This report discusses the status of ongoing analytical method development and research activities to support the development of ASTM standard practices and test methods to measure potential chemical emissions from spray polyurethane foam (SPF) insulation designed for on-site application in buildings. The consensus standards are being developed to evaluate SPF products to establish re-occupancy times for trade workers and residents as well as to assess indoor air quality after installation. Three generic foam formulations including closed-cell, open-cell and a low pressure kit formulation were used to evaluate the test protocols. An analytical method was developed with thermal desorption and GC/MS to measure volatile organic compounds (VOCs), e.g., blowing agents, in addition to semi-volatile organic compounds (SVOCs), e.g., flame retardants and amine catalysts. Sample preparation procedures were developed to test SPF samples in micro-scale chambers to accelerate testing. A holding time study was then conducted with the micro chambers to estimate the maximum time after spraying that SPF samples can be stored in sealed Mylar bags without significant loss of compounds of interest. Semi-volatile organic compounds such as methylenediphenyl diisocyanate (MDI), selected amine catalysts and flame retardant were evaluated for potential losses in the conventional small-scale and micro-scale test chambers due to potential wall effects. The conclusions from this research may be used as the basis to develop several ASTM standards on Committee D22 on Air Quality through Subcommittee D22.05 on Indoor Air.