The properties that might influence the sequestration of aflatoxin B1 (AfB1) were examined. Laser-diffraction, particle-size analysis (LDPSA) indicated that the particle size of the smectite influences the amount of AfB1 adsorbed. Effective adsorbent smectites disperse well under combined sodium hexametaphosphate solution and ultrasonic agitation. Particle size explained 66% of the variability for most of the samples investigated in an ‘as-received’ state. One effective adsorbent smectite was especially well aggregated and required additional physical dispersion, thus raising the correlation to 73%. Transmission electron microscope (TEM) images show typical smectites and reveal the very diverse morphology of smectites in bentonites. Thin, cloud-like smectite, in TEM images, related positively to AfB1-adsorption capacity. Particles that often fold and are usually ~0.5 μm across seem to be optimal. The selection of criteria for evaluating these smectites provides a scientific basis for their selection to obtain reliable performance. Particle size is of particular importance as outlined below, and use of LDPSA makes it possible to perform the analysis efficiently and with precision.