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The aim of the present research was to provide a strategy for the start‐up of upflow anaerobic sludge blanket (UASB) reactors treating sugar cane vinasse, with emphasis on the relevant sulfur compounds along the reactor height. To this end, a laboratory‐scale UASB reactor was started up and its performance under the applied conditions was studied.

Biomass was able to assimilate organic loading rates from 3 to 10 kg chemical oxygen demand (COD) m_R⁻³ d⁻¹, reducing VFAs accumulation, while increasing biogas production rate (BPR) from 0.92 to 4.12 m³ m_R⁻³ d⁻¹. The COD and sulfate (SO₄²⁻) were mainly removed in the reactor bed, showing homogenous distribution in the blanket and settler zones. However, from bottom to top of the reactor, a slight decrease of total and free sulfide concentrations was observed, indicating that the sludge bed in the UASB reactor was …