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In this paper, a novel lanthanum metal–organic framework La‐MOF was prepared via hydrothermal and reflux methods. The La‐MOF was achieved through the reaction of a 5‐amino‐isophthalic acid with 1, 2‐phenylenediamine and lanthanum chloride. The prepared La‐MOF structure was confirmed by XRD, mass spectrometry, IR, UV–Vis and elemental analysis, whereas the size, and morphology was examined by FE‐SEM/EDX and HR‐TEM. The results indicated that the La‐MOF prepared via both methods have the same structure and composition. Meanwhile, the MOF yield, reaction time, morphology, physiochemical and sensing properties were highly depended on the used preparation method. The photoluminescence (PL) study was carried out for the La‐MOF, and the results showed that La‐MOF exhibits strong emission at 558 nm after excitation at 369 nm. Moreover, the PL data indicating that the La‐MOF has highly selective sensing properties for iron (III) competing with different metal ions. The Stern‐Völmer graph shows a linear calibration curve which achieved over a concentration range 1.0–500 μM of Fe3+ with a correlation coefficient, detection, and quantitation limits 0.998, 1.35 μM and 4.08 μM, respectively. According to the remarkable quenching of the PL intensity of La‐MOF using various concentrations of Fe3+, it was successfully used as a sensor for Fe3+detecting in different water resources (pure and waste) samples. The quenching mechanism was studied and it has a dynamic type and due to efficient energy transfer between the La‐MOF and Fe3+. A novel La‐MOF was synthesized and well characterized via two simple method, a unique morphology of the prepared nano‐rods and nanosheets of La‐MOF remarkably quenched by Fe3+ and not effected by other common metal ions. The detection of fe3+ in different water waste and pure resources is achieved. The quenching mechanism is well studied. [ABSTRACT FROM AUTHOR]