Abstract: A method for the simultaneous determination of the trace contents of As, Sb, Bi and Hg in the same solution by Hydride Generation-Inductively Coupled Plasma-Atomic Emission Spectrometry (HG-ICP-AES) was established by using 10% hydrochloric acid as the dissolved medium. The soil sample was dissolved in water bath with aqua regia for one hour, and then ascorbic acid-thiourea solution was added to reduce As and Sb in advance without influence on the content of Hg. The elements were determined by a new type self-designed hydride generator coupled with ICP-AES with 10% hydrochloric acid, 0.5 L/min carrier gas and 10 g/L NaHB₄-NaOH as reductants. This method solved the problems of the inconvenience of multi-element determination and more reagent consumption. The sample pre-treatment and determination were easy, rapid and had no memory effect. The detection limits of the method were 0.01-0.06 ng/g, the recoveries of standard materials were between 92.0% and 102.0%, and RSD was less than 5%. This method is suitable for the simultaneous determination of the trace contents of As, Sb, Bi and Hg in environmental samples.