Home About us Contact
|
Home About us Contact | ||
|
|
||
SAXS Data (sax + data)
Selected AbstractsQuality control of protein standards for molecular mass determinations by small-angle X-ray scatteringJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 2 2010Shuji Akiyama Small-angle X-ray scattering (SAXS) is a powerful technique with which to evaluate the size and shape of biological macromolecules in solution. Forward scattering intensity normalized relative to the particle concentration, I(0)/c, is useful as a good measure of molecular mass. A general method for deducing the molecular mass from SAXS data is to determine the ratio of I(0)/c of a target protein to that of a standard protein with known molecular mass. The accuracy of this interprotein calibration is affected considerably by the monodispersity of the prepared standard, as well as by the precision in estimating its concentration. In the present study, chromatographic fractionation followed by hydrodynamic characterization is proposed as an effective procedure by which to prepare a series of monodispersed protein standards. The estimation of molecular mass within an average deviation of 8% is demonstrated using monodispersed bovine serum albumin as a standard. The present results demonstrate the importance of protein standard quality control in order to take full advantage of interprotein calibration. [source] Determination of the molecular weight of proteins in solution from a single small-angle X-ray scattering measurement on a relative scaleJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 1 2010H. Fischer This paper describes a new and simple method to determine the molecular weight of proteins in dilute solution, with an error smaller than ,10%, by using the experimental data of a single small-angle X-ray scattering (SAXS) curve measured on a relative scale. This procedure does not require the measurement of SAXS intensity on an absolute scale and does not involve a comparison with another SAXS curve determined from a known standard protein. The proposed procedure can be applied to monodisperse systems of proteins in dilute solution, either in monomeric or multimeric state, and it has been successfully tested on SAXS data experimentally determined for proteins with known molecular weights. It is shown here that the molecular weights determined by this procedure deviate from the known values by less than 10% in each case and the average error for the test set of 21 proteins was 5.3%. Importantly, this method allows for an unambiguous determination of the multimeric state of proteins with known molecular weights. [source] Structural refinement by restrained molecular-dynamics algorithm with small-angle X-ray scattering constraints for a biomoleculeJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 1 2004Masaki Kojima A new algorithm to refine protein structures in solution from small-angle X-ray scattering (SAXS) data was developed based on restrained molecular dynamics (MD). In the method, the sum of squared differences between calculated and observed SAXS intensities was used as a constraint energy function, and the calculation was started from given atomic coordinates, such as those of the crystal. In order to reduce the contribution of the hydration effect to the deviation from the experimental (objective) curve during the dynamics, and purely as an estimate of the efficiency of the algorithm, the calculation was first performed assuming the SAXS curve corresponding to the crystal structure as the objective curve. Next, the calculation was carried out with `real' experimental data, which yielded a structure that satisfied the experimental SAXS curve well. The SAXS data for ribonuclease T1, a single-chain globular protein, were used for the calculation, along with its crystal structure. The results showed that the present algorithm was very effective in the refinement and adjustment of the initial structure so that it could satisfy the objective SAXS data. [source] Pole figure analysis of mineral nanoparticle orientation in individual trabecula of human vertebral boneJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3-1 2003Daniel Jaschouz The spongious interior of human vertebral bone consists of interconnected trabecula with a thickness of about 0.2 mm. The texture of the bone material, a collagen-mineral nanocomposite, was studied within single trabecula by collecting two-dimensional small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD) data exactly at the same specimen positions with an X-ray beam of 0.2 mm diameter. Three-dimensional information was reconstructed by combining measurements with different specimen orientations. The XRD data, and for the first time also the SAXS data, were subjected to a pole figure analysis. The method provides a quantitative description of the crystallographic orientation distribution as well as the morphological orientation distribution of the plate shaped nanoparticles, both with respect to the orientation of the investigated trabecula. As a main result it could be shown that a fibre-texture exists in the trabecula, and that the plate shaped nanoparticles are aligned with the lamellae within the trabecula. [source] Modelling of small-angle X-ray scattering data using Hermite polynomialsJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2001A. K. Swain A new algorithm, called the term-selection algorithm (TSA), is derived to treat small-angle X-ray scattering (SAXS) data by fitting models to the scattering intensity using weighted Hermite polynomials. This algorithm exploits the orthogonal property of the Hermite polynomials and introduces an error-reduction ratio test to select the correct model terms or to determine which polynomials are to be included in the model and to estimate the associated unknown coefficients. With no a priori information about particle sizes, it is possible to evaluate the real-space distribution function as well as three- and one-dimensional correlation functions directly from the models fitted to raw experimental data. The success of this algorithm depends on the choice of a scale factor and the accuracy of orthogonality of the Hermite polynomials over a finite range of SAXS data. An algorithm to select a weighted orthogonal term is therefore derived to overcome the disadvantages of the TSA. This algorithm combines the properties and advantages of both weighted and orthogonal least-squares algorithms and is numerically more robust for the estimation of the parameters of the Hermite polynomial models. The weighting feature of the algorithm provides an additional degree of freedom to control the effects of noise and the orthogonal feature enables the reorthogonalization of the Hermite polynomials with respect to the weighting matrix. This considerably reduces the error in orthogonality of the Hermite polynomials. The performance of the algorithm has been demonstrated considering both simulated data and experimental data from SAXS measurements of dewaxed cotton fibre at different temperatures. [source] Improvement of SAXS measurements on Kratky slit systems by Göbel mirrors and imaging-plate detectorsJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 3-2 2000Alexander Bergmann Laboratory X-ray sources emit a highly divergent beam. The Kratky compact camera is constructed to maximize the intensity in the sample using a slit collimation system. The performance of this camera can be further increased if the primary beam is collimated from a divergent into a parallel beam. A recently developed device for this purpose is the so-called `Göbel mirror'. This mirror is made of parabolically bent multilayers, designed to collimate divergent X-rays from laboratory X-ray sources into a parallel and monochromatic beam of high brilliance. Modification of the block collimation system in combination with a Göbel mirror leads to a different beam geometry, resulting in an intensity increase by a factor of about 10. The gain in intensity implicates the use of imaging-plate detectors, which have a wide linear range in intensity and allow the full use of the increased intensity. Hence the quality of the SAXS data is improved by the higher intensity primary beam, the much lower background due to the exclusive use of Cu K, radiation, and a detection unit which is linear in the measured intensity regime. All these advantages, such as intensity gain, lower background, better quality of the data, are demonstrated with some selected experimental results. [source] DIATOM SILICA BIOMINERALIZATION: AT NANOSCALE LEVEL A CHEMICALLY UNIFORM PROCESSJOURNAL OF PHYCOLOGY, Issue 2000E. G. Vrieling Using a high-brilliance synchrotron X-ray source, combined small- and wide-angle X-ray scattering (SAXS and WAXS) was applied to study nanoscale characteristics, in particular pore size in the range of 3 to 65 nm, of a variety of unialgal cultures of centric and pennate diatoms, and of mixed diatom populations sampled in the field. Results of scattering analysis were compared with details of pore size, structure and orientation visible at the electron microscopic level. WAXS patterns did not reveal any crystalline phase or features of microcrystallinity (resolution 0.07 to 0.51 nm), which implies a totally amorphous character of the SiO2 matrix of the frustule material. SAXS data (resolution 3 to 65 nm) provided information on geometry, size, and distribution of pores in the silica. Overall, two pore regions were recognized that were common to the silica of all samples: the smallest (d less than 10 nm) regularly spaced and shaped spherically, the larger (up to 65 nm) being cylinders or slits. Apparently, at a nanoscale level diatomaceous silica is quite homologous among species, in agreement with the chemical principles of silica polymerization under the conditions of pH and precursor concentrations inside the silicon deposition vesicle. The final frustule "macro"-morphology is of course species-specific, being determined genetically. Synthetically-derived MCM-type silicas have a similarly organized pore distribution in an amorphous silica matrix as we found in all diatom species studied. We therefore suggest that organic molecules of a kind used as structure-directing agents to produce these artificial silicas play a role in the nucleation of the silica polymerization reaction and the shaping of pore morphology inside the silicon deposition vesicle of diatoms. Structure-directing molecules now await isolation from the SDV, followed by identification and characterisation by molecular techniques. [source] Tensile properties and morphological evolution of polypropylene and poly(ethylene- co -1-octene) blendsPOLYMER COMPOSITES, Issue 10 2009Na Song Extruded sheet of isotactic polypropylene and poly(ethylene- co -1-octene) blends extruded from a counterrotating twin-screw extruder were studied by scanning electron microscopy, tensile test, and small-angle X-ray scattering. The average characteristic length (,m) determined by the statistical computing from the SEM images increases linearly with increasing of dispersed phase concentration. When POE content is 50 wt% (double continuous phase), ,m is two or three times as big as that of other blends ratio. The analyses of SAXS data confirm this result. Comparison has been made between experimental data of tensile test and those predicted from several meso-mechanical models such as parallel model, series model, Halpin's model, Mori-Tanaka's model, and modified mixture model. The modified mixture model is an effective method for predicting Young's modulus in comparison with other models. POLYM. COMPOS., 2009. © 2008 Society of Plastics Engineers [source] The Structure of MetallomicellesCHEMISTRY - A EUROPEAN JOURNAL, Issue 8 2004P. C. Griffiths Dr. Abstract The morphology of micelles formed by two novel metallosurfactants has been studied by small-angle neutron scattering (SANS) and small-angle-X-ray scattering (SAXS). The two surfactants both contain a dodecyl chain as the hydrophobic moiety, but differ in the structure of the head group. The surfactants are CuII complexes of monopendant alcohol derivatives of a) the face-capping macrocycle 1,4,7-triazacyclanonane (tacn), and b) an analogue based upon the tetraazamacrocycle 1,4,7,10-tetraazacyclododecane. Here, neutron scattering has been used to study the overall size and shape of the surfactant micelles, in conjunction with X-ray scattering to locate the metal ions. For the 1,4,7,10-tetraazacyclododecane-based surfactant, oblate micelles are observed, which are smaller to the prolate micelles formed by the 1,4,7-triazacyclononane analogue. The X-ray scattering analysis shows that the metal ions are distributed throughout the polar head-group region, rather than at a well-defined radius; this is in good agreement with the SANS-derived dimensions of the micelle. Indeed, the same model for micelle morphology can be used to fit both the SANS and SAXS data. [source] | ||||||||||