The purpose of this study is to develop and evaluate disyllabic Mandarin speech test materials (MSTMs) in order to facilitate wider use of speech audiometry in Chinese audiology clinics. Phonologically balanced Mandarin disyllabic materials with high familiarity were designed based on the basic rules for developing speech materials and the particular characteristics of Mandarin, and recorded digitally. In order to establish the validity and reliability of these Mandarin disyllabic materials, equivalence of difficulty between the word lists was evaluated for a group of 60 subjects (age-range 18-25 years) with normal hearing. Subsequently, performance-intensity (PI) functions were measured in a group of 30 subjects with normal hearing (age-range 18-25 years), and a group of 35 subjects with sensineural hearing loss. The nine lists of Mandarin disyllabic materials were found to have sufficient reliability and validity to be used in clinical situations.