The semiconductor industry currently faces technical challenges in transistor design as traditional materials used for decades are being driven to their physical limits. High‐k materials (k>7 for Si3N4) are being developed as gate oxides for sub 100 nm MOSFETs to prevent electron tunneling between source and drain. Organometallic precursors under consideration could produce hazardous byproducts. Low‐k materials (k<3.9 for SiO2) are being developed as insulators or barriers in the dielectric stack to reduce RC time delays and cross talk between adjacent conductors. Precursors containing carbon or fluorine may increase the emission of CF4during chamber cleans. Heavily doped polysilicon or metals currently in use as gate electrodes may be replaced with metals or metal oxides having greater corrosion resistance or other advantageous properties. All of these new materials must be characterized from the standoint of process byproduct emissions and abatement performance. Gas‐phase analysis is critical to the safe and timely incorporation of these novel materials. Several new applications of Fourier transform infra‐red spectroscopy (FTIR) are presented, including techniques being applied to address some of the current challenges facing the semiconductor industry. This report describes the characterization of various chemical vapor deposition (CVD) processes. Applications of gas‐phase analytical methods to process optimization are also described. © 2003 American Institute of Physics