Structural characterization of iron oxide/hydroxide nanoparticles in nine different parenteral drugs for the treatment of iron deficiency anaemia by electron diffraction (ED) and X-ray powder diffraction (XRPD)
Drug products containing iron oxide and hydroxide nanoparticles (INPs) are important for the treatment of iron deficiency anaemia. Pharmaceuticals prepared by the complexation of different kinds of INPs and carbohydrates have different physicochemical and biopharmaceutic characteristics. The increasing number of parenteral non-biological complex drugs (NBCD) containing iron requires physicochemical methods for characterization and enabling of cross comparisons. In this context the structure and the level of crystallinity of the iron phases may be connected to the in vitro and in vivo dissolution rates, which etiologically determine the therapeutic and toxic effects. X-ray powder diffraction…
Zircon M257 - a homogeneous natural reference material for the ion microprobe U-Pb analysis of zircon
We introduce and propose zircon M257 as a future reference material for the determination of zircon U-Pb ages by means of secondary ion mass spectrometry. This light brownish, flawless, cut gemstone specimen from Sri Lanka weighed 5.14 g (25.7 carats). Zircon M257 has TIMS-determined, mean isotopic ratios (2s uncertainties) of 0.09100 ± 0.00003 for 206pb/238U and 0.7392 ± 0.0003 for 207pb/235U. Its 206pb/238U age is 561.3 ± 0.3 Ma (unweighted mean, uncertainty quoted at the 95% confidence level); the U-Pb system is concordant within uncertainty of decay constants. Zircon M257 contains ∼ 840 μg g−1 U (Th/U ∼ 0.27). The material exhibits remarkably low heterogeneity, with a virtual absence of…
The Ti-influence on the tourmaline color
Titanium was examined in different black tourmalines by spectrophotometric analyses in the region between 12500 and 27000 cm-1 (800-370 nm) using a microscope spectrophotometer MPV-5P, Leitz (Germany), and chemically analyzed on an electron microprobe Camebax Microbeam, Cameca (France) in WDS Mode. Fourteen tourmaline samples with their face oriented parallel to the principal axis, cut and polished down to thin sections, showed polarized spectra of two broad absorption bands at approximately 14000 cm-1 (715 nm) and 24000 cm-1 (417 nm). Precision thickness measurements were used to calculate the absorption coefficients α. For the absorption around 24000 cm-1, a linear correlation was observe…
Validation of Powder X-Ray Diffraction Following EN ISO/IEC 17025
: Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase iden…
Zircon M127 - A Homogeneous Reference Material for SIMS U-Pb Geochronology Combined with Hafnium, Oxygen and, Potentially, Lithium Isotope Analysis
Faculty of Geosciences, Geography and Astronomy, University of Vienna; Beijing SHRIMP Centre, Chinese Academy of Geological Sciences; European Commission [MEXC-CT-2005-024878]; FWF Austrian Science Fund [P20028-N10, P24448-N19]; U.S. National Science Foundation [EAR 1524336]
Micro-Raman spectroscopy of pigments contained in different calcium carbonate polymorphs from freshwater cultured pearls
The metastable calcium carbonate polymorph vaterite has recently been found to occur commonly in freshwater cultured pearls from Japan and China. Organic pigment molecules in these vaterite regions of freshwater cultured pearls were analysed by resonance and near-resonance micro-Raman spectroscopy, in single spectra and in mapping modes and are compared with their aragonitic counterparts. Four different excitation wavelengths (487.9, 514.5, 532.2 and 632.8 nm) were used, resulting in differential increase of resolution for the pigments. Although vaterite areas were always lightly coloured (light yellow, light brown or white), ten different pigments were identified and a single colour is for…
Rod-like ferrites obtained through thermal degradation of a molecular ferrimagnet
This paper presents the characteristics of iron oxides obtained through thermal degradation of a molecular ferrimagnet, {N(n-C4H9)4[Fe II
Geochemical provenance analyses of Roman lava millstones north of the Alps: a study of their distribution and implications for the beginning of Roman lava quarrying in the Eifel region (Germany)
Abstract In Roman times, rotary querns and different types of millstones, driven either by horse-capstan or water power, were produced in the lava quarries of the quaternary volcanic Eifel region and exported to many parts of the Empire. The geographic distribution of Roman lava millstones from the Eifel region provides important information about trade patterns and, in cases of well dated millstones, also allows an estimate as to when the Roman lava quarrying in the Eifel region began. Sixty-two millstones from Germany, France and Austria were sampled and analyzed for major and trace elements by X-ray fluorescence. To determine their provenance, the millstone data was evaluated by a combin…
Structural Investigation of K-Feldspar KAlSi3O8Crystals by XRD and Raman Spectroscopy: An Application to Petrological Study of Luc Yen Pegmatites, Yen Bai Province, Vietnam
K-feldspars in pegmatites from Luc Yen gem mining area, Yen Bai province, Vietnam were studied by X-ray fluorescence, X-ray powder diffraction and the Raman spectroscopy. Chemical analysis determined the K-feldspars in the form of (K0:8909Na0:0388Ca0:002Pb0:0042Cs0:0024Rb0:0338)(Al0:9975Fe0:0053Ti0:0004)Si2:988O8. Both X-ray powder diffraction and Raman spectroscopy indicated Luc Yen K-feldspars as orthoclase phase. Together with the values of Al content of the T1 tetrahedral sites in orthoclase, it is understood that Luc Yen pegmatites are of young ages (Cenozoic) and shallow intrusive types.
Study of phase transition in Bi3TiNbO9-BaBi2Nb2O9 ceramics
Abstract The subject of the paper is lead free bismuth layer structure oxides (1-x)Bi3TiNbO9-xBaBi2Nb2O9 (x=0; 1; 2; 3 mol). The influence of Bi3TiNbO9/BaBi2Nb2O9 ratio on dielectric and structural properties was studied in a wide range of temperatures. Change in the ratio causes a decrease in the maximum value of dielectric permittivity and shifts the temperature of ε’max to low values, leading to linear decreasing of average grain size and linear increasing of ceramics density. These results indicate an augment of the packing degree and the participation of pores are significantly decreased with the increase of BaBi2Nb2O9 compound intake. Moreover, for 0.7Bi3TiNbO9-0.3BaBi2Nb2O9 ceramics …
Structural characterization and chemical composition of aragonite and vaterite in freshwater cultured pearls
AbstractVaterite and aragonite polymorphs in freshwater cultured pearls from mussels of the genus Hyriopsis (Unionidae) were structurally and compositionally characterized by Raman spectroscopy, Micro computer tomography, high resolution field emission scanning electron microscopy, electron microprobe analysis and laser ablation inductively coupled plasma mass spectrometry. The appearance of vaterite in pearls is related to the initial stages of biomineralization, although we demonstrate that vaterite can not be a precursor to aragonite. It is not related to a particular crystal habit and therefore does not have a structural functionality in the pearls. Larger contents of elements typically…
Microstructural and magnetic characterization of fly ash from Kolaghat Thermal Power Plant in West Bengal, India
Abstract This paper reports on the physical nature of the fly ash sample of the Kolaghat Thermal Power Plant, India with an emphasis on its ultrafine nature. This paper also deals with the measurement of the magnetic properties of the fine particles of the fly ash sample. Particle sizes of this fly ash sample estimated from the SEM images lie within 0.16–5.50 μm, and the EDX spectral analysis indicates the presence of O, Al, Si, C, Fe, Mg, Na, K and Ti in this sample. From the XRD study, it is found that physical nature of conglomeration in the fly ash is crystalline and the major components are mullite (Al 6 Si 2 O 13 ) and quartz (SiO 2 ). Additionally, the presence of hematite, microclin…
Effects of natural radiation damage on back-scattered electron images of single crystals of minerals
Generally, it has been assumed that signal intensity variations in back-scattered electron (BSE) images of minerals are mainly controlled by chemical heterogeneity. This is especially true for images of single crystals, where effects of different crystal orientations with respect to the incident beam on the observed BSE are excluded. In contrast, we show that local variations of the structural state within single-crystals (i.e., degree of lattice order or lattice imperfectness) may also have dramatic effects on the back-scattering of electrons. As an example, we present BSE images of single-crystals of natural zircon, ZrSiO 4 , whose intensity patterns are predominantly controlled by struct…
Raman spectroscopy of synthetic, geological and biological vaterite: a Raman spectroscopic study
Raman spectroscopy was used to study vaterite samples of biological, geological and synthetic origin. The Raman band positions and the full width at half-maximum (FWHM) of the lattice modes and the internal modes of the carbonate ion of all specimens show no significant differences between vaterites of different origin. With increasing Mg concentrations, synthetic vaterite samples show increasing FWHM in the region of the lattice modes and the three ν1 bands, whereas no change in luminescence was detected. In contrast, in situ measurements of vaterite areas in freshwater cultured pearls (FWCPs) by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) together with the Rama…
Scolecite, Part I: Refinement of high-order data, separation of internal and external vibrational amplitudes from displacement parameters
A single crystal of scolecite, CaAl2Si3O10· 3H2O, was studied by X-ray diffraction methods at room temperature. The intensities were measured with MoKα radiation (λ=0.71069 A) in a complete sphere of reflection up to sinθ/λ=0.9 A−1. The structure was refined in the pseudo-orthorhombic setting of space group F1d1 instead of the conventional setting Cc for better comparison with natrolite (Fdd2). The cell parameters are: a=18.502(1) A, b=18.974(2) A, c=6.525(1) A, β=90.615(7)°, V=2290.6(3) A3, Z=8. A refinement of high-order diffraction data yielded residuals of R(F)=0.9%, R w (F)=0.9%, GoF=1.73 for 1831 high-angle reflections (0.7≤sinθ/λ≤0.9 A−1) and R(F)=1.2%, R w (F)=1.4%, GoF=3.22 for all…
Structural, thermal, dielectric and ferroelectric properties of Na0.5K0.5NbO3and Na0.5K0.5NbO3+0.5mol%MnO2ceramics
Lead-free Na0.5K0.5NbO3 and Na0.5K0.5NbO3+0.5mol%MnO2 ceramics were fabricated by solid state hot pressing sintering process. The phase structure and thermal, dielectric and ferroelectric properties of these ceramics were investigated. X-ray measurements showed that all samples have a single perovskite structure and possess orthorhombic–tetragonal and tetragonal–cubic phase transitions. Sequence of phase transitions was confirmed by differential scanning calorimetry (DSC) and dielectric measurements. Obtained results showed that optimal temperature sintering of Na0.5K0.5 NbO3+0.5mol%MnO2 ceramics is 1100 °C. The results show that investigated ceramics are one of the promising materials as e…
Rubies and Sapphires from Snezhnoe, Tajikistan
Nanostructure, composition and mechanisms of bivalve shell growth
Abstract Freshwater and marine cultured pearls form via identical processes to the shells of bivalves and can therefore serve as models for the biomineralization of bivalve shells in general. Their nanostructure consists of membrane-coated granules (vesicles) which contain amorphous calcium carbonate (ACC) at the beginning of the biomineralization sequence, preceding the crystallization of aragonite and vaterite. In contrast to the commonly accepted view, crystallization of ACC occurs rapidly and within the granular nano-compartments mediated by organic molecules much earlier than platelet formation. The interlamellar organic sheets in nacre that form the platelet structure of nacre themsel…
Prehnite: Structural similarity of the monoclinic and orthorhombic polymorphs and their Si/Al ordering
Abstract Two modifications of the naturally occurring mineral prehnite, Ca 2 Al(Si 3 AlO 10 )(OH) 2 , are characterized by precise single crystal diffraction methods. The two forms are topologically identical. They differ only in the siting of one Al and one Si atom per unit cell: these switch their places in two of the tetrahedrally coordinated sites. This appears to be the only known case where a silicate occurs with two differently ordered tetrahedral distributions of Al and Si atoms. The two forms are not polytypes according to the current definition of polytypes. The two modifications are so similar to each other that they differ only in the eighth coordination sphere.
Crystal Structure of the Microwave Dielectric Resonator Ba2Ti9O20
A single-crystal X-ray study of dibarium nonatitanate, Ba2Ti9O20, yielded the triclinic space group P 1 with a=0.7471(1), b= 1.4081(2), c= 1.4344(2) nm, α=89.94(2)°, β= 79.43(2)°, γ= 84.45(2)°, V = 1.476 nm3 Z = 4, and Dx= 4.61 Mg/m3. A refinement of atomic coordinates and isotropic thermal parameters led to a residual of 0.03. The structure consists of hexagonally closest-packed layers of Ba and O atoms in the sequence (hch)3. All Ti atoms reside in octahedral interstices of this closest packing. The various Ti coordination octahedra share only edges and corners with each other. One-half of the Ba atoms is twelve-coordinated by oxygen atoms, the other half is eleven-coordinated.
Roman lava quarries in the Eifel region (Germany): geochemical data for millstone provenance studies
Roman millstones of assumed Eifel origin were produced and exported in huge quantities to many parts of Roman Europe and can be used as tracers for trade patterns in Roman times. This study presents for the first time a raw-material centred geochemical definition of the 13 well-known Roman basaltic lava quarries in the Quaternary East and West Eifel volcanic fields. The aim is to find a way to characterize the individual exploitation sites precisely by means of their geochemical composition and to recommend a standard procedure for further millstone provenance analysis. Based on major and trace element composition analyses by XRF, a differentiation of each quarry is achieved by using a comb…
Crystal Inclusions in Diamonds and Other Crystals
Single crystal inclusions in natural single crystals bear a lot of information on the genesis and phase stabilities between host and guest crystals. Not only parameters of the natural environment of crystallization may be elucidated, also the history of up-rise within the earth to the surface and the development during procedures, eventually applied by mankind to enhance the physical properties of crystals, may be detectable. Structural reactions resulting in phase separation due to chemical stress during change of physical parameters shed light on the borders of solid solution and exsolution domains. Natural crystals of proper quality allow us to evaluate a time factor in phase stabilities…
Growth zoning and strain patterns inside diamond crystals as revealed by Raman maps
The Raman mapping technique provides a non-destructive means of studying internal growth textures and other micro-structural heterogeneity inside diamond single-crystals. Raman maps showing distribution patterns of the bandwidth (FWHM) of the main first-order lattice vibration of diamond ( LO=TO phonon at ~1332 cm −1 ) along two-dimensional planes inside diamond crystals may reveal the internal growth zoning of these crystals. The observed zoning is affected, and in some cases even obscured in micro-areas adjacent to inclusions, by patterns of heterogeneous strain in the diamond. We present Raman maps obtained from diamond crystals containing large, single-crystal graphite inclusions, from …
High Temperature Study of Metamict Steenstrupine
Metamict minerals contain radioactive elements that degrade their crystal structure. Unlike other metamict minerals, annealing process under ambient pressure do not lead to direct recrystallization of steenstrupine.
Amorphous, nanocrystalline and crystalline calcium carbonates in biological materials
Raman spectroscopy is a powerful tool in identifying different calcium carbonate polymorphs. Here, the method is applied to cultured pearls from freshwater (genus Hyriopsis) and marine bivalve species (Pinctada maxima) as well as to shells of Diplodon chilensis patagonicus bivalves. Raman spectra for vaterite, detected for the first time in an adult shell, and amorphous calcium carbonate (ACC) are discussed. Results for ACC are compared with those of synthetically produced ACC and with the Raman spectroscopic features of stable biogenic ACC from the crustacean Porcellio scaber. Decomposition of the most intense signal of all calcium carbonate polymorphs—the ν1 symmetric stretching mode of t…
ChemInform Abstract: Crystal Structure of the Microwave Dielectric Resonator Ba2Ti9O20.
A single-crystal X-ray study of dibarium nonatitanate, Ba2Ti9O20, yielded the triclinic space group P 1 with a=0.7471(1), b= 1.4081(2), c= 1.4344(2) nm, α=89.94(2)°, β= 79.43(2)°, γ= 84.45(2)°, V = 1.476 nm3 Z = 4, and Dx= 4.61 Mg/m3. A refinement of atomic coordinates and isotropic thermal parameters led to a residual of 0.03. The structure consists of hexagonally closest-packed layers of Ba and O atoms in the sequence (hch)3. All Ti atoms reside in octahedral interstices of this closest packing. The various Ti coordination octahedra share only edges and corners with each other. One-half of the Ba atoms is twelve-coordinated by oxygen atoms, the other half is eleven-coordinated.
A comparative study of the physicochemical properties of iron isomaltoside 1000 (Monofer®), a new intravenous iron preparation and its clinical implications
Abstract The treatment of iron deficiency anemia with polynuclear iron formulations is an established therapy in patients with chronic kidney disease but also in other disease areas like gastroenterology, cardiology, oncology, pre/post operatively and obstetrics’ and gynecology. Parenteral iron formulations represent colloidal systems in the lower nanometer size range which have traditionally been shown to consist of an iron core surrounded by a carbohydrate shell. In this publication, we for the first time describe the novel matrix structure of iron isomaltoside 1000 which differs from the traditional picture of an iron core surrounded by a carbohydrate. Despite some structural similaritie…
Chemical modification of Topaz surfaces
In chemisorption, one is typically faced with the problem that the two-dimensional structure of the organic layer does not match the structure of the inorganic substrate. This work describes the first steps toward an induced epitaxial correlation of organic compounds on an inorganic surface. The idea of this work was to use a single crystal with a two-dimensional surface structure, Topaz (001), that matches an alkyl chain lattice better than existing substrates. X-ray reflectivity and FTIR experiments prove the surface modification of the Topaz, which is probably an etherification of the reactive OH-groups on the Topaz (001) surface.
Sapphire-bearing magmatic rocks trace the boundary between paleo-continents: A case study of Ilmenogorsky alkaline complex, Uralian collision zone of Russia
Abstract Metamorphic gem corundum (mainly ruby) deposits are robust indicators of continent-continent collision processes. However, a systematic link of primary magmatic blue sapphire occurrences to orogenic belts is less understood. An example is the Ilmenogorsky alkaline complex, within the Ilmen Mountains region and part of the Uralian orogenic belt. The mobile belt is a product of the collision among Kazakhstania, Laurussia, and Siberia continents prior to the closure of the Paleo-Uralian ocean and formation of the Laurasia supercontinent (330–250 Ma). It is believed that the alkaline complex became inсluded into the separate Sysertsk-Ilmenogorsk microcontinent with unconstrained border…
Corundum Anorthosites-Kyshtymites from the South Urals, Russia: A Combined Mineralogical, Geochemical, and U-Pb Zircon Geochronological Study
Kyshtymites are the unique corundum-blue sapphire-bearing variety of anorthosites of debatable geological origin found in the Ilmenogorsky-Vishnevogorsky complex (IVC) in the South Urals, Russia. Their mineral association includes corundum-sapphire, plagioclase (An61&ndash
Spectroscopic 2D-tomography: Residual pressure and strain around mineral inclusions in diamonds
We have studied high-pressure inclusions (Ca-silicates, coesite, graphite) in three large diamonds, one from the Kankan district, Guinea, and the other two from the Panda kimberlite, Ekati diamond mines, Canada. Using the in situ point-by-point mapping technique with a confocal Raman system, the mineralogy of the inclusions, as well as their area distribution pattern ( e.g. , of different Ca-silicate phases) and their order-disorder distribution pattern (shown for graphite/disordered carbon), were determined. Raman mapping of the host diamonds yielded 2D-tomographic pressure and strain distribution patterns and provided information on the residual pressure of the inclusions (∼ 2.3 GPa for a…
A New Find of Danburite in the Luc Yen Mining Area, Vietnam
Crystallization of Vaterite Nanowires by the Cooperative Interaction of Tailor-Made Nucleation Surfaces and Polyelectrolytes
The concepts of template-induced crystallization on self-assembled monolayers (SAMs) and the use of polymer additives are combined into a new strategy, where, through the cooperative interaction of a SAM matrix involved in the nucleation process, poly(acrylic acid), a dissolved polyelectrolyte, and the dissolved ions, hierarchically ordered mineral structures are formed. The adsorption of poly(acrylic acid) to the SAM is monitored using a quartz microbalance. Transmission electron microscopy measurements on samples that are taken from polyacrylate solution in short intervals after the start of the reaction reveals that nanometer-sized particles pre-formed in solution are being attached to t…
High Temperature Study of Metamict Rinkite
Metamict minerals contain radioactive elements that degrade their crystal structure. During the annealing process under ambient pressure in argon atmosphere the sample of metamict rinkite recrystallizes to the primary crystalline form at 700°C. Further heating leads to the formation of a new crystalline phase.
Morphosynthesis of Strontianite Nanowires Using Polyacrylate Templates Tethered onto Self-Assembled Monolayers
Strontianite nanowires have been synthesized on self-assembled monolayers (SAM) in the presence of polyacrylate templates. The morphology of this product exhibits characteristic differences from that of products obtained in the absence of polyacrylate. It is demonstrated that the template-induced crystallization process involves the interaction between the SAM surface, polyacrylate (a dissolved polyelectrolyte), and the cations/anions in solution. By the combination of these components, hierarchically ordered mineral hybrid structures are formed.
Morphological and chemical evolution of corundum (ruby and sapphire): Crystal ontogeny reconstructed by EMPA, LA-ICP-MS, and Cr3+Raman mapping
The term “ ontogeny ,” which is commonly used in biology, was introduced into the Earth sciences in 1961 to include the genesis and evolution of single crystals and crystal aggregates. The term encompasses nucleation , growth , alteration , and destruction . We present results of studies concerning the ontogeny of natural corundum (rubies and sapphires), and the chemical and morphological evolution of corundum crystals from deposits in Africa (Kenya, Tanzania, Madagascar) and Southeast Asia (Vietnam). Trace-element compositions indicative for different corundum habits were determined by rim-to-rim LA-ICP-MS and electron microprobe analyses. Raman spectroscopy was applied for Cr 3+ photolumi…