本文提出了在(NH_4)_2SO_4—EDTA—Cu~(2+)—Ni~(2+)体系中以阴极溶出伏安法测定人发中微量硒的方法。并对方法的最佳条件选择及头发样品消化处理进行了研究。实验表明:在0.5M(NH_4)_2SO_4-2×10~(-4)MEDTA底液中,加入少量Cu~(2+)-Ni~(2+),可明显改善汞膜电极性能,提高测定灵敏度,结果有较好的重现性。此方法简便,易行,最低检出浓度可达5×10~(-9)M。 This paper presents a method for the determination of trace selenium in human hair by cathodic stripping voltammetry in (NH_4) _2SO_4-EDTA-Cu ~ (2 +) - Ni 2+ system. The optimal conditions of the method and the hair sample digestion were studied. Experiments show that the addition of a small amount of Cu2 +-Ni2 + in 0.5M (NH4) _2SO_4-2 × 10 ~ (-4) MEDTA can obviously improve the performance of the mercury electrode and improve the determination of Sensitivity, the results have better reproducibility. This method is simple and easy, the lowest detectable concentration of up to 5 × 10 ~ (-9) M.