Archive for the 'Actinides' Category

Aug 21 2008

ACS Day 4: New Uranium (VI) Chemistry (non uranyl)

Published by mitch under Actinides

Hayton, from Santa Barabara, presented his recent work with uranium (VI) compounds. The chemistry of Uranium (VI) is dominated by the formation of Uranyl (UO2)2+.  However, the Hayton group was able to synthesize and fully characterize U(OtBu)6 (1). The compound was reacted with aryl-alcohols in the hope of producing U(OAr)6 (2) compounds, shown below.

Unfortunately, due to the presence of lithium from earlier steps he prepared (3) and after doing a better job ridding his reagents of lithium produced (4).

The work highlights the difficulty in synthesizing stable uranium (VI) compounds, but perhaps if they don’t use the electron withdrawing fluorine on their arylalcohols they might better stabilize the U+6.

More Info: Synthesis and Characterization of Three Homoleptic Alkoxides of Uranium

Mitch


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Aug 17 2008

ACS Day1: New Actinide Solvent Extractors

Published by mitch under Actinides

The ability to selectively extract actinides out of nuclear waste remains a hot research topic. Today Hancock, from Wilmington, gave a presentation on several tetradentate ligands that bind to actinides more strongly than other smaller metals.  The systems he investigated are shown below.

The PDA ( system was highlighted for its rigidity, fluorescent potential, and the size of its cavity. Some formation data below.

These types of systems look promising and is a nice upgrade over traditional old-school extractors like Tributylphosphate(TBP).

Much of the talk was covered in this recent paper: Affinity of the Highly Preorganized Ligand PDA…

Mitch

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Jan 18 2008

Chemistry with uranyl dications

Published by mitch under Actinides

In this week’s issue of Nature magazine Arnold et al. have published an intriguing reactive complex of the notoriously stable uranyl dication [UO2]+ that cleaves C-Si bonds and yields a functionalized U=O bond. This was accomplished by first encapsulating the UO2 into a cyclic macrocycle, followed by the addition of the metal (either iron or zinc bound to the inner U=O bond) with a silylamide base. The major product is shown in the figure below.

reactive uranyl dication complexreactive uranyl dication complex crystal
Reprinted by permission from Macmillan Publishers Ltd: Nature, advance online publication, 17 January 2008 (doi:10.1038/nature06467)
The crystal structure was also taken and is shown above. This reactivity was explained by postulating an U(VI) K2 intermediate not observed. Postulated mechanism below.

Uranium K2 intermediate

Reprinted by permission from Macmillan Publishers Ltd: Nature, advance online publication, 17 January 2008 (doi:10.1038/nature06467)

A solution to the problem of determining the presence of the postulated intermediate might simply be to take mass specs along the course of the reaction; as one described prep takes 42 hours. In the end, this work literally builds the scaffold for future chemists to begin functionalizing uranyl. Although, no mention is given how to un-encapsulate the newly derivatized uranium. ;)

Note 1: Link to article — Reduction and selective oxo group silylation of the uranyl dication

Mitch

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Dec 13 2007

Plutonium Polymer Mystery Solved

Published by mitch under Actinides

Earlier this week a paper by L. Soderholm et al. in Angewandte Chemie may have solved the great plutonium polymer mystery. Plutonium polymer is the ubiquitous noun often spoken by plutonium chemists in regards to the un-extractable ill-defined hydrous oxides of plutonium that will form in any solution of aqueous plutonium lying about the bench top. Often plutonium polymerization can be inhibited by storing aqueous plutonium solutions at high acid concentrations. It was thought to form from a series of olation reactions:

Plutonium Olation Reaction: Pu—OH + Pu—OH2 —> Pu—OH—Pu + H2O

This old hypothesis is put to rest with the isolation of Li14(H2O)n[Pu38O56Cl54(H2O)8]. This occurred after repeated anion-exchange with an acidified alkaline peroxide solution of plutonium, that then crystallized in the presence of aqueous LiCl. This type of workup is common for samples containing plutonium polymer. The crystal is reported to have the same intracluster packing and structural topology as bulk PuO2. The crystal structure of the [Pu38O54(H2O)8]40+ is shown below.

Plutonium cation nanocluster

Copyright Wiley-VCH Verlag GmbH & Co. KGaA. Reproduced with permission.: Angewandte Chemie International Edition (Dec 2007).

The Plutonium is in green, oxygen from the oxide in red, and oxygen from water in blue. With this and other evidence of well defined Pu—O clusters and the lack of hard evidence for oxyhydroxides they expect plutonium to condensate through an oxolation reaction.

Plutonium Oxolation Reaction: 2Pu—OH —> Pu—O—Pu + H2O

The one caveat with this work is that it was performed with the more stable plutonuium-242 (t1/2=3.7 x 105 y) and not the typical reactor plutonium-239 (t1/2=2.4 x 104 y). Perhaps in the presence of the >10x more radioactive Pu-239 the nanoclusters would become either too structurally damaged to resolve nice crystalline structures, or more chemically reactive towards hydrous oxide formation or oxyhydroxide formation. Regardless, this work may still lead to better methods of extracting plutonium out of the nuclear fuel cycle and represents a nice resolution to the nebulous plutonium polymer conundrum.

Link to Paper: http://dx.doi.org/10.1002/anie.200704420

Mitch

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