This ASU review focuses on developments in applications of atomic spectrometry to the characterisation of metals, chemicals and materials. It is difficult to identify research trends solely from an annual review of the literature, but a certain perspective can be obtained from examining the developments described in recent years in this ASU review series. It is, for example, evident that there has been a decline in truly novel applications for the analysis of chemicals, perhaps indicative of the fact that, for most sample types, there is now an abundance of methods available in the literature. Those papers that have appeared in the year under review have either focused on specific problems not yet fully addressed (e.g. determination of Si in gasoline) or on incremental development of well-established approaches to sample preparation or measurement. Nevertheless, there has been a very noticeable increase in activity in relation to publication of methods for the characterisation of pharmaceuticals. This is directly linked to changes in the US Pharmacopeia requirements for registration of pharmaceuticals for human use that require assessments to be made for trace element content. Laser-induced breakdown spectrometry is becoming widely employed for applications involving the characterisation of a wide variety of metals, materials and other solid sample types. Efforts are being made to overcome the perceived weaknesses of the technique, such as lack of sensitivity, elemental fractionation, accuracy and/or precision. Advances have been made, for example, using dual-pulse lasers to improve sensitivity, or by employing chemometrics methods with full spectrum data to improve the robustness of calibration. Many of these reported LIBS developments draw from, and have relevance for, applications involving LA-ICP-MS, which continues to be a popular means of generating highly sensitive lateral and depth profiling and bulk compositional information for a wide range of materials and solids. The use of field portable instrumentation for in situ analysis continues grow, with LIBS and XRF techniques amongst those most frequently cited. The development of such instrumentation has had a substantial impact in the examination of cultural heritage artefacts, especially in relation to paintings, wall murals and other objects of unique historical value. The latter area of application has also seen continued use of combinations of surface (SIMS, XPS, SEM-EDS, PIXE, GD and laser ablation methods) and bulk (ICP-OES, ICP-MS, AAS, XRF) analysis techniques to reveal details of objects that would not otherwise be identified (for example preparatory sketches hidden under original works of art or materials provenance). This trend towards using a multi-technique based approach has also been apparent in the characterisation of multi-layer or heterogeneous organic and inorganic materials and metals. Finally, methods for the analysis of nanoparticles and nanostructures have been reported, based primarily on single particle (SP)-ICP-MS and flow field flow fractionation (A4F). The investigation of methods of drift correction, the use of flow injection and isotope dilution methodologies in combination with SP-ICP-MS are indicative of the further development of this field.

/pdf/atomic-spectrometry-update-review-of-advances-in-the-5dt9znhga2.pdf

Atomic spectrometry update. Review of advances in the analysis of metals, chemicals and materials

This review summarizes recent progress in solvent extraction of rare earth elements (REEs) using an ionic liquid (IL) as the extraction solvent. These IL extraction systems are advantageous owing to the affinity of ILs for both charged and neutral hydrophobic species, in contrast to conventional organic solvent extraction systems. Herein, REE extraction studies using ILs are detailed and classified based on the type of extraction system, namely extraction using anionic ligands, extraction using neutral ligands, synergistic extraction, extraction without extractants, and a specific system using task-specific ionic liquids (TSILs). In IL extraction systems, the extracted complexes are often different from those in organic solvent systems, and the REE extraction and separation efficiencies are often significantly enhanced. Synergistic IL extraction is an effective approach to improving the extractability and separability of REEs. The development of novel TSILs suitable for IL extraction systems is also effective for REE separation.

/pdf/recent-progress-in-ionic-liquid-extraction-for-the-1x0avgj6bq.pdf

Recent Progress in Ionic Liquid Extraction for the Separation of Rare Earth Elements

The chemical separation of minor actinides (MAs) over lanthanides from high-level waste (HLW) is one of the hottest and most difficult topics in international separation science. N, O-hybrid phenanthroline-derived extractants have shown good potential in the separation of minor actinides over lanthanides from highly acidic HNO3 solution by liquid–liquid solvent or solid extraction method. The 1,10-phenanthroline skeleton can serve as a platform to design various extractants for the separation of actinides. In this review, the recent progress made in the hard-soft donors combined 1,10-phenanthroline type extractants for separation and complexation with f-block elements is summarized. The structure–activity relationships between the extractants and their separation performances are discussed, which can provide practical strategies to design more efficient extractants for actinides separation. Finally, the future perspectives and trends in those phenanthroline-derived extractants for actinides separation are proposed. 

Separation and complexation of f-block elements using hard-soft donors combined phenanthroline extractants

Radiation-induced surface modification of silanized silica with n-alkyl-imidazolium ionic liquids and their applications for the removal of ReO4− as an analogue for TcO4−

Abstract Two full continuous countercurrent processes for the recovery of trivalent actinides (An(III)) from a simulated PUREX raffinate solution (HAR) were developed and demonstrated using miniature laboratory-scale centrifugal contactors: the innovative SANEX and the 1-cycle SANEX processes. The innovative SANEX process was successfully demonstrated in a 16 + 16 stage flow sheet. In the first 16 stages, Am(III), Cm(III), and Ln(III) were quantitatively co-extracted from the HAR by a TODGA-based extractant. The decontamination factors (DFs) for the major non-lanthanide fission products were >103. The loaded extractant was then subjected to two stripping steps using the second 16 stages of the flow sheet. The first stripping step concerned the selective stripping of Am(III) + Cm(III) at fairly high acidity (0.35 ML−1 HNO3) with the new hydrophilic N-chelating selective ligand SO3-Ph-BTP. High An(III) recoveries >99.8% were achieved with high decontamination factors toward the trivalent lanthanides. In the second step, the residual stripping of Ln(III) from loaded organic phase was carried out quantitatively using 0.5 ML−1 citric acid solution at pH 3. However, Ru proved to be the only exception and remained to a large extent (12.8%) in the spent extractant. A more challenging route also studied at our laboratories is the 1-cycle SANEX process, i.e. direct An(III) separation from HAR using an extractant mixture of CyMe4BTBP and TODGA in 1-octanol/TPH diluent. A demonstration process was also successfully implemented using a 16 + 16 stage flow sheet on the above-mentioned laboratory-scale centrifugal contactor rig. It was demonstrated that a selective extraction and high recovery of >99.8% of Am(III) and >99.4% Cm(III) was achieved with low contamination of fission products. Both new processes are major contributions to the field of partitioning and important steps forward toward the industrial implementation of MA partitioning.

Development and demonstration of innovative partitioning processes (i-SANEX and 1-cycle SANEX) for actinide partitioning

Pure and complete fractions of neodymium, samarium, europium, gadolinium and dysprosium were isolated by means of high performance ion chromatography, using a cation exchange column and gradient elution with alpha-hydroxyisobutyric acid solutions (α-HIBA). Intermediate precision and robustness of the isolation method was investigated, identifying eluent pH as the most important parameter. Investigation of the elution behaviour of the most important fission and activation products and actinides indicated that preventing the accumulation of cesium on the cation exchange column required further isocratic elution with a higher concentrated α-HIBA solution after elution of the lanthanides. A sample matrix free of carbon was achieved by means of acid digestion, followed by UV photo-oxidation, resulting in samples suitable for mass spectrometric analysis.

Isolation of lanthanides from spent nuclear fuel by means of high performance ion chromatography (HPIC) prior to mass spectrometric analysis

The extraction of Am(III), Cm(III) and Eu(III) by 2,9-bis(5,5,8,8-tetramethyl-5,6,7,8-tetrahydro-1,2,4-benzotriazin-3-yl)-1,10-phenanthroline (CyMe4BTPhen) from nitric acid solution was studied using the ionic liquid Aliquat-336 nitrate ([A336][NO3]) as diluent. Results show a high selectivity of the solvent for Am(III) and Cm(III) over Eu(III), but rather slow extraction kinetics. The kinetics of CyMe4BTPhen were largely improved by the addition of 0.005 mol L−1 N,N,N′,N′-tetra-n-octyl-diglycolamide (TODGA) as a phase transfer reagent and by the use of 1-octanol as co-diluent. The addition of the phase transfer catalyst and co-diluent did not compromise the selectivity towards the actinide/lanthanide separation and thus this four-component system can be successfully applied to separate Am(III) and Cm(III) from the lanthanides.

/pdf/selective-extraction-of-trivalent-actinides-using-3o5ibafliv.pdf

Selective extraction of trivalent actinides using CyMe4BTPhen in the ionic liquid Aliquat-336 nitrate

The extraction behavior of americium(III), curium(III) (minor actinides, MA), fission products (lanthanides (Ln(III)), Mo, Ru, Pd, and Rh), and corrosion products (Zr and Fe) was studied in batch s...

Solvent Extraction of Am(III), Cm(III), and Ln(III) Ions from Simulated Highly Active Raffinate Solutions by TODGA Diluted in Aliquat-336 Nitrate Ionic Liquid

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Isolation of lanthanides from spent nuclear fuel by means of high performance ion chromatography (HPIC) prior to mass spectrometric analysis

Selective extraction of trivalent actinides using CyMe4BTPhen in the ionic liquid Aliquat-336 nitrate

Solvent Extraction of Am(III), Cm(III), and Ln(III) Ions from Simulated Highly Active Raffinate Solutions by TODGA Diluted in Aliquat-336 Nitrate Ionic Liquid