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A new sample preparation protocol for high-purity titanium material has been developed for analysis by glow discharge mass spectrometry. The titanium material is machined using an aluminium oxide cut-off wheel followed by a double etching process with a hydrogen peroxide based acid etchant. This sample preparation method reduces conventional preparation time from 3 h to 20 min and pre-sputtering time from more than 1 h to 20 min.