A three-phase, 11-day training program designed to monitor elemental mercury (Hg0) emissions originating from gold shops was conducted in Georgetown and Bartica, Guyana, during May of 2019. The first phase consisted of interactive lectures and discussions on mercury use in artisanal and small-scale gold mining throughout Guyana, the region, and the world. In addition, specific training in the theory and use of analytical instrumentation to quantify Hg0 pollution associated with the processing of amalgams and sponge gold occurred. Trainees participated in the mapping of smelting facilities in Georgetown where, outside of one gold shop, Hg0 concentrations exceeded 100,000 ng/m3. During the second phase of training, a subset of trainees traveled to Bartica, where they mapped the town center to identify point sources of Hg0 pollution, all of which corresponded to the location of shops where amalgams and sponge gold were heated and purchased. Once mapped, Hg0 concentrations were measured during the smelting of gold inside the Guyana Gold Board (GGB) facility and two privately-owned gold shops. Maximum Hg0 concentrations at the GGB facility did not exceed 98,700 ng/m3 during the measurement period, while maximum concentrations at the two privately owned shops were measured as 527,500 ng/m3 and 302,200 ng/m3. With guidance from the training team, trainees were responsible for the collection and interpretation of all data. The third phase of the training involved the collaborative production of a report summarizing the findings from the training. This work represents the first formal training opportunity for the assessment of Hg0 concentrations in and around gold shops in Guyana, and provides baseline data to assist the government of Guyana to generate air quality standards for Hg0 emissions.