Hostname: page-component-8448b6f56d-dnltx Total loading time: 0 Render date: 2024-04-23T17:31:23.827Z Has data issue: false hasContentIssue false
  • English
  • Français

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
Get access Rights & Permissions [Opens in a new window]

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

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

ASTM E177 – 13 (2013). “Standard practice for use of the terms precision and bias in ASTM test methods,” in Annual Book of ASTM Standards (ASTM International, West Conshohocken, PA), Vol. 14.02.Google Scholar
ASTM E691 – 13 (2013). “Standard practice for conducting an interlaboratory study to determine the precision of a test method,” in Annual Book of ASTM Standards (ASTM International, West Conshohocken, PA), Vol. 14.02.Google Scholar
ASTM F1088 – 4 (2004). “Standard specification for beta-tricalcium phosphate for surgical implantation,” in Annual Book of ASTM Standards (ASTM International, West Conshohocken, PA), Vol. 13.01.Google Scholar
ASTM F1185 – 03 (2003). “Standard specification for composition of hydroxyapatite for surgical implants,” in Annual Book of ASTM Standards (ASTM International, West Conshohocken, PA), Vol. 13.01.Google Scholar
ASTM F2024 – 10 (2010). “Standard practice for X-ray diffraction determination of phase content of plasma-sprayed hydroxyapatite coatings,” in Annual Book of ASTM Standards (ASTM International, West Conshohocken, PA), Vol 13.01.Google Scholar
Bergmann, J., Friedel, P. and Kleeberg, R. (1998). “BGMN – a new fundamental parameters based Rietveld program for laboratory X-ray sources, it's use in quantitative analysis and structure investigations,” Commission of Powder Diffraction, International Union of Crystallography, CPD Newslett. 20, 5–8.Google Scholar
Bohner, M., Galea, L. and Doebelin, N. (2012). “Calcium phosphate bone graft substitutes: failures and hopes,” J. Eur. Ceram. Soc. 32, 2663–2671.CrossRefGoogle Scholar
Chow, L. C. (2001). “Solubility of calcium phosphates,” in Octacalcium Phosphate, edited by Chow, L. C. and Eanes, E. D. (Karger, Basel), Vol. 18, pp. 94–111.Google Scholar
Dickens, B., Schroeder, L. W. and Brown, W. E. (1974). “Crystallographic studies on the role of Mg as a stabilizing impurity in β-Ca3(PO4)2 I. The crystal structure of pure β-Ca3(PO4)2 ,” J. Solid State Chem. 10, 232–248.CrossRefGoogle Scholar
Dinnebier, R. E. and Billinge, S. J. L. (Eds.) (2008). Powder Diffraction: Theory and Practice (Royal Society of Chemistry, Cambridge).Google Scholar
Döbelin, N., Luginbühl, R. and Bohner, M. (2010). “Synthetic calcium phosphate ceramics for treatment of bone fractures,” Chimia 64, 723–729.Google Scholar
Dorozhkin, S. V. (2002). “A review on the dissolution models of calcium apatites,” Prog. Cryst. Growth Charact. Mater. 44, 45–61.Google Scholar
Dorozhkin, S. V. (2011). “Self-setting calcium orthophosphate formulations: cements, concretes, pastes and putties,” Int. J. Mater. Chem. 1, 1–48.Google Scholar
Elliott, J. C. (1994). Structure and Chemistry of the Apatites and other Calcium Orthophosphates (Elsevier, Amsterdam).Google Scholar
Enderle, R., Gotz-Neunhoeffer, F., Gobbels, M., Muller, F. A. and Greil, P. (2005). “Influence of magnesium doping on the phase transformation temperature of beta-TCP ceramics examined by Rietveld refinement,” Biomaterials 26, 3379–3384.CrossRefGoogle ScholarPubMed
Gopal, R. and Calvo, C. (1972). “Structural relationship of Whitlockite and βCa3(PO4)2 ,” Nat. Phys. Sci. 237, 30–32.Google Scholar
ICDD (2013). PDF-4+2013 (Database), edited by Dr. Soorya Kabekkodu, (International Centre for Diffraction Data, Newtown Square, PA, USA).Google Scholar
Ishikawa, K., Ducheyne, P. and Radin, S. (1993). “Determination of the Ca/P ratio in calcium-deficient hydroxyapatite using X-ray-diffraction analysis,” J. Mater. Sci.-Mater. Med. 4, 165–168.Google Scholar
ISO 13175-3 (2012). Implants for surgery - Calcium phosphates - Part 3: Hydroxyapatite and beta-tricalcium phosphate bone substitutes (ISO, Geneva, Switzerland).Google Scholar
ISO 13779-3 (2008). Implants for surgery - Calcium phosphates - Part 3: Chemical analysis and characterization of crystallinity and phase purity (ISO, Geneva, Switzerland).Google Scholar
Jackson, L. E., Barralet, J. E. and Wright, A. J. (2004). “Rietveld analysis in sintering studies of Ca-deficient hydroxyapatite,” Key Eng. Mater. 254–256, 297–300.Google Scholar
Keller, L. (1995). “X-ray powder diffraction patterns of calcium phosphates analyzed by the Rietveld method,” J. Biomed. Mater. Res. 29, 1403–1413.CrossRefGoogle ScholarPubMed
Madsen, I. C. and Scarlett, N. V. Y. (2008). “Quantitative phase analysis” in Powder Diffraction: Theory and Practice, edited by Dinnebier, R. E. and Billinge, S. J. L. (Royal Society of Chemistry, Cambridge), pp. 298–331.Google Scholar
McCusker, L. B., Von Dreele, R. B., Cox, D. E., Louer, D. and Scardi, P. (1999). “Rietveld refinement guidelines,” J. Appl. Crystallogr. 32, 36–50.CrossRefGoogle Scholar
Neira, I. S., Kolen'ko, Y. V., Lebedev, O. I., Van Tendeloo, G., Gupta, H. S., Guitián, F. and Yoshimura, M. (2009). “An effective morphology control of hydroxyapatite crystals via hydrothermal synthesis,” Cryst. Growth. Des. 9, 466–474.Google Scholar
Neuman, W. F. and Mulryan, B. J. (1971). “Synthetic hydroxyapatite crystals IV. Magnesium incorporation,” Calcif. Tissue Res. 7, 133–138.Google Scholar
Nilen, R. W. N. and Richter, P. W. (2008). “The thermal stability of hydroxyapatite in biphasic calcium phosphate ceramics,” J. Mater. Sci.: Mater. Med. 19, 1693–1702.Google ScholarPubMed
Raynaud, S., Champion, E., Bernache-Assolant, D. and Laval, J.-P. (2001). “Determination of calcium/phosphorus atomic ratio of calcium phosphate apatites using X-ray diffractometry,” J. Am. Ceram. Soc. 84, 359–366.CrossRefGoogle Scholar
Raynaud, S., Champion, E., Bernache-Assollant, D. and Thomas, P. (2002a). “Calcium phosphate apatites with variable Ca/P atomic ratio I. Synthesis, characterisation and thermal stability of powders,” Biomaterials 23, 1065–1072.Google Scholar
Raynaud, S., Champion, E. and Bernache-Assollant, D. (2002b). “Calcium phosphate apatites with variable Ca/P atomic ratio II. Calcination and sintering,” Biomaterials 23, 1073–1080.Google Scholar
Reid, J. W. and Hendry, J. A. (2006). “Rapid, accurate phase quantification of multiphase calcium phosphate materials using Rietveld refinement,” J. Appl. Crystallogr. 39, 536–543.Google Scholar
Riboud, P. V. (1973). “Composition et stabilité des phases a structure d'apatite dans le système CaO-P2O5-oxyde de Fer-H2O a haute temperature,” Ann. Chim. 8, 381–390.Google Scholar
Rietveld, H. M. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Crystallogr. 2, 65–71.Google Scholar
Schroeder, L. W., Dickens, B. and Brown, W. E. (1977). “Crystallographic studies of the role of Mg as a stabilizing impurity in β-Ca3(PO4)2 II. Refinement of Mg-containing β-Ca3(PO4)2 ,” J. Solid State Chem. 22, 253–262.Google Scholar
Stutzman, P. (2005). “Powder diffraction analysis of hydraulic cements: ASTM Rietveld round-robin results on precision,” Powder Diffr. 20, 97–100.CrossRefGoogle Scholar
Sudarsanan, K. and Young, R. A. (1969). “Significant precision in crystal structure details: Holly springs hydroxyapatite,” Acta Crystallogr. B25, 1534–1543.Google Scholar
Tõnsuaadu, K., Gross, K. A., Plusuma, L. and Veiderma, M. (2012). “A review on the thermal stability of calcium apatites,” J. Therm. Anal. Calorim. 110, 647–659.CrossRefGoogle Scholar
Toth, J. M., Hirthe, W. M., Hubbart, W. G., Brantley, W. A. and Lynch, K. L. (1991). “Determination of the ratio of HA/TCP mixtures by x-ray diffraction,” J. Appl. Biomater. 2, 37–40.Google Scholar
Welch, J. H. and Gutt, W. (1961). “High-temperature studies of the system calcium oxide-phosphorus pentoxide,” J. Chem. Soc. 874, 4442–4444.Google Scholar
Wilson, R. M., Elliott, J. C., Dowker, S. E. P. and Rodriguez-Lorenzo, L. M. (2005). “Rietveld refinements and spectroscopic studies of the structure of Ca-deficient apatite,” Biomaterials 26, 1317–1327.Google Scholar