pH control is not necessary during FNA pre-treatment on primary sludge (PS). FNA increases the solubility and reduces cell viability (<20%). At 1 h, FNA (with 650 mg N-NO2−) provided the highest methane production (MP). Similar enhancement on MP were obtained while subjecting the PS at mild at 2–5 h. FNA is not necessary to increase MP; mild agitations also improve MP (around 14–17%).