A direct test method for Cr(VI) determination in milk powder was developed.The method comprised the following steps: ashing sample at 550°C muffle, adding a complexing reagent thenoyltrifluoroacetone(TTA) and acetate acid-acetate ammonium buffer solution, then analyzing with GF-AAS after several hours.The Cr(III) in milk powder sample and TTA can form a complex Cr(TTA)3 which can volatile before atomization, so the remaining Cr(VI) can be determined directly.This method has good linearity within the concentration range 1 μg/L∼20 μg/L, and the correlation coefficient can reach 0.999.The recoveries exceed 75% when the spike concentration is no less than 50 μg/kg, and RSD is less then 12.6%.