We report on an interdisciplinary study of ceramic material excavated in 1999 and 2001 at a 1000-year old ceramic and metal production site, located at Huaca Sialupe in the La Leche valley on the north coast of Peru and dating to the Middle Sicán period (AD 900–1100). Sherds of Sicán red- and blackware, numerous moulds, several kilns and other evidence of pottery making were found. The pottery, in particular, is famous for its fine texture and perfect black surface finish. In addition, some clay lumps and sherds of unfired Sicán pottery were excavated. Within the same workshop several large inverted ceramic urns used as furnaces were found together with Middle Sicán metal working tools and debris. Various physical methods were applied to investigate this material. The ancient firing procedures could be elucidated by comparing the spectra observed for the ancient sherds with model spectra of laboratory and field fired clay samples. This shows that the fine ware made at Huaca Sialupe was intentionally fired under strongly reducing conditions at temperatures up to 900°C. Reoxidation at the end of the reducing firing took place only occasionally. Less care was taken in firing moulds used for pottery making.