A sequential extraction procedure was applied to acid sulfate soil materials from a soil profile to investigate the effect of sample pretreatment on the geochemical fractionation of selected metals. The samples were prepared for analysis by oven-drying, sieving and grinding the soil, or were examined as collected in field condition. The soil profile encompassed oxidising conditions near the surface, through to reducing conditions at depth. Six metals (Fe, Cr, Ni, Mn, Cu, and Zn) were measured during the sequential extraction procedure, and their fractionation determined in the oxidised and in the reduced zone. Although cumulative totals (the sum of all steps in the sequential extraction procedure) for the metals extracted from both the field condition and dried/ground samples were similar, some significant differences in fractionation within individual extraction steps were observed. Of particular interest was the redistribution of metals from the sulfide-bearing (pyrite-bound) fraction to the more readily available fractions (i.e. labile and acid-soluble), as a result of oven-drying and grinding. The results indicate that when assessing metal fractionation in acid sulfate soil materials, samples should be analysed in field condition in order to avoid the considerable metal fractionation artifacts that are induced by drying and grinding.