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A new kinetic spectrophotometric method has been developed for the determination of trace Ni (Ⅱ) in natural water. The method is based on the catalytic effect of Ni(Ⅱ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The concentration of nickel (Ⅱ) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ = 626 nm using the fix-time method. The influencing factors are investigated by the orthogonal experimental design. The obtained op- timum analytical conditions are: pH = 2.00, CRAWL = 5.00×10-5 molL-1, C