One of the most powerful predictive tools in sediment biogeochemistry is the electron acceptor layering model, which describes the order in which oxidised compounds are reduced by successions of respiring microbial populations, and how this layering is influenced by benthic macro-organism activity. However, techniques allowing convenient determination of heterogeneous distributions of reduced substances, such as iron(II) and sulfide, have been lacking. A combined diffusive gradients in thin films-diffusive equilibrium in thin films technique was used to quantitatively measure the two-dimensional iron(II) and sulfide distributions at high resolution in the vicinity of various sediment features, including macrofauna burrows, particulate organic matter and macrophyte roots. Substantial heterogeneity was observed for both analytes in all probes, especially in the vicinity of seagrass roots and particulate organic matter. Measured distributions tended to follow the general patterns predicted by the tertiary electron acceptor layering model. However, there was unexpected overlap of sulfide and iron(II) distributions at the millimetre to centimetre scale in several samples from different sediments, notably the more complex sediments containing particulate organic matter and seagrass roots. The cause of such overlap is unclear and further study is necessary to elucidate how such distributions can occur.