Abstract: The determination of F~-,Cl~-,NO_2~- and PO_4~(3-) ions in the presence of a large quantities of NO_2 ion is investigated in detail. In order to remove harmful and a great amount of cations that are contained in the liquid waste, especially the transition metal and other heavy metal ions. The pretreatment column with cation exchange resin is used; The sample is dilluted with the eluent to suppress the negative peak of water; The effect of a large amount of NO_3~- on the measurement of other anions are eliminated by choicing proper dillution times of sample. Because the method possesses higher sensitivity and allows much more dillution times of sample to decrease radiation, it is very fit for the analysis of high levelwaste.F~-,Cl~-,NO_2~- and PO_4~(3-) are recovered quantitatively in the method. The precision of the method is better than6 % for the determination of F~-,Cl~-,NO_2~- and PO_4~(3-).