Five selected insecticides were applied to four substrates and evaluated in laboratory studies for repellency and toxicity against the Pharaoh ant, Monomorium pharaonis (L.). We tested both repellent and nonrepellent formulations on outdoor (concrete and mulch) and indoor (ceramic and vinyl) substrates. Repellency was evaluated using a behavioral bioassay in which colonies were given a choice to leave the treated zone and move into empty nests provided in the untreated zone. We used a novel experimental design whereby ants walked on a Slinky coil suspended from a metal support frame, thus permitting a long foraging distance with a minimum use of space and resources. Cypermethrin, a repellent pyrethroid insecticide, resulted in colony budding, although the response was delayed. Toxicity of insecticides was evaluated as worker, queen, and brood mortality. The most effective treatment was fipronil, which provided 100% reduction in pretreatment activity by 2 d posttreatment on both concrete and mulch. Chlorfenapyr was highly effective on both outdoor and indoor substrates. Significant substrate effects were observed with insecticides applied to nonabsorbent substrates (ceramic tile), which performed better than insecticides applied to absorbent substrates (vinyl tile). Other highly absorbent materials (mulch and concrete), however, did not reduce insecticide efficacy. This is because ants relocated nests into and/or under these attractive nesting materials, thus increasing their exposure to toxic insecticide residues. Our results demonstrate efficacy of nonrepellent liquid insecticides as indoor treatments for the control of Pharaoh ants and possibly as exterior perimeter treatments.