12 samples from an assay process chain were submitted to qualitative and quantitative neutron activation analysis for the determination of gold. Gold was detected and quantitatively determined in three samples after a chemical separation consisting of solvent extraction and precipitation steps. Recoveries ranged between 81.0 and 93.6% and results of duplicated determinations were reproducible. Quantitative data were obtained from gamma-spectrometric photopeak-area counting. Interference from fast neutron reactions was negligible.