ASTM F1581-99

Standard Specification for Composition of Anorganic Bone for Surgical Implants

SCOPE
1.1 This specification covers material requirements for anorganic xenogeneic or allogeneic bone (hydroxylapatite) intended for surgical implants. For a material to be called anorganic or deorganified bone, it must conform to this specification (see Appendix XI).  
1.2 The biological response to hydroxylapatite in soft tissue and bone has been characterized by a history of clinical use (1, 2, 3, 4, 5)  and by laboratory studies (6, 7, 8). Xenogeneic bone, due to its organic component, has been shown to be antigenic in the human host (9) whereas the same material that has been completely deorganified has been shown to elicit no inflammatory or foreign body reactions in human clinical use (10, 11).  
1.3 This specification specifically excludes synthetic hydroxylapatite, hydroxylapatite coatings, ceramic glasses, tribasic calcium phosphate, whitlockite, and alpha- and beta-tricalcium phosphate.

General Information

• Status: Historical
• Publication Date: 09-Feb-1999
• ICS: 11.040.40 - Implants for surgery, prosthetics and orthotics
• Technical Committee: F04 - Medical and Surgical Materials and Devices
• Drafting Committee: F04.13 - Ceramic Materials

Relations

• Replaced By: ASTM F1581-08 - Standard Specification for Composition of Anorganic Bone for Surgical Implants
• Effective Date: 01-Feb-2008
• Referred By: ASTM F2027-16 - Standard Guide for Characterization and Testing of Raw or Starting Materials for Tissue-Engineered Medical Products
• Effective Date: 10-Feb-1999

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: F 1581 – 99
Standard Specification for
Composition of Anorganic Bone for Surgical Implants
This standard is issued under the fixed designation F 1581; 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 High Temperature Oxidation and Coulometric Detection
E 1184 Practice for Electrothermal (Graphite Furnace)
1.1 This specification covers material requirements for an-
Atomic Absorption Analysis
organic xenogeneic or allogeneic bone (apatite) intended for
F 748 Practice For Selecting Generic Biological Test Meth-
surgical implants. For a material to be called anorganic or
ods for Materials and Devices
deorganified bone, it must conform to this specification (see
F 1185 Specification for Composition of Ceramic Hydroxy-
Appendix X1).
lapatite for Surgical Implants
1.2 Thebiologicalresponsetoapatiteinsofttissueandbone
2 2.2 Code of Federal Regulations:
has been characterized by a history of clinical use and by
Title 21, Part 820
laboratory studies (1,2,3). Xenogeneic bone, with organic
2.3 National Formulary:
components present, has been shown to be antigenic in the
Tribasic Calcium Phosphate
human host (4) whereas the same material that has been
2.4 United States Pharmocopeia:
completely deorganified has been shown to elicit no inflam-
Identification Tests for Calcium and Phosphate <191>
matory or foreign body reactions in human clinical use (5, 6,
Lead <251>
7).
Mercury <261>
1.3 This specification specifically excludes synthetic hy-
Cadmium <461>
droxylapatite, hydroxylapatite coatings, ceramic glasses, triba-
Arnsenic <211>
sic calcium phosphate, whitlockite, and alpha- and beta-
Heavy Metals <231> Method 1
tricalcium phosphate.
Nitrogen Determination <4617>
1.4 This standard does not pruport to address all of the
2.5 U.S. Geological Survey Method:
safety concerns, such as health concerns due to the presence of
Cadmium
transmissible disease, associated with its use. It is the respon-
sibility of the user of this standard to establish appropriate
3. Terminology
safety and health practices and determine the applicability of
3.1 Definitions:
regulatory limitations prior to use.(See Appendix X2).
3.1.1 allogeneic, adj—derived from different individuals of
2. Referenced Documents the same species.
3.1.2 anorganic, adj—denoting tissue (for example, bone)
2.1 ASTM Standards:
from which the organic material has been totally removed.
D 513 Test Methods for Total and Dissolved Carbon Diox-
Also referred to as deorganified, deproteinized or deprotein-
ide in Water
3 ated.
D 1688 Test Methods for Copper in Water
3.1.3 apatite, n—the mineral substance having the molecu-
D 2972 Test Methods for Arsenic in Water
3 lar formula Ca (X) (PO ) where X=OH (hydroxyapatite or
D 3557 Test Methods for Cadmium in Water 10 2 4 6
hydroxylapatite), CO (carbonated apatite), F or C1 (8).
D 3559 Test Methods for Lead in Water
D 3919 Practice for Measuring Trace Elements in Water by
Graphite Furnace Atomic Absorption Spectrophotometry
Annual Book of ASTM Standards, Vol. 11.02.
D 4129 Test Method for Total and Organic Carbon in Water
Annual Book of ASTM Standards, Vol. 03.06.
Annual Book of ASTM Standards, Vol. 13.01.
AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
1 8
This specification is under the jurisdiction of ASTM Committee F04 on National Formulary XVI.Available from U.S. Pharmacopeia Convention, Inc.,
Medical and Surgical Materials and Devices and is under the direct responsibility of 12601 Twinbrook Parkway, Rockville, MD 20852.
Subcommittee F04.13 . United States Pharmacopeia XXI.Available from U.S. Pharmacopeia Conven-
Current edition approved Feb. 10, 1999. Published June 1999. Originally tion, Inc., 12601 Twinbrook Parkway, Rockville, MD 20852.
published as F 1581 – 95. Last previous edition F 1581 – 96. Crock, J. G., Felichte, F. E., and Briggs, P. H., “Determination of Elements in
The boldface numbers in parentheses refer to the list of references at the end of National Bureau of Standards Geological Reference Materials SRM 278 Obsidian
this specification. and SRM 688 Basalt by Inductively Coupled Argon Plasma—Atomic Emission
Annual Book of ASTM Standards, Vol. 11.01. Spectrometry.” Geostandards Newsletter, Vol 7, 1983, pp. 335–340.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F1581–99
NOTE 1—The Kjeldahl process for nitrogen determination (USP
3.1.4 xenogeneic, adj—derived from individuals of a differ-
<461>) is set forth by theAssociation of OfficialAnalytical Chemists(12)
ent, specified species. For example, bovine bone, when used as
as an appropriate measure of proteins. Alternatively, organic material
an implant material in humans, is xenogeneic.
(carbon) can be measured by the coulometric method (Test Method
D 4129). Subtract from this value the carbonate content, which can be
4. Chemical Requirements
determined by Test Methods D 513.
4.1 Elemental analysis for calcium and phosphorus will be
4.7 Functionalgroupswillbeidentifiedbyinfraredanalysis.
consistent with the expected composition of the source of the
Typical functional groups of apatites have been described by
biologically derived bone mineral (9).
Elliott (8), LeGeros et al (14), and Rey (15,16,17).
4.2 An X-ray diffraction analysis of the material shall be
4.8 Analysis of additional elements or ionic species associ-
consistent with PDF card #9-432 for hydroxyapatite (10) or
ated with the source or with processing conditions should be
PDF card #35–180 for calcium phosphate carbonate (carbon-
specified for this material.
ated apatite). Analysis of relative peak intensities shall be
consistent with published data.
5. Test Specimen Fabrication
4.3 The concentration of trace elements in the anorganic
5.1 Prepare test specimens from the same batch of material
bone shall be limited as follows:
and by the same processes as those employed in fabricating the
Element ppm, max
implant device.
As 3
Cd 5
Hg 5
6. Quality Program Requirements
Pb 30
6.1 ThemanufacturershallconformtoGoodManufacturing
total heavy metals (as lead) 50
Practices (see Title 21, Part 820, of the Code of Federal
For referee purposes, use either inductively coupled plasma/
Regulations ) or its equivalent.
mass spectroscopy (ICP/MS) (11) or the United States Phar-
mocopeia (USP) methods <191>, <251>, <261>, <211>,
7. Biocompatibility
<231> Method 1, < 4617> and for cadmium either <461> or
7.1 The biocompatibility of anorganic bone may depend
the U.S. Geological Survey Method on Cadmium. (See 2.4 and
upon processing conditions or source material history, or both,
2.5). Graphite furnace atomic absorption spectrophotometry
which may not be identified by the compositional requirements
may also be used for ananlysis of trace elements using (Test
of this specification. The biocompatibility of these products
MethodsD 2972),Cd(TestMethodD 1688),Pb(TestMethods
should be ensured by a combination of preclinical testing and
D 3559) with 1 g anorganic bone/100mL H O samples. G
process controls. Material derived under the desired process
eneral guides for the application of the graphite furnace are
conditions should be tested in accordance with the recommen-
given in Practices D 3919 and E 1184.
dations of Practice F 748 and manufacturing controls put in
4.4 The maximum allowable limit of all heavy metals
place to ensure that process variations outside o
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