A study has been made of the experimental conditions, errors, sensitivity, limits of detection and linear response range in the determination of beryllium by AAS in a nitrous oxide-acetylene flame, with aqueous or aqueous organic solutions or MIBK solutions containing the ion-pair [Be(SCN)(2-)(4)][(R(3)NH)(2+)(2)]. The interference of Al, Mg, Ti, V, Fe, Ca, Mn, Na, K, SiO(2-)(3), PO(3-)(4), Cl(-), SO(2-)(4), F(-), ClO(-)(4), H(2)BO(-)(3) and SCN(-) has been studied, and methods established for eliminating that of titanium, aluminium, fluoride and silicon.