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In this paper, a destabilization episode in a semicontinuous dry thermophilic acidogenic reactor was induced. The reactor was fed with different mixtures of organic fraction of municipal solid waste (OFMSW) and food waste (FW). The aim was to determinate the effect of the organic loading rate (OLR) and cosubstrate ratio on biohydrogen production by dark fermentation. OLR was increased from 21.0 to 88.8 g TVS/L/day testing three mixture ratios (OFMSW:FW) from 80:20 to 50:50 and four hydraulic retention times (HRTs; 6.6, 4.4, 2.4, and 1.9 days). Results have shown that an increment in the OLR (from 21.0 to 59.8 g TVS/L/day) and FW proportion (from 80:20 to 50:50) improves the yield process in terms of solubilized organic matter. However, from 50:50 ratio combined with OLRs higher than 70.3 g TVS/L/day and HRTs lower than 4.4 days showed a clear destabilization episode due to an imbalance of the hydrolytic phase. This fact has been corroborated by the values of two indirect parameters, “nonsolubilized carbon” and “acidogenic substrate as carbon”.

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