Absolute Intensity Measurements in Small‐Angle X‐Ray Scattering

1963 ◽  
Vol 34 (6) ◽  
pp. 691-696 ◽  
Author(s):  
D. L. Weinberg
2017 ◽  
Vol 50 (2) ◽  
pp. 462-474 ◽  
Author(s):  
Andrew J. Allen ◽  
Fan Zhang ◽  
R. Joseph Kline ◽  
William F. Guthrie ◽  
Jan Ilavsky

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.


1978 ◽  
Vol 11 (3) ◽  
pp. 196-205 ◽  
Author(s):  

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.


2020 ◽  
Vol 27 (6) ◽  
pp. 1601-1608
Author(s):  
Thomas Ferron ◽  
Devin Grabner ◽  
Terry McAfee ◽  
Brian Collins

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.


2014 ◽  
Vol 47 (2) ◽  
pp. 654-658 ◽  
Author(s):  
Noboru Ohta ◽  
Hiroshi Sekiguchi ◽  
Yuji C. Sasaki ◽  
Naoto Yagi

For small-angle X-ray scattering (SAXS) in solution, absolute intensity calibration is an important step to estimate the number of electrons of the sample. In this study, the excess scattering length of 1-bromododecane dispersed in dodecane was determined using that of 1-chlorododecane in the same solvent. The deviation of the experimental values from theoretical calculations obtained using atomic factors was around 1%. It is suggested that the 1-chlorododecane–dodecane system constitutes a new calibration approach that is applicable to various materials over a large energy range generally used in SAXS measurements, and could be less complex and more reliable than conventional methods.


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