The conformational order of sodium dodecyl sulfate (SDS) adsorbed at the D2O-CCl4 interface has been examined by total internal reflection sum-frequency vibrational spectroscopy. A change in conformation of the alkyl chain with increased surface coverage at the liquid-liquid interface is observed. A series of aqueous surfactant concentrations have been examined in order to determine the effect of surface coverage on the conformation of the alkyl chains at the interface. Polarization studies indicate that, for the concentration range examined, the symmetry axis of the terminal methyl group on the alkyl chain is oriented primarily along the surface normal. Identification of spectral features in the C-H region of the infrared region is facilitated by examination of the sum-frequency spectrum from an analogous deuterated compound.