Abstract: Alkalized cocoa nibs were produced using cocoa shell ash as an alkalizing agent. Conventionally, imported alkalizing agents are used to produce alkalized/dutched nibs in cocoa processing industries. Cocoa powder and cocoa butter were produced from nibs treated with cocoa shell’s ash as an alkalizing agent and compared with products from two industries which used imported alkali as the dutching agent. Cocoa products made from cocoa nibs alkalized with ash for the shell were evaluated for physicochemical properties in comparison with product from Oluji and Stanmark Industries located in Southwestern Nigeria. Flame photometry method was used to determine components of the ash. The pH value of cocoa powder were 6.72 and 6.56 for Oluji and Stanmark samples respectively while 6.59 was reported for the Experimental cocoa powder sample. Percent fat content was 11.56 for Stanmark, 12.20 for Oluji and 10.56 for the Experimental sample. Colour reflectance was highest in Stanmark sample with 8.69 while the least was recorded for Experimental sample (7.18). Percent ash was 6.58, 8.16 and 7.13 for Stanmark, Oluji and Experimental samples respectively. Fat parameters for cocoa butter from the three samples were found to be within International standard for cocoa butter. Percent fatty acid ranged from 1.46 to 1.59. Saponification value was 193 mg KOH g–1 sample for Experimental sample, while Stanmark and Oluji cocoa butter had 196 and 198 mg KOH g–1, respectively. Percent unsaponifiable matter content was 0.30 each for Stanmark and Oluji with 0.39 for Experimental sample. Iodine value was between 35.11 and 38.07 Wij’s. Peroxide value ranged from 26-29 ME kg–1. Major components of cocoa shell ash were found to be potassium, 3.1 g/100 g and sodium, 7.2 g/100 g while sodium carbonate was 33.1 g/100 g. The pH of the ash was 10.8. There were no significant differences (p< 0.05) in all the sensory parameter for cocoa powder. Although, chocolate aroma was found to be less pronounced in the Experimental sample when assessed by sensory panelists, it did not significantly affect the overall acceptability.