ASTM F2847-10

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: F2847 − 10
Standard Practice for
Reporting and Assessment of Residues on Single Use
Implants
This standard is issued under the fixed designation F2847; 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
2.1 ASTM Standards:
1.1 The purpose of this practice is to describe how the
E996 Practice for Reporting Data in Auger Electron Spec-
cleanliness of single use implants as manufactured shall be
troscopy and X-ray Photoelectron Spectroscopy
reported. This practice proposes how to approach the identifi-
E1078 Guide for Specimen Preparation and Mounting in
cation of critical compounds and suggests different analytical
Surface Analysis
methods.
E1504 PracticeforReportingMassSpectralDatainSecond-
1.2 The practice does not address substances which are
ary Ion Mass Spectrometry (SIMS)
intrinsic to the implant properties or design. In particular, it
E1635 Practice for Reporting Imaging Data in Secondary
doesnotaddresssubstancesreleasedduringimplantresorption,
Ion Mass Spectrometry (SIMS)
implant coatings, or leachables by design.
E1829 Guide for Handling Specimens Prior to Surface
Analysis
1.3 This practice does not address the cleanliness of im-
F561 Practice for Retrieval and Analysis of Medical
plants which are re-processed, re-cleaned after unpacking for
Devices, and Associated Tissues and Fluids
re-use in the hospital or by the manufacturer.
F748 PracticeforSelectingGenericBiologicalTestMethods
1.4 Thispracticedoesnotestablishlimitvaluesforresidues.
for Materials and Devices
F1251 Terminology Relating to Polymeric Biomaterials in
1.5 This practice suggests appropriate test methods for the
Medical and Surgical Devices (Withdrawn 2012)
general specification of residues and residue requirements of
F1877 Practice for Characterization of Particles
implants. This practice may also be used to characterize
F2459 Test Method for Extracting Residue from Metallic
semi-finished components for implants.
Medical Components and Quantifying via Gravimetric
1.6 Thetestmethodssuggestedanddescribedhereinreferto Analysis
F2809 Terminology Relating to Medical and Surgical Mate-
established analytical methods and to existing standard meth-
ods for chemical, biochemical, or biological analysis. rials and Devices
G121 Practice for Preparation of Contaminated Test Cou-
1.7 This practice is intended solely to provide guidance
pons for the Evaluation of Cleaning Agents
regarding suitable test methods and reporting conventions for
G131 PracticeforCleaningofMaterialsandComponentsby
residues, which may or may not affect implant biocompatibil-
Ultrasonic Techniques
ity. This practice does not suggest or recommend test methods
G136 Practice for Determination of Soluble Residual Con-
for biocompatibility, which may be found in Practice F748 or
taminants in Materials by Ultrasonic Extraction
in ISO 10993-1.
2.2 ISO Standards:
1.8 This standard does not purport to address all of the
ISO 10993-1 Biological Evaluation of Medical Devices—
safety concerns, if any, associated with its use. It is the
Part 1: Evaluation and Testing
responsibility of the user of this standard to establish appro-
ISO 10993-17 Biological Evaluation of Medical Devices—
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
ThispracticeisunderthejurisdictionofASTMCommitteeF04onMedicaland the ASTM website.
Surgical Materials and Devices and is the direct responsibility of Subcommittee The last approved version of this historical standard is referenced on
F04.15 on Material Test Methods. www.astm.org.
Current edition approved Dec. 1, 2010. Published January 2011. DOI: 10.1520/ Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
F2847–10. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F2847 − 10
Part 17: Establishment ofAllowable Limits for Leachable 3.2.2 exhaustive extraction, n—extraction until the cumula-
Substances tive residue change is analytically insignificant or less than
ISO 10993-18 Biological Evaluation of Medical Devices— 10 % of the initial extract.
Part 18: Chemical Characterization of Materials
3.2.3 limit value, n—the maximum allowable amount(s) of
ISO 11737-1 Sterilization of Medical Devices—
substance(s) at the surface of an implant not yet found to be
Microbiological Methods—Part 1: Determination of a
harmful for the surrounding tissues and organs. Its value is
Population of Microorganisms on Products
established and defined by the manufacturer.
2.3 United States Pharmacopeia (USP) Document:
3.2.4 model residue, n—a single substance or a mixture of
<85> Bacterial Endotoxin Test
substances that reflect the process materials likely to be
encountered and used during the manufacturing of the device.
2.4 European Pharmacopoeia (PhEUR) Documents:
2.2.23 Atomic Absorption Spectrometry
3.2.5 residue, n—a substance present at the surface of an
2.2.24 Absorption Spectrophotometry, Infrared
implant or embedded therein that is not explicitly recognized
2.2.25 Absorption Spectrophotometry, Ultraviolet and Vis-
and defined as part of the implant specification (special
ible
definition for residue analysis of surfaces). It includes process-
2.2.28 Gas Chromatography
based residues as well as contamination by environmental
2.2.29 Liquid Chromatography
factors (adsorbates).
2.2.43 Mass Spectrometry
3.2.6 single use implant, n—a medical device which in-
2.2.44 Total Organic Carbon in Water for Pharmaceutical
tended use is to be implanted permanently and that is not
Use
re-cleaned or re-worked for a second implantation after even-
2.2.48 Raman Spectrometry
tual removal.
2.2.55 Peptide Mapping
3.2.7 soiling, n—procedureofapplyingknownamountsofa
2.2.57 Inductively Coupled Plasma-Atomic Emission Spec-
substance onto a medical device for determination of process
trometry
capability, that is, cleaning efficiency and extraction yields.
2.2.58 Inductively Coupled Plasma-Mass Spectrometry
3.2.8 spiking, n—procedureofapplyingexactquantitiesofa
2.5 Association for the Advancement of Medical Instrumen-
substance to an analyte for instrumental calibration and deter-
tation (AAMI) Document:
mination reaction yield.
AAMI ST72 Bacterial Endotoxins—Test Methodologies,
3.2.9 surface area, n—the projected surface area of a part.
Routine Monitoring, and Alternatives to Batch Testing
This area does not include the internal porosity of parts with
2.6 Other References:
cancellous, porous, or wire structure. It does include factors
FDA Guideline on Validation of the Limulus Amebocyte
that correct for the estimated surface roughness.
Lysate Test as an End-Product Endotoxin Test for Human
and Animal Parenteral Drugs, Biological Products, and
4. Summary of Practice
Medical Device, 1987
4.1 This practice describes how to report residues on im-
200.7 EPA Methodologies for ICP
plant surfaces and indicates useful and typical applicable
8270C EPA Methodologies for GC-MS
analytical methods.
4.2 Application of the test methods contained within this
3. Terminology
practice does not guarantee clinical success of a finished
3.1 Unless provided otherwise in 3.2, terminology shall be
implant,butitwillhelptoensureconsistencyinitscleanliness.
in conformance with Terminology F1251 and with Terminol-
ogy F2809.
5. Significance and Use
3.2 Definitions:
5.1 The quality and consequently the clinical performance
3.2.1 action value, n—the amount(s) of substance(s) toler-
of implants may be affected by residues. Residues may induce
ated at the surface of an implant by the manufacturer before it
no tissue response, minor tissue irritations, or they may lead to
will interfere with the manufacturing process.
local inflammation of tissues surrounding the implant which
may lead to failure in short-term or long-term use. Residues
may also cause harm at locations away from the implant.
Residues may originate from manufacturing materials used in
Available from U.S. Pharmacopeia (USP), 12601Twinbrook Pkwy., Rockville,
MD 20852-1790, http://www.usp.org.
the course of processing, or may be the result of handling and
Available from European Directorate for the Quality of Medicines and
packaging (1-3).
HealthCare (EDQM), 7 allee Kastner, CS 30026, F67081, Strasbourg, France,
http://www.edqm.eu/en/News-and-General-Information-43.html.
5.2 Thispracticeshallbeusedtoreporttheresultsoftesting
Available from Association for the Advancement of Medical Instrumentation
for residue. All residues cannot necessarily be detected. It
(AAMI), 4301 North Fairfax Drive, Suite 301, Arlington, VA 22203, http://
suggests standard techniques that may be applied for analysis,
www.aami.org.
and provides suggestions for how limit values may be set.
Available from Food and Drug Administration (FDA), 5600 Fishers Ln.,
Rockville, MD 20857, http://www.fda.gov.
Available from United States Environmental Protection Agency (EPA), Ariel
Rios Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http:// The boldface numbers in parentheses refer to the list of references at the end
www.epa.gov. of this standard.
F2847 − 10
5.3 Residues may be of inorganic, organic, or biological 6.2.3.1 In this practice, microbiologic residues are to be
nature. They may exhibit as surface bound substance, or as an listedseparatelyanddifferentiatedasbioburdenandendotoxin.
adsorbate (for example, electrostatically held), an It should be noted that for medical devices sold sterile,
efflorescence, or a mechanically held substance. Residues may bioburden testing is often part of sterilization validation and is
be soluble in aqueous media, soluble in organic solvents, or
monitoredonapredeterminedscheduleforthepurposeofdose
may be insoluble particulates. audits or process control.
6.2.4 In this practice, particulate residues are referred to as
5.4 Data generated in validation processes, that is, cleaning
material insoluble in aqueous media or organic solvent, which
validation or sterility validation may be used as results or as
can be removed from the surface of an implant by physical-
basis for setting acceptance criteria in the report.
chemical means without interfering with the integrity of the
implant surface. Even though particulates shall be reported
6. Reporting of Residues on Implants
separately, they belong to one of the chemical classes men-
6.1 The reporting of cleanliness of implants shall include a
tioned above.
table that lists at least sections on (1) the chemical categories,
(2) the results of validation studies or of routine analysis, (3)
6.3 Reported Units:
the acceptance criteria if applicable, (4) the detection limits of
6.3.1 Results of inorganic and organic analysis shall be
the methods used, and (5) the methods of analysis (see Table
reported as mass per implant and/or mass per surface area (use
1).
SI units).
6.2 Categories of Residues:
6.3.2 Results of biological analysis shall be reported in the
6.2.1 Residues shall be classified, as needed, according to
specificunitsperimplant,thatis,enumerationmethodssuchas
the common description and reported accordingly as (I)
colony forming unit (CFU), or enzymatic assays such as for
inorganic,(II)organic,(III)biologic,(IV)microbiological,and
example, endotoxin units (EU).
(V) particulate residues.
6.3.3 Results of particulate analysis shall be reported in
6.2.2 In this practice, inorganic residues are referred to as
mass per implant, mass per surface area, number per device,
substances of all elements with the exception of carbon-
number per surface area, or atomic-%, or fraction per surface
containing substances. Carbonates, graphite or graphite-like
area. The size range of particulates considered in the analysis
structures (for example, diamond like coatings) are tradition-
(for example, based on filter pore sizes, capillaries, diffraction
ally listed as inorganic substances.
settings) shall be reported.
6.2.3 In this practice, organic residues are referred to as
6.3.4 Results of surface analysis shall be reported as
synthetic and natural carbon-based substances. It includes both
atomic-%, molecular-%, or fraction per surface area.
small molecules with low molecular mass (for example,
paraffin or low viscosity oil) and high molecular mass based 6.4 Identification of Residues—Residues that have been
synthetic polymers. Polysilanes and -oxanes are also consid- identified shall be listed separately in the report if they are
ered organic residues. considered significant by the practitioner of this practice.
TABLE 1 Suggested Table for Reporting of Residues
NOTE 1—The reported table shall reflect the mean value of all measurements of a product and the error including the error of the method.
NOTE2—ThecolumnAppliedAnalyticalMethodexemplifiesmethodsandapplicablestandards.Theycanbereplacedbyanymethod/standardprotocol
suitable for the particular residues.
Results of Set Limit Applied Analytical
Categories Detection Limit
Analysis Values Methods
Inorganic [mass/implant] [mass/implant] [mass/implant] ICP-OES
[mass/surface area] [mass/surface area] [mass/surface area] (PhEur 2.2.57)
Organic GC-MS
(PhEur 2.2.28,
EPA 8270C)
Biological e-spray MS
(PhEur 2.2.43)
Bioburden [CFU/implant] [CFU/implant] [CFU/implant] ISO 11737-1
A
Endotoxin [EU/implant] EU/implant [EU/implant] USP<85>
AAMI ST72
Particulate [mass/implant] [mass/implant] [mass/implant] SEM (internal protocol)
[mass/surface area] [mass/surface area] [mass/surface area] XPS (ASTM E996)
[Number/implant] [Number/ implant] [Number/implant]
2 2 2 2 2 2
or [cm /cm ] or [cm /cm ] or [cm /cm ]
[Atomic-%] [Atomic-%] [Atomic-%]
or [Molecular-%] or [Molecular-%] or [Molecular-%]
Visual Inspection [Optical observations] [Optical observations] [Optical observations] (internal protocol)
A
Limit value as defined for device types listed in FDA Guidance for Industry and Guideline on Validation of the Limulus Amebocyte Lysate Test as an End-Product
Endotoxin Text for Human and Animal Parenteral Drugs, Biological Products, and Medical Devices (December 1987).
F2847 − 10
7. Quality Assurance 7.6 Each method of analysis shall be establishe
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