Volatile Organic Compounds (VOCs) are unavoidable aspects of foods and their packaging. Some VOCs provide pleasant odors and contribute to flavor profiles, while others can cause negative health and environmental effects. VOCs are most commonly measured using headspace gas chromatography, and more recently, kinetic techniques such as solid phase microextraction (SPME). In microwave popcorn, diacetyl and possible other related substances (DAPORS) have recently become an emerging concern. Diacetyl was first discovered to cause bronchiolitis obliterans (BO) in microwave popcorn plant workers, but some claim levels of these compounds in microwave popcorn is of concern to consumers; particularly because of the high temperatures reached during cooking. Eight DAPORS were analyzed using SPME/GC-MS in both high-fat and low-fat varieties of microwave popcorn. Results found elevated levels of diacetyl and 2,3-pentanedione in low-fat varieties. Diacetyl was below the limit of detection in high-fat varieties. Because of the close proximity of these compounds to both plant workers and the consumers, solutions are now being developed to monitor VOC contamination in real time during manufacture of microwave popcorn. Additionally, real-time monitoring technologies can be applied to a wide variety of compounds and packaging substrates to monitor organic and inorganic contamination. A combination sensor array technology was developed in conjunction with a proprietary neural network. The array was successfully trained to detect and predict contamination in thermoplastics. This technology has application in detecting VOCs of interest both in total concentration, and speciation of certain chemical functional groups.