Various testing methods and techniques have been used to identify and quantify per- and polyfluoroalkyl substances (PFAS) in food packaging. A common indirect measurement of PFAS is total fluorine (TF) and total organic fluorine (TOF). These methods are critical in rapidly screening food packaging materials for the >9000 PFAS and are often globally used for regulatory limits. However, this destructive approach requires careful sample preparation, combustion, and the analysis of the solution by a fluoride-specific electrode. The method described herein is a cost-effective, rapid, quantitative, and externally validated initial screening of packaging materials for fluoro-chemistry. This study presents validated protocols for measuring TF and TOF in packaging substrates using oxygen combustion sample preparation coupled with fluoride ion-selective electrode (F-ISE); the materials and required equipment are provided, and the step-by-step procedure from sample preparation to the analysis are described, including critical steps to minimize contamination and interferences during sample preparation.