Absolute scale calibration with use of excess scattering length for small-angle X-ray scattering

2014 ◽  
Vol 47 (2) ◽  
pp. 654-658 ◽  
Author(s):  
Noboru Ohta ◽  
Hiroshi Sekiguchi ◽  
Yuji C. Sasaki ◽  
Naoto Yagi
Keyword(s):  
Small Angle ◽  
Theoretical Calculations ◽  
Scattering Length ◽  
Absolute Intensity ◽  
X Ray ◽  
X Ray Scattering ◽  
Scale Calibration ◽  
Experimental Values ◽  
Calibration Approach ◽  
Ray Scattering

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.

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 Carbonaceous Materials Investigated by Small-Angle X-ray and Neutron Scattering

2020 ◽  
Vol 6 (4) ◽  
pp. 82
Author(s):  
Eneli Härk ◽  
Matthias Ballauff
Keyword(s):  
Neutron Scattering ◽  
Small Angle ◽  
Small Angle Neutron Scattering ◽  
Carbon Nanomaterials ◽  
Scattering Length ◽  
Carbonaceous Materials ◽  
X Ray ◽  
Scattering Length Density ◽  
X Ray Scattering ◽  
Ray Scattering

Carbonaceous nanomaterials have become important materials with widespread applications in battery systems and supercapacitors. The application of these materials requires precise knowledge of their nanostructure. In particular, the porosity of the materials together with the shape of the pores and the total internal surface must be known accurately. Small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) present the methods of choice for this purpose. Here we review our recent investigations using SAXS and SANS. We first describe the theoretical basis of the analysis of carbonaceous material by small-angle scattering. The evaluation of the small-angle data relies on the powerful concept of the chord length distribution (CLD) which we explain in detail. As an example of such an evaluation, we use recent analysis by SAXS of carbide-derived carbons. Moreover, we present our SAXS analysis on commercially produced activated carbons (ACN, RP-20) and provide a comparison with small-angle neutron scattering data. This comparison demonstrates the wealth of additional information that would not be obtained by the application of either method alone. SANS allows us to change the contrast, and we summarize the main results using different contrast matching agents. The pores of the carbon nanomaterials can be filled gradually by deuterated p-xylene, which leads to a precise analysis of the pore size distribution. The X-ray scattering length density of carbon can be matched by the scattering length density of sulfur, which allows us to see the gradual filling of the nanopores by sulfur in a melt-impregnation procedure. This process is important for the application of carbonaceous materials as cathodes in lithium/sulfur batteries. All studies summarized in this review underscore the great power and precision with which carbon nanomaterials can be analyzed by SAXS and SANS.

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.

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.

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