Flameless atomic absorption spectroscopy with a carbon rod atomizer was used to determine lead, cadmium, and chromium in wholefish samples. Samples were dry-ashed, and the metals were separated by solvent extraction with ammonium pyrrolidine dithiocarbamate in methyl isobutyl ketone, and then back-partitioned into an aqueous acid solution for analysis. The back-partitioning step allows a direct comparison of sample solutions with aqueous solutions of the standard. Recoveries of the metals from fortified samples averaged 91% (±9.6) for lead and 100% (±5.6) for chromium at the 0.1–1 ppm level, and 100% (±13.3) for cadmium at the 0.01–0.1 ppm level.