Fine-scale phosphorus distribution in coral skeletons: combining X-ray mapping by electronprobe microanalysis and LA-ICP-MS

ABSTRACT Hingganite-(Nd), ideally Nd2□Be2Si2O8(OH)2, is a new gadolinite group, gadolinite supergroup mineral discovered at Zagi Mountain, near Kafoor Dheri, about 4 km S of Warsak and 30 km NW of Peshawar, Khyber Pakhtunkhwa Province, Pakistan. The new mineral forms zones measuring up to 1 × 1 mm2 in loose prismatic crystals up to 0.7 cm long, where it is intergrown with hingganite-(Y). Other associated minerals include aegirine, microcline, fergusonite-(Y), and zircon. Hingganite-(Nd) is dark greenish-brown, transparent, has vitreous luster and a white streak. It is brittle and has a conchoidal fracture. No cleavage or parting are observed. Mohs hardness is 5½–6. Dcalc. = 4.690 g/cm3. Hingganite-(Nd) is non-pleochroic, optically biaxial (+), α = 1.746(5), β = 1.766(5), γ = 1.792(6) (589 nm). 2Vmeas. = 80(7)°; 2Vcalc. = 84°. Dispersion of optical axes was not observed. The average chemical composition of hingganite-(Nd) is as follows (wt.%; electron microprobe, BeO, B2O3, and Lu2O3 content measured by LA-ICP-MS; H2O calculated by stoichiometry): BeO 9.64, CaO 0.45, MnO 0.10, FeO 3.03, B2O3 0.42, Y2O3 8.75, La2O3 1.63, Ce2O3 12.89, Pr2O3 3.09, Nd2O3 16.90, Sm2O3 5.97, Eu2O3 1.08, Gd2O3 5.15, Tb2O3 0.50, Dy2O3 2.50, Ho2O3 0.33, Er2O3 0.84, Tm2O3 0.10, Yb2O3 0.44, Lu2O3 0.04, ThO2 0.13, SiO2 23.55, H2O 2.72, total 100.25. The empirical formula calculated on the basis of 2 Si apfu is (Nd0.513Ce0.401Y0.395Sm0.175Gd0.145Pr0.096Dy0.068La0.051Ca0.041Eu0.031Er0.022Tb0.014Yb0.011Ho0.009Tm0.003Th0.003Lu0.001)Σ1.979(□0.778Fe2+0.215Mn0.007)Σ1.000(Be1.967B0.062)Σ2.029Si2O8.46(OH)1.54. Hingganite-(Nd) is monoclinic, space group P21/c with a = 4.77193(15), b = 7.6422(2), c = 9.9299(2) Å, β = 89.851(2)°, V = 362.123(14) Å3, and Z = 2. The strongest lines of the powder X-ray diffraction pattern [d, Å (I, %) (hkl)] are: 6.105 (95) (011), 4.959 (56) (002), 4.773 (100) (100), 3.462 (58) (102), 3.122 , 3.028 (61) (013), 2.864 (87) (121), 2.573 (89) (113). The crystal structure of hingganite-(Nd) was refined from single-crystal X-ray diffraction data to R = 0.034 for 2007 unique reflections with I > 2σ(I). The new mineral is named as an analogue of hingganite-(Y), hingganite-(Yb), and hingganite-(Ce), but with Nd dominant among the rare earth elements.

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GOLD PROVENANCE AND CHARACTERIZATION USING MICRO X-RAY FLUORESCENCE (µXRF): PRELIMINARY RESULTS/ PROVENIÊNCIA E CARACTERIZAÇÃO DE OURO COM MICRO FLUORESCÊNCIA DE RAIOS X (μXRF): RESULTADOS PRELIMINARES

Journal of Sedimentary Environments ◽

10.12957/jse.2018.37905 ◽

2018 ◽

Vol 3 (3) ◽

pp. 155-165

Author(s):

William Murussi Canto ◽

Hamilton Santos Gama Filho ◽

Marcelino José dos Anjos ◽

Armando Dias Tavares Jr. ◽

Mauro César Geraldes

Keyword(s):

Sample Preparation ◽

Pure Gold ◽

Noninvasive Technique ◽

X Ray ◽

Preliminary Results ◽

Icp Ms ◽

Para Determinar ◽

Made In ◽

Gold Digging

This work presents some preliminary results that allows to characterize gold samples using Micro X-Ray Fluorescence/µXRF. The first aim of this work is to apply a noninvasive technique, preserving the sample integrity, in order to identify the composition of gold samples and to recognize their possible geographical provenance. Samples have been obtained in geographically distinct gold-digging sites, in three Brazilian and one Colombian areas. These samples were processed only by fusion into a furnace at 1,200 ºC. The proportion of Au, Ag and Cu were measured in gold samples. The results of this work, allowed to characterize and to identify quite well the pure gold provenance, using µXRF instrumentation and related techniques. Further work is in progress to determine the behavior of mixed gold samples from different provenances. Besides that, measurements with different sample preparation will be made, in order to compare the results obtained in this work with those obtained by LA-ICP-MS techniques. ResumoEste trabalho apresenta resultados preliminares que permitem caracterizar amostras de ouro utilizando a Micro Fluorescência de Raios-X/ µXRF. O primeiro objetivo deste trabalho é aplicar uma técnica não invasiva, preservando a integridade da amostra, para identificar a composição de amostras de ouro e reconhecer a sua possível proveniência geográfica. As amostras foram obtidas em locais de exploração de ouro geograficamente distintos, em três áreas brasileiras e uma colombiana. Estas amostras foram sugeitas a fusão a 1.200 ºC, num forno. A proporção de Au, Ag e Cu foi medida em amostras de ouro. Os resultados deste trabalho permitiram caracterizar e claramente identificar a proveniência de ouro puro, utilizando resultados de µXRF. Estão em andamento outros trabalhos para determinar o comportamento da mistura de amostras de ouro de diferentes procedências. Além disso, serão efetuadas medições com diferentes preparações de amostras, a fim de comparar os resultados obtidos neste trabalho com os que estão sendo aquiridos com técnicas de LA-ICP-MS.

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X-ray linear dichroic ptychography

Proceedings of the National Academy of Sciences ◽

10.1073/pnas.2019068118 ◽

2021 ◽

Vol 118 (3) ◽

pp. e2019068118

Author(s):

Yuan Hung Lo ◽

Jihan Zhou ◽

Arjun Rana ◽

Drew Morrill ◽

Christian Gentry ◽

...

Keyword(s):

Tooth Enamel ◽

Phase Imaging ◽

Crystalline Materials ◽

X Ray ◽

Coral Skeletons ◽

Mineral Growth ◽

Multiple Length Scales ◽

Transmission Electron ◽

Scanning Transmission ◽

Amorphous Nanoparticle

Biominerals such as seashells, coral skeletons, bone, and tooth enamel are optically anisotropic crystalline materials with unique nanoscale and microscale organization that translates into exceptional macroscopic mechanical properties, providing inspiration for engineering new and superior biomimetic structures. Using Seriatopora aculeata coral skeleton as a model, here, we experimentally demonstrate X-ray linear dichroic ptychography and map the c-axis orientations of the aragonite (CaCO3) crystals. Linear dichroic phase imaging at the oxygen K-edge energy shows strong polarization-dependent contrast and reveals the presence of both narrow (<35°) and wide (>35°) c-axis angular spread in the coral samples. These X-ray ptychography results are corroborated by four-dimensional (4D) scanning transmission electron microscopy (STEM) on the same samples. Evidence of co-oriented, but disconnected, corallite subdomains indicates jagged crystal boundaries consistent with formation by amorphous nanoparticle attachment. We expect that the combination of X-ray linear dichroic ptychography and 4D STEM could be an important multimodal tool to study nano-crystallites, interfaces, nucleation, and mineral growth of optically anisotropic materials at multiple length scales.

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Sorption of As (III) and Se (IV) from aqueous solutions for subsequent determination by total reflection X-ray fluorescence

Industrial laboratory Diagnostics of materials ◽

10.26896/1028-6861-2021-87-8-19-22 ◽

2021 ◽

Vol 87 (8) ◽

pp. 19-22

Author(s):

D. G. Filatova ◽

A. A. Arkhipenko ◽

M. A. Statkus ◽

I. V. Mikheev ◽

V. B. Baranovskaya ◽

...

Keyword(s):

Raw Materials ◽

Total Reflection ◽

Phase Contact Time ◽

Sorbent Phase ◽

X Ray ◽

Icp Ms ◽

Subsequent Determination ◽

Processed Products ◽

Branched Structure

An approach to the simultaneous isolation of As (III) and Se (IV) from solutions on a new S,N-containing sorbent followed by determination of the analyte in the sorbent phase using total reflection X-ray fluorescence (TXRF) has been proposed. To match the goal, a sorbent with a branched structure was synthesized on the base of polyacrylamide modified with formaldehyde and hydrogen sulfide. This is a heteroatomic copolymer containing sulfide bridges in the chain and crosslinking by a tertiary amine. Conditions for the quantitative co-extraction of As (III) and Se (IV), i.e., sorption in solutions of 1 M HNO3 with calcium ions present, heating to 60°C and phase contact time of 1 h were determined. The mechanism of sorption interaction of the analytes under specified conditions is discussed. It is shown that a 100-fold excess of iron, zinc and copper does not interfere with the extraction of analytes, thus providing the possibility of As (III) and Se (IV) isolation from different types of raw materials and processed products using the synthesized sorbent. A method for the direct XRF quantification of arsenic and selenium with sr 0.09 and 0.08, respectively, in the sorbent phase has been developed. The correctness of the results was confirmed by the ICP-MS method in analysis of aqueous reference solution after dissolution of the sorbate in HNO3 (1:1).

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A Review on Metal Impurities in Pharmaceuticals

Asian Journal of Pharmaceutical Analysis ◽

10.52711/2231-5675.2021.00038 ◽

2021 ◽

pp. 212-222

Author(s):

Ashok B. Patel ◽

Avadhi R. Bundheliya ◽

Amitkumar J. Vyas ◽

Nilesh K. Patel ◽

Ajay I. Patel ◽

...

Keyword(s):

Drug Product ◽

Analytical Techniques ◽

Pharmaceutical Product ◽

Raw Material ◽

Impurity Level ◽

Metal Catalyst ◽

Metal Impurity ◽

X Ray ◽

Metal Impurities ◽

Icp Ms

Sources of metal impurities can from anywhere in drug product as raw material which may produce using metal catalyst, excipients, process materials, Water or any solvent used, manufacturing equipment, environment, packaging materials. So, it leads to metal impurity in high amount present in final drug product that is why it is important to check the impurity level in final drug product or as well as in process also that it should be present in low or acceptable amount. Any Drug product is not completely pure, some amount of metal impurities are always present in pharmaceutical product may cause various toxicity when it will be administered. Thus it is necessary to check impurity level is present at acceptable amount. The present review gives an account of updated information about metal impurities and reviews the regulatory aspects for such metal impurities in drug substance/drug product. In addition the aim of this article is to discuss the currently used different analytical techniques for detection of metals from drug product like spectrophotometry, X – Ray florescence spectrometry, AAS, INAA, ICP – AES, ICP – MS, MP – AES, Laser Ablation – ICP – MS etc which is used for quality control of metal impurities in pharmaceuticals.

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Mineralogical Study and Genetic Model of Efflorescent Salts and Crusts from Two Abandoned Tailings in the Taxco Mining District, Guerrero (Mexico)

Minerals ◽

10.3390/min10100871 ◽

2020 ◽

Vol 10 (10) ◽

pp. 871

Author(s):

Teresa Pi-Puig ◽

Jesús Solé ◽

Adriana Gómez Cruz

Keyword(s):

Genetic Model ◽

Rietveld Method ◽

Short Wave ◽

Mining District ◽

X Ray Diffraction ◽

Wet Season ◽

X Ray ◽

Icp Ms ◽

Mineralogical Study ◽

Plasma Mass Spectrometry

The mineralogy of surface crusts and efflorescent salts of two old abandoned tailings (Xochula and Remedios) of the mining district of Taxco, Guerrero, was studied by short-wave infrared spectroscopy (SWIR), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The chemistry of the selected samples was studied with induced coupled plasma mass spectrometry (ICP–MS). Principal mineralogy is composed of hydrated sulfates of iron (di-trivalent), other less-soluble sulfates such as gypsum and jarosite, and oxides–hydroxides of iron, all of which are the result of the weathering of sulfides (mainly pyrite) accumulated in mining waste. Using quantitative X-ray diffraction (Rietveld method) and the spatial distribution of secondary minerals, two main zones (lateral and central) have been established in both tailings. The genetic model for their formation shows that the secondary iron minerals (sulfates, oxides, and hydroxides) in these deposits have been formed at least in three different stages, mainly by oxidation, dissolution, and precipitation processes in combination with dehydration and primary sulfides neutralization reactions. The chemical analyses of some salts confirm the presence of potentially toxic elements (PTE) in their structure and therefore indicate that the dissolution of the efflorescences in these deposits is a potential source of contamination during the wet season.

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Pure Ni Single Crystal of Cube Orientation Deformed by Equal Channel Angular Extrusion

Solid State Phenomena ◽

10.4028/www.scientific.net/ssp.105.333 ◽

2005 ◽

Vol 105 ◽

pp. 333-338 ◽

Cited By ~ 7

Author(s):

D. Goran ◽

Jean-Jacques Fundenberger ◽

Satyam Suwas ◽

Emmanuel Bouzy ◽

László S. Tóth ◽

...

Keyword(s):

Single Crystal ◽

Equal Channel Angular Extrusion ◽

Fine Scale ◽

X Ray Diffraction ◽

Cube Orientation ◽

X Ray ◽

Angular Extrusion ◽

Global And Local

Texture and microstructure were investigated after 1 pass equal channel angular extrusion (ECAE) of a single crystal cube oriented Ni billet. Neutron and X-ray diffraction were used to determine global and local textures, respectively. To investigate the fine scale microstructural features EBSD was used. Substantial variations in texture and microstructure resulting from different efficiencies in the shearing process were locally recorded through the billet height.

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Chelidonic Acid and Its Derivatives from Saussurea Controversa: Isolation, Structural Elucidation and Influence on the Osteogenic Differentiation of Multipotent Mesenchymal Stromal Cells In Vitro

Biomolecules ◽

10.3390/biom9050189 ◽

2019 ◽

Vol 9 (5) ◽

pp. 189 ◽

Cited By ~ 3

Author(s):

Elena Avdeeva ◽

Elvira Shults ◽

Tatyana Rybalova ◽

Yaroslav Reshetov ◽

Ekaterina Porokhova ◽

...

Keyword(s):

Mesenchymal Stromal Cells ◽

Stromal Cells ◽

Cell Mass ◽

Multipotent Mesenchymal Stromal Cells ◽

Bone Tissue Regeneration ◽

X Ray ◽

Icp Ms ◽

First Time ◽

Asteraceae Family

4-oxo-4H-pyran-2.6-dicarboxylic acid (chelidonic acid, ChA) in the native state and in the complex with calcium [Ca(ChA)(H2O)3], named saucalchelin (CaChA), was isolated from the extract of Saussurea controversa leaves for the first time for the Asteraceae family. The structure of ChA was determined by NMR, MS and confirmed by X-ray analysis of its monomethyl ester, and CaChA was described by IR, ICP-MS, CHN analysis. The yield of ChA and CaChA was 45 mg/g and 70 mg/g of extract, respectively. The osteogenic activity of ChA, n-monobutyl ester of chelidonic acid, and CaChA has been studied in vitro in a 21-day culture of human adipose-derived multipotent mesenchymal stromal cells (hAMMSCs) in a standard nutrient medium without osteogenic supplements. CaChA significantly stimulated the growth of cell mass and differentiation of hAMMSCs into osteoblasts with subsequent mineralization of the culture and it may be a promising substance for accelerating bone tissue regeneration and engineering.

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ANÁLISIS DE LOS ELEMENTOS MINERALES ESENCIALES Y TÓXICOS EN TEJIDOS VEGETALES

Agrociencia ◽

10.47163/agrociencia.v54i3.1916 ◽

2020 ◽

Vol 54 (3) ◽

pp. 413-434

Author(s):

Juliana Padilla-Cuevas ◽

Hernani T. Yee-Madeira ◽

Agustín Merino-García ◽

Claudia Hidalgo ◽

Jorge D. Etchevers

Keyword(s):

Mass Spectrometry ◽

Inductively Coupled Plasma ◽

Ad Hoc ◽

Absorption Spectrometry ◽

Atomic Emission ◽

Atomic Emission Spectrometry ◽

Emission Spectrometry ◽

X Ray ◽

Inductively Coupled ◽

Icp Ms

Las técnicas para analizar los elementos esenciales o tóxicos para las plantas y los seres humanos, ha experimentado un acelerado desarrollo en los últimos tiempos, tanto en las convencionales o clásicas, que requieren la solubilización de la muestra, como en otras emergentes que no la requieren. Las técnicas convencionales avanzadas y las no destructivas se usan poco por los investigadores en genética, agronomía, nutrición, fisiología, biología, para evaluar la composición y calidad nutrimental de alimentos, cuantificar elementos metálicos esenciales y tóxicos, diagnosticar el estado nutrimental de los cultivos y estudiar alimentos funcionales. Estas técnicas analíticas se pueden aplicar, además, a suelos, abonos y fertilizantes. El objetivo de este ensayo es difundir las posibilidades de aplicación y los principios básicos de estas técnicas analíticas emergentes. La espectrometría de emisión por atomización con plasma inductivamente acoplado (ICP, Inductively coupled plasma) y la de ICP masas (ICP-MS, Mass spectrometry with inductive coupling plasma) tienen mayor interés que las técnicas clásicas usadas en los laboratorios de los países de escaso desarrollo, como las espectrometrías de emisión (AES, Atomic emission spectrometry) y absorción atómica (AAS, Atomic absorption spectrometry), que requieren solubilización de la matriz. La ICP-MS y la ICP tienen ventajas para el análisis simultáneo de contenidos totales de la mayoría de los elementos esenciales para el crecimiento de los vegetales. Entre las técnicas no destructivas de la matriz, la mayoría de las consideradas en este ensayo se basan en la interacción de los rayos X con la materia, como fotoemisión de rayos X (XPS, X-ray photoelectron spectrometry), emisión de rayos X inducida por partículas (PIXE, Particle induced X-ray emission), fluorescencia de rayos X (XRF, X-ray fluorescence) y espectrometría de dispersión de energía de rayos X (EDS, Energy-dispersive X-ray spectroscopy), similares en sus fundamentos. Estas técnicas, a diferencias de las anteriores, no requieren solubilizar la muestra o su preparación es mínima. Otras ventajas son su rapidez, la realización de análisis multielemental simultáneo, tamaño pequeño de muestra, adquisición de la distribución de elementos químicos en la muestra y generar mapas en dos dimensiones. Las cuatro técnicas descritas más arriba analizan contenidos totales. PIXE y XRF presentan mayor sensibilidad que las otras dos para cuantificar elementos traza en concentraciones de partes por millón, y estas dos más EDS se pueden acoplar a microscopios ad hoc para obtener la distribución de elementos químicos y hacer mapeos. La técnica XPS permite analizar fracciones iónicas en estudios de estados de oxidación de los elementos, pero las concentraciones en las muestras deben ser superiores a 0.1% en peso. Las aplicaciones de las técnicas no destructivas generan información complementaria a las clásicas y aportan conocimiento básico. Otras ventajas es que la preparación de las muestras requiere menos tiempo, excepto cuando se requieren mapeos. Su capacidad para ejecutar multianálisis permite reducir costos. En México y otros países hay grupos de investigación especializados en estas técnicas, pero es necesario desarrollar e implementar aplicaciones para realizar análisis de matrices biológicas como vegetales (semillas, hojas, etc.), alimentos, abonos y matriz orgánica de los suelos. Un conocimiento más profundo de estas técnicas permitirá la interacción de grupos de investigación y generar información para estudios de ciencia básica en agronomía y alimentos.

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