Diffuse reflectance infrared spectroscopy technique possesses a decided advantage to many classical transmission spectroscopic studies of petroleum fractions and related materials. where the solids are dispersed and encapsulated in a matrix. The detailed and comprehensive diffuse reflectance infrared spectroscopic study on the sediments derived from visbroken residues after prolonged storage at ambient aging conditions are reported. The technique provides a better degree of characterization and high quality data on the structure and chemistry of sediment formation during visbreaking and storage at ambient aging conditions. The study also provides a new insight into the visbreaking reactions, which especially influence the nature and extent of sediment formation.