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Interlaboratory study on the quantification of calcium phosphate phases by Rietveld refinement

Published online by Cambridge University Press:  11 August 2015

Nicola Döbelin
Nicola Döbelin*
Affiliation:
RMS Foundation, Bischmattstrasse 12, 2544 Bettlach, Switzerland
*
a) Author to whom correspondence should be addressed. Electronic mail: nicola.doebelin@rms-foundation.ch
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Abstract

An interlaboratory study (ILS, round robin) was conducted to assess the accuracy and precision of the phase quantification of calcium phosphate (CaP) bioceramics by X-ray diffraction (XRD) and Rietveld refinement. For that purpose, a mixture of hydroxyapatite and β-tricalcium phosphate, two CaP phases commonly used in synthetic bone graft substitutes, was prepared and sent to 12 laboratories for XRD analysis. Results from 26 different instruments were received and evaluated statistically according to ASTM E691 – 13. The statistical analysis revealed that the reproducibility standard deviation of phase quantities was approximately two times greater than the repeatability standard deviation, which is obtained by repeating the analysis on a single instrument configuration multiple times. The 95% reproducibility limit for phase quantities was R = ±1.67 wt%. The study also demonstrated that several participants overinterpreted their data in an attempt to refine crystallite sizes of the minor phase.

Keywords

phase quantificationRietveld refinementcalcium phosphateinterlaboratory studyrepeatabilityreproducibility

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Type
Technical Articles
Information
Powder Diffraction , Volume 30 , Issue 3 , September 2015 , pp. 231 - 241
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Copyright
Copyright © International Centre for Diffraction Data 2015 

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