Many hydrometallurgical and chemical processes produce large amounts of acid waste. This is illustrated by the copper S/X-E/W process used at the Mount Gordon mine in North Queensland, which produces a tank house bleed in the form of a concentrated sulphuric acid stream. The bleed stream is necessary to remove impurities such as iron that decrease the efficiency of the electrowinning process. However, this bleed stream comes at a high financial cost due to large quantities of make up sulphuric acid required as well as the need to neutralise the bleed stream prior to disposal. The present work describes the approach taken to develop a solvent extraction process for the selective recovery of sulphuric acid from copper tank house bleed liquor. The proposed extraction system was investigated using a branched long chain aliphatic tertiary amine tris(2-ethylhexyl)amine (TEHA) as the extractant, Shellsol 2046 as the diluent and octanol as a modifier. Computer simulations were used to determine the optimum operating conditions for the recovery process. It was found that the process was able to selectively recover up to 90 per cent of the sulphuric acid from the copper electrolyte. This is recovered as a pure aqueous acid stream at a concentration of up to 130 g/L that can be recycled back into the tank house circuit or other areas of the process. The raffinate acid concentration was reduced from 180 g/L to as low as 18 g/L, significantly reducing waste disposal and the environmental impact of the copper process. The equilibrium data and simulation results were also compared with an alternative extractant, CYANEXR 923. Finally the efficiency of the TEHA extraction system was investigated on a pilot-scale in a pulsed perforated plate column. This information was used in order to scale the process for an industrial application. The same methodology applied in this case study could be used to provide innovative and cost-effective solutions to waste streams encountered in other hydrometallurgical or chemical processes.