A solid-phase dispersive microextraction procedure has been developed using ferrite (Fe3O4), an inexpensive magnetic material, as an adsorbent for the separation and subsequent determination of Ga(III) and In(III). The ions were removed from an aqueous solution by adsorption on Fe3O4, which was next easily collected from the medium by the action of a magnet. The analytes were then desorbed using 50 µL of 2 M NaOH or 50 µL of a 4:1 mixture of 0.1 M EDTA and 2 M HNO3 for the determination of Ga(III) or In(III), respectively. The level of the elements in the desorption phase was measured by electrothermal atomic absorption spectrometry (ETAAS) by injecting 10 µL of this phase into the atomizer. The enrichment factor was 163, and detection limits of 0.02 and 0.01 µg L−1 were achieved for Ga(III) and In(III), respectively. The reliability of the procedure has been verified by means of standard reference materials and by means of standard additions. Results are given for waters, soils and samples obtained from various electronic devices. It is of note that the procedure could be the basis for a useful way of recovering these valuable elements from different matrices for reuse.