Silver nanoparticles (AgNPs) and gold nanoparticles (AuNPs) can be separated of their ions by a magnetic dispersive micro-solid phase extraction procedure using non-functionalised ferrite particles. The separation and speciation are based on careful control of the acidity of the medium, without involving oxidation-reduction processes. Thus, using a small amount of ferrite particles (2 mg for a typical 10 mL sample) which is added to the sample as a suspension, Ag(I) as well as both gold species are retained in the sorbent at pH 4, while AgNPs are retained at pH 8. For the selective retention of AuNPs, ammonium diethyl dithiophosphate is added to the medium and the extraction process is repeated at pH 4. In all cases, the analytes are desorbed by treating the solid phase separated by the magnet with 0.1 mL of a thiourea solution at pH 3 and determined by electrothermal atomization atomic absorption spectrometry. For the measurement of silver, a palladium salt is used as a chemical modifier. This is not required for the determination of gold. The enrichment factor is 97 and the detection limits are 12 and 4 ng L−1 for gold and silver, respectively. The reproducibility is close to 5% for the four analytes studied. The reliability of the procedures is checked by standard additions and by the use of four standard reference materials with certified total silver content. Several water samples are analysed, and speciation results are given.