Synchrotron Radiation X-Ray Fluorescence Analysis (SRXRF) for Measuring the Multielement Composition of Samples of Biogenic Nature

Koutzenogii, K.P.; Савченко, Т. И.; Chankina, O. V.; Kovalskaya, G. A.; Osipova, L. P.; Bgatov, A. V.

doi:10.1081/tma-120020265

Cited by 16 publications

(4 citation statements)

References 5 publications

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“…Trace elements from these samples are fundamental intrinsic components of the biological systems. Paleobiological studies are necessary to know more about the developmental and evolutionary changes occur over millions of years, such as, living organisms of invertebrates [3][4][5][6][7][8][9][10].…”

Section: Introductionmentioning

confidence: 99%

Synchrotron-based X-ray fluorescence, imaging and elemental mapping from biological samples

Rao¹,

Swapna²,

Cesáreo

et al. 2011

Pramana - J Phys

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The present study utilized the new hard X-ray microspectroscopy beamline facility, X27A, available at NSLS, BNL, USA, for elemental mapping. This facility provided the primary beam in a small spot of the order of similar to 10 mu m, for focussing. With this spatial resolution and high flux throughput, the synchrotron-based X-ray fluorescent intensities for Mn, Fe, Zn, Cr, Ti and Cu were measured using a liquid-nitrogen-cooled 13-element energy-dispersive high-purity germanium detector. The sample is scanned in a 'step-and-repeat' mode for fast elemental mapping measurements and generated elemental maps at 8, 10 and 12 keV, from a small animal shell (snail). The accumulated trace elements, from these biological samples, in small areas have been identified. Analysis of the small areas will be better suited to establish the physiology of metals in specific structures like small animal shell and the distribution of other elements

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Section: Introductionmentioning

confidence: 99%

Synchrotron-based X-ray fluorescence, imaging and elemental mapping from biological samples

Rao¹,

Swapna²,

Cesáreo

et al. 2011

Pramana - J Phys

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“…We are interested in the biological and medicinal chemistry of zirconium and the possibility of designing Zr compounds as therapeutic agents. Although Zr has no known natural biological role, it is reported to be present in the body at levels similar to the essential elements Co and Mo. − Current uses of Zr and Zr compounds in medicine center on artificial joints for limb and hip replacements, antiperspirants, , and adjuvants for antibody production . Attempts to design Zr complexes as anticancer agents have so far been unsuccessful; although Cp 2 TiCl 2 exhibits anticancer activity, Cp 2 ZrCl 2 is inactive .…”

Section: Introductionmentioning

confidence: 99%

Structure and Dynamics of Dinuclear Zirconium(IV) Complexes

et al. 2004

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We have determined by X-ray crystallography the structures of three dinuclear zirconium(IV) complexes containing the heptadentate ligand dhpta (where H(5)dhpta = 1,3-diamino-2-propanol-N,N,N',N'-tetraacetic acid, 1) and different countercations: K(2)[Zr(2)(dhpta)(2)].5H(2)O (2.5H(2)O), Na(2)[Zr(2)(dhpta)(2)].7H(2)O.C(2)H(5)OH (3.7H(2)O.C(2)H(5)OH), and Cs(2)[Zr(2)(dhpta)(2)].H(5)O(2).Cl.4H(2)O (4.H(5)O(2).Cl.4H(2)O). In the K(I) complex 2, crystallized from water, the two Zr(IV) ions are 3.5973(4) A apart and bridged via two alkoxo groups (average Zr-O 2.165 A). Each Zr(IV) is eight-coordinate and also bound to two N atoms (average Zr-N 2.448 A), and four carboxylate O atoms (average Zr-O 2.148 A). The two dhpta ligands in the dinuclear unit have different conformations. One face of the complex contains an array of 14 oxygen atoms and interacts strongly with the two K(I) ions, one of which is 6-coordinate, the other 8-coordinate, which are 3.922(4) A apart and bridged by a carboxylate O and by two water molecules. The structures of the dinuclear anion [Zr(2)(dhpta)(2)](2-) in the Na(I) complex 3 and in the Cs(I) complex 4 are essentially identical to that found in complex 2, although the alkali metal ions coordinate differently to the oxygen-rich face. All Zr(IV) ions have a distorted triangulated dodecahedral geometry. Although the crystal structure of complex 2 does not indicate the presence of acidic protons, in 4 an [H(5)O(2)](+) unit is strongly H-bonded to an oxygen atom of a coordinated carboxylate group. 1D and 2D (1)H and (13)C NMR spectroscopic and potentiometric studies reveal two deprotonations with pK(a) values of 9.0 and 10.0. At low pH, two carboxylate groups appear to undergo protonation accompanied by chelate ring-opening, and the complex exhibits dynamic fluxional behavior in which the two magnetically nonequivalent dhpta ligands exchange at a rate of 11 s(-1) at pH 3.30, 298 K, as determined from 2D EXSY NMR studies. Ligand interchange is not observed at high pH (>11). The same crystals of complex 2 were obtained from solutions at pH 3 or 12. The dynamic configurational change is therefore mediated by the aqueous solvent.

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“…XRF spectroscopy is well suited for quantitative analysis of the elements with Z > 11 of the human body tissues and fluids. [12][13][14] Reduction of the SR beam size to the micrometer scale with the use of capillary optics or other X-ray focusing elements, allows the 2-dimensional mapping of the distribution of the studied elements. 15 On the other hand, XAFS spectroscopy is a well-established technique for the investigation of the bonding environment of both metallic 16 17 and non metallic elements 18 in samples of biogenic nature.…”

Section: Introductionmentioning

confidence: 99%

Application of Conventional and Microbeam Synchrotron Radiation X-Ray Fluorescence and Absorption for the Characterization of Human Nails

Katsikini

Mavromati²,

Pinakidou³

et al. 2010

J. Nanosci. Nanotech.

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The synchrotron radiation based spectroscopies X-ray fluorescence and X-ray absorption fine structure are used to detect illness-related changes in the elemental distribution and bonding environment of metals in human nails. The effective atomic number of a collection of nails is determined using two methods, the X-ray transmittance and the scattering method, and is found equal to 7.5 +/- 0.5. X-ray fluorescence maps of the elemental distributions, recorded with a lateral resolution of 5 microm, reveal that S, Ca and Zn are distributed homogeneously while Fe tends to cluster. In the Fe-rich clusters, which have a diameter in the range 15-30 microm, the Fe concentration is 10 times higher than in the matrix. The Zn K edge X-ray Absorption Fine Structure spectra reveal that Zn, in the nails from healthy donors and patients suffering from lung diseases, is four-fold coordinated with N and S and the Zn-N and Zn-S distances are equal to 2.03 A and 2.25 A, respectively. Finally the signature of various bonds in the C-, O- and N- K near edge X-ray absorption fine structure spectra is discussed.

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Synchrotron Radiation X-Ray Fluorescence Analysis (SRXRF) for Measuring the Multielement Composition of Samples of Biogenic Nature

Cited by 16 publications

References 5 publications

Synchrotron-based X-ray fluorescence, imaging and elemental mapping from biological samples

Synchrotron-based X-ray fluorescence, imaging and elemental mapping from biological samples

Structure and Dynamics of Dinuclear Zirconium(IV) Complexes

Application of Conventional and Microbeam Synchrotron Radiation X-Ray Fluorescence and Absorption for the Characterization of Human Nails

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