Indoor Air Quality monitoring in cultural institutions is of particular concern to protect these places and the cultural heritage content. An indoor monitoring campaign was performed in three museums in Florence (Italy) to determine the occurrence and levels of volatile organic compounds (VOCs). VOCs of interest included BTEX (benzene, toluene, ethylbenzene, xylenes), terpenes, aldehydes, organic acids, and cyclic volatile methyl siloxanes (cVMS). The most abundant VOCs in all samples analyzed were BTEX, which were strictly related to the traffic source, followed by siloxanes and terpenes. Among BTEX, toluene was always the most abundant followed by xylenes, ethylbenzene, and benzene. cVMS in exhibition rooms with the presence of visitors showed higher values compared to samples collected when the museums were closed. Terpenes showed not only the influence of vegetation‐biogenic sources surrounding a museum but could also be related to the wood used for the construction of showcases and furniture and the use of cleaning products. Data obtained also showed the presence of organic acids and aldehydes whose source can be traced back to exhibits themselves and wood‐based furniture. Assessing the levels of organic acids in museums is important because, over time, it can cause deterioration of the artifacts.