This research is the study concerning in both qualitative and quantitative analysis of 4,4'-methylenebis (2-6-di-tert-butylphenol), phenolic antioxidant in lubricant using thin layer chromatography (TLC) technique coupled with diffuse reflectance infrared fourier transform (DRIFT) spectroscopy. The research consists of the qualitative analysis of the sample coated on TLC sheet compared with transmission technique the study of DRIFT spectroscopy, the determination of the sample coated on TLC sheet using DRIFT spectroscopy and the confirmation of the determined value from calibration curve by densitionmeter. It was found that this applied technique can be used well in both qualitative and quantitative analysis. Beyond this the sample separated by TLC technique can be used in situ with DRIFT spectroscopy that is so convenient, less operating cost, and chemical used. However, this technique can only be applied under limitation that the concentration of the sample must be high enough to overcome the absorption of silica gel coated on TLC sheet because silica gel can absorb infrared in the frequency region 1300-800 Cm-1