scholarly journals Absolute intensity calibration for carbon-edge soft X-ray scattering

2020 ◽  
Vol 27 (6) ◽  
pp. 1601-1608
Author(s):  
Thomas Ferron ◽  
Devin Grabner ◽  
Terry McAfee ◽  
Brian Collins
Keyword(s):  
Small Angle ◽  
Absolute Intensity ◽  
Small Angle Scattering ◽  
Interfacial Structure ◽  
Thin Polymer Film ◽  
X Ray ◽  
X Ray Scattering ◽  
Angle Scattering ◽  
Intensity Calibration ◽  
Ray Scattering

Resonant soft X-ray scattering (RSOXS) has become a premier probe to study complex three-dimensional nanostructures in soft matter through combining the robust structural characterization of small-angle scattering with the chemical sensitivity of spectroscopy. This technique borrows many of its analysis methods from alternative small-angle scattering measurements that utilize contrast variation, but thus far RSOXS has been unable to reliably achieve an absolute scattering intensity required for quantitative analysis of domain compositions, volume fraction, or interfacial structure. Here, a novel technique to calibrate RSOXS to an absolute intensity at the carbon absorption edge is introduced. It is shown that the X-ray fluorescence from a thin polymer film can be utilized as an angle-independent scattering standard. Verification of absolute intensity is then accomplished through measuring the Flory–Huggins interaction parameter in a phase-mixed polymer melt. The necessary steps for users to reproduce this intensity calibration in their own experiments to improve the scientific output from RSOXS measurements are discussed.

scholarly journals NIST Standard Reference Material 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering

2017 ◽  
Vol 50 (2) ◽  
pp. 462-474 ◽  
Author(s):  
Andrew J. Allen ◽  
Fan Zhang ◽  
R. Joseph Kline ◽  
William F. Guthrie ◽  
Jan Ilavsky
Keyword(s):  
Reference Material ◽  
Small Angle ◽  
Standard Reference Material ◽  
Absolute Intensity ◽  
Calibration Standard ◽  
X Ray ◽  
X Ray Scattering ◽  
Nist Standard Reference Material ◽  
Intensity Calibration ◽  
Ray Scattering

The certification of a new standard reference material for small-angle scattering [NIST Standard Reference Material (SRM) 3600: Absolute Intensity Calibration Standard for Small-Angle X-ray Scattering (SAXS)], based on glassy carbon, is presented. Creation of this SRM relies on the intrinsic primary calibration capabilities of the ultra-small-angle X-ray scattering technique. This article describes how the intensity calibration has been achieved and validated in the certifiedQrange,Q= 0.008–0.25 Å−1, together with the purpose, use and availability of the SRM. The intensity calibration afforded by this robust and stable SRM should be applicable universally to all SAXS instruments that employ a transmission measurement geometry, working with a wide range of X-ray energies or wavelengths. The validation of the SRM SAXS intensity calibration using small-angle neutron scattering (SANS) is discussed, together with the prospects for including SANS in a future renewal certification.

scholarly journals Two practical Java software tools for small-angle X-ray scattering analysis of biomolecules

2014 ◽  
Vol 47 (2) ◽  
pp. 810-815 ◽  
Author(s):  
Andreas Hofmann ◽  
Andrew E. Whitten
Keyword(s):  
Small Angle ◽  
Three Dimensional ◽  
Small Angle Scattering ◽  
Ease Of Use ◽  
Scattering Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Angle Scattering ◽  
Three Dimensional Models ◽  
Ray Scattering

Small-angle X-ray scattering has established itself as a common technique in structural biology research. Here, two novel Java applications to aid modelling of three-dimensional macromolecular structures based on small-angle scattering data are described.MolScatis an application that computes small-angle scattering intensities from user-provided three-dimensional models. The program can fit the theoretical scattering intensities to experimental X-ray scattering data.SAFIRis a program for interactive rigid-body modelling into low-resolution shapes restored from small-angle scattering data. The program has been designed with an emphasis on ease of use and intuitive handling. An embedded version ofMolScatis used to enable quick evaluation of the fit between the model and experimental scattering data.SAFIRalso provides options to refine macromolecular complexes with optional user-specified restraints against scattering data by means of a Monte Carlo approach.

Nanostructure of a-Si:H and Related Materials by Small-Angle X-Ray Scattering

1995 ◽  
Vol 377 ◽  
Author(s):  
D. L. Williamson
Keyword(s):  
Small Angle ◽  
Detailed Comparison ◽  
Small Angle Scattering ◽  
Atomic Scale ◽  
X Ray ◽  
X Ray Scattering ◽  
Current State ◽  
Angle Scattering ◽  
Wide Range ◽  
Ray Scattering

ABSTRACTThe use of small-angle x-ray scattering to examine nanostructural features of a-Si:H and the related alloys a-SiGe:H and a-SiC:H will be reviewed. A wide range of H, Ge, and C compositions has been investigated. The films examined came from several film- and device-making groups and represent current state-of-the-art solar cell material or attempts to develop improved and more stable material. A detailed comparison of the three classes of materials reveals dramatic differences in nanostructure. The diffuse component of the small-angle scattering, not recognized or discussed in previous small-angle scattering experiments on these materials by other groups, is shown to contain potentially valuable information on the atomic-scale structure.

scholarly journals Final Report of the International Project for the Calibration of Absolute Intensities in Small-Angle X-ray Scattering

1978 ◽  
Vol 11 (3) ◽  
pp. 196-205 ◽  
Author(s):  
Keyword(s):  
Small Angle ◽  
Absolute Intensity ◽  
Final Report ◽  
X Ray ◽  
X Ray Scattering ◽  
Calibration Methods ◽  
The Absolute ◽  
Calibration Techniques ◽  
Intensity Calibration ◽  
Ray Scattering

An international intercomparison project was performed to test the reproducibility and the comparative accuracy of the various absolute intensity calibration techniques in current use in small-angle X-ray scattering with the participation of fifteen investigators from eight different laboratories in six countries. In the project, the absolute differential X-ray scattering cross sections of standard samples of glassy carbon and polystyrene were calibrated using five different calibration techniques and two different X-ray wavelengths. The results have been intercompared with a variety of statistical techniques. It is concluded that angularly dependent errors associated with determining the zero of angle, dead-time corrections, collimation corrections, and insufficiently close data point spacing are more important in accounting for discrepancies between laboratories than are differences in the absolute intensity calibration methods themselves.

Interpretation of small-angle X-ray scattering patterns of crystalline triglyceride nanoparticles in dispersion

2007 ◽  
Vol 40 (6) ◽  
pp. 1008-1018 ◽  
Author(s):  
T. Unruh
Keyword(s):  
Small Angle ◽  
Simulation Analysis ◽  
Aqueous Dispersion ◽  
Small Angle Scattering ◽  
X Rays ◽  
X Ray ◽  
Scattering Model ◽  
X Ray Scattering ◽  
Angle Scattering ◽  
Ray Scattering

Triglyceride nanocrystals in aqueous dispersion produced by high-pressure melt homogenization exhibit platelet-like shapes and clear but broadened Bragg reflections in the small-angle scattering regime. Because the particle thickness, the thickness of the stabilizer layer, the length scale of the crystalline structure of the nanoparticles and often the interparticle distances are of the same order of magnitude, the scattering of these structures mutually interferes. This leads to complicated small-angle scattering patterns which exhibit a lot of features, but it is not straightforward to discover the contained information on the structure of the system. In this contribution, a scattering model for such systems will be described, which is based on the kinematic scattering theory of X-rays. Using this scattering model an X-ray powder pattern simulation analysis is introduced to gain information on tripalmitin nanosuspensions which have been investigated by synchrotron small-angle X-ray scattering. It will be demonstrated that the results of this method provide a consistent description of all structural details mentioned above. In particular, information on the extension and the molecular packing density of the stabilizer layers can be achieved because these layers exhibit a comparatively large scattering contrast.

Small-Angle X-ray Scattering at the ESRF High-Brilliance Beamline

1997 ◽  
Vol 30 (5) ◽  
pp. 867-871 ◽  
Author(s):  
P. Bösecke ◽  
O. Diat
Keyword(s):  
Small Angle ◽  
Small Angle Scattering ◽  
Optical Systems ◽  
Photon Flux ◽  
X Rays ◽  
Time Resolved ◽  
X Ray ◽  
X Ray Scattering ◽  
Angle Scattering ◽  
Ray Scattering

The high-brilliance beamline (BL4/ID2) at the European Synchrotron Radiation Facility (ESRF) in Grenoble has been constructed with the emphasis on time-resolved small-angle X-ray scattering and macromolecular crystallography. It has been open to users for two years. The beamline has opened up new areas in small-angle scattering research, facilitating (a) small-angle crystallography on structures with unit cells of several hundredths of nanometres, (b) overlap with the light scattering range for the study of optical systems, (c) high photon flux for time-resolved experiments and (d) a high spatial coherence allowing submicrometre imaging with X-rays. The set-up and the detector system of the small-angle scattering station are presented. A method for obtaining absolute scattering intensities is described. The parasitic background at the station is discussed in terms of absolute scattering intensities.

Performance and First Results of the ELETTRA High-Flux Beamline for Small-Angle X-ray Scattering

1997 ◽  
Vol 30 (5) ◽  
pp. 872-876 ◽  
Author(s):  
H. Amenitsch ◽  
S. Bernstorff ◽  
M. Kriechbaum ◽  
D. Lombardo ◽  
H. Mio ◽  
...  
Keyword(s):  
Small Angle ◽  
Small Angle Scattering ◽  
Design Parameters ◽  
High Flux ◽  
Time Resolved ◽  
X Ray ◽  
X Ray Scattering ◽  
Angle Scattering ◽  
Scattering Measurements ◽  
Ray Scattering

A new beamline for small-angle X-ray scattering (SAXS) has recently been constructed and is presently under final commissioning at the 2 GeV storage ring ELETTRA. It has been designed specifically for time-resolved studies of non-crystalline and fibrous materials and has been optimized for small-angle scattering measurements. The beamline operates with a SAXS resolution between 10 and about 1400 Å in d spacing (at 8 keV) and has been optimized with respect to high flux at the sample [of the order of 1013 photons s−1 for 8 keV photons (2 GeV, 400 mA)]. Soon it will be possible to perform simultaneously wide-angle diffraction measurements in the d-spacing range 1.2–8 Å (at 8 keV). In order to allow time-resolved (resolution ~1 ms) small-angle scattering measurements, a high-power 57-pole wiggler is used as the beamline source. From its beam, one of three discrete energies, 5.4, 8 and 16 keV, can be selected with a double-crystal monochromator, which contains three pairs of asymmetrically cut plane Si(111) crystals. Downstream, the beam is focused horizontally and vertically by a toroidal mirror. Commissioning tests of this new SAXS beamline showed that all design parameters have been realized.

Performance on absolute scattering intensity calibration and protein molecular weight determination at BL16B1, a dedicated SAXS beamline at SSRF

2017 ◽  
Vol 24 (2) ◽  
pp. 509-520 ◽  
Author(s):  
Jianrong Zeng ◽  
Fenggang Bian ◽  
Jie Wang ◽  
Xiuhong Li ◽  
Yuzhu Wang ◽  
...  
Keyword(s):  
Molecular Weight ◽  
Small Angle ◽  
Absolute Intensity ◽  
Molecular Weight Determination ◽  
X Ray ◽  
X Ray Scattering ◽  
Saxs Intensity ◽  
The Absolute ◽  
Intensity Calibration ◽  
Ray Scattering

The optical system and end-station of bending-magnet beamline BL16B1, dedicated to small-angle X-ray scattering (SAXS) at the Shanghai Synchrotron Radiation Facility, is described. Constructed in 2009 and upgraded in 2013, this beamline has been open to users since May 2009 and supports methodologies including SAXS, wide-angle X-ray scattering (WAXS), simultaneous SAXS/WAXS, grazing-incidence small-angle X-ray scattering (GISAXS) and anomalous small-angle X-ray scattering (ASAXS). Considering that an increasing necessity for absolute calibration of SAXS intensity has been recognized in in-depth investigations, SAXS intensity is re-stated according to the extent of data processing, and the absolute intensity is suggested to be a unified presentation of SAXS data in this article. Theory with a practical procedure for absolute intensity calibration is established based on BL16B1, using glass carbon and water as primary and secondary standards, respectively. The calibration procedure can be completed in minutes and shows good reliability under different conditions. An empirical line of scale factor estimation is also established for any specific SAXS setup at the beamline. Beamline performance on molecular weight (MW) determination is provided as a straightforward application and verification of the absolute intensity calibration. Results show good accuracy with a deviation of less than 10% compared with the known value, which is also the best attainable accuracy in recent studies using SAXS to measure protein MW. Fast MW measurement following the demonstrated method also enables an instant check or pre-diagnosis of the SAXS performance to improve the data acquisition.

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