Search PubMed⌕ Search

SEARCH · Search PubMed

Results for “Powder Diffraction”

Search indexed PubMed citations on genomics, clinical trials, systematic reviews and public health. Explore titles, authors and supplied subject terms, then open the PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 1,279 records · Page 71Linked to original sources
PubMed1995

Evidence for a causal relationship between the structure, size, and load of calcium pyrophosphate dihydrate crystals, and attacks of pseudogout.

OBJECTIVE: To investigate any relationship between the nature, size, and numbers of synovial fluid (SF) calcium pyrophosphate dihydrate (CPPD) crystals, and attacks of pseudogout. METHODS: Knee SF was aspirated from nine selected patients, first during an attack of pseudogout (acute sample) and again later when the attack had subsided (interval sample). CPPD crystals were extracted, weighed, examined by high resolution transmission electron microscopy (HRTEM), and characterised by size and crystal habit (monoclinic or triclinic). Structural analysis was carried out by x ray powder diffraction (XRD) and the proportions of monoclinic to triclinic CPPD were estimated from densitometric measurements of selected key reflections. RESULTS: The mean crystal size, by HRTEM, indicated that the crystals in the acute sample were larger than those in the interval sample. The ratio of monoclinic to triclinic CPPD, whether estimated from their morphological appearance by HRTEM, or from XRD, was greater in the acute than in the interval sample in all nine patients. The total amount of extracted mineral varied, but in every patient the concentration of CPPD per ml of fluid, and the total mineral per joint, were greater in the acute sample than in the interval sample. CONCLUSION: In this highly selected group of patients, the large numbers of CPPD crystals associated with attacks of pseudogout included a greater proportion of monoclinic crystals, and larger crystals, than those present when inflammation had subsided. A special, phlogistic population of crystals may exist, originating in different joint tissues, or cleared in a different manner, than the more common populations of smaller crystals with a greater proportion of triclinic CPPD, seen in chronic disease.

Acute Disease↗
PubMed1971

Hydroxyapatite in the pathogenesis of cystic fibrosis.

Submandibular saliva collected from cystic fibrosis patients and control subjects was separated by centrifugation into an insoluble deposit and a clear supernatant. The resulting calcium and phosphorus analyses performed on both fractions warranted a closer investigation as a consistent Ca/P molar ratio of 1.5 was found in the deposit of the cystic fibrosis patients, while no consistent ratio >1.0 was found in the deposit of the control subjects. The expected result, that calcium and phosphorus in the deposit of cystic fibrosis patients is present as the solid phase of hydroxyapatite, was confirmed by a detailed comparison of x-ray powder diffraction patterns of an ashed sample of this deposit and a similarly treated synthetic sample of hydroxyapatite.

Adolescent↗
PubMed1973

The nature and incidence of gallstones containing calcium.

The crystalline constituents of gallstones determined by x-ray powder diffraction can be broadly classified as cholesterols and calcium salts. On this basis there are three main types of stones consisting of cholesterol, calcium salts, and mixtures of these. In a study of the composition of 481 gallstones from 11 countries, the percentage incidence of each was 59.9, 13.1, and 27.0 respectively. The presence of calcium compounds in 40.1% of the calculi showed the importance of these constituents in the nucleation and/or growth of many specimens. Men are just as likely as women to form stones consisting entirely of calcium salts, but female patients outnumber males by about 3:1 for both calculi of cholesterol and those of cholesterol with calcium salts. A description is given of the appearance, texture, and structure of calcium-containing stones subdivided according to the calcium salt(s) present.

Age Factors↗
PubMed1984

In vitro cytotoxicity and quantitative silica analysis of diatomaceous earth products.

Mouse peritoneal macrophages were used to evaluate the relative cytotoxicity of a series of diatomaceous earth products in vitro. The amorphous and crystalline silica content of the products was determined by a combination of infrared spectroscopy and x ray powder diffraction techniques. The cytotoxicities of the high cristobalite content flux calcined materials were similar to that of the standard cristobalite ; both the natural and straight calcined materials had significantly greater activities than the flux calcined materials. Thus within the limitations of the macrophage cytotoxicity test the hypothesis that crystalline content is the only determinant of fibrogenicity of diatomaceous earth is not supported.

Animals↗
PubMed1996

Evidence of calcium phosphate supersaturation in the loop of Henle.

We have used published rat micropuncture data to construct a matrix of ion concentrations along the rat nephron. With an iterative computer model of known ion interactions, we calculated relative supersaturation ratios in all nephron segments. The collecting ducts and urine showed expected supersaturation with stone-forming salts. Fluid in the thin segment of the loop of Henle may be supersaturated with calcium carbonate and calcium phosphate under certain conditions. Because calculations cannot predict the actual course of crystallization, we made solutions to mimic, in vitro, presumed conditions in the loop of Henle. The solid phases that formed were analyzed by X-ray powder diffraction, electron microprobe, and infrared spectroscopy. All samples were identified as poorly crystallized or immature apatite. The descending limb of Henle's loop creates a unique condition as it extracts water but not sodium, bicarbonate, calcium, or phosphate, giving a calcium concentration at the bend of 3 mM, pH 7.4, and a phosphate concentration that varies from 0.8 to 48 mM, depending on parathyroid hormone and dietary phosphate. We conclude that conditions in the thin segment potentially could create a solid calcium phosphate phase, which may initiate nucleation of calcium oxalate salts in the collecting ducts, potentiating nephrolithiasis and nephrocalcinosis.

Animals↗
PubMed1986

Critical aspects of urine and stone analysis. Appearance of iatrogenic urinary calculi.

In 25% of the samples the often applied qualitative chemical analysis of urinary stones leads to entirely wrong results with severe therapeutic consequences. The appropriate techniques for stone analysis are infrared spectroscopy and X-ray powder diffraction. These techniques make also possible the identification of iatrogenic urinary calculi. Four types of such stones were detected here, caused by modern medication. N4-acetylsulfamethoxazole, N4-acetylsulfadiazine, mefenamic acid and silicon dioxide. It is only the correct preanalytical treatment of urine samples that prevents considerable impairment of analytical results. Without precautions especially, the oxalate concentration in urine may be doubled or tripled during one day of storage.

False Positive Reactions↗
PubMed1989

Formation of bobierrite (magnesium phosphate) crystal aggregates by bacteria from human urine and renal calculi.

The formation of extracellular crystal aggregates of bobierrite [Mg3(PO4)2.8H2O] by bacteria isolated from renal calculi and urine of urolithiasic patients is found with the use of B-17 and B-43 media. The crystal aggregates were observed in the colonies as deposits of brown-yellow coloration, and were identified by X-ray powder diffraction, chemical analysis and scanning electron microscopy. The production of bobierrite by bacteria from human urine and renal calculi implies further versatility of crystal formation by microorganisms, and it may be interesting to investigate the possible relationships between calculi precipitation and urinary infection.

Bacteria↗
PubMed2004

Synthesis and characterization of titania-coated silver nanoparticles.

Silver particles of 70 +/- 10 nm mean diameter were coated with uniform layers of amorphous titania by the hydrolysis and polycondensation process using titanium(IV) n-butoxide in aqueous solution. Because of the large dielectric function of titania, a shift to the longer wavelengths was observed for the plasmon resonance maximum of coated silver nanoparticles. By changing the alkoxide to particles ratio in the reaction mixture, thickness ranging from 5 to 20 nm was obtained. Hydrothermal treatment performed on coated particles at 350 degrees C for 4 h converted amorphous titania to the anatase crystalline form. The anatase form was confirmed by X-ray powder diffraction. More red shift of the plasmon resonance was observed for the hydrothermally treated samples compared with the particles coated with amorphous titania.

Coated Materials, Biocompatible↗
PubMed2004

A room-temperature synthesis of titanium nitride hollow spheres.

Titanium nitride hollow spheres were synthesized by the reaction of TiCl4 and NaNH2 at room temperature. X-ray powder diffraction (XRD) pattern could be indexed as cubic TiN with the lattice constants of a = 4.236 A. Transmission electron microscopy (TEM) images showed hollow spheres with diameter about 200 nm. A possible formation mechanism of TiN hollow spheres was discussed.

Coated Materials, Biocompatible↗
PubMed2005

Synthesis and characterization of superconducting nanocrystalline niobium nitride.

Nanocrystalline niobium nitride (NbN0.9) was successfully synthesized at 600 degrees C through a solid-state reaction. The synthesis was carried out in an autoclave by using NbCl5 and NaN3 as the reactants. The X-ray powder diffraction pattern indicates the formation of cubic NbN0.9. Transmission electron microscopy images show that typical NbN0.9 crystallites are composed of uniform particles with an average size of about 30 nm and nanorod crystallites with a typical size of about 40 x 2500 nm. Magnetic measurements exhibited that a superconducting transition occurred at 15.4 K for the NbN0.9 product.

Crystallization↗
PubMed2005

Nanocrystallization of ferroelectric strontium bismuth vanadium niobate in lithium tetraborate glasses.

Transparent glass samples in (100-3x) (Li2O-2B2O3)-x(SrO-Bi2O3-0.7Nb2O5-0.3V2O5) (10 < or = x < or = 60, in molar ratio) system have been fabricated via conventional melt-quenching technique. The as-quenched samples, of all the compositions under study have been confirmed to be amorphous, by X-ray powder diffraction (XRD) studies. Differential thermal analysis (DTA) was employed to confirm the glassy nature of the as-quenched glasses. Glass composites comprising vanadium doped strontium bismuth niobate nanocrystallites were obtained by controlled heat-treatment of the as-quenched glasses at 783 K for 6 h. Perovskite SrBi2(Nb0.7VO3)2O9-delta phase formation was found to be preceded by an intermediate fluorite phase which was established via XRD and transmission electron microscopy (TEM). The dielectric constants (epsilonr) of the as-quenched glasses as well as the glass nanocrystal composites decreased with increase in frequency (100 Hz-10 kHz) at 300 K. Interestingly, the dielectric constant of the glass nanocrystal composite (heat-treated at 783 K/6 h) undergoes a maximum in the vicinity of the crystallization temperature of the host glass (Li2B4O7) reaching an anomalously high value (approximately 10(6)) at 800 K. Different dielectric mixture formulae were employed to rationalize the dielectric properties of the glass nanocrystal composite. The optical transmission properties of these glass nanocrystal composites were found to have strong compositional dependence.

Bismuth↗
PubMed2006

Microemulsion-mediated solvothermal synthesis and morphological evolution of MnCO3 nanocrystals.

The morphology- and size-controlled synthesis of MnCO3 nanocrystals was successfully achieved by cationic surfactant-CTAB-microemulsion-mediated solvothermal method. Various comparison experiments with different reactant concentrations and molar ratios between water and CTAB, showed the evolvement law of the morphology and size of the as-synthesized MnCO3 nanocrystals. With slowly increasing the concentration of reactants and/or molar ratio between water and CTAB, the morphology of MnCO3 nanocrystals changed gradually from cube to parallelepiped, and then rhombohedron, whereas the size decreased a little. The effect of the experimental parameters on the shapes and sizes of samples, such as the source of carbonate salts, reaction time, and temperature, were also discussed. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microscopy (HRTEM) were used to characterize the products.

Carbonates↗
PubMed2006

Preparation of Mg-vermiculite nanoparticles using potassium persulfate treatment.

Delamination/exfoliation process of the Mg-vermiculite (Letovice, Czech Republic), particles with size less than 5 microm, was studied after potassium persulfate treatment and compared with known method utilized hydrogen peroxide treatment. X-ray powder diffraction (XRPD) patterns showed that treatment of Mg-vermiculite with different molar concentration of potassium persulfate: c = 0.02, 0.04, and 0.08 mol x dm(-3) at the temperature 60 degrees C for 2 hr caused reduction of relative intensity (I(rel.)) of the basal 001 diffraction to the 15%, 9%, and 4%, respectively, compared to intensity of 001 diffraction of untreated Mg-vermiculite (I(rel.) = 100%). On the other hand I(rel.) of the 001 diffraction of Mg-vermiculite after treatment with 30% and 50% (c = 9.8 and 17.4 mol x dm(-3)) hydrogen peroxide at the 60 degrees C for 2 hr decreased only to I(rel.) = 36% and 32%, respectively. Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) verified effect of potassium persulfate treatment on structure degradation which is connected with higher degree of delamination/exfoliation of the particles and their cracking into nano-sized particles.

Aluminum Silicates↗
PubMedDate not supplied

Observations on normal and degenerating human otoconia.

Specimens of human otoconia obtained from autopsy material and representing various stages from fetal to advanced old age, were studied by microdissection, scanning electron microscopy, electron microprobe analysis, and x-ray powder diffraction. The typical adult otoconial configuration is a cylindrical, finely serrated body with pointed ends; crystallographically, it corresponds to a single crystal of calcite. Other, less numerous typed include jointed otoconia, pure rhombohedrons and multifaceted, presumably immature forms. Many otoconia achieve the adult configuration during fetal development. The multifaceted otoconia are most numerous, and the rhombohedrons proliferate, during childhon in the young adult, but saccular otoconia are the larger. In middle and advanced age the otoconia decrease in number, especially in the saccule. Saccular otoconia degenerate progressively in a posteroanterior direction across the macula; they assume a specific, fibours, hollowed-out appearance, which is not duplicated by either chemical etching or autolysis. Neogenesis and growth of otoconia appear to occur postnatally, with different characteristic growth potentials for those of the saccule and the utricle. Age-related saccular otoconial degeneration appears to involve the organic material, which disappears either before or simultaneously with the mineral substance.

Adolescent↗
PubMedDate not supplied

Vaterite otoconia in two cases of otoconial membrane dysplasia.

Scanning electron microscopy, electron microprobe analysis, and x-ray powder diffraction were used to study temporal bone specimens obtained at autopsy from an infant with Potter syndrome and from a second trimester fetus, which was the product of an elective abortion. The mothers of both the infant and fetus were juvenile-onset rheumatoid arthritis patients who took prostaglandin inhibitors during pregnancy. The infant's external ears were low set and the left ear canal was stenotic. The vestibular maculae on the left were covered by aberrant otoconia composed of vaterite. In the right inner ear, otoconia were entirely absent, although the gelatinous otoconial membranes were intact. Only the left saccule and right utricle from the fetus were studied; both contained vaterite crystals similar to those in the infant. In addition, apatite was present in the fetal utricle, apparently lying on the macula beneath the vaterite otoconia.

Abnormalities, Multiple↗
PubMed1981

Determination of the AuCu superlattice formation region in gold-copper-silver ternary system.

The composition and temperature range of the AuCu-type superlattice formation in the Au-Cu-Ag ternary system was determined by X-ray powder diffraction. Four distinguishable phase transformations were detected, i.e., 1) alpha (disordered FCC phase) leads to AuCu I, 2) alpha leads to AuCu II, 3) alpha leads to alpha 1 (Cu-rich FCC phase) + alpha 2 (Ag-rich FCC phase). and 4) alpha leads to AuCu3. The stable temperature range of the AuCu I-type superlattice was restricted to a lower temperature range by adding silver to stoichiometric and off-stoichiometric Au-Cu alloys. Depending on the increase in silver content, the co-existing region of the AuCu II-type superlattice and the silver-rich alpha 2 phase extended to the lower temperature and over a wide composition range.

Chemical Phenomena↗
PubMed2001

pH-Dependent dissolving nano- and microparticles for improved peroral delivery of a highly lipophilic compound in dogs.

RR01, a new highly lipophilic drug showing extremely low water solubility and poor oral bioavailability, has been incorporated into pH-dependent dissolving particles made of a poly(methacrylic acid-co-ethylacrylate) copolymer. The physicochemical properties of the particles were determined using laser-light-scattering techniques, scanning electron microscopy, high-performance liquid chromatography, and x-ray powder diffraction. Suspension of the free drug in a solution of hydroxypropylcellulose (reference formulation) and aqueous dispersions of pH-sensitive RR01-loaded nanoparticles or microparticles were administered orally to Beagle dogs according to a 2-block Latin square design (n = 6). Plasma samples were obtained over the course of 48 hours and analyzed by gas chromatography/mass spectrometry. The administration of the reference formulation resulted in a particularly high interindividual variability of pharmacokinetic parameters, with low exposure to compound RR01 (AUC0-48h of 6.5 microg x h/mL and coefficient of variation (CV) of 116%) and much higher Tmax, as compared to both pH-sensitive formulations. With respect to exposure and interindividual variability, nanoparticles were superior to microparticles (AUC0-48h of 27.1 microg x h/mL versus 17.7 microg x h/mL with CV of 19% and 40%, respectively), indicating that the particle size may play an important role in the absorption of compound RR01. The performance of pH-sensitive particles is attributed to their ability to release the drug selectively in the upper part of the intestine in a molecular or amorphous form. In conclusion, pH-dependent dissolving particles have a great potential as oral delivery systems for drugs with low water solubility and acceptable permeation properties.

Acrylic Resins↗
PubMed2003

Sublimation characterization and vapor pressure estimation of an HIV nonnucleoside reverse transcriptase inhibitor using thermogravimetric analysis.

The purpose of this research is to investigate the sublimation process of DPC 963, a second-generation nonnucleoside reverse transcriptase inhibitor for HIV-1 retrovirus, and to better understand the effect of sublimation during active pharmaceutical ingredient (API) manufacture and formulation development, especially the drying processes. Sublimation of DPC 963 at 150 degrees C and above was determined by thermogravimetric analysis-Fourier transform infrared (TGA-FTIR). The rates of sublimation at different temperatures were measured using isothermal TGA. Condensed material was collected and analyzed by differential scanning calorimetry (DSC), x-ray powder diffraction (XRPD), and infrared (IR) spectrometry. Benzoic acid was used as a reference standard to derive a linear logarithmic relationship between sublimation/evaporation rate and vapor pressure specific to the TGA system used in this study. Sublimation and evaporation of DPC 963 were found to follow apparent zero-order kinetics. Using the Eyring equation, the enthalpy and entropy of the sublimation and evaporation processes were obtained. The enthalpies of sublimation and evaporation were found to be 29 and 22 kcal/mol, respectively. The condensed material from the vapor phase was found to exist in 2 physical forms, amorphous and crystalline. Using benzoic acid as a reference standard, vapor pressure of DPC 963 at different temperatures was calculated using the linear logarithmic relationship obtained. DPC 963 undergoes sublimation at appreciable rates at 150 degrees C and above but this is not likely to pose a serious issue during the manufacturing process. Vapor pressure estimation using thermogravimetric analysis provided sufficient accuracy to be used as a fast, simple, and safe alternative to the traditional methods of vapor pressure determination.

Chemical Phenomena↗