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

Technetium-99 is a long-lived, high-abundance fission product which has been widely distributed in the environment through atmospheric testing, the nuclear fuel cycle, and nuclear medicine. It has a high potential for migration in the environment as the pertechnetate anion. At the Center for Accelerator Mass Spectrometry, methods are being developed for the detection of this radionuclide by accelerator mass spectrometry (AMS), including extraction from environmental samples, concentration and purification of the 99Tc, conversion to a form appropriate for AMS analysis, and quantification by AMS. Besides interference from the stable (though relatively rare) atomic isobar 99Ru, the detection of 99Tc by AMS presents some technical challenges which are not present for the other radionuclides typically measured by AMS. These challenges are related to the lack of a stable Tc isotope. Here we present the status of our 99Tc methods including discussion of interferences and sensitivity, and recent results for environmental samples and the IAEA reference material IAEA-381, Irish Sea Water. Sensitivity is presently ∼10 μBq (∼1×108 atoms) per sample, limited primarily by 99Ru introduced from process chemicals, and precision/reproducibility is ∼15–25%.

/pdf/technetium-measurements-by-accelerator-mass-spectrometry-at-56a8mj6ay4.pdf

Technetium measurements by accelerator mass spectrometry at LLNL

Rapid diagnostic method for transplutonium isotope production in high flux reactors

In the frame of studies on the safe disposal of nuclear waste, there is a great interest for understanding the migration behavior of 99Tc. 99Tc originating from nuclear energy production and global fallout shows environmental levels down to 107 atoms/g of soil (∼2 fg/g). Extremely low concentrations are also expected in groundwater after diffusion of 99Tc through the bentonite constituting the technical barrier for nuclear waste disposal. The main limitation to the sensitivity of the mass spectrometric analysis of 99Tc is the background of its stable isobar 99Ru. For ultratrace analysis, the Accelerator Mass Spectrometry (AMS) setup of the Technical University of Munich using a Gas-Filled Analyzing Magnet System (GAMS) and a 14 MV Tandem accelerator is greatly effective in suppressing this interference. In the present study, the GAMS setup is used for the analysis of 99Tc in samples of the seawater reference material IAEA-443, a peat bog lake, and groundwater from an experiment of in situ diffusion throug...

Ultratrace Determination of 99Tc in Small Natural Water Samples by Accelerator Mass Spectrometry with the Gas-Filled Analyzing Magnet System.

Plutonium is a major contributor to the radiotoxicity in a long-term nuclear waste repository; therefore, many studies have focused on interactions of plutonium with the technical, geotechnical, and geological barriers of a possible nuclear waste storage site. In order to gain new insights into the sorption on surfaces and diffusion of actinides through these complex heterogeneous materials, a highly sensitive method with spatial resolution is required. Resonant laser secondary neutral mass spectrometry (Laser-SNMS) uses the spatial resolution available in time-of-flight secondary ion mass spectrometry (TOF-SIMS) in combination with the high selectivity, sensitivity, and low background noise of resonance ionization mass spectrometry (RIMS) and is, therefore, a promising method for the study and analysis of the geochemical behavior of plutonium in long-term nuclear waste storage. The authors present an approach with a combined setup consisting of a commercial TOF-SIMS instrument and a Ti:sapphire (Ti:Sa) laser system, as well as its optimization, characterization, and improvements compared to the original proof of concept by Erdmann et al. (2009). As a first application, the spatial distributions of plutonium and other elements on the surface of a pyrite particle and a cement thin section were measured by Laser-SNMS and TOF-SIMS, respectively. These results exemplify the potential of these techniques for the surface analysis of heterogeneous materials in the context of nuclear safety research.

/pdf/development-characterization-and-first-application-of-a-2esrmaddpa.pdf

Development, characterization, and first application of a resonant laser secondary neutral mass spectrometry setup for the research of plutonium in the context of long-term nuclear waste storage.

This work shows the ability of resonance ionization mass spectrometry (RIMS) to determine 99gTc at the ultratrace level. The characterization of the prepared samples by X-ray photoelectron spectroscopy (XPS) and optimization of the RIMS setup for this purpose, as well as the application of the RIMS method to a soil sample, are presented in this article. 97Tc was used as a tracer isotope to determine the amount of 99gTc in a soil sample with RIMS. With 8.8 × 1010 atoms of 97Tc as the tracer, the concentration of 99gTc was found to be 1.5 × 109 atoms per gram of dried sample material, demonstrating the sensitivity of the method. Furthermore, it could be shown that the 97Tc solution contained 98Tc as well. This is the first time that 97,98,99gTc have been simultaneously measured with RIMS.

Application of Resonance Ionization Mass Spectrometry for Ultratrace Analysis of Technetium

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Development, characterization, and first application of a resonant laser secondary neutral mass spectrometry setup for the research of plutonium in the context of long-term nuclear waste storage.

Application of Resonance Ionization Mass Spectrometry for Ultratrace Analysis of Technetium