X-ray fluorescence spectroscopic determination of heavy metals and trace elements in aerial parts of Origanum sipyleum L from Turkey

Purpose: To determine the heavy metal and trace element composition of the powdered aerial parts of Origanum sipyleum L. and its water extract. Methods: The heavy metal and trace elements content of the powdered plant material and 2 % aqueous extract were evaluated by x-ray fluorescence spectroscopy with silicon drift detector SDD at a resolution of 145 eV and 10,000 pulses. The process conditions were 0.1 g sample weight, process time of 300 s at a voltage of 25 kV and 50 kV, and at a current of 0.5 and 1.0 mA under helium atmosphere. Results: The major elements, K, Ca and Na, known as macronutrients, constituted 11990, 10490 and 970 ppm of the powdered drug and 8910, 2991 and 810 ppm of the water extract, respectively. Among other constituents, arsenic, lead and uranium levels were < 1, 2.1 and < 3 ppm, respectively, in the powdered material while in the aqueous extract, the levels were < 1, < 2 and 200 ppm, respectively. Conclusion: O. sipyleum is a potential source of macro- and micronutrients from which useful food additives and health supplements can be derived.

Advanced X-ray techniques for the structural characterisation of Prussian Blue Analogue cathode materials

The thesis is dedicated to the implementation of advanced x-ray-based techniques for the investigation of the battery systems, more predominantly, the cathode materials. The implemented characterisation methods include synchrotron based x-ray absorption spectroscopy, powder x-ray diffraction, 2-dimensional x-ray fluorescence, full field transmission soft x-ray microscopy, and laboratory x-ray photoelectron spectroscopy. The research highlights the different areas of expertise for each described method, in terms of material characterisation, exploring their complementarities and intersections. The results are focused over manganese hexacyanoferrate and partially Ni substituted manganese hexacyanoferrate, through both organic and aqueous battery systems. In aqueous system, the modification of cathode composition has been observed with various techniques, indicating to the processes occurring in bulk, surface, locally or in long-range, including with the speciation by 2-dimensional scanning, and the time-resolution, by the implementation of the operando measurements. In organic media, the inhomogenisation of the cathode material during the aging process was investigated by the development of the special image treatment procedure for the maps, obtained from the transmission soft x-ray microscopy. It worth mentioning, that apart from the combination of the outcomes from the various x-ray measurements, the exploration of the new capabilities was also conducted, namely, probing the oxidation state of the element with the synchrotron-based 2-dimensional x-ray fluorescence technique, which, generally, with conventional set up, is not possible to achieve. The results and methodology from this thesis can, of course, be generalised on the characterisation of the other battery systems, and not only, as the x-ray techniques are one of the most informative and sophisticated methods for advanced structural investigation of the materials.

Fast And Direct Na And K Determination In Table, Marine, And Low-sodium Salts By X-ray Fluorescence And Chemometrics.

X-ray fluorescence (XRF) is a fast, low-cost, nondestructive, and truly multielement analytical technique. The objectives of this study are to quantify the amount of Na(+) and K(+) in samples of table salt (refined, marine, and light) and to compare three different methodologies of quantification using XRF. A fundamental parameter method revealed difficulties in quantifying accurately lighter elements (Z < 22). A univariate methodology based on peak area calibration is an attractive alternative, even though additional steps of data manipulation might consume some time. Quantifications were performed with good correlations for both Na (r = 0.974) and K (r = 0.992). A partial least-squares (PLS) regression method with five latent variables was very fast. Na(+) quantifications provided calibration errors lower than 16% and a correlation of 0.995. Of great concern was the observation of high Na(+) levels in low-sodium salts. The presented application may be performed in a fast and multielement fashion, in accordance with Green Chemistry specifications.

Are Human Peripheral Nerves Sensitive To X-ray Imaging?

Diagnostic imaging techniques play an important role in assessing the exact location, cause, and extent of a nerve lesion, thus allowing clinicians to diagnose and manage more effectively a variety of pathological conditions, such as entrapment syndromes, traumatic injuries, and space-occupying lesions. Ultrasound and nuclear magnetic resonance imaging are becoming useful methods for this purpose, but they still lack spatial resolution. In this regard, recent phase contrast x-ray imaging experiments of peripheral nerve allowed the visualization of each nerve fiber surrounded by its myelin sheath as clearly as optical microscopy. In the present study, we attempted to produce high-resolution x-ray phase contrast images of a human sciatic nerve by using synchrotron radiation propagation-based imaging. The images showed high contrast and high spatial resolution, allowing clear identification of each fascicle structure and surrounding connective tissue. The outstanding result is the detection of such structures by phase contrast x-ray tomography of a thick human sciatic nerve section. This may further enable the identification of diverse pathological patterns, such as Wallerian degeneration, hypertrophic neuropathy, inflammatory infiltration, leprosy neuropathy and amyloid deposits. To the best of our knowledge, this is the first successful phase contrast x-ray imaging experiment of a human peripheral nerve sample. Our long-term goal is to develop peripheral nerve imaging methods that could supersede biopsy procedures.

Different coordination modes for disulfoxides towards diorganotin(IV) dichlorides. X-ray crystal structures of 1,2-cis-bis-(phenylsulfinyl)ethene (rac-,cis-cbpse) and adducts [{Ph2SnCl2(meso-bpse)}n] and [{n-Bu2SnCl2(pdtd)}2]

The reactions of meso-1,2-bis(phenylsulfinyl)ethane (meso-bpse) with Ph2SnCl2, 2-phenyl-1,3-dithiane trans-1-trans-3-dioxide (pdtd) with n-Bu2SnCl2 and 1,2-cis-bis-(phenylsulfinyl)ethene (rac-,cis-cbpse) with Ph2SnCl2, in 1:1 molar ratio, yielded [{Ph2SnCl2(meso-bpse)}n], [{n-Bu2SnCl2(pdtd)}2] and [{Ph2SnCl2(rac,cis-cbpse)}x] (x = 2 or n), respectively. All adducts were studied by IR, Mössbauer and 119Sn NMR spectroscopic methods, elemental analysis and single crystal X-ray diffractometry. The X-ray crystal structure of [{Ph2SnCl2(meso-bpse)}n] revealed the occurrence of infinite chains in which the tin(IV) atoms appear in a distorted octahedral geometry with Cl atoms in cis and Ph groups in trans positions. The X-ray crystal structure of [{n-Bu2SnCl2(pdtd)}2] revealed discrete centrosymmetric dimeric species in which the tin(IV) atoms possess a distorted octahedral geometry with bridging disulfoxides in cis and n-butyl moieties in trans positions. The spectroscopic data indicated that the adduct containing the rac,cis-cbpse ligand can be dimeric or polymeric. The X-ray structural analysis of the free rac-,cis-cbpse sulfoxide revealed that the crystals belong to the C2/c space group.

Synthesis of novel O-acylated-D-ribono-1,5-lactones and structural assignment supported by conventional NOESY-NMR and x-ray analysis

A practical method for the structural assignment of 3,4-O-benzylidene-D-ribono-1,5-lactones and analogues using conventional NMR techniques and NOESY measurements in solution is described. 2-O-Acyl-3,4-O-benzylidene-D-ribono-1,5-lactones were prepared in good yields by acylation of Zinner’s lactone with acyl chlorides under mildly basic conditions. Structural determination of 2-O-(4-nitrobenzoyl)-3,4-O-benzylidene-D-ribono-1,5-lactone was achieved by single crystal x-ray diffraction, which supports the results based on spectroscopic data.

Estudo das interações entre o complexo polieletrolítico trimetilquitosana/carboximetilcelulose e Cu+2, ácido húmico e atrazina em solução aquosa

The polyelectrolyte complex (PEC) resulting from the reaction of sodium carboxymethylcellulose (CMC) and N,N,N-trimethylchitosan hydrochloride (TMQ) was prepared and then characterized by infrared spectroscopy and energy dispersive X rays analysis. The interactions involving the PEC and Cu2+ ions, humic acid and atrazine in aqueous medium were studied. From the adsorption isotherms the maximum amount adsorbed (Xmax) was determined as 61 mg Cu2+/g PEC, 171 mg humic acid/g PEC and 5 mg atrazine/g PEC. The results show that the CMC/TMQ complex has a high affinity for the studied species, indicating its potential application to remove them from aqueous media.

Study of calcium oxalate monohydrate of kidney stones by X-ray diffraction

X-ray powder diffraction was used to study the phase composition of human renal calculi. The stones were collected from 56 donors in Vitoria, Espirito Santo state, southeastern Brazil. An XRD phase quantification revealed that 61% of the studied renal stones were composed exclusively of calcium oxalate [34% formed only by calcium oxalate rnonohydrate (COM) and 27% presents both monohydrate and dihydratate calcium oxalate]. The 39% multi-composed calculi have various other phases such as uric acid and calcium phosphate. Rietveld refinement of XRD data of one apparent monophasic (COM) renal calculus revealed the presence of a small amount of hydroxyapatite. The presence of this second phase and the morphology of the stone (ellipsoidal) indicated that this calculus can be classified as non-papillary type and its nucleation process developed in closed kidney cavities. In order to show some advantages of the X-ray powder diffraction technique, a study of the phase transformation of monohydrate calcium oxalate into calcium carbonate (CaCO(3)) was carried out by annealing of a monophasic COM calculi at 200, 300, and 400 degrees C for 48 h in a N(2) gas atmosphere. The results of the XRD for the heat treated samples is ill good agreement with the thermogravimetric analysis found in the literature and shows that X-ray powder diffraction can be used as a suitable technique to study the composition and phase diagram of renal calculi. (C) 2008 International Centre for Diffraction Data.

WOOD DENSITY VARIATION AND TREE RING DEMARCATION IN Gmelina arborea TREES USING X-RAY DENSITOMETRY

Due to its relationship with other properties, wood density is the main wood quality parameter. Modern, accurate methods - such as X-ray densitometry - are applied to determine the spatial distribution of density in wood sections and to evaluate wood quality. The objectives of this study were to determinate the influence of growing conditions on wood density variation and tree ring demarcation of gmelina trees from fast growing plantations in Costa Rica. The wood density was determined by X-ray densitometry method. Wood samples were cut from gmelina trees and were exposed to low X-rays. The radiographic films were developed and scanned using a 256 gray scale with 1000 dpi resolution and the wood density was determined by CRAD and CERD software. The results showed tree-ring boundaries were distinctly delimited in trees growing in site with rainfall lower than 25 10 mm/year. It was demonstrated that tree age, climatic conditions and management of plantation affects wood density and its variability. The specific effect of variables on wood density was quantified by for multiple regression method. It was determined that tree year explained 25.8% of the total variation of density and 19.9% were caused by climatic condition where the tree growing. Wood density was less affected by the intensity of forest management with 5.9% of total variation.

Analysis of breast cancer by small angle X-ray scattering (SAXS)

Small angle X-ray scattering (SAXS) images of normal breast tissue and benign and malignant breast tumour tissues, fixed in formalin, were measured at the momentum transfer range of 0.063 nm(-1) <= q (=4 pi sin(theta/2)/lambda) <= 2.720 nm(-1). Four intrinsic parameters were extracted from the scattering profiles (1D SAXS image reduced) and, from the combination of these parameters, another three parameters were also created. All parameters, intrinsic and derived, were subject to discriminant analysis, and it was verified that parameters such as the area of diffuse scatter at the momentum transfer range 0.50 <= q <= 0.56 nm(-1), the ratio between areas of fifth-order axial and third-order lateral peaks and third-order axial spacing provide the most significant information for diagnosis (p < 0.001). Thus, in this work it was verified that by combining these three parameters it was possible to classify human breast tissues as normal, benign lesion or malignant lesion with a sensitivity of 83% and a specificity of 100%.

Optical identification of the transient supersoft X-ray source RX J0527.8-6954, in the LMC

Context. Close binary supersoft X-ray sources (CBSS) are binary systems that contain a white dwarf with stable nuclear burning on its surface. These sources, first discovered in the Magellanic Clouds, have high accretion rates and near-Eddington luminosities (10(37)-10(38) erg s(-1)) with high temperatures (T = 2-7 x 10(5) K). Aims. The total number of known objects in the MC is still small and, in our galaxy, even smaller. We observed the field of the unidentified transient supersoft X-ray source RX J0527.8-6954 in order to identify its optical counterpart. Methods. The observation was made with the IFU-GMOS on the Gemini South telescope with the purpose of identifying stars with possible He II or Balmer emission or else of observing nebular extended jets or ionization cones, features that may be expected in CBSS. Results. The X-ray source is identified with a B5e V star that is associated with subarcsecond extended H alpha emission, possibly bipolar. Conclusions. If the primary star is a white dwarf, as suggested by the supersoft X-ray spectrum, the expected orbital period exceeds 21 h; therefore, we believe that the 9.4 h period found so far is not associated to this system.

PRECESSING JETS AND X-RAY BUBBLES FROM NGC 1275 (3C 84) IN THE PERSEUS GALAXY CLUSTER: A VIEW FROM THREE-DIMENSIONAL NUMERICAL SIMULATIONS

The Perseus galaxy cluster is known to present multiple and misaligned pairs of cavities seen in X-rays, as well as twisted kiloparsec-scale jets at radio wavelengths; both morphologies suggest that the active galactic nucleus (AGN) jet is subject to precession. In this work, we performed three-dimensional hydrodynamical simulations of the interaction between a precessing AGN jet and the warm intracluster medium plasma, whose dynamics are coupled to a Navarro-Frenk-White dark matter gravitational potential. The AGN jet inflates cavities that become buoyantly unstable and rise up out of the cluster core. We found that under certain circumstances precession can originate multiple pairs of bubbles. For the physical conditions in the Perseus cluster, multiple pairs of bubbles are obtained for a jet precession opening angle >40 degrees acting for at least three precession periods, reproducing both radio and X-ray maps well. Based on such conditions, assuming that the Bardeen-Peterson effect is dominant, we studied the evolution of the precession opening angle of this system. We were able to constrain the ratio between the accretion disk and the black hole angular momenta as 0.7-1.4. We were also able to constrain the present precession angle to 30 degrees-40 degrees, as well as the approximate age of the inflated bubbles to 100-150 Myr.

Star formation history of Canis Major R1 I. Wide-Field X-ray study of the young stellar population

Aims. The CMa R1 star-forming region contains several compact clusters as well as many young early-B stars. It is associated with a well-known bright rimmed nebula, the nature of which is unclear (fossil HII region or supernova remnant). To help elucidate the nature of the nebula, our goal was to reconstruct the star-formation history of the CMa R1 region, including the previously unknown older, fainter low-mass stellar population, using X-rays. Methods. We analyzed images obtained with the ROSAT satellite, covering similar to 5 sq. deg. Complementary VRI photometry was performed with the Gemini South telescope. Colour-magnitude and colour-colour diagrams were used in conjunction with pre-main sequence evolutionary tracks to derive the masses and ages of the X-ray sources. Results. The ROSAT images show two distinct clusters. One is associated with the known optical clusters near Z CMa, to which similar to 40 members are added. The other, which we name the ""GU CMa"" cluster, is new, and contains similar to 60 members. The ROSAT sources are young stars with masses down to M(star) similar to 0.5 M(circle dot), and ages up to 10 Myr. The mass functions of the two clusters are similar, but the GU CMa cluster is older than the cluster around Z CMa by at least a few Myr. Also, the GU CMa cluster is away from any molecular cloud, implying that star formation must have ceased; on the contrary (as already known), star formation is very active in the Z CMa region.

Crystallization and preliminary X-ray analysis of LipL32 from Leptospira interrogans serovar Copenhageni

LipL32 is a major surface protein that is expressed during infection by pathogenic Leptospira. Here, the crystallization of recombinant LipL32(21-272), which corresponds to the mature LipL32 protein minus its N-terminal lipid-anchored cysteine residue, is described. Selenomethionine-labelled LipL32(21-272) crystals diffracted to 2.25 angstrom resolution at a synchrotron source. The space group was P3(1)21 or P3(2)21 and the unit-cell parameters were a = b = 126.7, c = 96.0 angstrom.

X-ray phase measurements as a probe of small structural changes in doped nonlinear optical crystals

X-ray multiple diffraction experiments with synchrotron radiation were carried out on pure and doped nonlinear optical crystals: NH(4)H(2)PO(4) and KH(2)PO(4) doped with Ni and Mn, respectively. Variations in the intensity profiles were observed from pure to doped samples, and these variations correlated with shifts in the structure factor phases, also known as triplet phases. This result demonstrates the potential of X-ray phase measurements to study doping in this type of single crystal. Different methodologies for probing structural changes were developed. Dynamical diffraction simulations and curve fitting procedures were also necessary for accurate phase determination. Structural changes causing the observed phase shifts are discussed.