Thallium is a typical hazardous waste. In the process of mineral selecting and smelting, the thallium in the recycled zinc raw material is discharged into the environment in the form of oxide or dust, which poses a serious threat to the environment and human health. The regenerated zinc composition is very complex. If the sample digestion is not complete, it directly affect the accuracy of the measurement results. In this paper, the effects of microwave digestion and electric hot plate digestion at atmospheric pressure were compared, and the results showed that the microwave digestion method was fast and environmentally friendly, but for the regenerated zinc samples that were difficult to digest, there was a significant decrease in the oxidative capacity without the addition of perchloric acid. So the sample was not completely dissolved, which directly resulting in the low thallium measurement results. However, the sample dissolved by a mixed acid composed of perchloric acid, nitric acid, hydrochloric acid-and hydrofluoric acid, covered with polytetrafluoroethylene cover at low temperature, and on electric heating plate under constant pressure, which effectively solved the pretreatment problem of regenerated zinc samples. In this experiment, the samples were digested by a mixed acid composed of nitric acid, hydrochloric acid, hydrofluoric acid and hydrochloric acid (volume ratio is 10 : 5 : 5 : 3), extracted by 5% hydrochloric acid. Tl 190. 794 nm was selected as the analysis line. The analytical method for measuring thallium in regenerated zinc by inductively coupled plasma atomic emission spectroscopy (ICP-AES) was established. Under the set optimal instrument conditions, when Tl mass concentration was 0. 10 jug/mL to 5. 00 jng/mL, the emitted light intensity showed a good linear relationship with the mass concentration, the linear regression equation was y= 180. 77a: -- 0. 46, the correlation coefficient was 0.999 98. The interference experiments showed that at the set upper limit of coexisting ion interference, Pb, Zn, Cu, Fe, Ca, Bi, Sb, Sn, As, Al, Cd, Si, Ag had almost no effect on the determination of thallium in regenerated zinc. According to the test method, thallium in five regenerated zinc samples with different content levels was measured 11 independent times, and the measurement range was CD (Tl) 0.0041%--0.21%, the detection limit of the method was 0.004 jug/mL, the experimental relative quasi deviation (RSD) was 2. 1%--3. 2%, and the recovery of spike was 97. 3%--108%. The method is simple and operable, which can quickly and accurately determine thallium in regenerated zinc. [ABSTRACT FROM AUTHOR]