Short peptide sequences consisting of hydrophobic and hydrophilic amino acid units are capable of self-assembly to lead to interfacial adsorption and solution nano-aggregation. Because these peptide molecules bear basic resemblance to conventional alkyl chain surfactants, it is useful to compare their surface and interfacial activity and to explore how surfactant science can be applied to this new series of surface active species. Peptide surfactants differ from alkyl chain surfactants in that they are essentially short graft polymers and that the backbone carries labile hydrogens capable of hydrogen bonding. This work will mainly focus on the use of peptide surfactants such as A3K1, A6K1 and A9K1 to work out the main structural features of interfacial layers. Partially deuterated peptide surfactants will be used to enhance structural resolution within the adsorbed layer.