The distribution equilibrium: AuCl4-+(Bu4N+, ClO4-)HCCl3 ⇌ (Bu4N+, AuCl4-)HCCl3+C1O4-, has been examined. With acidic aqueous chloride solutions in which -log ([H+] [Cl-]) 1 2 is greater than 2, the apparent equilibrium constant, KA, is a constant equal to the equilibrium constant of the distribution reaction above; a value of 2.88·103 was obtained. Combination of the extraction with a direct spectrophotometric determination of AuCl4- in chloroform at 312 nm provides a simple, rapid, and accurate analytical method for the separation and determining of gold in the μg-range. © 1969.