Abstract

Commercial glassy carbon plates being used as absolute intensity calibration standards in small-angle X-ray scattering applications (NIST SRM 3600) have been characterized in several recent publications. This contribution adds to the characterization by measuring the hydrogen content of a plate to be (4.8 ± 0.2)× 10-4 (mol H)/(mol C), and by measuring the vibrational spectrum by neutron inelastic scattering. The spectrum bears a strong resemblance to published measurements on graphite, allowing the identification of several spectral features. The measured spectrum is used to calculate the heat capacity of low-hydrogen-content glassy carbon for comparison with measurements reported here from 20 to 295 K.

Highlights

  • A study (Zhang et al, 2010) at the Advanced Photon Source (APS) of Argonne National Laboratory characterized glassy carbon plates obtained from Alfa Aesar1 for use in absolute intensity calibrations for small-angle X-ray scattering (SAXS) applications

  • Commercial Alfa Aesar Type-2 glassy carbon plates have been developed as absolute intensity calibration standards in SAXS measurements and designated as new NIST Standard Reference Material SRM 3600

  • We have further characterized this material by sampling a plate provided to us from APS and found that it has a hydrogen content of (4.8 Æ 0.2) Â 10À4/(mol C)

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Summary

Introduction

A study (Zhang et al, 2010) at the Advanced Photon Source (APS) of Argonne National Laboratory characterized glassy carbon plates obtained from Alfa Aesar for use in absolute intensity calibrations for small-angle X-ray scattering (SAXS) applications. Zhang et al demonstrated that selected commercially available glassy carbon plates are sufficiently homogeneous and stable to serve as calibration standards and have made these plates available to several laboratories for this purpose. This material has been more formally developed as a new NIST Standard Reference Material (SRM 3600, 2017), as described in a recent article in this journal (Allen et al, 2017). To further characterize these same plates, we have determined their hydrogen content and performed neutron inelastic scattering measurements to determine the lattice vibrational spectrum. This, in turn, is used to calculate the heat capacity for comparison with measurements presented here on a similar sample

Properties and structure of NIST SRM 3600
Hydrogen content of NIST SRM 3600
Methods and results of neutron scattering measurements
Neutron scattering measurements on glassy carbon samples: discussion
Summary
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