This project developed and tested advanced Fourier transform infrared (FT-IR) instruments for process monitoring of black liquor recovery boilers. The state-of-the-art FT-IR instruments successfully operated in the harsh environment of a black liquor recovery boiler and provided a wealth of real-time process information. Concentrations of multiple gas species were simultaneously monitored in-situ across the combustion flow of the boiler and extractively at the stack. Sensitivity to changes of particulate fume and carryover levels in the process flow were also demonstrated. Boiler set-up and operation is a complex balance of conditions that influence the chemical and physical processes in the combustion flow. Operating parameters include black liquor flow rate, liquor temperature, nozzle pressure, primary air, secondary air, tertiary air, boiler excess oxygen and others. The in-process information provided by the FT-IR monitors can be used as a boiler control tool since species indicative of combustion efficiency (carbon monoxide, methane) and pollutant emissions (sulfur dioxide, hydrochloric acid and fume) were monitored in real-time and observed to fluctuate as operating conditions were varied. A high priority need of the U.S. industrial boiler market is improved measurement and control technology. The sensor technology demonstrated in this project is applicable to the need of industry.