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Rationally designed multiple hydroxyl-group-based chemosensors L1–L4 containing arene-based fluorophores are presented for the selective detection of Al³⁺ and Ga³⁺ ions. Changes in the absorption and emission spectra of L1–L4 in ethanol were easily observable upon the addition of Al³⁺ and Ga³⁺ ions. Competitive binding studies, detection limits, and binding constants illustrate significant sensing abilities of these chemosensors with L4, showing the best results. The interaction of Al³⁺/Ga³⁺ ions with chemosensor L4 was investigated by fluorescence lifetime measurements, whereas Job’s plot, high-resolution mass spectrometry, and ¹H NMR spectral titrations substantiated the stoichiometry between L4 and Al³⁺/Ga³⁺ ions. The solution-generated [L-M³⁺] species further detected pyrophosphate ion (PPi) by exhibiting emission enhancement and a visible color change. The binding of Al³⁺/Ga³⁺ ions with …