The determination of total oil and grease (TOG) in water is important mainly for the petroleum industry due to the high amount of water coproduced with oil. Many countries establish regulations determining a maximum limit of TOG. In Brazil, for example, TOG should be measured by gravimetric methods. Other methodologies may be accepted when providing statistical correlation with the gravimetric method, which is extremely laborious, takes a long time to be performed, provokes great losses of material, produces relatively large standard deviations, and cannot be used in offshore oil platforms. Spectroscopy methods, such as fluorimetry, can be used as a simpler alternative to determine TOG. However, consent of the regulation agency to use other methods requires an accurate statistical correlation between their results. In this work, TOG values determined by the gravimetric method (using two different extraction solvents: n-hexane and xylene) and fluorimetry (using n-hexane as the extraction solvent) were compared for oily water in the theoretical oil concentration range of 10 to 100 ppm, using a heavy oil to prepare the oily water. Good correlations were obtained for both gravimetry vs fluorimetry, both using n-hexane (R 2 = 0.9630), and gravimetry using xylene vs fluorimetry using n-hexane (R 2 = 0.9857). Moreover, TOG measured by fluorimetry was closer to the real oil concentrations. Therefore, although a specific correlation must be obtained for each kind of crude oil, fluorimetry is a simple, fast, and accurate method, and the correlation is relatively simple to obtain.