Different types of iron ore and pyrite were used to craft a wide variety of reflective artifacts in pre-Columbian Mesoamerica, including “mirrors,” pectorals, necklaces, and dental inlays, among others. In the Maya region, most of these have only been visually assessed, without using analytical techniques. Consequently, our understanding of the diversity of raw materials used in artifact production has been limited. This article presents preliminary results from a pilot study aiming to identify the raw materials used in the manufacture of different reflective objects from a small sample of finds from the sites of La Corona and Cancuen, located in Guatemala, through the use of scanning electron microscopy with EDS detectors (SEM-EDS), energy-dispersive X-ray fluorescence (EDXRF), X-ray diffraction (XRD), and Raman spectroscopy. Although further analyses are needed to confirm the representativeness of the sample, these results indicate the use of hematite and goethite (iron oxides), but not pyrite (iron sulfide). This study also shows how improved knowledge of raw material use can elicit previously unknown patterns of distribution and exchange, and highlight patterns of inter- and intrasite variability in the production, use, and exchange of reflective objects over time in the Maya region throughout the Classic period.