The kinetics of thermal decomposition of samarium and praseodymium hexadecanoate (palmitate) was found to be of zero order and the energy of activation for the decomposition reaction for samarium and praseodymium hexadecanoate was in the range of 30-35 KJ mol-1 .The X-ray analysis showed that samarium and praseodymium hexadecanoate soaps have double layer structure with molecular axis slightly inclined to the basal plane. The IR results confirmed that the fatty acids exists with dimeric structure through hydrogen bonding between the carboxyl groups of two acid molecules, whereas the metal soaps have an ionic character.