ASTM F1609-95
(Specification)Standard Specification for Calcium Phosphate Coatings for Implantable Materials
Standard Specification for Calcium Phosphate Coatings for Implantable Materials
SCOPE
1.1 This specification covers the material requirements for calcium phosphate coatings for surgical implant applications.
1.2 In particulate and monolithic form, the calcium phosphate materials system has been well-characterized regarding biological response (1, 2) and laboratory characterization (2-4). Several publications (5-10) have documented the in vitro and in vivo properties of selected calcium phosphate coating systems.
1.3 This specification includes hydroxylapatite coatings, tricalcium phosphate coatings, or combinations thereof, with or without intentional minor additions (10% or less, as opposed to trace elements) of other ceramic or metallics, and applied by methods including, but not limited to, the following: ( ) mechanical capture, ( ) plasma spray deposition, ( ) dipping/sintering, ( ) electrophoretic deposition, ( ) porcelainizing, and ( ) sputtering.
1.4 Substrates may include smooth, porous, textured, and other implantable topographical forms.
1.5 This specification excludes organic coatings that may contain calcium and phosphate ionic species.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: F 1609 – 95
Standard Specification for
Calcium Phosphate Coatings for Implantable Materials
This standard is issued under the fixed designation F 1609; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Magnetic-Field or Eddy-Current (Electromagnetic) Test
Methods
1.1 This specification covers the material requirements for
F 1044 Test Method for Shear Testing of Porous Metal
calcium phosphate coatings for surgical implant applications.
Coatings
1.2 In particulate and monolithic form, the calcium phos-
F 1088 Specification for Beta-Tricalcium Phosphate for
phate materials system has been well-characterized regarding
Surgical Implantation
biological response (1, 2) and laboratory characterization
F 1147 Test Method for Tension Testing of Porous Metal
(2–4). Several publications (5–10) have documented the in
Coatings
vitro and in vivo properties of selected calcium phosphate
F 1185 Specification for Composition of Ceramic Hydroxy-
coating systems.
lapatite for Surgical Implants
1.3 This specification includes hydroxylapatite coatings,
2.2 Pharmacopeia Convention Documents:
tricalcium phosphate coatings, or combinations thereof, with or
National Formulary XVI, Tribasic Calcium Phosphate
without intentional minor additions (10 % or less, as opposed
United States Pharmacopeia:
to trace elements) of other ceramic or metallics, and applied by
U.S. Pharmacopeia XXI, Chemical Tests CaP (191), Lead
methods including, but not limited to, the following: (1)
<251>, Mercury <261>, Arsenic< 211>, and Heavy Met-
mechanical capture, (2) plasma spray deposition, (3) dipping/
als <231> Method (1)
sintering, (4) electrophoretic deposition, (5) porcelainizing,
2.3 Other Documents:
and (6) sputtering.
U.S. Geological Survey Method, Cadmium
1.4 Substrates may include smooth, porous, textured, and
21 CFR 820
other implantable topographical forms.
X-Ray Diffraction Analyses
1.5 This specification excludes organic coatings that may
contain calcium and phosphate ionic species.
3. Terminology
2. Referenced Documents 3.1 Definitions:
3.1.1 beta tricalcium phosphate—a calcium phosphate sub-
2.1 ASTM Standards:
stance of empirical chemical formula, Ca (PO ) (see Specifi-
3 4 2
C 313 Test Method for Adherence of Porcelain Enamel and
cation F 1088).
Ceramic Coatings to Sheet Metal
3.1.2 calcium phosphate—any one of a number of inorganic
C 501 Test Method for Relative Resistance to Wear of
chemical compounds containing calcium and phosphate ions as
Unglazed Ceramic Tile by the Taber Abraser
its principal constituents.
C 633 Test Method for Adhesion or Cohesive Strength of
3.1.3 coating—a layer of mechanically or chemically at-
Flame-Sprayed Coatings
tached material covering a substrate material.
C 674 Test Methods for Flexural Properties of Ceramic
Whiteware Materials
C 949 Test Method for Porosity in Vitreous Whitewares by
Annual Book of ASTM Standards, Vol 03.03.
Dye Penetration
Annual Book of ASTM Standards, Vol 13.01.
E 376 Practice for Measuring Coating Thickness by
Available from U.S. Pharmacopeia Convention, Inc., 12601 Twinbrook Park-
way, Rockville, MD 20852.
Crock, J. G., Felichte, F. E., and Briggs, P. H., “Determination of Elements in
National Bureau of Standards Geological Reference Materials SRM 278 Obsidian
This specification is under the jurisdiction of ASTM Committee F04 on and SRM 688 Basalt by Inductively Coupled Argon Plasma—Atomic Emission
Medical and Surgical Materials and Devices and is the direct responsibility of Spectrometry,” Geostandards Newsletter, Vol 7, 1983, pp. 335–340.
Subcommittee F04.13 on Ceramic Materials. Available from Standardization Documents Order Desk, Bldg. 4 Section D,
Current edition approved Aug. 15, 1995. Published September 1995. 700 Robbins Ave., Philadelphia, PA 19111-5098, Attn: NPODS.
2 11
The boldface numbers in parentheses refer to the list of references at the end of The Joint Committee on Powdered Diffraction has established a Powder
this specification. Diffraction File. The committee operates on an international basis and cooperates
Discontinued 1991—See 1990 Annual Book of ASTM Standards, Vol 15.02. closely with the Data Commission of the International Union of Crystallinity and
Annual Book of ASTM Standards, Vol 15.02. ASTM. Hydroxylapatite data can be found on file card No. 9-432; beta tricalcium
Annual Book of ASTM Standards, Vol 02.05. phosphate data can be found on file card No. 9-169.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
F 1609
3.1.4 hydroxylapatite—A calcium phosphate crystalline may be required if applicable for the specific coating method.
compound of empirical chemical formula, Ca (PO ) OH (see Scanning electron microscopy shall be used to establish the
5 4 3
Specification F 1185). coating surface and cross-section morphology.
5.6 Other Characterizations—Other characterizations may
4. Chemical or Crystallographic Requirements, or Both
be required or applicable, depending on the end-use applica-
4.1 Chemical:
tion. Standard test methods should be used in all cases, where
4.1.1 Elemental analysis for calcium and phosphorous and
available, or acceptable alternatives developed. An additional
intentional additions (other than trace elements) will be con-
ASTM test that may apply is Test Methods C 674.
sistent with the expected stoichiometry of the specific calcium
phosphate compound(s).
6. Mechanical Characterization
4.1.2 Trace Element Analysis—The concentration of trace
6.1 The following mechanical characterizations may be
elements in the coating shall be limited as follows:
applicable to a coating, depending on the substrate material or
Element ppm, max
geometry, coating thickness or location, and coating meth-
As 3
Cd 5 ods(s), or some combination thereof. Characterization reports
Hg 5
shall contain sufficient information regarding the test tech-
Pb 30
niques, procedures, and standards used and details such as
total heavy metals (as lead) 50
specimen orientation and proportional depth of thickness in
For reference purposes, the U.S. Pharmacopeia XXI and U.S.
order to represent the analysis accurately.
Geological Survey Method, Cadmium, shall be used.
6.1.1 The tensile bond strength of the coating to the sub-
4.1.3 The analysis of other trace elements may be required,
strate shall be measured using a non-penetrating adhesive such
based on the conditions, apparatus, or environments specific to
as FM-1000 Adhesive Film. The measurement technique shall
the coating application technique used.
follow the general procedure of Test Methods C 633 and
4.1.4 The analysis of intentional additional elements or
F 1147. The tensile test shall be considered invalid if any
compounds such as fluorine, manganese, magnesium, carbon-
portion of the metal substrate is exposed to the surface before
ate, etc. must be specified for calcium phosphate coatings.
testing, allowing direct bonding of the adhesive to the metal.
4.2 Crystallographic Characterization:
6.1.2 Shear strength determinations shall be consistent with
4.2.1 This involves the degree of crystallinity, determined as
Test Method F 1044, or a demonstrated equivalent technique,
a weight percent of the total substance.
as long as the adhesive is demonstrated to be non-penetrating
4.2.2 This involves the identification of crystalline species
and the test technique allows for the coating to be placed in a
and their weight percentages, expressed as a percent of the total
pure shear condition, minimizing “peeling stress” modes.
substance.
6.1.3 The fatigue strength shall be determined on an appli-
4.2.3 This involves the identification of functional groups
cable full-scale device and as a materials system using appro-
by infrared analysis.
priate testing methods applicable to the various service condi-
4.3 Environmental Stab
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