N2 coherent anti-Stokes Raman spectroscopy (CARS) and H2-O2 multiplex CARS employing a single dye laser have been explored to simultaneously determine the temperature and concentrations of H2 and O2 in a premixed H2/air flat flame burner. Systematic calibrations were performed through the well-characterized flame. In particular, the temperature measurement was accomplished using the intensity ratio of the H2 S(5) and S(6) rotational lines, while the extraction of H2 and O2 concentrations was obtained from the H2 S(6) and O2 Q-branches, respectively. Details of the calibration procedure and data reduction are discussed. The associated detection limits as well as calibration errors are also identified.