<p> In this thesis the Mössbauer spectroscopic technique was applied to a wide variety of antimony compounds. </p> <p> Antimony chalcogenides, oxides and a phosphate were studied. No evidence could be found to support the existence of Sb₂S₅. Sb₂O₄ was found to contain Sb(III) and Sb(V) rather than Sb(IV). SbPO₄ and the Sb(III) site in Sb₂O₄ had similar Mössbauer parameters in agreement with their structures. </p> <p> Hexahalo complexes of antimony, some of which contain both (III) and (V) oxidation states, have been examined. These exhibit extremely large isomer shifts which are interpreted as indicating no involvement of the 5s electron pair of Sb in the bonding scheme. </p> <p> A study was made of some antimony-fluorine systems. The spectra of KSbF₅, KSbF₄ and KSb₂F₇ and similar salts were interpreted in terms of the known structures. Other complex antimony fluorides and fluorosulphates have also been examined and possible structures suggested. </p> <p> Three antimony-containing minerals, nadorite, tetrahedrite, and boulangerite have been examined, and attempts made to rationalise the Mössbauer data in terms of known structural parameters. </p> / Thesis / Master of Science (MSc)