Fish offal and other high protein substrates are generally not suitable for anaerobic digestion because of the high levels of ammonia produced as a result of their biodegradation. In order to efficiently use these types of substrates to produce methane, co-digestion is used to balance the amounts of carbon and nitrogen in the feedstock. In this experiment an optimization procedure for maximizing the methane potential of fish offal, using river tamarind as the co-substrates was developed. Our experimental design tested the effects of substrate to substrate mixtures, as well as overall substrate to inoculum combinations, on the methane potentials. This was performed using batch style biochemical methane potential assays, which employed a methodology developed in our laboratory. The optimum of the 25 combinations tested was 50% fish offal to 50% river tamarind at a substrate to inoculum ratio of 0.03, with a specific methane yield of 144 ± 6 NmL/gFM (330 ± 14 NmL/goDM). This gave much improvement when compared with the fish offal alone, which reached 63 ± 4 NmL/gFM (317 ± 20 NmL/goDM) at maximum. These results indicate that with the correct mixture, rivertamarind is a suitable co-substrate for anaerobic co-digestion of fish offal.