Gaining a better understanding of the processes and linkages operating in agricultural catchments is essential in understanding how diffuse sources of pollution influence the water quality of fluvial systems. One of the key limitations is the lack of available data at a range of spatial scales, which is necessary in order to improve process understanding and model development. Carefully designed field-based research has the potential to improve predictions of water quality in agricultural catchments, which is particularly important given the context of changing climate and land use. Event-based fluxes of sediment and phosphorus were monitored at different scales in a first-order agricultural catchment in Herefordshire, UK, and the data have enabled characterisation of their behaviour and identification of relationships at various scales from hillslope patches of 60 m length to a 30 ha first-order catchment. The results shown here indicate the differing behaviour of both sediment and phosphorus over six events throughout two hydrological years between two scales of observation: the hillslope and the catchment.