scholarly journals Spectroscopic, Raman, EMPA, Micro-XRF and Micro-XANES Analyses of Sulphur Concentration and Oxidation State of Natural Apatite Crystals

Crystals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1032
Author(s):  
Bo Xu ◽  
Guanyu Kou ◽  
Barbara Etschmann ◽  
Daiyue Liu ◽  
Joël Brugger
Keyword(s):  
Reference Material ◽  
Oxidation State ◽  
Inductively Coupled Plasma ◽  
Small Contribution ◽  
Volatile Element ◽  
Edge Structure ◽  
X Ray ◽  
Sulphur Concentration ◽  
S Oxidation ◽  
Natural Apatite

Sulphur is the third most abundant volatile element in deep Earth systems. Analytical methods for accurately and efficiently determining the sulphur content and oxidation state in natural minerals are still lacking. Natural apatite is widely distributed in the Earth and incorporates a large amount of sulphur. Therefore, apatite is an ideal mineral for performing sulphur measurements. Here, we used spectroscopic, Raman, X-ray diffraction, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), electron microprobe (EMPA) and micro-X-ray fluorescence spectrometry (micro-XRF) analysis techniques and developed a new analytical approach (i.e., micro-X-ray absorption near-edge structure (micro-XANES) analysis of the sulphur K-edge) to investigate the chemical characteristics of natural apatite. These multiple methods were developed to measure in situ sulphur concentration and S oxidation states and to assess a potential natural apatite reference material. Apatite contains chemically homogeneous sulphur, with micro-XANES located at the peak energies corresponding to S6+ (sulphate; ~2482 eV), S4+ (sulfite; ~2478 eV), and S2− (sulphide; ~2467, 2470 and 2474 eV). The Durango apatite contains total S presented as SO3 at amount of 0.332 ± 0.012 wt.% (1σ), with a large amount of S6+ and a small contribution of S4+. The Kovdor apatite contains 44–100 ppm of S and is dominated by S6+. These results indicate that the Durango apatite crystallised under relative oxidising conditions, and the Kovdor apatite has a higher oxygen fugacity than Durango. In addition, this study indicates the potential use of the natural apatite reference material with its S composition and S oxidation state.

scholarly journals An X-ray Absorption Near-Edge Structure (XANES) Study on the Oxidation State of Chromophores in Natural Kunzite Samples from Nuristan, Afghanistan

Minerals ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 463
Author(s):  
Habib Ur Rehman ◽  
Gerhard Martens ◽  
Ying Lai Tsai ◽  
Chawalit Chankhantha ◽  
Pinit Kidkhunthod ◽  
...  
Keyword(s):  
Oxidation State ◽  
Inductively Coupled Plasma ◽  
Oxidation States ◽  
Transition Elements ◽  
Edge Structure ◽  
X Ray ◽  
Inductively Coupled ◽  
Valence States ◽  
Icp Ms ◽  
X Ray Absorption

Kunzite, the pink variety of spodumene is famous and desirable among gemstone lovers. Due to its tenebrescent properties, kunzite always remains a hot research candidate among physicists and mineralogists. The present work is continuing the effort towards value addition to kunzite by enhancing its color using different treatments. Before color enhancement, it is essential to identify the chromophores and their oxidation states. In this paper, the authors investigated the main impurities in natural kunzite from the Nuristan area in Afghanistan and their valence states. Some impurities in the LiAlSi2O6 spodumene structure were identified and quantified by using sensitive techniques, including Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), UV−VIS and X-ray absorption near-edge structure (XANES). LA-ICP-MS indicated many trace elements as impurities in kunzite, among which Fe and Mn are the main elements responsible for coloration. The oxidation states of these two transition elements were determined by the XANES technique. The study reveals that Mn is present in both Mn2+ and Mn3+ oxidation states, while Fe is present only in Fe3+ oxidation state.

Microstructure of TiC/Amorphous Hydrocarbon Nanocomposite Coatings

2000 ◽  
Vol 6 (S2) ◽  
pp. 440-441
Author(s):  
D. M. Cao ◽  
J. C. Jiang ◽  
B. Feng ◽  
W. J. Meng
Keyword(s):  
Inductively Coupled Plasma ◽  
High Hardness ◽  
Ceramic Surface ◽  
Edge Structure ◽  
X Ray ◽  
Inductively Coupled ◽  
Transmission Electron ◽  
Wide Range ◽  
Mechanical Components ◽  
X Ray Absorption

Application of an appropriate ceramic surface coating to mechanical components such as bearings and gears can provide longer life and increased performance reliability. Metal-containing hydrocarbon (Me-C:H) coatings possess high hardness, together with low friction and low wear rate. They have also been suggested to adhere better to metallic substrates. This combination of attractive mechanical/tribological properties makes Me-C:H coatings potentially useful for surface modification of a wide range of mechanical components.Using the technique of inductively coupled plasma (ICP) assisted vapor deposition[1], we have synthesized Ti-containing hydrocarbon (Ti-C:H) coatings with a wide range of Ti compositions[2]. Coating mechanical properties such as modulus and hardness have been measured by the technique of nanoindentation and correlated to Ti and hydrogen compositions[2,3].We have performed detailed microstructural examination of Ti-C:H coatings by transmission electron microscopy (TEM), Extended X-ray Absorption Fine Structure (EXAFS) spectroscopy, and X-ray Absorption Near Edge Structure (XANES) spectroscopy.

Oxygen Reduction Effect on T’-Pr2-xCexCuO4 Nanopowders in the Underdoped Regime Studied by X-Ray Absorption near Edge Structure

2018 ◽  
Vol 936 ◽  
pp. 93-97 ◽  
Author(s):  
Irfanita Resky ◽  
Putu Eka Dharma Putra ◽  
Triono Bambang ◽  
Saiyasombat Chatree ◽  
Kamonsuangkasem Krongthong ◽  
...  
Keyword(s):  
Oxidation State ◽  
Oxidation States ◽  
Edge Structure ◽  
X Ray ◽  
Reduction Annealing ◽  
Gas Atmosphere ◽  
Reduction Effect ◽  
Ar Gas ◽  
X Ray Absorption ◽  
Cu Ions

This research is aimed to examine oxidation state of Copper (Cu) in both as-synthesized and reduced T’-Pr2-xCexCuO4 (T’-PCCO) with x = 0, 0.10, and 0.15 using Cu K-edge x-ray absorption near edge structure (XANES). The T‘-PCCO nanopowders were successfully synthesized by the chemically dissolved method with HNO3 as a dissolving agent continued by calcination at 1000°C for 15 h. The reduced T’-PCCO nanopowders were obtained by reduction annealing process at 700°C for 5 h under Ar gas atmosphere. The analyses of XANES spectra show that oxidation states of the Cu ions in all of the T'-PCCO nanopowders have values between +1 and +2. This indicates the existence of electron doping in the CuO2 planes, even in the undoped T’-structure. It is found that the oxidation states of the Cu ions change after reduction annealing depending on the existence of apical oxygen in the T'-structure. Based on the XANES analyses, it is revealed that the change of oxidation state is influenced by the presence of both electron and hole carriers in the two-carrier model of T’-structure.

Using X-ray absorption near edge structure (XANES) spectroscopy to determine selenium oxidation states in animal mineral supplements and feeds

2004 ◽  
Vol 84 (2) ◽  
pp. 171-175 ◽  
Author(s):  
C. R. Christensen ◽  
J. N. Cutler ◽  
D. A. Christensen
Keyword(s):  
Oxidation State ◽  
Animal Feed ◽  
Xanes Spectroscopy ◽  
Elemental Selenium ◽  
Selenium Speciation ◽  
Edge Structure ◽  
X Ray ◽  
Mineral Supplements ◽  
Animal Feeds ◽  
X Ray Absorption

Synchrotron-based X-ray absorption near edge structure (XANES) spectroscopy is a relatively new technique within the life sciences. XANES has been utilized to identify the location, oxidation state and spatial distribution of heavy metal elements in plants , neurons, blood and DNA, but has not been widely used in the animal sciences. Selenium content in animal feeds is monitored, as both selenium deficiencies and toxicities are associated with physiological disorders. Selenium is available as an animal feed in both inorganic and organic states. The bioavailability of selenium species has been tested in numerous animal trials; however, a simple, non-destructive test for selenium speciation is not available. The objective of this study was to determine whether XANES spectroscopy could be used to determine the selenium oxidation state found in various commercial animal feed products. A comparison of absorption spectra indicated that the animal mineral supplements contained an organoselenium or selenite. The processed animal feeds had a spectral profile similar to that of elemental selenium. Further experiments are necessary to determine the implication of selenium speciation on animal physiology. Key words: Selenium speciation, mineral supplements, ruminants, non-ruminants, synchrotron, XANES, X-ray

Oxidation State of Ti Atoms and Ti-O Bond Length on Natural Sapphire Gem-Materials Probed by X-Ray Absorption Spectroscopy

2017 ◽  
Vol 737 ◽  
pp. 585-589 ◽  
Author(s):  
Natthapong Monarumit ◽  
Wiwat Wongkokua ◽  
Somruedee Satitkune
Keyword(s):  
Bond Length ◽  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Germanium Detector ◽  
Blue Color ◽  
Edge Structure ◽  
X Ray ◽  
Fe Content ◽  
X Ray Absorption ◽  
Exafs Spectra

Sapphire, an inorganic gem-material in a variety of corundum, mainly consists of alpha-alumina (α-Al2O3) structure. The geological origins of sapphire are related to either basaltic or metamorphic rocks. The causes of the color on sapphire are some trace elements such as Cr, Fe, and Ti. It could be mentioned that Ti atoms have cooperated with Fe atoms for creating the blue color. In this study, X-ray absorption spectroscopy (XAS) technique focused on the x-ray absorption near edge structure (XANES) and the extended x-ray absorption fine structure (EXAFS) is employed to identify the oxidation state of Ti atoms and Ti-O bond length on sapphire samples. The Ti K-edge XANES and EXAFS spectra of natural sapphires were carried out using the 13-channel array germanium detector in fluorescence mode. The XANES spectra showed that the oxidation state of Ti was Ti4+ regardless of Fe content. Moreover, the Ti-O bond length on a-Al2O3 was equal to the Ti-O bond length on rutile (TiO2) analyzed from the EXAFS spectra. From these results, it could be concluded that the oxidation state of Ti atoms on natural sapphires was Ti4+ which substitutes Al3+ on the sapphire structure.

Study of the Oxidation State of Arsenic and Uranium in Individual Particles From Uranium Mine Tailings, Hungary

2007 ◽  
Author(s):  
A. Alsecz ◽  
J. Osa´n ◽  
J. Pa´lfalvi ◽  
I. Sajo´ ◽  
Z. Ma´the´ ◽  
...  
Keyword(s):  
Oxidation State ◽  
Mine Tailings ◽  
Track Detector ◽  
Uranium Mine ◽  
Nuclear Track Detector ◽  
Mobile Form ◽  
Edge Structure ◽  
X Ray ◽  
Uranium Ore ◽  
Distribution Of Elements

Uranium ore mining and milling have been terminated in the Mecsek Mountains (southwest Hungary) in 1997. Mine tailings ponds are located between two important water bases, which are resources of the drinking water of the city of Pe´cs and the neighbouring villages. The average U concentration of the tailings material is 71.73 μg/g, but it is inhomogeneous. Some microscopic particles contain orders of magnitude more U than the rest of the tailings material. Other potentially toxic elements are As and Pb of which chemical state is important to estimate mobility, because in mobile form they can risk the water basis and the public health. Individual U-rich particles were selected with solid state nuclear track detector (SSNTD) and after localisation the particles were investigated by synchrotron radiation based microanalytical techniques. The distribution of elements over the particles was studied by micro beam X-ray fluorescence (μ-XRF) and the oxidation state of uranium and arsenic was determined by micro X-ray absorption near edge structure (μ-XANES) spectroscopy. Some of the measured U-rich particles were chosen for studying the heterogeneity with μ-XRF tomography. Arsenic was present mainly in As(V) and uranium in U(VI) form in the original uranium ore particles, but in the mine tailings samples uranium was present mainly in the less mobile U(IV) form. Correlation was found between the oxidation state of As and U in the same analyzed particles. These results suggest that dissolution of uranium is not expected in short term period.

Direct determination of oxidation state of gold deposits in metal-reducing bacterium Shewanella algae using X-ray absorption near-edge structure spectroscopy (XANES)

2007 ◽  
Vol 103 (6) ◽  
pp. 568-571 ◽  
Author(s):  
Yasuhiro Konishi ◽  
Takeshi Tsukiyama ◽  
Norizoh Saitoh ◽  
Toshiyuki Nomura ◽  
Shinsuke Nagamine ◽  
...  
Keyword(s):  
Oxidation State ◽  
Direct Determination ◽  
Gold Deposits ◽  
Edge Structure ◽  
X Ray ◽  
Shewanella Algae ◽  
X Ray Absorption

scholarly journals Seleno-l-Methionine Is the Predominant Organic Form of Selenium in Cupriavidus metallidurans CH34 Exposed to Selenite or Selenate

2006 ◽  
Vol 72 (9) ◽  
pp. 6414-6416 ◽  
Author(s):  
Laure Avoscan ◽  
Richard Collins ◽  
Marie Carriere ◽  
Barbara Gouget ◽  
Jacques Cov�s
Keyword(s):  
Inductively Coupled Plasma ◽  
High Performance ◽  
Organic Form ◽  
Edge Structure ◽  
Cupriavidus Metallidurans Ch34 ◽  
X Ray ◽  
Inductively Coupled ◽  
Cupriavidus Metallidurans ◽  
Plasma Mass Spectrometry ◽  
X Ray Absorption

ABSTRACT The accumulated organic form of selenium previously detected by X-ray absorption near-edge structure (XANES) analyses in Cupriavidus metallidurans CH34 exposed to selenite or selenate was identified as seleno-l-methionine by coupling high-performance liquid chromatography to inductively coupled plasma-mass spectrometry.

scholarly journals A compact furnace for in situ X-ray absorption spectroscopy: design, fabrication and study of cationic oxidation states in Pr6O11 and NiO

2021 ◽  
Vol 28 (2) ◽  
pp. 455-460
Author(s):  
Suchinda Sattayaporn ◽  
Somboonsup Rodporn ◽  
Pinit Kidkhunthod ◽  
Narong Chanlek ◽  
Chutarat Yonchai ◽  
...  
Keyword(s):  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Heating Temperature ◽  
Reduction Process ◽  
Oxidation States ◽  
Quartz Tube ◽  
Edge Structure ◽  
X Ray ◽  
X Ray Absorption

A well designed compact furnace has been designed for in situ X-ray absorption spectroscopy (XAS). It enables various heat ramps from 300 K to 1473 K. The furnace consists of heaters, a quartz tube, a circulated refrigerator and a power controller. It can generate ohmic heating via an induction process with tantalum filaments. The maximum heating rate exceeds 20 K min−1. A quartz tube with gas feedthroughs allows the mixing of gases and adjustment of the flow rate. The use of this compact furnace allows in situ XAS investigations to be carried out in transmission or fluorescence modes under controlled temperature and atmosphere. Moreover, the furnace is compact, light and well compatible to XAS. The furnace was used to study cationic oxidation states in Pr6O11 and NiO compounds under elevated temperature and reduced atmosphere using the in situ X-ray absorption near-edge structure (XANES) technique at beamline 5.2 SUT-NANOTEC-SLRI of the Synchrotron Light Research Institute, Thailand. At room temperature, Pr6O11 contains a mixture of Pr3+ and Pr4+ cations, resulting in an average oxidation state of +3.67. In situ XANES spectra of Pr (L 3-edge) show that the oxidation state of Pr4+ cations was totally reduced to +3.00 at 1273 K under H2 atmosphere. Considering NiO, Ni2+ species were present under ambient conditions. At 573 K, the reduction process of Ni2+ occurred. The Ni0/Ni2+ ratio increased linearly with respect to the heating temperature. Finally, the reduction process of Ni2+ was completely finished at 770 K.

scholarly journals The State of Trace Elements (In, Cu, Ag) in Sphalerite Studied by X-Ray Absorption Spectroscopy of Synthetic Minerals

Minerals ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 640 ◽  
Author(s):  
Nikolay D. Trofimov ◽  
Alexander L. Trigub ◽  
Boris R. Tagirov ◽  
Olga N. Filimonova ◽  
Polina V. Evstigneeva ◽  
...  
Keyword(s):  
Solid Solution ◽  
Oxidation State ◽  
Absorption Spectroscopy ◽  
Atomic Structure ◽  
Salt Flux ◽  
Ionic Radii ◽  
Edge Structure ◽  
X Ray ◽  
X Ray Absorption ◽  
Exafs Spectra

The oxidation state and local atomic environment of admixtures of In, Cu, and Ag in synthetic sphalerite crystals were determined by X-ray absorption spectroscopy (XAS). The sphalerite crystals doped with In, Cu, Ag, In–Cu, and In–Ag were synthesized utilizing gas transport, salt flux, and dry synthesis techniques. Oxidation states of dopants were determined using X-ray absorption near edge structure (XANES) technique. The local atomic structure was studied by X-ray absorption fine structure spectroscopy (EXAFS). The spectra were recorded at Zn, In, Ag, and Cu K-edges. In all studied samples, In was in the 3+ oxidation state and replaced Zn in the structure of sphalerite, which occurs with the expansion of the nearest coordination shells due to the large In ionic radius. In the presence of In, the oxidation state of Cu and Ag is 1+, and both metals can form an isomorphous solid solution where they substitute for Zn according to the coupled substitution scheme 2Zn2+ ↔ Me+ + In3+. Moreover, Ag K-edges EXAFS spectra fitting, combined with the results obtained for In- and Au-bearing sphalerite shows that the Me-S distances in the first coordination shell in the solid solution state are correlated with the ionic radii and increase in the order of Cu < Ag < Au. The distortion of the atomic structure increases in the same order. The distant (second and third) coordination shells of Cu and Ag in sphalerite are split into two subshells, and the splitting is more pronounced for Ag. Analysis of the EXAFS spectra, coupled with the results of DFT (Density Function Theory) simulations, showed that the In–In and Me+–In3+ clustering is absent when the metals are present in the sphalerite solid solution. Therefore, all studied admixtures (In, Cu, Ag), as well as Au, are randomly distributed in the matrix of sphalerite, where the concentration of the elements in the “invisible” form can reach a few tens wt.%.

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