The preparation of palynomorphs for microscopy has traditionally used hydrochloric acid (HCl), hydrofluoric acid (HF) and nitric acid (HNO 3). The use of these acids is both expensive and hazardous. An effective technique of preparation using sodium hexametaphosphate [(NaPO 3) 6 ] has been developed. The cleaned, crushed and softened sample is treated with (NaPO 3) 6. The deflocculated clay is then sieved away and the residue centrifuged. This method has been successfully tested on seven Jurassic to Quaternary sample sets from the United Kingdom (UK) and Antarctica. In five of these sets, the rock/sediment was prepared using the mineral acid technique and the (NaPO 3) 6 procedure. Four of these five sample suites were prepared by both methods quantitatively, so that the concentrations of palynomorphs can be compared. The (NaPO 3) 6 method largely proved to be equally as effective as the mineral acid procedure. The Lower Toarcian Whitby Mudstone Formation of Leicestershire and the Middle and Upper Albian Gault Formation of Kent both produced similar palynomorph/kerogen associations. Some differences between the two procedures were, however, noted. The (NaPO 3) 6 method produced significantly better results than acid preparations for the uppermost Cretaceous (Maastrichtian) of Antarctica and the Pleistocene Till of northern England. By contrast, the majority of the samples from the in situ late Campanian-early Maastrichtian White Chalk Subgroup of north Norfolk prepared using HCl, were significantly richer in palynomorphs than those treated with (NaPO 3) 6.