The Ammonia Fiber Explosion (AFEX) process was used as a pretreatment method to increase enzyme digestibility of bagasse and cane leaf matter (CLM). The AFEX process parameters including reaction time, reaction temperature, ammonia loading, and moisture content of the biomass were varied to find a set(s) of conditions that result in the highest glucose and xylose yield. The efficiency of the AFEX process was evaluated via enzyme hydrolysis. The highest glucose and xylose yield for both bagasse and CLM were obtained from AFEX treatment with process conditions of 100-110ºC, 40-60% moisture content, 2:1 ammonia loading to dry biomass, and 30 min reaction time. Enzyme hyrdolysate of AFEX-treated bagasse and CLM was assessed via separate hydrolysis and fermentation (SHF) processes for ethanol and succinic acid production. In these SHF processes two different solid loadings were used. Zymomonas mobilis (pZB5) was used for ethanol fermentation; and for succinic acid fermentation, Actinobacillus succinogenes (FZ45) was used. Both organisms are able to utilize glucose and xylose. The experimental details, maximum glucose and xylose yields obtained from AFEX-treated bagasse and CLM, furfural and HMF analysis, ethanol yield and succinic acid yield will be presented.