Specimens spanning 10 m across the Cretaceous/Tertiary (K/T) boundary in Core 32 at DSDP Site 527, Walvis Ridge, were analyzed for trace elements and for evidence of shock deformation. Results from INAA/RNAA chemistry of the 45 samples suggest that multiple events are recorded at this site, including at least two enrichments of chalcophile elements possibly related to basaltic volcanism. A major event, coincident with the paleontological K/T boundary, is marked by a strong Ir anomaly and high frequency of shock deformation in quartz and feldspar. A strong secondary peak in elemental enrichment and mosaicism occurs at 1.87 m below the K/T boundary, suggesting appreciable volcanic activity about 10⁵ years prior to the K/T event. Carbon and oxygen isotopes from the site also suggest that changes in climate began before the shock event at the boundary. Correlations between biostratigraphy, isotopes, and the data from this study suggest that the decline in marine productivity over an extended period of time may be the result of complex coupling of basaltic volcanism to climate change.