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PubMed2001

Structure Analysis of Montmorillonite Intercalated with Cetylpyridinium and Cetyltrimethylammonium: Molecular Simulations and XRD Analysis.

Molecular mechanics and molecular dynamics simulations combined with X-ray powder diffraction were used in structure investigation of montmorillonite intercalated with cetylpyridinium (CP) and cethyltrimethylammonium (CTA) cations. Molecular modeling revealed the interlayer structure and differences in intercalation behavior of CP and CTA cations in montmorillonite. The experimental and calculated values of basal spacing were in good agreement for both intercalates: in the case of CP-montmorillonite d(exp)=20.59 Å, d(calc)=20.60 Å; for CTA-montmorillonite d(exp)=18.00 Å and d(calc)=18.10 Å. CTA-montmorillonite exhibits significantly higher total sublimation energy and higher host-guest interaction energy than the CP-montmorillonite. The main difference between both intercalates is in charge distribution on the host layers and guest species. The charge transfer from the guest species to the host layer is higher in CTA-montmorillonite than in CP-montmorillonite, and consequently the charge polarization between the host and guest layers is much higher in CTA-montmorillonite. This leads to much stronger host-guest electrostatic interaction in the case of CTA-montmorillonite. Copyright 2001 Academic Press.

Journal Article↗
PubMed2001

Ultrasound-Induced Formation of CdS Nanostructures in Oil-in-Water Microemulsions.

In this study the formation of approximately spherical assemblies of nanocrystalline primary particles of CdS in a CS(2)-water-ethylenediamine (CWE) microemulsion induced by ultrasonic irradiation is described. CS(2) was employed as the sulfur source for CdS and also as the oil phase in the microemulsion. The particles were studied with X-ray powder diffraction, transmission electron microscopy, UV/Vis absorption spectroscopy, and photoluminescence spectroscopy. A blue shift compared to bulk CdS was observed in absorption and photoluminescence spectra. Copyright 2001 Academic Press.

Journal Article↗
PubMed2001

Preparation and Characterization of Metal Sulfides in Ethylenediamine under Ambient Conditions through a gamma-Irradiation Route.

The gamma-irradiation technique has been extended to irradiate liquid ethylenediamine containing metal ions and sulfur powder, and a series of uniform metal sulfide particles including CdS, PbS, Cu(2)S, and Ag(2)S have been prepared at room temperature. X-ray powder diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and UV-visible spectra have been used to characterize the products. In addition, the discussion shows that ethylenediamine and solvated electrons formed in ethylenediamine play crucial roles during the synthetic process. The stability constants of the metal chelates with ethylenediamine, the solubility product constants of the metal sulfides, and the standard electrode potentials of the metal ions also directly control the formation of metal sulfides. Copyright 2001 Academic Press.

Journal Article↗
PubMed2002

Intercalation of octadecylamine into montmorillonite: molecular simulations and XRD analysis.

Intercalation of octadecylamine (ODAMIN) into Na montmorillonite based on the ion-dipole interaction was investigated using molecular mechanics and molecular dynamics simulations combined with X-ray powder diffraction. Molecular modeling revealed the interlayer structure of the ODAMIN-montmorillonite intercalate, the charge distribution on the host layer and guest species, and the energy characteristics, i.e., the total sublimation energy and it's individual contributions (electrostatic and Van der Waals). The present study showed the development of the interlayer structure, basal spacing, and exfoliation energy in dependence on the ODAMIN content.

Journal Article↗
PubMed2002

A 3-D structural model of solid self-assembled chlorophyll a/H(2)O from multispin labeling and MAS NMR 2-D dipolar correlation spectroscopy in high magnetic field.

Magic angle spinning (MAS) NMR with Lee-Goldburg cross-polarization (LG-CP) is used to promote long-range heteronuclear transfer of magnetization and to constrain a structural model for uniformly labeled chlorophyll a/H(2)O. An effective maximum transfer range d(max) can be determined experimentally from the detection of a gradually decreasing series of intramolecular correlations with the (13)C along the molecular skeleton. To probe intermolecular contacts, d(max) can be set to approximately 4.2 A by choosing an LG-CP contact time of 2 ms. Long-range (1)H-(13)C correlations are used in conjunction with carbon and proton aggregation shifts to establish the stacking of the chlorophyll a (Chl a) molecules. First, high-field (14.1 T) 2-D MAS NMR homonuclear ((13)C-(13)C) dipolar correlation spectra provide a complete assignment of the carbon chemical shifts. Second, proton chemical shifts are obtained from (1)H-(13)C heteronuclear dipolar correlation spectroscopy in high magnetic field. The shift constraints and long-range (1)H-(13)C intermolecular correlations reveal a 2-D stacking homologous to the molecular arrangement in crystalline solid ethyl-chlorophyllide a. A doubling of a small subset of the carbon resonances, in the 7-methyl region of the molecule, provides evidence for two marginally different well-defined molecular environments. Evidence is found for the presence of neutral structural water molecules forming a hydrogen-bonded network to stabilize Chl a sheets. In line with the microcrystalline order observed for the rings, the long T(1)'s, and absence of conformational shifts for the (13)C in the phytyl tails, it is proposed that the Chl a form a rigid 3-D space-filling structure. Probably the only way this can be realized with the sheets is by forming bilayers with interpenetration of elongated tails. Such a 3-D space-filling organization of the aggregated Chl a from MAS NMR would match existing models inferred from electron microscopy and low-resolution X-ray powder diffraction, while a micellar model based on neutron diffraction and antiparallel stacking observed in solution can be discarded.

Carbon Isotopes↗
PubMed1986

Crystalluria in marathon runners. 1. Standard marathon--males.

Epidemiological evidence suggests that marathon runners have a higher incidence of renal stone formation than occurs in the general population. Since crystalluria and stone disease are thought to be related, we subjected urine samples from a group of marathon runners to particle counting and sizing in a Coulter Counter equipped with a population accessory unit. The volume-size distribution curves so obtained were bimodal with one peak occurring in the 2-5 micron diameter range and a second in the 15-32 micron diameter range - a pattern that is remarkably similar to the distributions reported for recurrent idiopathic stone formers and distinctly different to those recorded for control subjects. Analyses by scanning electron microscopy and X-ray powder diffraction revealed other features which are regarded as typical of stone formers' crystalluria. These physicochemical data indicate that marathon runners may be at increased risk of urinary stone formation.

Adult↗
PubMed1986

An unusual complication of a myocardial electrode--apatite mantle on the platinum-iridium spurs.

A case of a high excitation threshold that occurred 2 years 5 months after the initial implantation of pacemaker electrodes is described in a girl 4 years 3 months of age. This complication was considered to be due to calcification of the platinum-iridium electrode spurs. The calcified material was shown to be a kind of apatite using the X-ray powder diffraction method. This complication is rare, but it must be kept in mind since battery longevity has markedly improved in recent years.

Apatites↗
PubMed1983

Correlated physiochemical and age changes in embryonic bovine enamel.

Whole enamel scrapings from unerupted teeth of embryonic calves have been separated into fractions of varying density by stepwise centrifugation in bromoform-toluene mixtures of increasing specific gravity. Partition of enamel in this manner yields individual fractions of increasing mineral phase age and maturation. Whole scrapings and isolated fractions of the fetal bovine enamel were examined by X-ray powder diffraction, scanning electron microscopy, and atomic absorption and infrared spectroscopy to determine time-related changes in the physiochemical nature of the constituent mineral phase particles. These analyses showed poorly crystalline hydroxyapatite (HA) as the only detectable solid phase of calcium phosphate present in all fractions, its degree of crystallinity increasing with increasing density. Molar Ca/P ratios and magnesium content were highest in lowest density fractions. Carbonate vibration bands at 875 and 1420-1450 cm-1, common to mineralized tissue, were observed in intermediate and higher density fractions and in whole unfractionated enamel. Another carbonate band at approximately 705 cm-1, unusual to vertebrate calcified tissue, was detected in low density fractions and disappeared rapidly with increasing enamel maturation. Its precise relation with the enamel mineral phase has not been determined.

Animals↗
PubMed1986

Pancreatic calculi containing brushite: ultrastructure and pathogenesis.

Six pancreatic calculi were analyzed by X-ray powder diffraction and scanning electron microscopy. All were found to contain calcite; however, small amounts of two other morphologically distinct deposits containing only Ca were also detected in some of the stones. It is suggested that these substances may be vaterite and aragonite. In addition, significant deposits of brushite, CaHPO4 X 2H2O, were identified on the outer surfaces of three of the stones. This substance has not been previously reported as a constituent of pancreatic calculi, and its presence is surprising since physico-chemical factors such as phosphate concentration and fluid pH do not favor its deposition. We suggest that precipitation of calcite in the pancreatic duct occurs as the primary event in the formation of pancreatic calculi and that it may continue until the duct is completely occluded. Thereafter, further growth causes injury to the duct wall resulting in the calcite core being exposed to phosphate in the tissue fluid. Deposition of brushite follows.

Calcium Carbonate↗
PubMed1987

Formation of octacalcium phosphate and subsequent transformation to hydroxyapatite at low supersaturation: a model for cartilage calcification.

By means of X-ray powder diffraction (XRD), octacalcium phosphate (OCP, Ca8H2(PO4)6 X 5H2O, Ca/P = 1.33) has been shown to be a metastable precursor of hydroxyapatite (HA, Ca10(PO4)6(OH)2, Ca/P = 1.67) during de novo HA formation in aqueous solutions containing [CaCl2] = 1.0-2.0 mM and [Na2HPO4] less than or equal to 3 mM, kept at 37 degrees C, 300 mosM and stirred gently at 150 rpm. At the precipitation boundary with initial pH = 7.4, OCP is stable for at least 24 hours when [Ca] = 1.0 mM, and is less stable when [Ca] = 2.0 mM, transforming into a mixture of OCP and HA within 24 hours. Almost complete transformation to HA within 24 hours takes place with high [Ca] and high [Pi]. Statistical analysis of the pH 7.4 precipitation boundary data supports the XRD findings: although [Ca][Pi] values vary significantly (P less than 0.001) with [Ca] (2.70 +/- 0.05 mM2 for [Ca] = 1.0 mM and 2.00 +/- 0.10 mM2 for [Ca] = 2.0 mM), [Ca]1.33[Pi] values do not vary with [Ca] suggesting that the initial precipitation process is 6(1.33 Ca + Pi)----OCP. With initial pH = 7.6, a different precipitation boundary with lower [Ca][Pi] values has been determined. These findings strongly support the fact that rat epiphyseal cartilage fluid which has [CaUF][PiUF] = 2.6 mM2 (UF = ultrafiltrate) and pH 7.6 [2] should be able to support de novo calcification.

Calcification, Physiologic↗
PubMed1979

Review of five cases of limy bile--particularly on radiological, chemical and crystallographic studies--.

Incidence of "limy bile" is relatively rare and only 120 cases have been recorded in Japan so far. The present report is to add five more cases operated on at our clinic. On chemical analysis by atomic absorption spectrophotometry calcium carbonate was the major constituent of solid portion and ranged from 73.5 to 88.5%. On crystallographic analyses, the infrared spectra by means of KBr-disk method gave patterns of calcium carbonate in all cases, and the X-ray powder diffraction studies disclosed those of aragonite only in cases 2 and 4, and aragonite-calcite mixture in cases 1 and 3. The exact etiology of formation of limy bile in the gallbladder has not yet been understood completely.

Adult↗
PubMed1986

Chemical and crystallographic studies on 33 cases of calcium carbonate gallstone (so-called limy bile).

Chemical analyses by atomic absorption spectrophotometry and crystallographic studies by the X-ray powder diffraction method and infrared spectrometry (KBr-disk method) were made on 33 cases of calcium carbonate gallstone or so-called limy bile. Chemically, calcium carbonate was the major constituent, ranged from 33.7 to 91.6% and averaged 77.8%. Crystallographically, calcium carbonate has three different polymorphic crystalline forms; calcite, aragonite and vaterite. In nature the most stable calcite (hexagonal) is most commonly found and aragonite (rhombic) is next. On the other hand vaterite, which is unstable hexagonal modification, rarely occurs in biological systems. But in our gallstone series in man, aragonite was most commonly found, with an occurrence rate of 90.6%, while that of calcite was 62.5%. Even vaterite was found in 28.1%. Moreover three cases contained all three forms of calcium carbonate polymorphs; calcite, aragonite and vaterite. This was a very unusual condition. Some environmental factors controlling the growth of these crystals, such as specificity of the bile, are suggested.

Calcium Carbonate↗
PubMed2004

Crystal forms of ketorolac.

Four crystal forms of ketorolac have been obtained by recrystallization in organic solvents under variable conditions. Different ketorolac polymorphs and pseudopolymorph were characterized by X-ray powder diffraction crystallography (XRD), Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In the dissolution studies in water at 37 +/- 0.5 degrees C, four crystal forms showed different patterns. The solubility of Form I were the highest. The solubility decreased in rank order: Form I > Form II > Form III > Form IV. Form land Form III were shown to have a good physical stability at room temperature for 60 days. However, Form II is converted to Form III and Form IV is converted to Form I after 60 days storage. Therefore, these observations indicate that crystalline polymorphism for ketorolac is readily inter-convertible and the relationship may have to taken into consideration in the formulation of the drug.

Chemistry, Pharmaceutical↗
PubMed2002

A core-shell structured BaTiO3 precursor preparation, characterization and potential.

A new procedure for the preparation of a core-shell-structured BaTiO(3) precursor (core=TiO(2); shell=BaCO(3)) will be described. The structure of this precursor is characterized by electron microscopy (environmental scanning electron microscopy; energy disperse X-ray spectroscopy), whereas the development of phases during thermal treatment is followed by X-ray powder diffraction.

Journal Article↗
PubMed2005

Analytical evidence of amorphous microdomains within nitridosilicate and nitridoaluminosilicate single crystals.

Single crystals of new nitridosilicates and nitridoaluminosilicates with excellent R values in X-ray investigations were analysed quantitatively using 30 to 60 microm single-spot LA-ICP-MS. Significant discrepancies between expected and measured chemical composition could not be explained by the crystallographic data. High spatial resolution analysis using electron probe microanalysis (EPMA, 10 microm) leads to the discovery of inhomogeneities in the crystalline material. The application of standard single-spot LA-ICP-MS with a spatial resolution of 30 to 60 microm is not suitable for the analysis of these crystals as the existing inhomogeneities dominate and alter the determined concentrations. However, owing to the better detection capabilities, a scanning LA-ICP-MS procedure enables a more representative analysis of single crystals of Ca(5)Si(2)Al(2)N(8) than single-spot LA-ICP-MS as a result of a larger sampling volume. It is highly likely that these impurities consist of amorphous, vitreous phases as powder diffraction X-ray data indicates the existence of a significant fraction of an X-ray amorphous material besides crystalline silicates. These microdomains contain less aluminium, silicon and calcium or are nearly free of aluminium, which explains the detected discrepancies in the chemical composition.

Journal Article↗
PubMed2002

Effect of age on rat bone solubility and crystallinity.

It has been shown that biominerals such as dental enamel and bone demonstrate a non-thermodynamic equilibrium state following initial dissolution where no further mineral dissolution or precipitation occurs; this state is termed metastable equilibrium solubility (MES). Furthermore, these minerals are composed of a distribution of domains each with their own MES. Recent studies have also demonstrated a linear relationship between crystallinity and the mean MES of these minerals, with solubility decreasing with increasing crystallinity. This study investigates the effect of age on the MES and crystallinity of rat bone mineral. The bone mineral samples were prepared by protein extraction with a series of hydrazine and alcohol solutions. The MES distributions of the bone mineral were measured by exposure to 0.1 M acetate buffers containing a range of calculated amounts of calcium (Ca) and phosphate for 48 h. The amount of mineral dissolved in each solution was determined from Ca and phosphate analyses of the undissolved residue. The full width of the half maximum (FWHM) of the 002 reflection of the X-ray powder diffraction was used as an indicator of crystallinity. The MES of mineral from bone of rats of different ages (1-25 months) were compared. Results of this study indicate that (l) there is a difference in the mean MES of bone mineral from rats of different ages, with older bone mineral being less soluble and more crystalline than bone mineral from younger rats; (2) the nature of the solubility distribution changes from a narrow to a broader distribution with age; and (3) all of the bone samples demonstrated an inverse-linear correlation between crystallinity and mean MES value consistent with previous results obtained with synthetic apatites and dental enamel.

Aging↗
PubMed2004

Nucleation of calcium oxalate crystals on an imprinted polymer surface from pure aqueous solution and urine.

Calcium oxalate (CaOx) is the most common component of human kidney stones. Heterogeneous nucleation is regarded as the key mechanism in this process. In this study, we have used an imprinted 6-methacrylamidohexanoic acid/divinylbenzene co-polymer as a biomimetic surface to nucleate CaOx crystal formation. The polymer was imprinted with either calcium oxalate monohydrate (COM) or dihydrate (COD) template crystals. These were washed out of the polymer, which was then immersed in various test solutions. The test solutions were an aqueous solution of calcium chloride and sodium oxalate, artificial urine and a sample of real urine. Crystals that formed on the polymer surface were characterized by X-ray powder diffraction, Fourier transform infrared spectroscopy, atomic absorption spectroscopy and scanning electron microscopy. Results showed that in the aqueous solution the COM-imprinted polymer induced the nucleation of COM. The COD-imprinted polymer induced only trace amounts of COD crystallization, together with larger quantities of COM. In artificial and real urines, COM also specifically precipitated on the COM-imprinted surface. The results show that, at least to some extent, the imprinted polymers direct formation of their morphologically matched crystals. In the case of COD, however, it appears that either rapid hydrate transformation of COD to COM occurs, or the more stable COM polymorph is directly co-precipitated by the polymer. Our results support the hypothesis that heterogeneous nucleation plays a key role in CaOx stone formation and that the imprinted polymer model could provide an additional and superior diagnostic tool for stone researchers to assess stone-risk in urine.

Acrylamides↗
PubMed1999

[Roentgen spectrometry comparison of currently available bone substitutes].

INTRODUCTION: The crystalline structure of hydroxyapatite (HA) and tricalciumphosphate (TCP) used as bone regeneration materials affects their physical and probably also their biological properties. Varying velocities of the HA solution process seem to be correlated to different results in powder diffraction analysis (RDX) [1], a validated, routine procedure in minerology [2, 6] to analyse crystallized materials. As far we know there are no comparative RDX analyses for the TCP materials in clinical use. GOALS: The dimension and quality of the crystallization of several bone regeneration materials are analysed by RDX. MATERIAL AND METHODS: The materials analysed were divided in different groups: hydroxyapatite, tricalciumphosphate and bioglass. The materials are characterized by the specific intensity curve measurements. RESULTS: The HA products, with the exception of Algipore, seem to be monophasic. Ceros80 and Endobone were the only ones which seem to be totally crystallized. The TCP products Biobase and Cerasorb are nearly monophasic, whereas Ceros82 seems to contain a mixture of 30% HA and 70% beta-TCP. All TCPs show a high crystallization. The bioglasses did--as suspected--not show crystalline structures. DISCUSSION: There are many possible causes for inhomogeneous crystallization of the investigated materials, as they are composites of different foreign ions, extremely small crystals or abnormal (deficient) apatites. How this affects the biological behaviour is not known. SUMMARY: We found differences between the examined materials; how this affects the biological behaviour is unknown. Further investigations are necessary to correlate the characteristics of the materials to the clinical outcome.

Bone Substitutes↗