Abstract: Annual Neosinocalamus affinis was treated in four kinds of maceration solutions, i.e. HNO3-KClO3 (a), NaClO (b), H2O2-HAc (c) and NaOH (d), respectively. Effects of different chemical maceration methods, maceration time and ultrasonic test on contact angle of single fiber and hollow fiber were studied. The results showed that the maceration time of four methods was largely different (ta tb td tc), contact angles of single fiber were dissimilar (CaCdCbCc) and hollow fibers were diverse (HcHd). In the maceration process, ultrasonic wave can accelerate the maceration rate, shorten the maceration time and reduce the contact angle of single fiber.