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Standard Reference Material (SRM 1990) For Single Crystal Diffractometer Alignment.

W Wong-Ng1, T Siegrist2, G T DeTitta3

  • 1National Institute of Standards and Technology, Gaithersburg, MD 20899-0001.

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Summary
This summary is machine-generated.

An international project successfully certified ruby spheres as a Standard Reference Material for single crystal diffractometer alignment. This involved a round-robin study and precise lattice parameter measurements, ensuring accuracy for X-ray diffraction applications.

Keywords:
Cr-contentNIST SRM 1990alignment standardinternational round robinruby spheressingle crystal x-ray diffractometers

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Area of Science:

  • Materials Science
  • Crystallography
  • Metrology

Background:

  • Accurate single crystal diffractometer alignment is crucial for reliable crystallographic measurements.
  • Standard Reference Materials (SRMs) are essential for calibrating and validating experimental setups.
  • Chromium-doped aluminum oxide (ruby) spheres were selected for their suitable crystallographic properties.

Purpose of the Study:

  • To demonstrate the viability of ruby spheres as a standard for diffractometer alignment through a global round-robin study.
  • To certify the precise lattice parameters of SRM 1990, a ruby sphere Standard Reference Material.
  • To establish a reliable standard for X-ray diffraction laboratories worldwide.

Main Methods:

  • An international round-robin study involving 32 laboratories determining lattice parameters of ruby spheres and zeolite crystals.
  • Certification of lattice parameters using four single crystal diffractometers at Lucent Technologies and NRC Canada.
  • Quantification of chromium content via microprobe and SEM/EDS, and mosaicity evaluation using double-crystal spectrometry.
  • Confirmation of lattice parameters using a Guinier-Hägg camera and application of thermal expansion and refraction corrections.

Main Results:

  • The international round-robin study yielded mean lattice parameters for ruby spheres: a=4.7608 ű0.0062 Å and c=12.9979 ű0.020 Å.
  • Certified mean unit cell parameters for SRM 1990 were determined as a=4.76080±0.00029 Å and c=12.99568 ű0.00087 Å.
  • Results from single crystal diffractometry and Guinier-Hägg measurements showed excellent agreement, validating the certified values.

Conclusions:

  • The international project successfully established SRM 1990, ruby spheres, as a reliable standard for single crystal diffractometer alignment.
  • The certified lattice parameters are highly accurate and consistent with results from a global collaborative study.
  • This SRM will enhance the accuracy and comparability of crystallographic data generated by X-ray diffraction laboratories.