SUMMARYSamples may be obtained from outcrops, cuttings, cores, modern sediments and old collections. Coals, brown or grey siltstones and fine‐grained sandstones generally yield the most satisfactory organic matter for maturation analysis, while red beds and evaporites are often barren. Shales with a high organic content are not especially desirable for optical studies of maturation because the organic matter is likely to be very fine‐grained and high in pyrite. The whole rock or a concentrate of organic particles may be prepared for microscopical study, the former being preferred for analysis of solid bitumens and fluorescence study, the latter for measurement of vitrinite reflectance, microspore translucency and refractive index. Crushing, ultrasonic disintegration, handpicking, heavy liquid separation, flotation, settling, sieving and demineralization with HC1 and HF are used to concentrate organic particles. Preparations include polished rock slabs, concentrate briquettes and strew mounts.The constituents with the lowest maturation in a rock must be selected if maturation indigenous to the rock is to be measured. Organic matter that has been previously altered at its site of origin, reworked and altered during diagenesis, or redeposited from older rocks, must be excluded from consideration. The organic constituents are recognized most easily by reflected light microscopy. A combination of fluorescence and reflectance techniques is useful for low rank samp