ASTM F2024-10
(Practice)Standard Practice for X-ray Diffraction Determination of Phase Content of Plasma-Sprayed Hydroxyapatite Coatings
Standard Practice for X-ray Diffraction Determination of Phase Content of Plasma-Sprayed Hydroxyapatite Coatings
SIGNIFICANCE AND USE
Calcium phosphate coatings have been shown in animal and clinical studies to be biocompatible and to enhance the early attachment of bone to implant surfaces (see Refs. 1-5)
It is believed that the form of calcium phosphate ceramic and its purity with respect to secondary crystalline phases and amorphous material have an effect on its physical, mechanical, and biological properties. However, no definitive studies of effects on biological properties have been completed. To achieve reproducible clinical results and to permit the determination of the effects of properties of the coating on biological performance, it is essential that the properties of both clinical and experimental materials be well-characterized and consistent.
This practice provides procedures for determination of the percentage by weight of the crystalline phases identified as hydroxyapatite, β-TCP and CaO in plasma-sprayed hydroxyapatite coatings.
SCOPE
1.1 This practice is for the determination, by the Reference Intensity Ratio External Standard Method, of the percent by weight of the crystalline phases, hydroxyapatite (HA), beta-(whitlockite) tricalcium phosphate (β-TCP), and calcium oxide (CaO) in coatings deposited upon metallic substrates by plasma-spraying hydroxyapatite.
1.2 A major component in plasma-sprayed HA coatings other than HA is expected to be amorphous calcium phosphate (ACP). Crystalline components other than HA that may be present include alpha- and beta- (whitlockite) tricalcium phosphates, tetracalcium phosphate (TTCP), calcium oxide, and calcium pyrophosphates. Quantification of the minor crystalline components has proven to be very unreliable due to extreme overlap and confounding of X-ray diffraction peaks. Therefore, this practice addresses the quantification of only HA, β-TCP, and CaO.
1.3 This practice was developed for plasma-sprayed HA coatings with HA contents of at least 50 % of the total coating. It is recognized that the analysis of the crystalline components uses diffraction from regions of the pattern that also includes a small contribution from the amorphous component. However, within the limits of applicability of this practice, the effect of such interference is believed to be negligible.
1.4 The coating analyzed shall be produced and processed under equivalent manufacturing conditions to that on the device of interest.
1.5 This practice requires the use of monochromated copper Kα radiation and flat samples.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: F2024 − 10
StandardPractice for
X-ray Diffraction Determination of Phase Content of Plasma-
1
Sprayed Hydroxyapatite Coatings
This standard is issued under the fixed designation F2024; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
1.1 This practice is for the determination, by the Reference
bility of regulatory limitations prior to use.
Intensity Ratio External Standard Method, of the percent by
weight of the crystalline phases, hydroxyapatite (HA), beta-
2. Terminology
(whitlockite) tricalcium phosphate (β-TCP), and calcium oxide
(CaO) in coatings deposited upon metallic substrates by
2.1 Definitions:
plasma-spraying hydroxyapatite.
2.1.1 crystalline phases:
1.2 A major component in plasma-sprayed HA coatings
2
Chemical and Mineral Formula PDF Card No.
other than HAis expected to be amorphous calcium phosphate Names
(ACP). Crystalline components other than HA that may be
whitlockite β-Ca (PO ) 9-169
3 4 2
present include alpha- and beta- (whitlockite) tricalcium
beta-tricalcium phosphate
phosphates, tetracalcium phosphate (TTCP), calcium oxide,
calcium phosphate α-Ca (PO ) 9-348
3 4 2
and calcium pyrophosphates. Quantification of the minor
alpha-tricalcium phosphate
crystalline components has proven to be very unreliable due to
lime CaO 37-1497
extreme overlap and confounding of X-ray diffraction peaks.
calcium oxide
Therefore, this practice addresses the quantification of only
HA, β-TCP, and CaO.
hydroxyapatite Ca (PO ) OH 9-432
5 4 3
(hydroxylapatite)
1.3 This practice was developed for plasma-sprayed HA
2.2 plasma-sprayed hydroxyapatite coating—a coating,
coatings with HAcontents of at least 50 % of the total coating.
consisting of at least 50 % hydroxyapatite by weight, prepared
It is recognized that the analysis of the crystalline components
by plasma-spraying hydroxyapatite on a substrate.
uses diffraction from regions of the pattern that also includes a
small contribution from the amorphous component. However,
3. Significance and Use
within the limits of applicability of this practice, the effect of
such interference is believed to be negligible.
3.1 Calcium phosphate coatings have been shown in animal
1.4 The coating analyzed shall be produced and processed
and clinical studies to be biocompatible and to enhance the
3
under equivalent manufacturing conditions to that on the
early attachment of bone to implant surfaces (see Refs. 1-5)
device of interest.
3.2 It is believed that the form of calcium phosphate
1.5 This practice requires the use of monochromated copper
ceramic and its purity with respect to secondary crystalline
Kα radiation and flat samples.
phases and amorphous material have an effect on its physical,
mechanical, and biological properties. However, no definitive
1.6 The values stated in SI units are to be regarded as
studiesofeffectsonbiologicalpropertieshavebeencompleted.
standard. No other units of measurement are included in this
To achieve reproducible clinical results and to permit the
standard.
determination of the effects of properties of the coating on
1.7 This standard does not purport to address all of the
biological performance, it is essential that the properties of
safety concerns, if any, associated with its use. It is the
both clinical and experimental materials be well-characterized
and consistent.
1
ThispracticeisunderthejurisdictionofASTMCommitteeF04onMedicaland
Surgical Materials and Devices and is the direct responsibility of Subcommittee
F04.13 on Ceramic Materials.
2
Current edition approved June 1, 2010. Published June 2010. Originally Joint Committee on Powder Diffraction Standards, Swarthmore, PA.
3
approved in 2000. Last previous edition approved in 2000 as F2024–00 which was The boldface numbers in parentheses refer to the list of references at the end of
withdrawn in January 2009 and reinstated in June 2010. DOI: 10.1520/F2024–10. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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F2024 − 10
3.3 This practice provides procedures for determination of overlapping peaks, a diffracted beam monochromator is re-
the percentage by weight of the crystalline phases identified as quired unless a solid-state detector is used. Linearity of the
hydroxyapatite, β-TCP and CaO in plasma-sprayed hydroxy- instrument and associated electronics must be verified daily
apatite coatings. prior
...
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