The application of a micro-Fourier transform infrared, (μ-FTIR), spectroscopic system, using synchrotron radiation as a light source, for photoresist chemical analysis has been investigated. The better signal to noise due to the high brightness of the infrared radiation from the synchrotron permits higher spatial resolution scans than with a conventional glowbar. This permits a new technique of μ-FTIR spectroscopy, which potentially can get close to diffraction limited resolution, with high chemical sensitivity, for mid-IR wavelengths ranging from 2.3 μm (4400 cm−1) to 9 μm (1100 cm−1). An example of application of imaging the local chemistry changes of a chemically amplified photoresist with post-exposure bake shows the exciting capability of this technique for nondestructive resist exposure process control. © 1997 American Institute of Physics.