An algorithm has been derived, forming the basis of a computer program called BBCCURV, which calculates a Bragg-Brentano X-ray diffractometer intensity correction curve (intensity correction factor Kivs. 2θi) given the diffractometer and sample dimensions, and the effective (not theoretical) linear absorption coefficient of the sample. Use of this calibration curve gives a set of intensity data free from aberrations, which are caused mainly by sample transparency, curvature of the diffraction cones passing through the receiving slit and possible beam overflow past the specimen at low angles.
The algorithm was confirmed with a full-profile Rietveld refinement of Bragg-Brentano X-ray diffraction data from a H+-ZSM5 zeolite sample. On introducing a BBCCURV correction curve, the profile R-factor over the pattern points dropped from 30.8% to 16.5%, a significantly better fit when the data were corrected with a BBCCURV curve.
BBCCURV intensity calibration curves from LiF (μ= 1.5 mm−1) through zeolites, clays, ZnO, rutile, Pb(NO3)2and finally solid metal (μ= 1000 mm−1) (CoKα) indicate upward revision of the measured diffractometer intensities by factors of between 2 and 10 at 2θ= 5° for these sample types, normalised to a correction factor of 1.0 at 2θ= 44°. Corrections of this magnitude to Bragg-Brentano data are thus significant in full-profile structure refinement and quantitative analysis with Bragg-Brentano data. Use of a variable divergence slit (VDS) is not appropriate in full-profile refinements as the intensity aberrations are magnified, and conversion from VDS data to aberration-free data is sample- and transparency-dependent, and not the simple area (sinθ)−1function generally assumed. Use of a fixed divergence slit with a BBCCURV-type calibration is recommended.