Abstract: The extractive property of dibenzyl sulfoxide (DBSO) toward Pd(Ⅱ) was studied,and mixture of DBSO and C18 reverse phase bonding silica gel was used for SPE separation of Pd(Ⅱ).A HCl solution of pH 2.0 containing Pd(Ⅱ) was passed through the SPE column at a flow rate of 1.0-2.0 mL·min-1.A solution of 50 g·L-1 thiourea in 0.01 mol·L-1 HCl was used as eluant to desorb Pd(Ⅱ) from the column,and Pd(Ⅱ) in the eluate was determined photometrically.Values of recovery were found to be more than 90%.The proposed method was used in the analysis of two samples,the results obtained were in consistency with those obtained by AAS.