Copper ferrite spinel oxide (CuFe2O4) samples with calcination temperatures ranging from 500 to 900 degrees C were synthesized using the sol-gel combustion method with citric-nitrate precursors. Each calcined sample was further characterized and carefully analyzed for its structure, morphology, porosity, magnetic property and reducibility. For the first time, the catalytic performance of the ferrite spinels was examined for palm oil methanolysis. The characterization results from X-ray diffraction (XRD), extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge structure (XANES) analyses revealed that the major part of the active species was divalent ions of Cu2+ and Fe2+ and that they played a crucial role in the activity of the considered spinel. catalysts. The catalytic behaviors strongly depended on the crystallinity of spinel structures and operating parameters, such as the catalyst loading and methanol to oil molar ratio. The CuFe2O4 calcined at 700 degrees C was the most active and selective for methanolysis with palm oil. No activity decline was observed over the catalyst after it was reused for 5-cycles without any post-treatment. Easy and effective catalyst separation could be obtained when magnetization was applied to the magnetic spinel catalysts. (C) 2016 Elsevier B.V. All rights reserved.