In this paper, the cloud point extraction and separation of scandium and yttrium (III) via use of Triton X-114 with and without 8-hydroquiloline (HQ) as an added chelate agent are investigated. The effects of various parameters, such as the aqueous phase pH, HQ concentration, Triton X-114 concentration, heating temperature, and incubation time, on the cloud point extraction of scandium and yttrium (III) are studied. The results demonstrate that, there are different extraction and separation behaviors for scandium and yttrium (III) with and without HQ as an added chelate. And in contrast to solvent extraction, cloud point extraction is an excellent method to extract and separate scandium and yttrium (III).