A dissertation submitted to the Faculty of Science, University of the Witwatersrand, Johannesburg, in fulfilment of requirements for the degree of Master of Science. Johannesburg, 2015. / Excavations conducted at Thaba Nkulu, an Early Farming Community homestead with associated metal working debris, led to the recovery of iron slag, tuyères, furnace lining, iron ore, copper artefacts and iron artefacts. Using the material recovered, this dissertation identified chemical signatures for metal artefacts and metal smelting and smithing associated material. This was achieved through the use of a combination of X-ray fluorescence spectrometry (XRF) and Scanning Electron Microscopy coupled with Energy-Dispersive X-Ray Spectroscopy (SEM-EDX). The artefacts recovered were analysed, and 3 sets of possible chemical signatures were recorded.