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This work developed a method based on solid phase microextraction followed by gas chromatography/mass spectrometry (SPME-GC/MS) for the measurement of fluorotelomer alcohols (FTOHs) in gas samples. The method quantification limit (MQL) is 6-7 ng/L for 6:2 fluorotelomer alcohols (6:2 FTOH) and 8:2 fluorotelomer alcohols (8:2 FTOH). In contrast to common methods such as thermal desorption combined with GC-MS, it needs neither pre-concentration equipment nor large sample volume. The extraction-evaporation-GC/MS is commonly used in literature for FTOHs measurement in solids samples. We developed a method to measure FTOHs in solid samples by adding solvent extraction prior to headspace SPME-GC/MS. The extraction-headspace SPME-GC/MS method has a quantification limit of 40-43 ng per gram for 6:2 FTOH and 8:2 FTOH in solid samples. This is comparable to the MQLs for the extraction-evaporation-GC/MS method. Removing the solvent evaporation step decreased the risk of contamination and loss of analytes. The developed methods were successfully used in three examples of solid waste study: 1) measuring 6:2 FTOH and 8:2 FTOH above the MQL in gas emissions from a closed landfill, 2) finding 6:2 FTOH above MQL in 9 of 31 solid consumer products, and 3) finding that the release of 6:2 FTOH in simulated landfills containing popcorn bags was linear at a rate of 3.15 ng/g popcorn bags-day and that partial 6:2 FTOH was from the hydrolysis of precursors., Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests:Youneng Tang reports financial support was provided by Hinkley Center for Solid and Hazardous Waste Management., (Copyright © 2023 Elsevier Ltd. All rights reserved.)