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A two-step chromatographic purification method for Ni for its isotopic analysis by MC-ICP-MS

Lingke Li,Fei Wu,Yongsheng Liu,Tao He,Jie Lin,Wen Zhang,Rui Li,Haihong Chen,Keqing Zong,Zhen Zeng,Zhaochu Hu

Stable nickel (Ni) isotopes have shown great potential for investigating planetary accretion processes, mantle–crust magmatism, and paleo-marine evolution. The development of an economical and time-efficient separation method for Ni isotope analysis holds significant value within the realm of Ni isotope research. Previous purification methods for Ni isotope analysis have typically relied on either multi-column procedures or the utilization of significant quantities of organic reagents, such as acetic acid, acetone, and dimethylglyoxime. In this study, a novel two-column chromatographic separation procedure was presented for the determination of Ni isotope compositions in geological materials. A cation resin (AG50W-X8) was utilized in conjunction with diluted HCl and HF to effectively remove a substantial portion of matrix elements. Subsequently, trace amounts (100–200 μL) of Ni-spec resin were used for further purification of Ni. This relatively simple purification scheme for Ni isotope analysis effectively reduces the use of organic reagents and the amount of Ni-spec resin compared to previous methods that relied on multi-column separation and organic reagent extraction. Ni isotopic compositions were analyzed using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The instrumental mass discrimination of Ni isotopic ratios was corrected for using the double spike (DS) combined with the sample–standard bracketing (SSB) method. The Ni isotope compositions (δ60Ni) of in-house standards (SCP and CUG) were −0.06 ± 0.05‰ (2 SD, n = 104) and 0.36 ± 0.06‰ (2 SD, n = 97), respectively. Furthermore, the measured δ60Ni values of various geological reference materials (BCR-2, BHVO-2, BIR-1, DTS-1, DTS-2b, SDO-1, GSP-2, and W-2a from the USGS; JB-1b from the GSJ; GSR-2, GSR-3, GSR-4, GSR-5, and GSR-10 from the NRCGA) were consistent with previous studies within measurement error. Additionally, the δ60Ni values of AGV-1 from the USGS, as well as those of GSR-10, GSR-12, GSR-15, GSR-17, GSR-18, and GSR-19 from the NRCGA are reported here for the first time. Based on repeated measurements of pure solutions and reference materials, the long-term reproducibility of δ60Ni values was better than ± 0.06‰ (2 SD). Consequently, our study presents a relatively straightforward purification method for Ni for its isotopic analysis using only trace amounts of organic reagents and Ni-spec resin.