Efficient pre-treatment has been found to be crucial step before enzymatic hydrolysis of cellulose into fuels or chemicals. As a result various pretreatment methods have been developed to facilitate these bio-conversion processes, and this research focuses on the effect of two pretreatment methods such as liquid hot water and sulphuric acid pre-treatment to remove some of the components like lignin and hemicellulose which form structural barrier to enzymatic accessibility of cellulose in corn cobs and sawdust. The cellulosic materials were first dried in oven at 65 oC for 24 hours,  and using   solid to liquid ratio of 1:10, the two methods were carried out at resident times ranging from 10 - 40 minutes. The liquid hot water method involved heating the cellulosic materials in water at 120 oC and 1atmosphere in a pressure vessel, and for the second method, the dried cellulosic materials were refluxed in 5 % sulphuric acid at a temperature of 120 oC. Pretreated samples were filtered and liquid fractions were analyzed for the presence of reducing sugars, while solid residues were dried in the oven and weighed to measure the mass lost during pretreatment as a pointer to lignin breakdown. It was observed that the mass lost increased with time for both pretreatment methods, but the liquid hot water pretreatment gave higher lignin and hemicellulose removal when compared to the sulphuric acid pre-treatment. The pretreated materials were hydrolyzed with two combinations of commercial enzymes namely cellulase/ hemicellulase and cellulase/β glucosidase. The reducing sugar was measured using Dinitrosalycilic acid (DNSA) method and the sugar yields from corn cobs were higher than that of sawdust when subjected to similar process conditions, and the enzyme combination of cellulase/glucosidase gave higher yields of reducing sugars.  A model equation which describes the hydrolysis process was developed from first principles and the experimental data obtained gave a good fit.