Abstract: HG-AFS was applied to the simultaneous determination of selenium and germanium in poultry offal. The sample was digested with HNO3 and H2O2 in a microwave digestor. Thiourea was added to the sample solution as pre-reductant and 20 g·L-1 KBH4 solution (dissolved in 5 g·L-1 KOH solution) was added as reductant. Linear relationships between values of fluorescence intensity and mass concentration of selenium and germanium were found in the same range within 500 μg·L-1, with detection limits (3s/k) of 0.001 08 μg·L-1 and 0.017 1 μg·L-1, respectively. Values of recovery found by standard addition method were in the range of 98.9%-102% for selenium and 97.4%-102% for germanium.