comparative analysis of oxalic acid produced from rice husk and cocoa seed was carried out by nitric acid oxidation of carbohydrates in order to ascertain which waste sample produced a better yield. The results obtained showed that HNO3:H2SO4 acid ratio of 50:50 for rice husk sample gave a percentage yield of 48.0, 63.2, and 49.3 at temperatures of 55°C, 75°C, and 85°C respectively. At 60:40 acid ratio, the percentage yields were 47.8, 67.8 and 46.6 at the three different temperatures respectively. At 80:20 acid ratio, the percentage yields were 50.2, 67.0 and 45.4 at the three different temperatures .For cocoa seed, a percentage at 50:50 acid ratio, were 44.6, 54.7 and 47.4 at temperatures of 55°C, 75°c and 85°C respectively. At 60:40 acid ratio, the percentage yields were 45, 54.8 and 46.4 at these three different temperatures. At 80:20 acid ratio, the percentage yields were 47.6 51.3 and 45.8 at the above stated temperatures. The variable ratio of 60: 40 gave the maximum yield at the maximum temperature of 75°C for the both samples. But in comparison, it was found that the oxalic acid produced from rice husk gave higher yield by 13% than that from cocoa seed. The use of these raw materials to produce oxalic acid will minimize environmental pollution.