The purpose of this paper is to present a report on the characterization of crude glycerol derived from biodiesel processed from cashew, melon and rubber seed oils. Crude glycerol is a co-product frombiodiesel production. To make the crude glycerol economically useful, it is imperative to characterize it. Investigative tests were carried out on the vegetable oils and on the crude glycerol that were separated fromthe biodiesel fuels with a separating funnel. The fatty acid profile was obtained using a gas chromatography analyzer and the physicochemical properties of the glycerol sludge were measured. Some of these physicochemical properties are flash point, ash content and material organic non-glycerin (MONG). Further works can still nutritional, industrial and pharmaceutical qualities and uses.