The amount of glycerol derived from the biodiesel industry is increasing exponentially worldwide. Therefore, the purification of the crude glycerol by-product has the potential to improve the profitability of biodiesel in a bio-refinery scenario coupled with the fact that glycerol is an important industrial chemical. This research was carried out using crude glycerol from biodiesel production of neem seed oil and waste cooking vegetable oil (W.C.V.O). Variables like glycerol content of the crude glycerine, pH, density,ash content percentage purity and the extraction solvent to glycerol ratio were examined. The crude glycerine content of the neem seed oil source and waste cooking vegetable oilsource were found to be about 41.33% and about 35.66% respectively. Dilute phosphoric acid was used to neutralise the highly basic crude glycerolcausing a separation between the phases which converts the catalyst to salt. The optimal pH for the separation of the glycerol-rich phase for the neem oil source and the waste cooking vegetable oil source was found to be 6.5 and 6.0 respectively. Both the refined glycerol and crude glycerine samples were characterized using the Gas Chromatograph Mass Spectrometer (G. C. M. S.). The purity levels were found to be about 97% for both sources, density was found to be about 1.24g/cm3and1.234g/cm3for the neem source and for the waste cooking vegetable oil source respectively. The ash content was found to be 1.30% for the purified glycerol from a crude glycerine value of 4.31% from the neem source and 1.10% for the waste cooking vegetable oil source from a crude glycerine with 4.08% content. The heavy metal content, chloride, phosphate and a few other tests have also been done on the samples produced.