The microscopic structure of skeletonized films of cadmium arachidate has been studied by atomic force microscopy (AFM)-skeletonization is the removal of free acid from a mixed Langmuir-Blodgett (LB) film consisting of a fatty acid salt and the free acid. The preparation of the LB films and the AFM methods used are detailed, AFM images and results from a two-dimensional fast Fourier transform analysis are discussed, and factors affecting the overall cadmium arachidate content of the transferred film are considered.