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The chemical properties of actinide materials are often predefined and described based on the data available for isostructural species. This is the case for potassium plutonyl (PuVI) carbonate, K4PuVIO2(CO3)3(cr), a complex relevant for nuclear technology and the environment, of which the crystallographic and thermodynamic properties of which are still lacking. We report here the synthesis and characterization of PuVI achieved by single-crystal X-ray diffraction analysis and high-energy-resolution fluorescence-detected X-ray absorption near-edge structure at the Pu M4-edge coupled with electronic structure calculations. The crystallographic properties of PuVI are compared with isostructural uranium (U) and neptunium (Np) compounds. Actinyl (AnVI) axial bond lengths, [O-AnVI-O]2+, are correlated between solid, K4AnVIO2(CO3)3(cr), and aqueous, [AnVIO2(CO3)3]4-(aq) species for the UVI-NpVI-PuVI series. The spectroscopic data are compared to KPuVO2CO3(cr) and PuIVO2(cr) to tackle the trend in the electronic structure of PuVI regarding the oxidation state changes and local structural modifications around the Pu atom.

The nanoscience field often produces results more mystifying than any other discipline. It has been argued that changes of the plutonium dioxide (PuO2) particle size from bulk to nano can have a drastic effect on PuO2 properties. Here we report a full characterization of PuO2 nanoparticles (NPs) at the atomic level, explore their stability and probe their local and electronic structure. The particles were synthesized from precursors with different oxidation states (Pu III, IV and V) under various environmentally and waste storage relevant conditions (pH 8 and pH 12). We demonstrate that well dispersed, crystalline NPs with a size of ~2.5 nm in diameter are always formed in spite of diverse chemical conditions. Identical crystal structures and the presence of only Pu(IV) oxidation state in all NPs indicate that their fundamental properties, rather than being fancy and exotic, are identical to those of the bulk PuO2.

One of the long standing debates in actinide chemistry is the level of localization and participation of the actinide 5f valence orbitals in covalent bonds across the actinide series. Here we illuminate the role of the 5f valence orbitals of uranium, neptunium and plutonium in chemical bonding using advanced spectroscopies: actinide M4,5 HR-XANES and 3d4f RIXS. Results reveal that the 5f orbitals are active in the chemical bonding for uranium and neptunium, shown by significant variations in the level of their localization evidenced in the spectra. In contrast, the 5f orbitals of plutonium appear localized and surprisingly insensitive to different bonding environments. We envisage that this report of using relative energy differences between the 5fδ/ϕ and 5fπ*/5fσ* orbitals as a qualitative measure of overlap-driven actinyl bond covalency will spark activity, and extend to numerous applications of RIXS and HR-XANES to gain new insights into the electronic structures of the actinide elements., Understanding the chemistry of heavy radioactive elements is crucial to harnessing them for fuel and medicine. Here, the authors combine advanced X-ray spectroscopy and modelling to the study the chemical bonding of the 5f valence orbitals of uranium, neptunium and plutonium.

We report here experimental evidence that the formation of PuO2 nanoparticles from oxidized Pu(VI) under environmentally relevant conditions proceeds through the formation of an intermediate Pu(V) solid phase, similar to NH4PuO2CO3, which is stable over a period of several months. State-of-the-art experiments at Pu M4 and L3 absorption edges combined with theoretical calculations unambiguously allowed us to determine the oxidation state and the local structure of this intermediate phase

In this work a combination of multiple synchrotron and laboratory based micro-techniques is utilized to unveil the speciation, heterogeneities and degradation of uranium (U) micro-mineral phases accumulated on rock outcrop from natural U deposit area. The investigated system is sampled from the abandoned Krunkelbach U mine in Southern Germany with 2-3 km surrounding area which represents a natural analogue site with an unique accumulation of U minerals suitable for investigations of potential mobilization-immobilization processes expected in a real spent nuclear fuel repository. A specific feature of the site is the occurrence of more than forty secondary U minerals, from uraninite, mixed U oxy-hydroxides to uranyl silicates, representing a wide scale of U ore weathering events. Available data on the age of the secondary U mineralization indicates that oxidizing processes at the site started some 340,000 years ago and continues up to date. Several phases close to Cu(UO2)2(PO4)2-x(AsO4)x·8H2O are identified on 1×2 mm2 area with presumably older, more evenly distributed uranyl silicate and uranyl tungstate mineralization. Based on a multi-technique investigation 10-200 μm Cu(UO2)2(PO4)2-x(AsO4)x·8H2O particles with widely varying arsenic-phosphorus (As-P) content are analyzed. The evidences of a degradation on some zones of selected crystals are found which are associated with higher As content. This observation can be apparently attributed to different degradation properties of the mixed As-P phases depending on As-P ratio and originate from drastically different solubility properties of Cu(UO2)2(PO4)2·8H2O and Cu(UO2)2(AsO4)2·8H2O species. The conditions for preferential formation of As rich Cu(UO2)2(XO4)2·8H2O [X=As, P] phases and its possible role on U transport in environment under oxidizing conditions are discussed.

X-ray Absorption Spectroscopy (XAS) is an invaluable tool in nuclear material research, allowing to probe the oxidation state and the local coordination of selected atomic species. The first part of the spectrum, the X-ray Near Edge Structure (XANES), is less exploited than the Extended X-ray Absorption Fine Structure (EXAFS). However XANES conceals a wealth of information on the electronic structure and on the local geometry around the absorber. What prevents XANES to become a more common technique is the complexity of its analysis, which still gives more qualitative than quantitative information. Nowadays important progresses in the interpretation of XANES have been made thanks to i) the development of dedicated ab-initio codes using powerful computational resources and ii) the use of High Energy Fluorescence Detected (HERFD) XANES, which boosted spectral resolution especially in the case of actinides. These recent developments make the systematic studies based on XANES simulations an invaluable tool to strengthen our understanding of XANES. In this regards we present a detailed investigation on how the local coordination of U⁵⁺ and U⁶⁺ affects the U L₃ edge HERFD XANES. By simulating a large number of structures containing U⁵⁺ and/or U⁶⁺ in different local coordination geometries we found systematic trends, especially correlated with the presence of longer or shorter U – O bonds. It is well established that the presence of the short uranyl bond shows up in U L₃ edge XANES by the presence of a characteristic post-edge feature [1]. Interestingly, some experimental investigations reported that the uranyl post-edge feature shifts to lower energy when going from the uranyl to the uranate coordination, i.e. identical U – O distances [2,3]. Our systematic investigation confirms that this behavior correlates with the presence of U coordinated with 6 oxygen atoms in a regular octahedron and it is a consequence of the splitting of U 6d Density of States (DOS) induced by the crystal field. The possibility to detect the presence of U⁵⁺ in systems with both U⁵⁺ and U⁶⁺ by HERFD XANES will be discussed on the bases of our systematic investigation.

Plutonium is one of the most complicated element among actinides. It can exist in four different oxidation states (III, IV, V, VI) under environmental conditions. Due to the small value of standard electrode potentials among these linked oxidation states plutonium can change its oxidation state easily. Moreover, plutonium may exist in several oxidation states simultaneously, which makes its chemistry even more complex. It was previously shown that plutonium migrates in colloidal form in the subsurface environment with the distance of several kilometers. It turned out that so called “colloidal Pu(IV) polymers” are in fact aggregates of PuO2 nanoparticles with diameters ~ 2 nm. However, the certain structure and stoichiometry of these colloids, as well as presence of other oxidation states but Pu(IV) is still debated. This contribution will show results of plutonium oxide nanoparticle studies at the large-scale facility – The European Synchrotron (ESRF) by complementary methods that used X-rays in different regimes to probe the Pu oxide nanoparticles. Samples were prepared by rapid chemical precipitation using precursors in the different oxidation states (Pu(III), Pu(IV), Pu(V) and Pu(VI)). These precursors were obtained by chemical reduction or oxidation of Pu stock solution. The obtained nanoparticles were characterized at the different beamlines at the ESRF. It gives the opportunity to study our samples with various techniques: X-ray diffraction (XRD), pair distribution function analysis (PDF), and several types of spectroscopies: high energy resolution fluorescence detection (HERFD) at L3 and M5-edges, X-ray emission spectroscopy (XES) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The applying multifold synchrotron methods benefits to discover features, which may be unclear or even indistinguishable, these approach is also crucial to confirm results, obtained with individual methods. It was found that small (2 nm) nanoparticles are formed from the Pu(III), Pu(IV), Pu(V) aqueous solutions, with the crystal structure close to PuO2, without any other Pu-O contributions or oxidation states of Pu except Pu(IV).

The abandoned Krunkelbach uranium (U) mine, Southern Germany, with 2-3 km surrounding area represents a unique natural analogue site with accumulation of U minerals suitable for investigations of potential mobilization-immobilization processes expected in a real spent nuclear fuel repository. A specific feature of the site is the occurrence of more than forty secondary U minerals, from mixed redox U oxy-hydroxides to alkaline metal uranyl silicates, thus representing a wide scale of U ore weathering events. In this work the combination of synchrotron and laboratory techniques is used to unveil U speciation and micro heterogeneities in U phases accumulated on granitic rock outcrop from U deposit area. Available data on the age of the secondary U mineralization indicates that oxidizing processes at the site started some 340,000 years ago and continues up to date. Several phases close to Cu(UO2)2(PO4)2-x(AsO4)x·8H2O are identified on 1×2 mm2 area with presumably older, more evenly distributed Cu(UO2)2(SiO3OH)2·6H2O and (Fe, Ba, Pb)(UO2)2(WO4) (OH)4·12H2O, mineralization. Based on a multi-technique investigation 10-200 µm Cu(UO2)2(PO4)2-x(AsO4)x·8H2O particles with widely varying As-P content are analyzed. The evidences of a degradation occurred on some zones on the selected crystals are found associated with higher As and decreased P content. This observation can be apparently attributed to different degradation properties of the mixed As-P phases depending on As-P ratio and originate from different solubility properties of Cu(UO2)2(PO4)2·8H2O and Cu(UO2)2(AsO4)2·8H2O species. The conditions for preferential formation of As rich Cu(UO2)2(XO4)2·8H2O [X=As, P] phases and its possible role on U transport in environment under oxidizing conditions are discussed.

The release of radioactive plutonium (Pu) into the environment is of general concern due to the high radiotoxicity and long half-life of its main isotopes. Previous research has shown that plutonium migrates in the subsurface environment on the kilometer scale at some previously contaminated sites [1-4]. Additionally, previous research demonstrated the spontaneous formation of Pu oxide nanoparticles under certain environmental conditions [5]. However, fundamental properties of such Pu oxide nanoparticles, including their local, crystal and electronic structure, remain largely unexplored, hence it is difficult to understand their formation or to predict their transport in the environment. Plutonium may exist in four oxidation states, III, IV, V, VI, in aqueous solution under environmental conditions, which can change relatively easily. While Pu(IV) is the dominant oxidation state in such PuO2-like nanoparticles, their exact composition in terms of oxidation states and local structure remains an open question. Therefore, it is necessary to advance the fundamental understanding of the Pu oxide nanoparticles and to review the processes, through which the formation of Pu oxide nanoparticles takes place. This contribution will give an overview on the results of Pu oxide nanoparticle research conducted at the Rossendorf Beamline at The European Synchrotron (ESRF) [6]. Pu oxide nanoparticles were prepared by rapid chemical precipitation using precursors in the different oxidation states (Pu(III), Pu(IV), Pu(V) and Pu(VI)). These precursors were obtained by chemical reduction or oxidation of Pu stock solution. The recently upgraded ROBL beamline at the ESRF, dedicated to actinide science, provides now a unique opportunity to characterize actinide materials by several experimental techniques simultaneously. We will show how the detailed information about local and electronic structure and Pu oxidation state in different nanoparticles can be obtained using the variety of methods: Extended X-ray absorption fine structure (EXAFS [7]), X-ray absorption near edge structure (XANES), high-energy resolution fluorescence detection (HERFD) X-ray absorption spectroscopy [8-10], resonant inelastic X-ray scattering (RIXS [11]), and X-ray diffraction techniques.

Plutonium is a chemical element of a most significant concern at the nuclear legacy sites. The problem of the plutonium migration plays an important role in the environmental radioactivity because of its high radiological toxicity. It was shown previously that plutonium migrates in the subsurface environment on the kilometer scale at some previously contaminated sites [1-2]. During the last few years due to the evolution of spectroscopic and microscopic techniques it was found that so called “colloidal Pu(IV) polymers” actually represents as aggregates of PuO2 nanoparticles with size ~ 2 nm. [3-4]. Investigation of plutonium oxides nanoparticles is complicated, as plutonium can exist in four partially unstable oxidation states in aqueous solution: III, IV, V, VI under environmental conditions. At the same time, presence of Pu in different oxidation states in PuO2 structure is still an open question. This contribution will show first results of plutonium oxide nanoparticles studies at the large-scale facility – The European Synchrotron (ESRF) by X-ray spectroscopy and X-ray diffraction methods. Plutonium nanoparticles were prepared by rapid chemical precipitation using precursors in the different oxidation states. These precursors were obtained by chemical reduction or oxidation of Pu stock solution. The obtained nanoparticles were characterized by high energy resolution fluorescence detection (HERFD) [5] X-ray absorption spectroscopy, extended X-ray absorption fine structure (EXAFS) and X-ray diffraction (XRD) techniques. The experiments were performed at the Rossendorf Beamline (ROBL) at the ESRF, dedicated to actinide science, where we recently installed a novel X-ray emission spectrometer with ground-breaking detection limits. The recently upgraded ROBL beamline at the ESRF provides now a unique opportunity to study actinide materials by several experimental techniques - HERFD, XES, RIXS [6], EXAFS and XRD simultaneously. We will show how the detailed information about local and electronic structure and plutonium oxidation state in different nanoparticles can be obtained using the variety of methods at large scale facilities. References [1] A.B. Kersting et al., Nature 397, 56, (1999). [2] A.P. Novikov et al., Science 314, 638 (2006). [3] B.A. Powell et al., Environ. Sci. Technol. 45, 2698 (2011). [4] A.R. Romanchuk et al., Geochim. Cosmochim. Acta. 121, 29 (2013). [5] K.O. Kvashnina et al., Phys. Rev. Lett. 111, 253002 (2013). [6] K.O. Kvashnina et al., J. Electron. Spectrosc. Relat. Phenom. 194, 27 (2013).

Uranium redox states and speciation in magnetite nanoparticles co-precipitated with U(VI) for uranium loadings varying from 1,000 to 10,000 ppm are investigated by X-ray absorption spectroscopy (XAS). It is demonstrated that the U M4 high energy resolution X-ray absorption near edge structure (HR-XANES) method is capable to clearly characterize U(IV), U(V) and U(VI) existing simultaneously in the same sample. The contributions of the three different uranium redox states present in the samples are quantified with the iterative transformation factor analysis (ITFA) method. U(V) incorporated in octahedral magnetite sites remains stable over 226 days under ambient conditions as unambiguously shown for the magnetite nanoparticles containing 1,000 ppm uranium. U L3 XAS and transmission electron microscopy (TEM) studies reveal that initially precipitated U(VI) phases recrystallize to non-stoichiometric UO2+x nanoclusters within 147 days when stored under anoxic conditions. XAS results are supported by density functional theory (DFT) calculations. Further characterization of the samples include powder X-ray diffraction (pXRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS).

Local atomic and electronic structure investigations of uranium trioxide (UO3) crystalline phases performed by the U M4 edge HR-XANES technique is presented. The experimental U M4 edge HR-XANES spectra of α-UO3, β-UO3 and γ-UO3 polymorphic phases are compared with spectra of uranate (CaU2O7) and uranyl (UO3•1-2(H2O)) compounds. We describe a finger print approach valuable for characterization of variations of U-O axial bond lengths. Theoretical calculations of spectra using full-multiple-scattering theory (FEFF9.6 code) are performed. We have tested and selected input parameters, which provide best agreement between experimental and calculated spectra.

The redox variations and changes in local atomic environment of uranium (U) interacted with the magnetite nanoparticles were studied in a proof of principle experiment by the U L3 and M4 edges high energy resolution X-ray absorption near edge structure (HR-XANES) technique. We designed and applied a mixed flow reactor (MFR) set-up to maintain dynamic flow conditions during U-magnetite interactions. Formation of hydrolyzed, bi- and poly-nuclear U species were excluded by slow continuous injection of U(VI) (10-6 M) and pH control integrated in the MFR set-up. The applied U HR-XANES technique is more sensitive to minor changes in the U redox states and bonding compared to the conventional XANES method. Major U(VI) contribution in uranyl type of bonding is found in the magnetite nanoparticles after three days operation time of the MFR. Indications for shortening of the U-Oaxial bond length for the magnetite compared to the maghemite system are present too.

In this work, redox states and speciation of U in U coprecipitated with and sorbed on magnetite nanoparticles are investigated by U M₄ HR-XANES, L₃ EXAFS, XPS and TEM techniques. Coexistence of U(V), U(IV) and U(VI) in varying ratios is clearly detect by the U M₄ HR-XANES technique. Mainly U(V) stable for more than 240 days of contact time is found In a coprecipitated sample with lowest U loading (1000 ppm U). Coprecipitated sample with highest U loading (10000 ppm) undergoes reduction to U(IV) within less than 7 days. Reduction kinetics of U and long term stability of U(V) is discussed for both batch sorption and coprecipitation systems.

In this work four electrochemically aqueous plutonium (Pu) species prepared in perchloric acid solution at different oxidation states (III, IV, V, VI) as well as Pu(IV) colloids are characterized for the first time by Pu L₃ and M₅ edge high energy resolution X-ray absorption near-edge structure spectroscopy (HR-XANES). A Johann type five-analyzer crystal spectrometer recently installed and commissioned at the INE-Beamline for actinide research at the ANKA synchrotron radiation facility, Karlsruhe, Germany was applied. Different to conventional XANES several spectral features could be identified. The most intense absorption resonances (White Line, WL) have higher intensities for all Pu L₃ HR-XANES spectra compared to the conventional XANES. Additionally, the Pu(V) and Pu(VI) L₃ HR-XANES spectra exhibit better resolved post-edge features. The energy distance between the WL and this resonance is sensitive to the bond distance between the Pu and axial O atoms in Pu(V) and Pu(VI). Extended X-ray absorption fine structure (EXAFS) investigation is performed to correlate oxidation states with average Pu-O bonding distances. For the Pu(VI) M₅ edge HR-XANES two additional features at higher energy is well resolved, which are expected to be sensitive to changes in Pu-O bond length and to the level of hybridization of metal and axial oxygen valence orbitals. The origin of hitherto unresolved features is elucidated by quantum chemical calculations using the FEFF9.6 code. The HR-XANES experimental technique provides new insights into the actinides electronic structure and allows detection of minor contributions of Pu oxidation states in oxidation state mixtures.

Genuine radioactive glass sampled from the vitrification plant Karlsruhe and actinide doped model 2 glasses are investigated by U/Pu/Np M4/M5 high energy resolution X‐ray absorption near edge structure (HR‐XANES), U L3 EXAFS and XPS spectroscopy techniques to characterize and compare the U, Pu and Np oxidation states and their local atomic environments. The importance of the results will be discussed in terms of the strategy of using simplified simulated waste glasses to understand more complex industrial glass samples. The final goal of these studies is to predict the long term behavior of vitrified nuclear waste stored in a nuclear waste repository. Highly active waste concentrate (HAWC) from nuclear fuel reprocessing is immobilized in borosilicate glass matrices to generate a disposable waste form [1]. Between 2009 and 2010, the vitrification plant Karlsruhe (VEK) was operated for vitrification of liquid process residues left over from operation of the former reprocessing plant Karlsruhe (WAK). About 56 m3 HAWC were processed, resulting in 50 t of waste glass [2]. The long term radiotoxicity of U, Np, Pu and other actinide elements (An), minor constitute of the reprocessed waste, is of great concern in safety assessment studies of nuclear waste repositories. For example, in case of water intrusion and interaction with the glass matrix, corrosion processes will take place which might facilitate the release of radionuclides into the geosphere. The An redox state and bonding characteristics in the glass matrix determine their release mechanisms and retention processes taking place in near and far field of the repository [3]. Understanding the long term behavior of vitrified nuclear waste requires full and detailed characterization of the materials including their characteristics as synthesized and after exposure to groundwater. Genuine radioactive waste glass has a complex chemical composition. Therefore we take a simplified approach by investigating and comparing the oxidation states of U, Pu and Np in high level waste (HLW) glass sampled from the VEK vitrification process (VEK glass) and in model glasses. The model glasses doped with U and Pu have the same borosilicate glass frit composition as the VEK glass, whereas the model glass doped with Np has a base glass composition (R7T7) typically used for vitrification of HLW in France. U/Pu/Np M4/M5 edge high energy resolution X‐ray absorption near edge structure (HR‐XANES) spectroscopy technique [4] is applied to characterize the An oxidation states

One of the long standing debates in actinide chemistry is the level of localization and participation of the actinide 5f valence orbitals in covalent bonds across the actinide series. Here we illuminate the role of the 5f valence orbitals of uranium, neptunium and plutonium in chemical bonding using advanced spectroscopies: actinide M4,5 HR-XANES and 3d4f RIXS. Results reveal that the 5f orbitals are active in the chemical bonding for uranium and neptunium, shown by significant variations in the level of their localization evidenced in the spectra. In contrast, the 5f orbitals of plutonium appear localized and surprisingly insensitive to different bonding environments. We envisage that this report of using relative energy differences between the 5fδ/φ and 5fπ*/5fσ* orbitals as a qualitative measure of overlap-driven actinyl bond covalency will spark activity, and extend to numerous applications of RIXS and HR-XANES to gain new insights into the electronic structures of the actinide elements.

Herein, a multi-technique study was performed to reveal the elemental speciation and microphase composition in altered granitic rock collected from the Krunkelbach Valley uranium (U) deposit area near an abandoned U mine, Black Forest, Southern Germany. The former Krunkelbach U mine with 1–2 km surrounding area represents a unique natural analogue site with the rich accumulation of secondary U minerals suitable for radionuclide migration studies from a spent nuclear fuel (SNF) repository. Based on a micro-technique analysis using several synchrotron-based techniques such as X-ray fluorescence analysis, X-ray absorption spectroscopy, powder X-ray diffraction and laboratory-based scanning electron microscopy and Raman spectroscopy, the complex mineral assemblage was identified. While on the surface of granite, heavily altered metazeunerite–metatorbernite (Cu(UO$_{2}$)$_{2}$(AsO$_{4}$)$_{2-x}$(PO$_{4}$)$_{x}$·8H$_{2}$O) microcrystals were found together with diluted coatings similar to cuprosklodowskite (Cu(UO$_{2}$)$_{2}$(SiO$_{3}$OH)$_{2}$·6H$_{2}$O), in the cavities of the rock predominantly well-preserved microcrystals close to metatorbernite (Cu(UO$_{2}$)$_{2}$(PO$_{4}$)$_{2}$·8H$_{2}$O) were identified. The Cu(UO$_{2}$)$_{2}$(AsO$_{4}$)$_{2-x}$(PO$_{4}$)$_{x}$·8H$_{2}$O species exhibit uneven morphology and varies in its elemental composition, depending on the microcrystal part ranging from well-preserved to heavily altered on a scale of ∼200 μm. The microcrystal phase alteration could be presumably attributed to the microcrystal morphology, variations in chemical composition, and geochemical conditions at the site. The occurrence of uranyl-arsenate-phosphate and uranyl-silicate mineralisation on the surface of the same rock indicates the signatures of different geochemical conditions that took place after the oxidative weathering of the primary U- and arsenic (As)-bearing ores. The relevance of uranyl minerals to SNF storage and the potential role of uranyl-arsenate mineral species in the mobilization of U and As into the environment is discussed.

INTRODUCTION Plutonium is a chemical element of significant environmental and toxicological concern. At nuclear legacy sites, previous research has demonstrated that plutonium can migrate in colloidal form in the subsurface environment across several kilometers [1-2]. Recent spectroscopic and microscopic investigations showed that so called “colloidal Pu(IV) polymers” are in fact aggregates of PuO2 nanoparticles with diameters ~ 2 nm [3-4]. The exact stoichiometry and structure of such nanoparticles remain, however, still questionable, especially with respect to surface hydration and hydroxylation, as well as the purity of the tetravalent oxidation state considering the existence of four different oxidation states (with relatively small energy barriers III, IV, V, and VI) under environmental conditions. RESULTS This contribution will show first results of plutonium oxide nanoparticle studies at the large-scale facility – The European Synchrotron (ESRF) by X-ray spectroscopy and X-ray diffraction methods. Pu oxide nanoparticles were prepared by rapid chemical precipitation using precursors in the different oxidation states (Pu(III), Pu(IV), Pu(V) and Pu(VI)). These precursors were obtained by chemical reduction or oxidation of Pu stock solution. The obtained nanoparticles were characterized at the Rossendorf Beamline (ROBL) at the ESRF, dedicated to actinide science. The recently upgraded ROBL beamline provides unique opportunities to study actinide materials by several experimental techniques: high energy resolution fluorescence detection (HERFD) [5], X-ray emission spectroscopy (XES), resonant inelastic x-ray scattering (RIXS) [6], extended X-ray absorption fine structure (EXAFS) spectroscopy and X-ray diffraction (XRD) simultaneously. We will show how the detailed information about local and electronic structure and plutonium oxidation state in different nanoparticles can be obtained using the variety of methods.