Laboratory demonstrations of synergistic mixture interactions in human odor perception have been rare. The current study examined perithreshold mixture interactions between maple lactone (ML) and selected carboxylic acids. An air-dilution olfactometer allowed precise stimulus control. Experimenters measured stimulus concentrations in vapor phase using a combination of solid-phase microextraction and gas chromatography/mass spectrometry. A probability of detection versus concentration, or a psychometric, functions was measured for pure ML. Psychometric functions were also measured for ML with the addition of fixed, subthreshold concentrations of carboxylic acids. Relative to statistical independence in detection, clear synergy occurred over a range of ML concentrations. To the best of our knowledge, the current results constitute the first clear demonstration of synergy in odor detection by humans from an experiment that combined precise stimulus control, vapor-phase calibration of stimuli, and a clear statistical definition of synergy.