I'm stuck in a biodiesel synthesis using fish endo- and exoskeleton ash as a catalyst, but the biodiesel isn't separating from the glycerol. I've worked with ash calcined at 900°C and 1000°C, oil-to-methanol molar ratios of 1:6 and 1:9, reaction times of 2, 3, 4, and 5 hours, and reaction temperatures of 60°C and 65°C. The oil is used and has less than 1% free fatty acids. I tested the oil with ashes from other fruits and obtained good separations of biodiesel from glycerol. Could you help me?