ASTM F2224-09(2020)
(Specification)Standard Specification for High Purity Calcium Sulfate Hemihydrate or Dihydrate for Surgical Implants
Standard Specification for High Purity Calcium Sulfate Hemihydrate or Dihydrate for Surgical Implants
ABSTRACT
This specification covers unfabricated and fabricated forms of high purity hydrated calcium sulfate hemihydrate or dihydrate for surgical implants. The requirements of this specification apply to calcium sulfate combined with two molecules of water or two calcium sulfate molecules with one water mole but does not include calcium sulfate anhydrite and calcium sulfate forms that contain reinforcing phases, medicaments, biological agents, and other such additives. All covered materials should conform to the requirements for set time, compressive strength, and in vitro degradation.
SCOPE
1.1 This specification covers material requirements for unfabricated and fabricated forms of hydrated calcium sulfate intended for surgical implants. Fabricated forms may include pressed and cast surgical implants in various geometric shapes. The calcium sulfate hemihydrate in the unfabricated form can be converted with the addition of water or other water-containing solutions to a fabricated calcium sulfate dihydrate form.
1.2 The requirements of this specification apply to calcium sulfate combined with two molecules of water or two calcium sulfate molecules sharing one water molecule.
Approximate chemical formulae:
Calcium Sulfate Dihydrate
CaSO4·2H2O
Calcium Sulfate Hemihydrate
CaSO4·1/2H2O or CaSO4·H2O·CaSO4
1.3 This specification specifically excludes calcium sulfate anhydrite and calcium sulfate forms that contain additives such as reinforcing phases, medicaments, biological agents, and so forth.
1.4 The presence of processing aids does not exclude a product from the physical and mechanical requirements of this specification.
1.5 Some provisions of Specification C59/C59M and Test Methods C472 apply. Special requirements that are detailed in this specification are included to characterize the material which will be used in surgical implants.
1.6 The biological response to calcium sulfate in bone tissue has been well characterized by a history of clinical use (1-14)2 and by laboratory studies (15-18).
1.7 The following precautionary caveat pertains only to the test method portion, Sections 4, 5, and 6, of this specification. 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: F2224 −09 (Reapproved 2020)
Standard Specification for
High Purity Calcium Sulfate Hemihydrate or Dihydrate for
Surgical Implants
This standard is issued under the fixed designation F2224; 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 This standard does not purport to address all of the safety
concerns, if any, associated with its use. It is the responsibility
1.1 This specification covers material requirements for un-
of the user of this standard to establish appropriate safety,
fabricated and fabricated forms of hydrated calcium sulfate
health, and environmental practices and determine the appli-
intended for surgical implants. Fabricated forms may include
cability of regulatory limitations prior to use.
pressed and cast surgical implants in various geometric shapes.
1.8 This international standard was developed in accor-
The calcium sulfate hemihydrate in the unfabricated form can
dance with internationally recognized principles on standard-
be converted with the addition of water or other water-
ization established in the Decision on Principles for the
containing solutions to a fabricated calcium sulfate dihydrate
Development of International Standards, Guides and Recom-
form.
mendations issued by the World Trade Organization Technical
1.2 The requirements of this specification apply to calcium
Barriers to Trade (TBT) Committee.
sulfate combined with two molecules of water or two calcium
sulfate molecules sharing one water molecule.
2. Referenced Documents
Approximate chemical formulae:
2.1 ASTM Standards:
Calcium Sulfate Dihydrate
C59/C59M Specification for Gypsum Casting Plaster and
CaSO ·2H O
4 2
Gypsum Molding Plaster
Calcium Sulfate Hemihydrate
C472 Test Methods for Physical Testing of Gypsum, Gyp-
CaSO ·1/2H O or CaSO ·H O·CaSO
4 2 4 2 4
sum Plasters, and Gypsum Concrete
1.3 This specification specifically excludes calcium sulfate
F648 Specification for Ultra-High-Molecular-Weight Poly-
anhydrite and calcium sulfate forms that contain additives such
ethylene Powder and Fabricated Form for Surgical Im-
as reinforcing phases, medicaments, biological agents, and so
plants
forth.
F756 Practice for Assessment of Hemolytic Properties of
Materials
1.4 The presence of processing aids does not exclude a
product from the physical and mechanical requirements of this F763 Practice for Short-Term Screening of Implant Materi-
als
specification.
F813 Practice for Direct Contact Cell Culture Evaluation of
1.5 Some provisions of Specification C59/C59M and Test
Materials for Medical Devices
Methods C472 apply. Special requirements that are detailed in
F895 TestMethodforAgarDiffusionCellCultureScreening
this specification are included to characterize the material
for Cytotoxicity
which will be used in surgical implants.
F981 Practice for Assessment of Compatibility of Biomate-
1.6 Thebiologicalresponsetocalciumsulfateinbonetissue
rials for Surgical Implants with Respect to Effect of
has been well characterized by a history of clinical use (1-14)
Materials on Muscle and Insertion into Bone
and by laboratory studies (15-18).
F1088 Specification for Beta-Tricalcium Phosphate for Sur-
1.7 The following precautionary caveat pertains only to the gical Implantation
test method portion, Sections 4, 5, and 6, of this specification. F1635 Test Method for in vitro Degradation Testing of
HydrolyticallyDegradablePolymerResinsandFabricated
Forms for Surgical Implants
This specification is under the jurisdiction of ASTM Committee F04 on
Medical and Surgical Materials and Devices and is the direct responsibility of
Subcommittee F04.13 on Ceramic Materials.
Current edition approved Aug. 1, 2020. Published August 2020. Originally
approved in 2003. Last previous edition approved in 2014 as F2224 – 09 (2014). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
DOI: 10.1520/F2224-09R20. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
The boldface numbers in parentheses refer to the list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F2224 − 09 (2020)
2.2 Other Documents: 4.2 The total concentration of heavy metals (for example,
BS 6463-102: 2001 Quicklime, Hydrated Lime and Natural lead, arsenic, cadmium, antimony, bismuth, and mercury) in
Calcium Carbonate—Part 102: Methods for Chemical
the calcium sulfate raw material shall be limited to less than 10
Analysis
ppm. Other trace elements, such as iron, may also affect
US Pharmacopeia XXIV (USP 24) NF-19
implant performance and should be kept to a minimum. For
CFR Title 21, Part 820 Quality System Requirements
example, for calcium sulfate to meet USP grade, the iron
Food Chemical Codex (FCC)
concentration should not be higher than 100 ppm. Methods for
European Pharmacopeia
measuring these trace elements are described in Specification
ISO 10993-1 Biological Evaluation of Medical Devices
F1088 (Coupled Plasma—Atomic Absorption Spectrometry),
the United States Pharmacopeia (USP), European
3. Terminology
Pharmacopeia, or Food Chemical Codex (FCC). A second
3.1 Definitions:
method that may be used to analyze acid insoluble impurities
3.1.1 calcium sulfate anhydrite—a chemical substance hav-
is described in BS 6463-102.
ing approximate molecular formula of CaSO .
4.2.1 When calcium sulfate dihydrate is converted into
3.1.2 calcium sulfate dihydrate—a chemical having the
calcium sulfate hemihydrate, the mass of the material is
approximate molecular formula of CaSO ·2H O. This sub-
4 2
reducedbyapproximately15 %duetodehydration.Depending
stance is also known as gypsum.
on the conversion process, the quantities (total mass) of most
3.1.3 calcium sulfate hemihydrate—a chemical substance
or all of the trace elements present in the dihydrate are not
having approximate molecular formula of CaSO ·1/2HOor
4 2
affected. Therefore, the concentration of those trace elements
CaSO ·H O·CaSO . The mineral name of this substance is
4 2 4
in the resulting hemihydrate material can be expected to
bassanite and the substance is also known as Plaster of Paris in
increase by approximately 15 %. This should be taken into
the clinical literature.
account when setting acceptance criteria for a calcium sulfate
3.1.4 processing aids—any constituent intentionally used in
dihydrate raw material that will be used to produce a hemihy-
the processing of the raw material to fulfill a certain techno-
drate final product that is expected to conform to this specifi-
logical purpose during treatment or processing. Some ex-
cation.
amples would be: binders, lubricants, compaction aids,
disintegrants, plasticizers, deflocculants, wetting agents, water
5. Physical and Mechanical Characterization
retention agents, antistatic agents, antifoam agents, foam
stabilizers, chelating or sequestering agents, phase stabilizers,
5.1 The following physical and mechanical characterization
and so forth.
may be applicable to calcium sulfate for surgical implant
3.1.4.1 Discussion—Use of a processing aid may result in
applications in either the fabricated form or intra-operative
the unintentional but technically unavoidable presence of
fabricated form.When characterization test results are reported
residues of the substance or its derivatives in the final product.
in labeling, the test methods associated with these results shall
3.1.5 set time—foramixtureofcalciumsulfatehemihydrate
be referenced. Labeling can be defined as but is not limited to
and an aqueous solution, set time is defined as the elapsed time
the product label, brochures, technical monographs, and other
between the onset of mixing and the development of sufficient
related documentation.
mechanical properties to meet a specific criteria (for example,
5.2 Set Time—If set time is an applicable property, it should
hardness or resistance to indentation).
be reported along with the method by which it was determined
4. Chemical Requirements
in order to inform the final user. Test Methods C472 as
4.1 Calcium sulfate for surgical implants (raw material) described in Specification C59/C59M can be used to define a
typical set time. The actual method used for set time determi-
shall have a purity of not less than 98 % for calcium sulfate
(absent of water) when measured by USP 24 NF 19. (This nation shall be described or referenced in labeling.
purity measurement method may not be applicable to the
5.3 Compressive Strength—Calcium
...
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