X-ray diffraction line profile analysis has been used to study the microstructure of (111) oriented gold and platinum thin films deposited by thermal evaporation and DC magnetron sputtering. In addition to crystallite size broadening, the profiles from these films displayed broadening arising from dislocations. A parallel investigation, using transmission electron microscopy (TEM) was undertaken to study the nature of dislocations formed, and to provide information on the dimensions of the crystallite columns in the films. X-ray data were collected at room temperature to determine the anisotropy of the broadening with (hkl), using a Siemens D5000 powder diffractometer (CuK alpha radiation) and two high-resolution synchrotron instruments (BM 16 at the ESRF [lambda =0.35 Angstrom] and station 2.3 at the Daresbury laboratory [lambda =1.0 Angstrom]). Two approaches to instrument deconvolution were investigated, Fourier deconvolution and fundamental parameters profile fitting, using Lab,, as a reference material to determine the instrument profile function. After removal of the crystallite size broadening contribution from the measured integral breadths, the residual microstrain broadening was modelled assuming dislocations based on a FCC a/2 < 110 > {111} slip system. The results of the X-ray analysis agreed with dark field TEM micrographs, which showed that many of the crystallites contained dislocations of mixed character (screw-edge).