A uranium-based metal–organic framework, [(UO2)­(H2DTATC)] (HNU-39, H4DTATC = 5,5′-(9,10-dihydroxy-4a,9,9a,10-tetrahydroanthracene-9,10-diyl)­diisophthalic acid) was successfully prepared by a hydrothermal method. The structure of HNU-39 comprises UO8 hexagonal bipyramids linked by doubly protonated DTATC ligands, forming a ribbon arrangement. It is worth noting that the DTATC ligand was transformed in situ from 5,5′-(anthracene-9,10-diyl)­diisophthalic acid (H4DPATC) during the synthesis of HNU-39. Research on fluorescence properties has shown that HNU-39 exhibits fluorescence turn-on response under alkaline conditions and could be used as a potential pH sensor. Moreover, HNU-39 can also be successfully applied for pH sensing in real samples from a sewage treatment plant. The sensing mechanism can be interpreted as OH– ions reacting with the protons in the organic ligand of HNU-39.