The influence of acid volatile sulfide (AVS) on the partitioning of Cd, Ni, and Zn in porewater (PW) and sediment as reactive metals (SEM, simultaneously extracted metals) was investigated in laboratory microcosms. Two spiking procedures were compared, and the effects of vertical geochemical gradients and infaunal activity were evaluated. Sediments were spiked with a Cd−Ni−Zn mixture (0.06, 3, 7.5 μmol/g, respectively) containing four levels of AVS (0.5, 7.5, 15, 35 μmol/g). The results were compared to sediments spiked with four levels of Cd−Ni−Zn mixtures at one AVS concentration (7.5 μmol/g). A vertical redox gradient was generated in each treatment by an 18-d incubation with an oxidized water column. [AVS] in the surface sediments decreased by 65−95% due to oxidation during incubation; initial [AVS] was maintained at 0.5−7.5 cm depth. PW metal concentrations were correlated with [SEM − AVS] among all data. But PW metal concentrations were variable, causing the distribution coefficient, Kd_pw (the ratio of [SEM] to PW metal concentrations) to vary by 2−3 orders of magnitude at a given [SEM − AVS]. One reason for the variability was that vertical profiles in PW metal concentrations appeared to be influenced by diffusion as well as [SEM − AVS]. The presence of animals appeared to enhance the diffusion of at least Zn. The generalization that PW metal concentrations are controlled by [SEM − AVS] is subject to some important qualifications if vertical gradients are complicated, metal concentrations vary, or equilibration times differ.