Studies on coupling process of sphalerite concentrate leaching in H2SO4-HNO3 and tetrachloroethylene extracting of sulfur were reported. Mechanism of coupling leaching and effects of adding amounts of C(2)l(4), temperature and liquid-to-solid ratio on leaching process were investigated separately. The results indicated that the zinc recovery was up to 99.6 % after 3 h of leaching at 85 degrees C, 0.1 MPa O-2, with 20 g sphalerite concentrate in 200 ml leaching solution of 2.0 mol/l H2SO4 and 0.2 mol/l HNO3, in the presence of 10ml C2O4. The leaching time was 50 % shorter than the common leaching. The coupling effect was distinct. (c) 2004 Elsevier Ltd. All rights reserved.