The analysis of toxaphene, a highly complex mixture of chlorinated bornanes, bornenes and camphenes, is a challenging problem, especially as individual congeners are present at trace levels in biota and other relevant samples. The complicated nomenclature of the compounds of interest is briefly discussed. Gas chromatographic techniques are the most important tools in toxaphene analysis because of their high resolution. The main focus of attention is devoted to important steps in the GC-based analytical procedure, such as sample preparation and injection, separation by single-column and multidimensional GC, both heart-cut and comprehensive, and detection by electron capture and, increasingly, MS-based detection/identification. The gradual shift from total toxaphene to individual compound analysis is discussed, and the growing interest in enantiomer-selective separations is highlighted. The problems encountered when selecting appropriate indicator compounds for rapid toxaphene screening are also addressed.