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Comprehensive Summary: The second example of tetravalent plutonium carboxyl‐based organic framework, 242Pu(OH)[PO[(C6H4)COO]3]·H2O, termed as PuTPO (TPO = tris(4‐carboxylphenyl)‐phosphineoxide), was reported in this work. A series of characterizations of PuTPO, such as X‐ray crystallography and solid‐state UV‐Vis‐NIR spectroscopy, were carried out to expatiate its structure and physicochemical properties. PuTPO is constructed by dimers of the plutonium‐oxygen subunit of [Pu2O16]. Characteristic peaks located at approximately 1100 nm can be considered to be the fingerprint peaks of tetravalent plutonium. While PuTPO can maintain high crystallinity within several months after synthesis, it exhibits a radiation‐induced swelling effect probed by the expansion of cell parameter of b axis after self‐irradiation from α‐decay of 242Pu. This result enriches the inventory of tetravalent plutonium compounds and provides an insight into the irradiation resistance of metal‐organic frameworks. [ABSTRACT FROM AUTHOR]

Summary of main observation and conclusion: We present a new method for generating europium oxalate compounds by decomposing of N‐methyl 2‐pyrrolidone in HNO3 media. The reaction exhibits high selectivity towards Eu3+ over UO22+, which suggests that these conditions could be applied to a selective crystallization based separation system for trivalent lanthanides and hexavalent actinides. In this work, a new method for the separation of trivalent Eu3+ and hexavalent UO22+ in initial high‐acidity HNO3 solution is presented. N‐Methyl 2‐pyrrolidone was added in the HNO3 solution where Eu3+ and UO22+ coexisted, then the solution was heated. Eu3+ will react with oxalic acid and dimethylamine produced by N‐methyl 2‐pyrrolidone and form compound NH2(CH3)2[Eu(C2O4)2(H2O)], while UO22+ remains in the solution. This method provide a new strategy for separation of trivalent Eu3+ and hexavalent UO22+. [ABSTRACT FROM AUTHOR]