To meet the growing demand for personal protective equipment following the beginning of the COVID-19 pandemic, face mask production from existing and new manufacturers increased drastically. Testing masks to confirm they do not contain chemical residues, such as volatile organic compounds (VOCs), that may off-gas during normal wear is an integral part of this quality control process. This application note presents a method based on ISO-18562 and ISO-10093 to detect and quantify VOCs in face masks. Utilizing a solvent-free headspace extraction and GC/MS analysis, this method is ideal for PPE producers seeking a quick and precise method to ensure safety and quality standards are met during the production process.