A novel method for the determination of nickel and palladium in environmental samples by low temperature ETV-ICP-OES with dimethylglyoxime(DMG) as both the extractant and chemical modifier has been developed. In this study, it was found that nickel and palladium can form complexes with dimethylglyoxime(0. 05%, mass fraction) at pH 6.0 and can be extracted into chloroform quantitatively. The complexes can be evaporated into plasma at a suita-ble temperature( 1400℃) for ICP-OES detection. Under the optimized conditions, the detection limits of nickel and palladium are 0.48 and 0. 40 ng/mL, respectively, while the RSD values are separately 5.0% and 3.1% (p = 50 ng/mL, n = 7). The proposed method was applied to the determination of the target analytes in environmental sam-ples with satisfactory results.