A methacrylate adhesive marketed for high temperature applications was screened in combination with environmentally sustainable TT-C-490F surface pretreatments. Testing consisted of single-lap-joint testing using aluminum and steel specimens at room temperature along with hot/wet conditioning (water immersion for 14 days at 63 °C) and in-situ at elevated temperature (71 °C). The methacrylate adhesive showed high initial bond strength and hot/wet durability, but significant loss of strength retention at elevated temperature. The environmentally sustainable TT-C-490F Type IV inorganic pretreatments resulted in little to no loss of adhesive bond strength during hot/wet conditioning and their potential use as bonding pretreatments is worth further investigation.