A new microsystem will be presented which will enable quantitative analysis of the type and concentration of surface species present in real time during quantified NSR reactions, in a geometry identical to a commercial monolith and along the monolith reaction channel, and with simultaneous temperature measurement. The silicon microreactor contains 16 parallel channels (400 µm x 400 µm x 30 mm each) with on-chip heaters and temperature sensors spaced down the length of the channels at 5 mm intervals. Fast, spatially resolved Fourier-Transform Infrared (FTIR) analysis is used in this study to quantify the surface species (adsorbed carbonates, nitrates, and nitrites, etc.) along the catalytic converter channel at 500 µm intervals and up to 1600 Hz sampling rates. Gold-coated optical channels are integrated with path lengths near 20 mm to enable simultaneous product gas analysis for quantitative reactivity assessment. This high speed FTIR technique allows analysis of the transient processes occurring during capture and regeneration cycles of the NSR catalyst. Further, this microfabricated system will also allow determination of the temperature of the catalyst as a function of length along the channel with a degree of accuracy never before reported to aid in the development of NSR reactor models.