The increasing generation of organic waste from the food processing industry has created opportunities for converting biodegradable residues into renewable energy. Cassava sludge and tofu wastewater contain biodegradable organic matter and may serve as substrates for anaerobic digestion. This study aimed to characterize the initial physicochemical properties of cassava sludge and tofu wastewater and assess their characteristics and endpoint gas profiles under different substrate formulations. Four formulations were evaluated: cassava sludge (S1), cassava sludge mixed with tofu wastewater (S2), tofu wastewater (S3), and cassava sludge supplemented with a microbial inoculum (S4). Activated Effective Microorganisms 4 (EM4) was applied to all formulations. Initial characterization included pH, temperature, total nitrogen (TN), total suspended solids (TSS), turbidity, chemical oxygen demand (COD), and biochemical oxygen demand (BOD). Reactor pH and temperature were monitored every three days for 21 days batch digestion period, followed by endpoint gas composition analysis. Cassava sludge exhibited the highest initial COD and BOD concentrations, at 19,409 and 8,640 mg/L, respectively, with TSS and TN concentrations of 680 and 270 mg/L. The cassava sludge tofu wastewater formulation showed COD and BOD concentrations of (13,355 mg/L and 6,028 mg/L), respectively, whereas tofu wastewater showed values of (6,644 mg/L and 2,974 mg/L). S4 exhibited lower initial COD and BOD concentrations of 389 and 175 mg/L, respectively, reflecting the initial characteristics of the formulation containing additional microbial inoculum. During the digestion period, temperatures ranged from (25.1–32.2 °C). while pH generally increased across the formulations. At the end of the 21 days digestion period, S4 showed the highest CH₄ reading (65.4%LEL), followed by S1 (9.7%LEL), S3 (4.7%LEL), and S2 (3.9%LEL). The observed results indicate differences in endpoint gas characteristics among the substrate formulations under the experimental conditions. Overall, the initial physicochemical characteristics and endpoint gas profiles provide a basis for assessing cassava sludge and tofu wastewater as substrates for anaerobic digestion.
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