ASTM F1609-08(2014)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: F1609 − 08 (Reapproved 2014)
Standard Specification for
Calcium Phosphate Coatings for Implantable Materials
This standard is issued under the fixed designation F1609; 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 2. Referenced Documents
1.1 This specification covers the material requirements for 2.1 ASTM Standards:
calcium phosphate coatings for surgical implant applications. E376 Practice for Measuring Coating Thickness by
Magnetic-Field or Eddy Current (Electromagnetic) Test-
1.2 In particulate and monolithic form, the calcium phos-
ing Methods
phate materials system has been well-characterized regarding
F1044 Test Method for Shear Testing of Calcium Phosphate
biological response (1,2) and laboratory characterization (2-
Coatings and Metallic Coatings
4). Several publications (5-10) have documented the in vitro
F1088 Specification for Beta-Tricalcium Phosphate for Sur-
and in vivo properties of selected calcium phosphate coating
gical Implantation
systems.
F1147 Test Method for Tension Testing of Calcium Phos-
1.3 This specification includes hydroxylapatite coatings,
phate and Metallic Coatings
tricalcium phosphate coatings, or combinations thereof, with or
F1160 Test Method for Shear and Bending Fatigue Testing
without intentional minor additions of other ceramic or
of Calcium Phosphate and Metallic Medical and Compos-
metallic, and applied by methods including, but not limited to,
ite Calcium Phosphate/Metallic Coatings
the following: (1) mechanical capture, (2) plasma spray
F1185 Specification for Composition of Hydroxylapatite for
deposition, (3) dipping/sintering, (4) electrophoretic
Surgical Implants
deposition, (5) porcelainizing, and (6) sputtering.
F1854 Test Method for Stereological Evaluation of Porous
1.4 Substrates may include smooth, porous, textured, and
Coatings on Medical Implants
other implantable topographical forms.
F1926 Test Method for Dissolution Testing of Calcium
Phosphate Granules, Fabricated Forms, and Coatings
1.5 This specification excludes organic coatings that may
F2024 Practice for X-ray Diffraction Determination of Phase
contain calcium and phosphate ionic species.
Content of Plasma-Sprayed Hydroxyapatite Coatings
1.6 Warning—Mercury has been designated by EPA and
2.2 Pharmacopeia Convention Documents:
many state agencies as a hazardous material that can cause
National Formulary XVI, Tribasic Calcium Phosphate
central nervous system, kidney, and liver damage. Mercury, or
United States Pharmacopeia:
its vapor, may be hazardous to health and corrosive to
U.S. Pharmacopeia (most current), Chemical Tests: Calcium
materials. Caution should be taken when handling mercury and
(191), Phosphorous (191), Lead <251>, Mercury <261>,
mercury-containing products. See the applicable product Ma-
Arsenic < 211>, and Heavy Metals <231> Method (1)
terial Safety Data Sheet (MSDS) for details and EPA’s website
2.3 Other Documents:
(http://www.epa.gov/mercury/faq.htm) for additional informa-
U.S. Geological Survey Method, Cadmium
tion. Users should be aware that selling mercury or mercury-
U.S. Code of Federal Regulations Title 21 (CFR 21), Part
containing products, or both, in your state may be prohibited by
820–Quality System Regulation
state law.
1 4
This specification is under the jurisdiction of ASTM Committee F04 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Medical and Surgical Materials and Devicesand is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee F04.13 on Ceramic Materials. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved March 1, 2014. Published March 2014. Originally the ASTM website.
approved in 1995. Last previous edition approved in 2008 as F1609 – 08. DOI: Available from U.S. Pharmacopeia (USP), 12601 Twinbrook Pkwy., Rockville,
10.1520/F1609-08R14. MD 20852-1790, http://www.usp.org.
2 6
The boldface numbers in parentheses refer to the list of references at the end of Crock, J. G., Felichte, F. E., and Briggs, P. H., “Determination of Elements in
this specification. National Bureau of Standards Geological Reference Materials SRM 278 Obsidian
The Joint Committee on Powdered Diffraction has established a Powder and SRM 688 Basalt by Inductively Coupled Argon Plasma—Atomic Emission
Diffraction File. The committee operates on an international basis and cooperates Spectrometry,” Geostandards Newsletter, Vol 7, 1983, pp. 335–340.
closely with the Data Commission of the International Union of Crystallinity and Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
ASTM. Hydroxylapatite data can be found on file card No. 9-432; beta tricalcium Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
phosphate data can be found on file card No. 9-169. dodssp.daps.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1609 − 08 (2014)
X-Ray Diffraction Analyses 5. Physical Characterization
5.1 Coverage of Substrate:
3. Terminology
5.1.1 Microscopic examination of the surface will be made
3.1 Definitions: at 10× magnification; “bare” areas, “pinholes,” cracking, for-
3.1.1 amorphous calcium phosphate—a non-crystalline cal- eign debris, unmelts, chips, delamination and the appearance at
cium phosphate. the coating/substrate interface, and so forth shall be reported.
3.1.2 beta tricalcium phosphate—a calcium phosphate sub- 5.2 Thickness—The thickness shall be measured from cross
stance of empirical chemical formula, Ca (PO ) (see Specifi-
sections in accordance with Test Method F1854. If distinct
3 4 2
cation F1088). layers exist, they should be reported.
5.2.1 Alternatively, a magnetic field or eddy current tech-
3.1.3 calcium phosphate—any one of a number of inorganic
nique may be used if it has been shown to be equivalent to Test
chemical compounds containing calcium and phosphate ions as
Method F1854.
its principal constituents.
5.3 Porosity—The microporosity and macroporosity charac-
3.1.4 coating—a layer of mechanically or chemically at-
terization shall be determined in accordance with Test Method
tached material covering a substrate material.
F1854.
3.1.5 hydroxylapatite—a calcium phosphate crystalline
5.4 Color—A macroscopic examination of color should be
compound of empirical chemical formula, Ca (PO ) OH (see
5 4 3
performed to guarantee a uniform and consistent appearance,
Specification F1185).
in consideration of the specific process, substrate material and
geometry, and coating thickness.
4. Chemical or Crystallographic Requirements, or Both
5.5 Surface Topography—The surface topography shall be
4.1 Chemical:
measured using equipment designed to determine surface
4.1.1 Elemental analysis for calcium and phosphorous and
roughness. Characterization of the surface topography of the
intentional additions (other than trace elements) shall be
underlying substrate may be required, if applicable, for the
consistent with the expected stoichiometry of the specific
specific coating method. Scanning electron microscopy shall
calcium phosphate compound(s).
be used to provide a visual representation of the coating surface
4.1.2 Trace Element Analysis for Hydroxylapatite and Beta
characteristics.
Tricalcium Phosphate—The concentration of trace elements in
the coating shall be limited as follows: 5.6 Density—Density of both the powder and coated forms
shall be performed using a suitable method.
Element ppm, max
As 3
Cd 5
6. Mechanical Characterization
Hg 5
Pb 30
6.1 The following mechanical characterizations may be
total heavy metals (as lead) 50
applicable to a coating, depending on the substrate material or
For reference purposes, the U.S. Pharmacopeia (most cur-
geometry, coating thickness or location, or coating method(s).
rent) and U.S. Geological Survey Method, Cadmium, shall be
Characterization reports shall contain sufficient information
used.
regarding the test techniques, procedures, and standards used
4.1.3 The analysis of other trace elements may be required,
and details such as specimen orientation and proportional d
...