This paper reports on the non-destructive analysis of 42 samples of copper alloy and glass from sites in Libya, using semi-quantitative μXRF, carried out as part of the work of the Trans-Sahara Project funded by the European Research Council. These are among the first chemical analyses to be performed on metals and glasses of any period found in Libya, and the results – though preliminary – raise some interesting possibilities. In particular, we discuss some possible indications with regard to the practice of recycling glasses, as evidenced through heterogeneous, malformed glass beads with variable quantities of lead. A glass mirror from Ghirza was also found to be backed in lead, and was probably the result of a glass-making technique still practised in recent times in India. The metal analysis has revealed evidence of a pre-Islamic trade in brass in the northern Sahara, as well as showing the presence of objects made from the mixing of different types of scrap metal, a process probably taking place at the Garamantian metalworking site of Saniat Jibril among other locations. The importance of further analysis of available Libyan and other North African metal artefacts and glasses for the contextualisation and extension of these findings is emphasised.