ISO 17853:2003

Wear of implant materials — Polymer and metal wear particles — Isolation, characterization and quantification

ISO 17853:2003 specifies methods for sampling wear debris generated by total joint prostheses in humans and in joint simulators. It specifies the apparatus, reagents and test methods to isolate, characterize and quantify both polymer and metal wear debris from samples of tissue excised from around the joint prosthesis, obtained at revision surgery or post mortem, and from samples of joint-simulator test fluids. The method given in ISO 17853:2003 does not quantify the level of wear the implant produces, nor does it determine the amount of wear from any particular surface. ISO 17853:2003 does not cover the biological effect of wear debris or provide a method for evaluation of biological safety. The method given in ISO 17853:2003 is not applicable to the measurement of poly(methyl methacrylate) (PMMA) debris.

Usure des matériaux d'implant — Particules d'usure des polymères et des métaux — Isolation, caractérisation et quantification

General Information

• Status: Withdrawn
• Publication Date: 02-Jul-2003
• Withdrawal Date: 02-Jul-2003
• ICS: 11.040.40 - Implants for surgery, prosthetics and orthotics
• Technical Committee: ISO/TC 150/SC 4 - Bone and joint replacements
• Drafting Committee: ISO/TC 150/SC 4 - Bone and joint replacements
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 07-Jun-2010

Relations

• Revised: ISO 17853:2010 - Wear of implant materials — Polymer and metal wear particles — Isolation and characterization
• Effective Date: 15-Apr-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 17853
First edition
2003-07-01
Wear of implant materials — Polymer and
metal wear particles — Isolation,
characterization and quantification
Usure des matériaux d'implant — Particules d'usure des polymères et
des métaux — Isolation, caractérisation et quantification

Reference number
ISO 17853:2003(E)
©
ISO 2003

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ISO 17853:2003(E)
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ISO 17853:2003(E)
Contents Page
1 Scope . 1
2 Terms and definitions . 1
3 Methods of sampling and analysis of polymer and metal wear debris from tissue samples . 1
3.1 Principle . 1
3.2 Reagents . 1
3.3 Apparatus . 2
3.4 Storage and preparation of samples . 3
3.5 Procedure for polymer particle isolation . 3
3.6 Procedure for metal particle isolation . 4
3.7 Collection of particles . 4
3.8 Particle size and shape characterization . 5
3.9 Control study . 5
3.10 Calculation of the number of particles . 5
3.11 UHMWPE particle verification . 6
3.12 Metal particle verification . 6
4 Methods of sampling and analysis of polymer and metal particles from joint simulator
lubricants . 7
5 Test report . 7
Bibliography . 8
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ISO 17853:2003(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International
Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 17853 was prepared by Technical Committee ISO/TC 150, Implants for surgery, Subcommittee SC 4, Bone
and joint replacements.
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ISO 17853:2003(E)
Introduction
The biological responses to wear debris contribute to the failure of joint prostheses through bone resorption and
consequent implant loosening. A standardized method of particle retrieval from the tissue, followed by debris
characterization and quantification, is required for a uniform approach to debris response investigations. The
examination of the debris generated from implants in joint simulators also provides valuable information on the
wear properties and performance of the implant being studied.
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vi

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INTERNATIONAL STANDARD ISO 17853:2003(E)
Wear of implant materials — Polymer and metal wear particles —
Isolation, characterization and quantification
1Scope
This International Standard specifies methods for sampling wear debris generated by total joint prostheses in
humans and in joint simulators. It specifies the apparatus, reagents and test methods to isolate, characterize
and quantify both polymer and metal wear debris from samples of tissue excised from around the joint
prosthesis, obtained at revision surgery or post mortem, and from samples of joint-simulator test fluids.
The method given in this International Standard does not quantify the level of wear the implant produces, nor
does it determine the amount of wear from any particular surface. This International Standard does not cover
the biological effect of wear debris or provide a method for evaluation of biological safety.
The method given in this International Standard is not applicable to the measurement of poly(methyl
methacrylate) (PMMA) debris.
2 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
2.1
polymer wear debris
particles of ultra-high molecular weight polyethylene (UHMWPE) generated from the wear of polymeric
components of a joint prosthesis
2.2
metal wear debris
particles and particulate corrosion products generated from the wear of metal components of a joint prosthesis
3 Methods of sampling and analysis of polymer and metal wear debris from tissue
samples
3.1 Principle
Particles of polymeric and metal wear debris are released from tissue samples by digestion (see 3.5.1 and
3.6.1). The yield of each particle species is then purified by eliminating any remaining organic debris.
NOTE The methods involved in polymer and metal particle isolation are slightly different and are described in 3.5 and 3.6,
respectively.
The particles are collected, and are characterized and counted using scanning electron microscopy (SEM) or
transmission electron microscopy (TEM). The concentration of particles in the original tissue sample is then
calculated.
3.2 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and distilled
water or water of equivalent purity.
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ISO 17853:2003(E)
All reagent solutions shall be filtered through a filter of 0,2µm pore size or less (3.3.4) prior to use, to avoid
contamination of the sample by extraneous particles.
c = 0,1 mol/l 5 mol/l
3.2.1 Sodium hydroxide solutions (NaOH), and .
3.2.2 Hydrochloric acid solution (HCl), c = 0,01 mol/l.
3 3 3 3 3
3.2.3 Sucrose solutions, ρ = 1,35 g/cm, 1,17 g/cm, , 1,08 g/cm 1,04 g/cmand 1,02 g/cm.
3 3
3.2.4 Isopropanol-water mixtures, ρ = 0,96 g/cmand .ρ = 0,90 g/cm
3.2.5 Distilled water.
3.2.6 Papain solution.
Mix 100µm of pure papain, 3,26 mg of N-acetylcysteine, 9ml of distilled water and 1ml of phosphate buffer
(3.2.7).
3.2.7 Phosphate buffer.
Dissolve 3,55 gNa HPO and 3,45 g of NaH PO in 100 ml of distilled water to obtain a solution of pH 6,5; add
2 4 2 4
0,744 g EDTA added after pH titration.
3.2.8 Ethylenediaminetetraacetic acid solution (EDTA).
Dissolve 250 g of EDTA salt in 1,75 l of distilled water.
3.2.9 Fixative, e.g. formalin.
< 10µm
3.2.10 High density polyethylene (HDPE) powder (particle length ).
3.2.11 Titanium powder (particle length < 10µm).
3.3 Apparatus
All apparatus shall be cleaned and triple-rinsed with distilled water which has been filtered through a filter of
0,2µm
pore size or less (3.3.4) before use, to remove any contaminant particles.
3.3.1 Lint-free cloth.
3.3.2 Ultracentrifuge.
3.3.3 Ultracentrifuge tubes.
3.3.4 Filters, with pore size of 0,2µm or less for filtering reagents and distilled water.
3.3.5 Polycarbonate membrane filters, of pore sizes 0,1µm and 0,02µm, for collecting particles.
3.3.6 Agitating temperature-controlled water bath.
3.3.7 Pipettes, at least one of which is fine-tipped.
3.3.8 Petri dishes, with lids.
3.3.9 Ultrasonicator.
3.3.10 Polarizing light microscope.
3.3.11 Scanning electron microscope (SEM).
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ISO 17853:2003(E)
3.3.12 Transmission electron microscope (TEM).
3.3.13 Aluminium stub.
3.3.14 Carbon sticker.
3.3.15 Fourier transform infra-red (FTIR) spectroscope.
3.3.16 Syringe, with wide-bore needle.
3.3.17 Filtration unit.
3.3.18 Balance, with an accuracy of at least 0,1 mg.
3.4 Storage and preparation of samples
◦
Store the tissue frozen in a freezer at −70 C or in a fixative such as formalin. Thaw the tissue, if applicable,
and rinse it thoroughly in distilled water before continuing with the extraction method. Remove excess water
from the rinsed tissue by blotting with a lint-free cloth. Accurately measure the wet mass of the tissue and record
the volume of the subsequently applied solutions to enable the calculation of the number of wear particles per
gram of wet tissue (see 3.10).
Unfixed tissue should be handled under universal conditions.
Dry tissue may also be used, and the number of wear particles per gram of dry tissue calculated.
The nature of surgical instruments used for sample retrieval should be recorded in case of contamination.
NOTE Sampling variability due to specimen origin may occur.
3.5 Procedure for polymer particle isolation
3.5.1 Tissue digestion
Cut the tissue into smaller pieces using a scalpel and blade before digestion, to speed up the digestion times.
Extract the lipids from the minced tissue by placing into a 2:1 (volume ratio) chloroform: methanol mixture for
24 h or until the tissue sinks to the bottom of container. Remove and rinse the tissue.
Add 5 mol/l NaOH to the tissue in a ratio 10 ml of NaOH to 5 g tissue, and leave to digest for 1 h to 3 h in an
◦
agitating water bath at 65 C. Digestion can be judged to be complete when no visible solid pieces of tissue
remain in the suspension.
3.5.2 Purification of the polymer particle yield
3
ρ = 1,02 g/cm
Place sucrose solution ( ) into ultracentrifuge tubes so that the tubes are roughly three-quarters
full, and apply measured aliquots of the digested tissue suspension to the surface of the sucrose solution in
◦
each tube. Ultracentrifuge at 100 000g for 3h at 2 C. Carefully collect the top layer into a sterile tube and
◦
dilute with distilled water at 65 C to help dilute the residual sucrose. Ultrasonicate for 10 min to break up the
◦
agglomerated particles and then heat for 1h at 80 C to dissolve the sucrose.
3
Apply measured volumes of the suspension to two layers of isopropanol-water mixture of densities 0,90 g/cm
3 ◦
and 0,96 g/cm formed in the ultracentrifuge tubes. Ultracentrifuge these at 100 000g for 1h at 20 C. After
removing the tubes from the ultracentrifuge rotor, a layer of white particles should be visib
...