A novel spectroscopic method was developed to measure quantitatively and simultaneously solids volume fraction (1Àe) and gaseous species composition (Y i ) in a gas/ solid system. The method was comprised of an FT-IR coupled to a fiber-optic probe that could perform real-time and in situ measurements of absorbance. The effect of (1Àe) and Y i on the absorbance spectra were additive and could be independently calibrated. Experiments were conducted with alkane/nitrogen mixtures and two types of particles: sand and FCC. Fuel mole fractions and (1Àe) were varied between 1.8-10.1 mol % and 0-0.45, respectively. The relative errors for Y i time-averaged measurements were below 6% and the error increased significantly with decreasing beam intensity. A proof of concept for a novel application in fluidized beds was also completed: the fiber-optic probe was used to measure the molar fraction of a tracer gas inside the emulsion and bubble phases during gas tracer experiments.