The goal of the project reported herein was to develop and apply methodsfor the analysis of the major components of the solvent system used in the Caustic-Side Solvent Extraction Process (CSSX). These include the calix(4)arene, the modifier, 1-(2,2,3,3-tetrafluoro propoxy)-3-(4-sec- butylphenoxy)-2-propanol and tri-n-octylamine. In addition, it was an objective to develop methods that would allow visualization of other components under process conditions. These analyses would include quantitative laboratory methodsfor each of the components, quantitative analysis of expected breakdown products (4-sec-butylphenol and di-n-octylamine), and qualitative investigations of possible additional breakdown products under a varietyof process extremes. These methods would also provide a framework for process analysis should a pilot facility be developed.