ASTM F2459-2018 Standard Test Method for Extracting Residue from Metallic Medical Components and Quantifying via Gravimetric Analysis《从金属医疗部件中提取残留物并通过重量分析定量的标准试验方法》.pdf

1、Designation: F2459 18Standard 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 adoption or, in the case

2、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 ofthe amount of residue obtained from met

3、allic medical compo-nents when extracted with aqueous or organic solvents.1.2 This test method does not advocate an acceptable levelof cleanliness. It identifies two techniques to quantify extract-able residue on metallic medical components. In addition, it isrecognized that this test method may not

4、 be the only method todetermine and quantify extractables.1.3 Although these methods may give the investigator ameans to compare the relative levels of component cleanliness,it is recognized that some forms of component residue may notbe accounted for by these methods.1.4 The applicability of these

5、general gravimetric methodshave been demonstrated by many literature reports; however,the specific suitability for applications to all-metal medicalcomponents will be validated by an Interlaboratory Study (ILS)conducted according to Practice E691.1.5 This test method is not intended to evaluate the

6、residuelevel in medical components that have been cleaned for reuse.This test method is also not intended to extract residue for usein biocompatibility testing.NOTE 1For extraction of samples intended for the biological evalu-ation of devices or materials, refer to ISO 1099312.1.6 The values stated

7、in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 This standard may involve hazardous orenvironmentally-restricted materials, operations, and equip-ment. This standard does not purport to address all of thesafety concerns, if any, associated wi

8、th its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accor-dance with internationally recognized

9、principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2E691 Practice for Conductin

10、g an Interlaboratory Study toDetermine the Precision of a Test MethodG121 Practice for Preparation of Contaminated Test Cou-pons for the Evaluation of Cleaning AgentsG131 Practice for Cleaning of Materials and Components byUltrasonic TechniquesG136 Practice for Determination of Soluble Residual Con-

11、taminants in Materials by Ultrasonic Extraction2.2 ISO Standard:3ISO 1099312 Biological EvaluationSample Preparationand Reference Materials3. Terminology3.1 Definitions:3.1.1 ionic compounds/water soluble residueresidue thatis soluble in water, including surfactants and salts.3.1.2 non-soluble debri

12、sresidue including metals, organicsolids, inorganic solids, and ceramics.3.1.3 non-water soluble residueresidue soluble in solventsother than water. Inclusive in this are oils, greases,hydrocarbons, and low molecular weight polymers. Typicalsolvents used to dissolve these residues include chlorinate

13、d orfluorinated solvents, or low molecular weight hydrocarbons.3.1.4 reflux systeman apparatus containing an extractionvessel and a solvent return system. It is designed to allow1This test method is under the jurisdiction of ASTM Committee F04 on Medicaland Surgical Materials and Devices and is the

14、direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Feb. 1, 2018. Published March 2018. Originallyapproved in 2005. Last previous edition approved in 2012 as F2459 12. DOI:10.1520/F2459-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org,

15、 orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Cop

16、yright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of Internat

17、ional Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1boiling of the solvent in the extraction vessel and to return anyvaporized solvent to the extraction vessel.3.1.5 reusethe repeated or multiple use of any medicalcomponent

18、(whether labeled SUD or reusable) with reprocess-ing (cleaning, disinfection, or sterilization, or combinationthereof) between patient uses.3.1.6 single use device (SUD)a disposable component thatis intended to be used on one patient during a single procedure.3.1.7 surface areathe projected surface

19、area of a part. Thisarea does not include the internal porosity of parts withcancellous, porous, or wire structure.3.2 Symbols:m1= weight of extraction vessel, foil, and component beforeextractionm2= weight of extraction vessel, component, foil, andsolvent after extractionm3= mass of clean beaker an

20、d foil used to hold removedaliquot of extracted solutionm4= mass of beaker, foil, and aliquot of solution beforedryingm5= mass of beaker, foil, and residue after evaporatingsolventm6= mass of new filterm7= mass of filter following filtration and dryingm8= mass of pre-dried sample specimen prior to e

21、xtractionm9= mass of pre-dried sample specimen after extractionma= 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, correctedfor the blank runsmi= weight of insoluble debrismt=

22、 mass of soluble and insoluble residueE = extraction efficiency4. Summary of Test Method4.1 This test method describes the extraction and quantita-tive analysis procedures used to detect and quantify the totalamount of extractable residue from metallic medical compo-nents. The residues are grouped i

23、nto three categories: (1)water-soluble extractables; (2) non-water soluble extractables;and (3) non-soluble debris.5. Significance and Use5.1 This test method is suitable for determination of the totalamount of extractable residue in metallic medical components.Extractable residue includes aqueous a

24、nd non-aqueous residue,as well as non-soluble residue.5.2 This test method recommends the use of a sonicationtechnique to extract residue from the medical component.Other techniques, such as solvent reflux extraction, could beused but have been shown to be less efficient in some tests, asdiscussed i

25、n X1.2.5.3 This test method is not applicable for evaluating theextractable residue for the reuse of a single-use component(SUD).6. Apparatus6.1 Ultrasonic Bath, for extraction. The bath must be largeenough to hold an extraction beaker containing the medicalcomponent. This apparatus is used with the

26、 technique de-scribed in 11.5. Alternatively, an ultrasonic probe can be usedwith 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. Aheating manifold or hotplate stirrer

27、 capable of reaching theboiling point of the solvent is also included. This apparatus isused in the procedure described in 11.3. A Soxhlet extractor, asshown in Fig. 2, could be used as well using the proceduredescribed in 11.3.6.3 Analytical Balance, with 0.1 mg accuracy or better.6.4 Balance, with

28、 accuracy of 10 mg or better and sufficientcapacity to weigh the extraction beaker with the medicalcomponent and solvent combined.6.5 Glass Beaker and Extraction Vessel, large enough tohold sufficient solvent to cover the medical component in theextraction vessel. Additionally, metal beakers could b

29、e used.Plastic beakers should not be used as low molecular weightresidues could be extracted from the beakers.6.6 Desiccator.6.7 Pipets, for transferring liquid. Some solvents can leachextractable compounds from plastic pipets. Glass or metallicpipets are recommended for organic solvents.6.8 Aluminu

30、m Foil, degreased in extraction solvent.6.9 Forceps, Tweezers, or Tongs, cleaned with acetone orextraction solvent.6.10 Filtration Apparatus, containing a removable 0.2 mfilter medium that is non-soluble in the extraction solvent.6.11 Non-Corrosive (Glass or Non-Corrosive Metal) Trays.6.12 Laborator

31、y Oven or rotary evaporator.7. Reagents and Materials7.1 Each user needs to demonstrate solubility of all of theirsuspect sources of residue in the solvent(s) of choice. Severalsolvents may be required if more than one type of residue maybe present on the component. The selected solvent shall notdis

32、solve or change the implant material.7.2 Spectroscopy or ACS-grade solvents should be used.7.3 High purity, deionized, or equivalent water should beused.8. Hazards8.1 Many organic solvents are toxic, flammable, or explo-sive and should be handled only with chemically protectivelaboratory gloves and

33、used in a fume hood.8.2 If sonication is used, the user should make sure that thesolvent is not heated, directly or through sonication, to atemperature above the flash point of the solvent.F2459 1829. Sampling, Test Specimens, and Test Units9.1 Metallic medical components should be taken in randomgr

34、oupings from different lots if available.9.2 It is up to the user to determine the number of medicalcomponents that need to be used to establish known reproduc-ibility.9.3 It is up to the user to determine the number of test blanksthat need to be used to establish known reproducibility.9.4 Separate

35、components should be tested for organic andaqueous extractions.9.5 If a long medical component is cut, it is recommendedthat the original length and the cut lengths be recorded beforethe final cleaning operation for validation purposes. Individualcut lengths may be separately extracted and the resul

36、ts com-bined to provide a total residue value for the medical compo-nent. Cutting lubricants must be avoided in this procedure.10. Limits of Detection and Recovery Efficiency10.1 Standardized test coupons can be prepared accordingto Practice G121. Limits of detection for the two extractiontechniques

37、 described in Section 11 can be assessed by placingknown amounts of residues on the test coupons, and perform-ing the extraction and analyses described in Section 11.10.2 Recovery EffciencyThe recovery efficiency of theselected extraction technique can be determined by dopingpre-cleaned medical comp

38、onents with known amounts of thetarget residue, then extracting and quantifying the targetresidue. When using this method, the extraction efficiency E isthe ratio of the amount of recovered residue to the dopedamount of residue. Recovery efficiency may also be deter-mined by exhaustive extraction. T

39、he exhaustive extractiontechnique uses medical components which have not beencleaned and contain unknown amounts of the target residue(s).These components should be extracted using the selectedextraction technique until no significant increase in the cumu-lative residue level is detected upon re-ext

40、raction, or until theincremental amount extracted is less than 10 % of what wasdetected in the first extraction. When using this approach, theextraction efficiency E is the ratio of the amount of recoveredresidue from the first extraction to the total amount ofrecovered residue from all extractions

41、performed.10.3 The user should adjust the extraction parameters in11.3.11, 11.5.8,or11.7.12, and/or select the appropriatesolvent, in order to achieve an extraction efficiency of E 75 %. This step should be performed if target residues areknown a priori. In the case of mixed residues, extractioneffi

42、ciency may not be able to be determined and the exhaustiveextraction of the test specimen may be performed.11. Procedure11.1 If more than one specimen is to be extractedcollectively, record the number of specimens.FIG. 1 Sample Solvent Reflux Extractor AssemblyF2459 18311.2 If multiple specimens are

43、 to be extracted collectively,they must be of the same type and size.11.3 Reflux Extraction by Extract Mass:11.3.1 Equipment may need to be cleaned with nitric acid orother appropriate means prior to solvent cleaning.11.3.2 Clean the extraction equipment by rinsing at leastthree times with spectrosc

44、opy-grade hexane or another suitablesolvent. The extraction solvent may be used.11.3.3 Air or oven dry all beakers and glassware at roomtemperature in a fume hood and store in a dessicator prior touse.11.3.4 Assemble the extraction apparatus as shown in Fig.1.11.3.5 Do not use any type of joint grea

45、se on the extractionassembly. It can dissolve in the solvent and contaminate thesolution. Polytetrafluoroethylene (PTFE) sleeves or tape can beused to seal the joints if necessary.11.3.6 Place the sample component in the extractor vesseland add a magnetic stirring bar or PTFE boiling stones toreduce

46、 the potential for boiling retardation in the system duringreflux. The stir bar or boiling stones, or both, should becarefully cleaned in a suitable solvent prior to use.11.3.7 Weigh the extractor vessel with the component on abalance and record the weight, m1.11.3.8 Charge the flask with enough sol

47、vent to completelycover 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 tomaintain the solvent at a brisk boil with moderate constantstirring.11.3.11 Extract the component(s) for 4 h or f

48、or approxi-mately 10 cycles if using a Soxhlet extractor, or the amount oftime needed to achieve an extraction efficiency greater than 75%. The extraction time or number of cycles can be adjusted bythe user based on internal. The extraction time or number ofcycles can be adjusted by the user based o

49、n internal validationof their target residue.11.3.12 After the extraction period is complete, turn off thehot plate and allow the system to cool. Carefully open theapparatus. If a Soxhlet extractor is used, heavy debris may stayin the top part of the extractor. This debris can be washed downinto the collection vessel with fresh extraction solvent.11.3.13 Weigh the extraction vessel, component, andsolvent, and record the weight as m2.11.3.14 Weigh an aliquot beaker large enough to hold analiquot of the extraction vessel along with a clean piece of foiland record the