A method of experimentally obtaining both neutron and gamma‐ray spectra in a scattering medium is described. The method utilizes a liquid‐organic scintillator (NE‐213) coupled with a pulse‐shape discrimination circuit. This allows the separation of the neutron‐induced pulse‐height data from the gamma‐ray pulse‐height data. Using mathematical unfolding techniques, the two sets of pulse‐height data were transformed to obtain the neutron and gamma‐ray energy spectra. A small spherical detector was designed and constructed to reduce the errors incurred by attempting spectral measurements in a scattering medium. Demonstration of the utility of the system to obtain the neutron and gamma‐ray spectra in a scattering medium was performed by characterizing the neutron and gamma‐ray spectra at various sites about a 3.7‐μg (1.5 cm active length) californium‐252 source in a tissue‐equivalent medium.