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It is widely accepted that air entrainment, a purposeful introduction of small air bubbles in concrete, is critical to the long-term durability of concrete in freeze-thaw environments. Air entraining admixtures (AEA) are added to the mixture to stabilize air bubbles created during mixing, ensuring a proper air void system in the hardened concrete. Despite the complexity of creating a suitable air void system in concrete, previous study and experience established the reliability and robustness of such systems under a variety of conditions through use of neutralized vinsol resin (NVR) AEA products. In recent years, synthetic AEAs have been used more frequently due to limited supply of NVR to the concrete industry. With the use of synthetic AEAs, there are more reports of new problems including difficulties in accurately measuring the air content. This study was conducted to find the root cause of the increasing difficulties in controlling the air contents in portland cement concrete associated with synthetic AEAs. Main challenges included the lack of existing techniques to evaluate AEAs and air bubbles in concrete, and lack of data to help identify causes. Given these challenges, a multi-scale experimental study that included testing of field and laboratory concrete, and testing of foam and individual air bubbles was undertaken. The results indicate that the disparity between QC test results and the actual air contents in concrete pavements associated with the use of synthetic AEAs could be attributed to less robust air bubbles stabilized with synthetic AEAs compared to those entrained with NVR and the resulting increased loss of these air bubbles during concrete sampling. The cause of this decreased robustness and resulting air loss was traced directly to the properties of the bubble shells. The shells of air bubbles in concrete entrained with synthetic AEAs were thinner and less stiff than those associated with an NVR AEA. Through this research new test protocols were developed to measure stiffness and thickness of the shell of air bubbles extracted from cement paste and to quantify stability of foams of AEAs in a cementitious environment. These tests could be used by researchers and practitioners who are interested in developing new admixtures and/or identifying admixtures with undesirable performance.