The use of an alkaline sample solution for the determination of Se by the hydride generation technique offers the possibility of eliminating the interference from very high concentrations of Ni2+, CO2+, Fe3+ and Cr3+. In order to achieve this, complexing agents were employed to mask the interfering metal ions, After addition of the masking agent, the pH was adjusted to 12-13 with NaOH, and sodium tetrahydroborate was finally added in order to reduce selenite to selenide ions. The selenium hydride was generated by acidifying the solution with HCl in a flow system. Ethylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid (DTPA) were found to be effective masking agents for Ni2+ and Co2+; the, interference from up to 8000 mg l(-1) of Ni2+ or Co2+ was eliminated. Tartrate was found to be a suitable masking agent for Fe3+ and Cr3+ UP to 5000 mg l(-1). Accurate results were obtained for the National Institute of Standards and Technology Standard Reference Materials 671 Nickel Oxide and 364 Low-alloy Steel, using combinations of DTPA and tartrate as masking agents. The detection limits were 0.1 mu g g(-1) for the Nickel Oxide and 0.3 mu g g(-1) for the Low-alloy Steel.