HF solutions, which allows direct and effective separation of Cd from Sn and other complex sample matrices. We used this procedure and the double-spike MC-ICP-MS method to determine the δ^114/110Cd_{NIST SRM 3108} values for Mn nodule, igneous rock, shale, soil, and sediment reference materials, and obtained results that agree within analytical uncertainty with the values reported in previous studies. In addition, the δ^114/110Cd_{NIST SRM 3108} values of soil (GSS-1a), sediment (GSD-4a), and dolomite (GSR-12) standard reference materials are reported for the first time in this paper. The described purification procedure allows efficient and rapid Cd isotopic analysis in different types of geological and environmental samples.