Kilogram-size samples can be analysed via Large Sample Instrumental Neutron
Activation Analysis (LS-INAA), a method developed for samples which are in
homogeneous at the scale of a small sampling portion but which are assumed
to be macroscopically homogeneous. However, extreme inhomogeneities affecti
ng the total gamma-ray detection efficiency, may severely affect the qualit
y of the analysis. A method has been developed to monitor large activated s
amples for the presence of such extreme inhomogeneities. In addition, a met
hod has been developed for the determination of the spatial distribution of
the induced radioactivity. These methods have been tested using a cylindri
cal phantom, simulating a large activated sample, with a local inhomogeneit
y. With a collimated detector, the activity was measured stepwise at 2 cm h
eight intervals and 120 degrees rotation intervals, resulting in 150 gamma-
ray spectra at 45 seconds per spectrum. The activity distribution is retrie
ved from the measured spectra, employing a linear least squares matrix inve
rsion of the detection efficiency matrix. This matrix is based on Monte Car
lo computed detector responses and experimentally determined transmission c
oefficients. It is concluded that the proposed method can be employed in a
system for 3D-LNAA of large samples.