1、Designation:F245905 Designation: F2459 12Standard Test Method forExtracting Residue from Metallic Medical Components andQuantifying via Gravimetric Analysis1This standard is issued under the fixed designation F2459; the number immediately following the designation indicates the year oforiginal adopt
2、ion or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the quantitative assessment of the amount of resi
3、due obtained from metallic medical componentswhen extracted with aqueous or organic solvents.1.2 This test method does not advocate an acceptable level of cleanliness. It identifies one technique to quantify extractableresidue on metallic medical components. In addition, it is recognized that this t
4、est method may not be the only method to determineand quantify extractables.1.3 Although these methods may give the investigator a means to compare the relative levels of component cleanliness, it isrecognized that some forms of component residue may not be accounted for by these methods.1.4 The app
5、licability of these general gravimetric methods have been demonstrated by many literature reports; however, thespecific suitability for applications to all-metal medical components will be validated by an Interlaboratory Study (ILS) conductedaccording to Practice E691.1.5 This test method is not int
6、ended to evaluate the residue level in medical components that have been cleaned for reuse. Thistest method is also not intended to extract residue for use in biocompatibility testing.1.6The values stated in SI units are to be regarded as the standard. The values given in parentheses are for informa
7、tion only.NOTE 1For extraction of samples intended for the biological evaluation of devices or materials, refer to ISO 1099312.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard may involve hazardous or envi
8、ronmentally-restricted materials, operations, and equipment. This standarddoes not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of thisstandard to establish appropriate safety and health practices and determine the applicability
9、 of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodG121 Practice for Preparation of Contaminated Test Coupons for the Evaluation of Cleaning AgentsG131 Practice for Cleani
10、ng of Materials and Components by Ultrasonic TechniquesG136 Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction2.2 ISO Standard:3ISO 1099312 Biological EvaluationSample Preparation and Reference Materials3. Terminology3.1 Definitions:3.1.1 ionic compound
11、s/water soluble residueresidue that is soluble in water, including surfactants and salts.3.1.2 non-soluble debrisresidue including metals, organic solids, inorganic solids, and ceramics.1This test method is under the jurisdiction of ASTM Committee F04 on Medical and Surgical Materials and Devices an
12、d is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Aug. 1, 2005. Published August 2005. DOI: 10.1520/F2459-05.Current edition approved March 1, 2012. Published March 2012. Originally approved in 2005. Last previous edition approved in 2005 as F2459
13、 05. DOI:10.1520/F2459-12.2For extraction of samples intended for the biological evaluation of devices or materials, refer to ISO 10993-12 Biological EvaluationSample Preparation and ReferenceMaterials.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Ser
14、vice at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsv
15、olume information, refer to the standards Document Summary page on the ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.1This document is not an ASTM standard and is intended only to provide the user of an AS
16、TM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published
17、 by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.3 non-water soluble residueresidue soluble in solvents other than water. Inclusive in this are oils, greases, hydrocarbons,and low
18、molecular weight polymers. Typical solvents used to dissolve these residues include chlorinated or fluorinated solvents,or low molecular weight hydrocarbons.3.1.4 reflux systeman apparatus containing an extraction vessel and a solvent return system. It is designed to allow boilingof the solvent in t
19、he extraction vessel and to return any vaporized solvent to the extraction vessel.3.1.5 reusethe repeated or multiple use of any medical component (whether labeled SUD or reusable) with reprocessing(cleaning, disinfection, or sterilization, or combination thereof) between patient uses.3.1.6 single u
20、se component (SUD)a disposable component; intended to be used on one patient during a single procedure.3.1.7 surface areathe projected surface area of a part. This area does not include the internal porosity of parts with cancellous,porous, or wire structure.3.2 Symbols:m1= weight of extraction vess
21、el and component before extractionm2= weight of extraction vessel, component, foil, and solvent after extractionm3= mass of clean beaker and foil used to hold removed aliquot of extracted solutionm4= mass of beaker, foil, and aliquot of solution before dryingm5= mass of beaker, foil, and residue aft
22、er evaporating solventm6= mass of new filterm7= mass of filter following filtration and dryingma= mass of residue in removed aliquotcr= concentration of residue in solutioncb= concentration of residue in blank solutionsmr= mass of soluble residue in the overall extract, corrected for the blank runsm
23、i= weight of insoluble debrismt= mass of soluble and insoluble residueE = extraction efficiency4. Summary of Test Method4.1 This test method describes the extraction and quantitative analysis procedures used to detect and quantify extractable residuefrom metallic medical components. The residues are
24、 grouped into three categories: (1) water-soluble extractables; (2) non-watersoluble extractables; and (3) non-soluble debris.5. Significance and Use5.1 This test method is suitable for determination of the extractable residue in metallic medical components. Extractable residueincludes aqueous and n
25、on-aqueous residue, as well as non-soluble residue.5.2 This test method recommends the use of a sonication technique to extract residue from the medical component. Othertechniques, such as solvent reflux extraction, could be used but have been shown to be less efficient in some tests, as discussedin
26、 X1.2.5.3 This test method is not applicable for evaluating the extractable residue for the reuse of a single-use component (SUD).6. Apparatus6.1 Ultrasonic Bath, for extraction. The bath must be large enough to hold an extraction beaker containing the medicalcomponent. This apparatus is used with t
27、he technique described in 11.5. Alternatively, an ultrasonic probe can be used with a bath.6.2 Solvent Reflux Extraction Assembly, shown in Fig. 1. This assembly is composed of a vessel large enough to hold themedical component, and a water-cooled refluxing column. A heating manifold or hotplate sti
28、rrer capable of reaching the boilingpoint of the solvent is also included. This apparatus is used in the procedure described in 11.3. A Soxhlet extractor, as shown inFig. 2, could be used as well using the procedure described in 11.3.6.3 Analytical Balance, with 0.1 mg accuracy or better.6.4 Balance
29、, with accuracy of 10 mg of better and sufficient capacity to weigh the extraction beaker with the medical componentand solvent combined.6.5 Glass Beaker and Extraction Vessel, large enough to hold sufficient solvent to cover the medical component in the extractionvessel. Additionally, metal beakers
30、 could be used. Plastic beakers should not be used as low molecular weight residues could beextracted from the beakers.6.6 Desiccator.6.7 Pipets, for transferring liquid. Some solvents can leach extractable compounds from plastic pipets. Glass or metallic pipetsare recommended for organic solvents.6
31、.8 Aluminum Foil, degreased in extraction solvent.6.9 Forceps, Tweezers, or Tongs, cleaned with acetone or extraction solvent.6.10 Filtration Apparatus, containing a removable 0.2 m filter medium that is non-soluble in the extraction solvent.F2459 1227. Reagents and Materials7.1 Each user needs to d
32、emonstrate solubility of all of their suspect sources of residue in the solvent(s) of choice. Severalsolvents may be required if more than one type of residue may be present on the component.7.2 Spectroscopy or ACS-grade solvents should be used.8. Hazards8.1 Many organic solvents are toxic, flammabl
33、e, or explosive and should be handled only with chemically protective laboratorygloves and used in a fume hood.8.2 If sonication is used, the user should make sure that the solvent is not heated, directly or through sonication, to a temperatureabove the flash point of the solvent.9. Sampling, Test S
34、pecimens, and Test Units9.1 Metallic medical components should be taken in random groupings from different lots if available.9.2 It is up to the user to determine the number of medical components that need to be used to establish known reproducibility.9.3 It is up to the user to determine the number
35、 of test blanks that need to be used to establish known reproducibility.9.4 Separate components should be tested for organic and aqueous extractions.9.5 If a long medical component is cut, it is recommended that the original length and the cut lengths be recorded before thefinal cleaning operation f
36、or validation purposes. Individual cut lengths may be separately extracted and the results combined toprovide a total residue value for the medical component. Cutting lubricants must be avoided in this procedure.10. Limits of Detection and Recovery Efficiency10.1 Standardized test coupons can be pre
37、pared according to Practice G121. Limits of detection with the two techniques canbe assessed by placing known amounts of residues on the test coupons, and performing the extraction and analyses described inSection . Limits of detection for the two extraction techniques described in Section 11 . The
38、recovery efficiency of the selectedextraction technique should be determined by doping pre-cleaned medical components with known amounts of the target residue,then extracting and quantifying the target residue. The extraction efficiency can be assessed by placing known amounts of residueson the test
39、 coupons, and performing the extraction and analyses described in Section 11.FIG. 1 Sample Solvent Reflux Extractor AssemblyF2459 12310.2 Recovery EffciencyThe recovery efficiency of the selected extraction technique can be determined by dopingpre-cleaned medical components with known amounts of the
40、 target residue, then extracting and quantifying the target residue.When using this method, the extraction efficiency E is the ratio of the amount of recovered residue to the doped amount of residue.10.2The user should adjust the extraction parameters in is the ratio of the amount of recovered resid
41、ue to the doped amount ofresidue. Recovery efficiency may also be determined by exhaustive extraction. The exhaustive extraction technique uses medicalcomponents which have not been cleaned and contain unknown amounts of the target residue(s). These components should beextracted using the selected e
42、xtraction technique until no significant increase in the cumulative residue level is detected uponre-extraction, or until the incremental amount extracted is less than 10 % of what was detected in the first extraction. When usingthis approach, the extraction efficiency E is the ratio of the amount o
43、f recovered residue from the first extraction to the total amountof recovered residue from all extractions performed.10.3 The user should adjust the extraction parameters in 11.3.11 or 11.5.8, or select the appropriate solvent, or both, in orderto achieve an extraction efficiency of E 75%. 75 %. Thi
44、s step should be performed if target residues are known a priori. Inthe case of mixed residues, extraction efficiency may not be able to be determined.11. Procedure11.1 If more than one specimen is to be extracted collectively, record the number of specimens.11.2 If multiple specimens are to be extr
45、acted collectively, they must be of the same type and size.11.3 Reflux Extraction:11.3.1 Equipment may need to be cleaned with nitric acid or other appropriate means prior to solvent cleaning.11.3.2 Clean the extraction equipment by rinsing at least three times with spectroscopy-grade hexane or anot
46、her suitable solvent.The extraction solvent may be used.11.3.3 Air dry all beakers and glassware at room temperature in a fume hood and store in a dessicator prior to use.11.3.4 Assemble the extraction apparatus as shown in Fig. 1.11.3.5 Do not use any type of joint grease on the extraction assembly
47、. It can dissolve in the solvent and contaminate the solution.Polytetrafluoroethylene (PTFE) sleeves or tape can be used to seal the joints if necessary.11.3.6 Place the sample component in the extractor vessel and add a magnetic stirring bar or PTFE boiling stones to reduce thepotential for boiling
48、 retardation in the system during reflux. The stir bar or boiling stones, or both, should be carefully cleaned ina suitable solvent prior to use.FIG. 2 Sample Soxhlet Extractor AssemblyF2459 12411.3.7 Weigh the extractor vessel with the component on a balance and record the weight m1.11.3.8 Charge t
49、he flask with enough solvent to completely cover the component(s) and assemble the reflux system.11.3.9 Start flow of cooling water through the condenser.11.3.10 Adjust the hotplate stirrer or heating manifold to maintain the solvent at a brisk boil with moderate constant stirring.11.3.11 Extract the component(s) for4horforapproximately 10 cycles if using a Soxhlet extractor. The extraction time ornumber of cycles can be adjusted by the user based on internal validation of their target residue.11.3.12 After the extraction period is complete, turn off the hot p
