This research aims to study the air pollution due to fine Particulate Matter of radius less than 2.5µm (PM2.5) and Black Carbon concentration (BC) in air samples. Aerosol PM2.5 samples were collected from the rooftop of the National Oncology Center site in Al-Zubairy area in Sana’a Yemen. A Microprocessor Controlled Aerosol Sampling device ISAP1050e (Gerhard Schulze Automation Engineering, Germany company) was used to collect samples. The mass concentration of PM2.5 of collected samples ranged from 14.27 to 159.09 µg/m3 with an average of 32.66µg/m3. The PM2.5 results were compared with the World Health Organization (WHO) 2005 guideline of PM2.5 concentration in air. Statistical analysis showed a positive correlation between PM2.5 concentrations and temperature for both fall and summer samples. However, analysis showed a positive correlation between PM2.5 concentrations and relative humidity for fall samples and a negative correlation for summer samples. The black carbon (BC) concentrations in PM2.5 samples were measured using a Smoke Stain Reflectometer (SSR) device. The BC concentration ranged from 1.84 to 3.90 µg/m3 with an average of 2.90 µg/m3. The BC results were compared with some international reported results. The Air Quality Index (AQI) of 78.95% of PM2.5 concentrations was higher than the standard limit (AQI < 100) developed by the United States Environmental Protection Agency (EPA).