A surface pretreatment for aluminum and titanium involving the reaction of phosphonic acid (RPO(OH)2), R=butyl or vinyl for aluminum and R=vinyl for titanium, has been investigated. The durability of phosphonic acid-pretreated samples was compared with that for P2-etched (ferric sulfate-sulfuric acid) adherends. Samples were bonded with LaRC-IA adhesive in a wedge test geometry. Environmental testing consisted of static and cyclical exposure for 240 hours in three atmospheres: 1) 170°C, 2 torr; 2) -20°C; 3) 60°C, 70% relative humidity. Crack propagation arrested within 48 hours. The order of durability in static environmental tests for aluminum was vinyl phosphonic acid > P2 > butyl phosphonic acid. The durability performance was reversed for cyclic testing. The durability of specimens using P2-etched titanium was superior to that for vinyl phosphonic acid-treated titanium in all environmental tests. / Master of Science