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Hexanal, octanal, nonanal, decanal, hexanoic acid, octanoic acid, nonanoic acid, and decanoic acid were identified in the volatile emissions from fifth instars of Schistocerca gregaria by coupled gas chromatography-electroantennography (GC-EAD) detection and coupled CC-mass spectrometry (MS). In laboratory assays, synthetic blends of the eight compounds, with acids and aldehydes tested separately, evoked strong aggregation responses from fifth instars, similar to responses evoked by a crude volatile extract of the nymphs. A nymphal fecal volatile phenolic blend of guaiacol and phenol, which we have previously shown to evoke an aggregative response from different stages of the insect, significantly synergized the activity of the blend of eight compounds, suggesting mutually augmentative roles for nymphal and fecal volatiles in evoking aggregation. These results indicate that the aggregation behavior of gregarious second to fifth instars is modulated by three sets of pheromonal compounds: aldehydes and acids emitted by the nymphs themselves and phenols associated with their feces.