A new Compton suppression system (CSS) for the gamma-ray spectrometer portion of the neutron activation analysis (NAA) was set up at the RPI/ITN. The pneumatic transfer system, SIPRA, for short-lived nuclides and cyclic irradiations was improved. A full calibration procedure of the CSS and SIPRA systems was performed. Two certified reference materials, NIST-SRM-1572 (Citrus Leaves) and NIST-SRM-1633a (Coal Fly Ash) were analyzed using the calibration factors. The CSS was instrumental in lowering the detection limits of Cr, Fe, Hg, Rb, Sr, Th and Zn by reducing background and/or spectral interference considerably. The analytical results were evaluated by comparison to the NIST certified values with deviations ranging from 2% to 8% for the above mentioned elements, except Zn ranging from 10% to 15% for biological and environmental samples, respectively.