Carbon fiber reinforced thermoset composites such as carbon fiber epoxy composites are widely used in aircraft and aerospace, and are being increasingly used in automotive applications because of their lightweight characteristics, high specific strength, and stiffness. The carbon fiber content in the composite plays a critical role in enhancing structural performance. The carbon fibers contribute to the strength and stiffness; therefore, the mechanical properties of the composite are greatly influenced by the carbon fiber content. Measurement of carbon fiber content is essential for product quality control and process optimization. In this work, a novel carbonization-in-nitrogen (CIN) method is developed to characterize the fiber content in carbon fiber thermoset composites. A carbon fiber composite sample is carbonized in a nitrogen environment at elevated temperatures, alongside a neat resin sample. The carbon fibers are protected from oxidization while the resin (the neat resin and the resin matrix in the composite sample) is carbonized under nitrogen environment. The neat resin sample is used to calibrate the resin carbonization rate and calculate the amount of the resin matrix in the composite sample. The new method has been validated on several thermoset resin systems, and found to yield accurate estimation of fiber content in carbon fiber thermoset composites.