The properties of xylooligosaceharides separation by gel permeation chromatography was investigated. Xylooligosaecharides was separated with Bio-Gel P-4 by the first time and Bio-Gel P-2 by the second time. The results showed that the purity of fraction xylobiose, xylotriose, xylopentaose, xylohexaose and xyloheptaose separated with Bio-Gel P-4 were 98.18%, 88.54%, 97.52%, 78.80% and 86.67%, respectively. The content of arabinosyl groups in xylooligosaccharides was 14.75%, and xylobiose and xylotriose were not substituted with arabinosyl groups. The purity of fraction xylotriose can be raised from 88.54 % to 94.19% with Bio-Gel P-2 by the second separation.