In the context of workplace safety, activated carbon in the fiber form (i.e., activated carbon fiber, ACF) represents an alternative adsorbent to granular activated carbon (GAC) for use in organic vapor respiratory protection devices. ACFs are high surface area carbonaceous materials that are often available in a self-supporting non-woven form. The physical form of ACF suggests the potential for a filtration medium that is capable of supporting both organic vapor adsorption and particulate filtration. To study the application of these materials in respiratory protection devices, ACFs (ACFF 1200 m2/g, ACFF 1800 m2/g, and ACFF 2000 m2/g) were challenged with representative organic vapors (toluene, hexane, and methyl ethyl ketone (MEK)) at an occupationally relevant concentration (200 ppm). Breakthrough curves were generated for at least three different bed weights of adsorbent. Pressure drop (i.e., the resistance across the filtration media) was also measured to determine maximum ACF bed depths for use in respiratory protection devices. Breakthrough experiments indicate that ACFF 2000 has the highest adsorption capacity for toluene (381 mg/g), followed by ACFF 1800 and ACFF 1200 (344 mg/g and 239 mg/g, respectively). A similar trend was observed for hexane: 221 mg/g, 196 mg/g, and 146 mg/g for ACFF 2000, ACFF 1800, and ACFF 1200, respectively. ACFF 1200 showed the highest adsorption capacity for the polar adsorbate MEK (168 mg/g), followed by ACFF 1800 and ACFF 2000 (166 mg/g and 147 mg/g, respectively). Based on the constraints of pressure drop, it seems unlikely the exclusive use of ACF in a filtering facepiece respirator can provide an adsorbent mass sufficient for full shift protection against organic vapor contaminants at or above the legally enforceable permissible exposure level (PEL). Nevertheless, the incorporation of ACF into a facepiece respirator appears promising for “nuisance odor” applications; i.e., the further reduction of organic vapor concentrations when workplace exposures are already below PEL concentrations. Implications: This research brings innovation to the field of occupational health and air pollution control technology by investigating the adsorption performance of activated carbon fiber (ACF) media in the context of worker respiratory protection. ACF properties such as high specific surface area (m2/g), high permeability to airflow, and rapid adsorption kinetics make it ideal for use in thin, N95-style respirators for organic vapors. Respiratory protection is an exciting and relevant application for ACF media. A lightweight adsorbent such as ACF, if incorporated into an N95-style respirator, could potentially provide nuisance-level VOC protection in a physical form that is accessible to workers and consistent with OSHA’s voluntary use provisions for facepiece respirators. The research presented in this manuscript represents one of several steps planned in the characterization of ACF media for this particular application.