A new technique for on-line sample preparation and D/H determination is described. The technique is suitable for the preparation of fresh and brine waters, as well as natural gases and organic solvents, A 5-mu L sample of water or hydrogen equivalent is injected and reduced by means of hot manganese metal in a specially designed reaction tube surrounded by a tube furnace and attached directly to the mass spectrometer inlet without modification,The hydrogen gas flows directly into the MS to be analyzed by reference/sample comparison. The reproducibility varied between 0.7 and 1.8 parts per thousand for all liquid and gas samples. The accuracy of this technique is confirmed by analysis of IAEA standard waters V-SMOW, GISP, and SLAP, as well as NGS-3 (IAEA methane intercomparison material).