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A quantitative X-ray Photoelectron Spectroscopy (XPS) analysis of deposits formed from a microwave sustained hexamethyl disiloxane (HMDSO) plasma is undertaken. Curve fitting of the Si 2p core level has been achieved using component peak binding energies determined from standard compounds. The pure HMDSO plasma deposit was dominated by Si(–O)₂ (44%) environments indicating a large proportion of siloxane bond formation in the plasma environment. The introduction of 200 sccm (standard cubic centimetres per minute) of oxygen to the plasma produced a deposit in which half the silicon atoms were co-ordinated with four oxygen atoms while the majority of the remaining silicon was co-ordinated to three.