Oxalic acid (or its dissociated form oxalate) is a result of protein metabolism and is among the important nutrients in the human diet. Regular consumption of large amounts of food with high oxalate contents over a long period may result in nutrient deficiencies notably calcium and contribute to kidney stone formation. The aim of current research is to determine some physicochemical characteristics as well as the oxalate content of cassava in addition to sweet potato grown in Areka, Ethiopia using titration and UV-visible spectrophotometric methods. The moisture content of dry flour and fresh roots of cassava was found to be 10.33 and 55.27 %, respectively, while the moisture content of dry flour and fresh tuber of sweet potato was 9.07 and 68.47 %, respectively. The ash content of the flour sample of cassava and sweet potato was 3.60 and 4.13 %, respectively. The pH of the flour sample of cassava and sweet potato was 6.23 and 6.13, respectively. Oxalate content determination was done using titration and UV-visible spectrophotometer methods. The oxalate level of samples using the titration method gave 77.66 and 197.90 mg/100g for cassava and sweet potato, respectively. By the UV-visible spectrophotometer, the oxalate content was 151.19 and 153.56 mg/100g for cassava and sweet potato, respectively. Statistical analysis on the generated data indicated that all physicochemical investigated in this study have significance difference at p≤ 0.05.