Methodology and Application of Hafnium Isotopes in Ilmenite and Rutile by MC‐ICP‐MS

The high abundances of the high field‐strength elements in ilmenite and rutile make these minerals particularly suitable for hafnium isotopic investigations. We present a technique for separating Hf by ion exchange chemistry from high‐TiO₂ (> 40% m/m) minerals to achieve precise Hf isotopic composition analyses by MC (multiple collector)‐ICP‐MS. Following digestion and conversion to chlorides, the first elution column is used to separate iron and the rare earth elements, the second column is designed to separate most of the titanium from Hf, an evaporation step using HClO₄ is then performed to remove any trace of HF in preparation for the third column, which is needed to eliminate any remaining trace of titanium. The modified chemistry helped to improve the yields from < 10 to > 78% as well as the analytical precision of the processed samples (e.g., sample 2033‐A1, ¹⁷⁶Hf/¹⁷⁷Hf = 0.282251 ± 25 before vs. 0.282225 ± 6 after). The technique was tested on a case study in which the Hf isotopic ratios of ilmenite and rutile (analysed prior to the chemistry improvement) were determined and permitted to evaluate that the origin of rutile‐bearing ilmenite deposits is from the same or similar magma than their, respectively, associated Proterozoic anorthosite massifs (Saint‐Urbain and Lac Allard) of the Grenville Province in Québec, Canada.