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Ti‐isotope fractionation on the most Ti‐rich minerals on Earth has not been reported. Therefore, we present a chemical preparation and separation technique for Ti‐rich minerals for mineralogic, petrologic, and economic geologic studies. A two‐stage ion‐exchange column procedure modified from the previous literature is used in the current study to separate Ti from Fe‐rich samples, while α‐TiO2 does not require chemical separation. Purified solutions in conjunction with solution standards were measured on two different instruments with dry plasma and medium‐resolution mode providing mass‐dependent results with the lowest errors. 49/47TiOL‐Ti for the solution and solids analyzed here demonstrate a range of >5‰ far greater than the whole procedural 1 error of 0.10‰ for a synthetic compound and 0.07‰ for the mineral magnetite; thus, the procedure produces results is resolvable within the current range of measured Ti‐isotope fractionation in these minerals.