A dilute acid hydrolysis of rice husk (RH), wheat straw (WS), and their extractive-free residues was investigated with the objective of recovering the highest yield of xylose while keeping at minimum its conversion into furfural. The hydrolysis conditions were determined for different concentrations of sulfuric acid and different reaction times at 121 °C. The pre-extraction with ethanol-water (1:1, v/v) was also examined as a parameter. Using response surface methodology, the optimum conditions for xylose production were identified as 1.8% of acid and 41.4 min of hydrolysis time for RH, while those for its counterpart EF-RH (extractives-free rice husks) were 1.0% acid concentration, for 60 min. The same conditions were also predicted for WS and its EF-WS. Under these conditions, the xylose yield was 79.6%, 82.8%, 94.3%, and 88.6% for RH, EF-RH, WS, and EF-RW, respectively. Under these conditions the minimal furfural yields obtained were 1.2% and 1.3% for RH and EF-RH, and 0.8% and 1.5%, for WS and EF-WS, respectively. These results suggested that the pre-extraction step before the acid hydrolysis affected, at least in part, the xylose recovery from RH, but it was not necessary for a better xylose yield of WS for its bioconversion into valuable bioproducts like xylitol.