1、Designation: F 2459 05Standard Test Method forExtracting Residue from Metallic Medical Components andQuantifying via Gravimetric Analysis1This standard is issued under the fixed designation F 2459; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、metallic medical compo-nents when extracted with aqueous or organic solvents.1.2 This test method does not advocate an acceptable levelof cleanliness. It identifies one technique to quantify extract-able residue on metallic medical components. In addition, it isrecognized that this test method may n
4、ot 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 thes
5、e 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 E 691.1.5 This test method is not intended to evaluate t
6、he residuelevel in medical components that have been cleaned for reuse.This test method is also not intended to extract residue for usein biocompatibility testing.21.6 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.7 This st
7、andard may involve hazardous orenvironmentally-restricted materials, operations, and equip-ment. This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health prac
8、tices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodG 121 Practice for the Preparation of Contaminated Cou-pons for the Evaluation of
9、Cleaning AgentsG 131 Practice for Cleaning of Materials and Componentsby Ultrasonic TechniquesG 136 Practice for Determination of Soluble Residual Con-taminants in Materials by Ultrasonic Extraction3. Terminology3.1 Definitions:3.1.1 ionic compounds/water soluble residueresidue thatis soluble in wat
10、er, including surfactants and salts.3.1.2 non-soluble debrisresidue including metals, organicsolids, inorganic solids, and ceramics.3.1.3 non-water soluble residueresidue soluble in sol-vents other than water. Inclusive in this are oils, greases,hydrocarbons, and low molecular weight polymers. Typic
11、alsolvents used to dissolve these residues include chlorinated 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 allowboiling of the solvent in the extraction vessel and to return
12、 anyvaporized solvent to the extraction vessel.3.1.5 reusethe repeated or multiple use of any medicalcomponent (whether labeled SUD or reusable) with reprocess-ing (cleaning, disinfection, or sterilization, or combinationthereof) between patient uses.3.1.6 single use component (SUD)a disposable comp
13、o-nent; intended to be used on one patient during a singleprocedure.1This test method is under the jurisdiction of ASTM Committee F04 on Medicaland Surgical Materials and Devices and is the direct responsibility of SubcommitteeF04.15 on Material Test Methods.Current edition approved Aug. 1, 2005. Pu
14、blished August 2005.2For extraction of samples intended for the biological evaluation of devices ormaterials, refer to ISO 10993-12 Biological EvaluationSample Preparation andReference Materials.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
15、serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.7 surface areathe projected surface area of a p
16、art.This area does not include the internal porosity of parts withcancellous, porous, or wire structure.3.2 Symbols:m1= weight of extraction vessel and component beforeextractionm2= weight of extraction vessel, component, and solventafter extractionm3= mass of clean beaker used to hold removed aliqu
17、ot ofextracted solutionm4= mass of beaker and aliquot of solution before dryingm5= mass of beaker and residue after evaporating solventm6= mass of new filterm7= mass of filter following filtration and dryingma= mass of residue in removed aliquotcr= concentration of residue in solutioncb= concentrati
18、on of residue in blank solutionsmr= mass of soluble residue in the overall extract, cor-rected for the blank runsmi= weight of insoluble debrismt= mass of soluble and insoluble residueE = extraction efficiency4. Summary of Test Method4.1 This test method describes the extraction and quantita-tive an
19、alysis procedures used to detect and quantify extractableresidue from metallic medical components. The residues aregrouped into 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
20、determination of theextractable residue in metallic medical components. Extract-able residue includes aqueous and non-aqueous residue, as wellas non-soluble residue.5.2 This test method recommends the use of a sonicationtechnique to extract residue from the medical component.Other techniques, such a
21、s solvent reflux extraction, could beused but have been shown to be less efficient in some tests, asdiscussed in 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 mu
22、st be largeenough to hold an extraction beaker containing the medicalcomponent. This apparatus is used with the 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
23、enough to hold themedical component, and a water-cooled refluxing column. AFIG. 1 Sample Solvent Reflux Extractor AssemblyF2459052heating manifold or hotplate stirrer capable of reaching theboiling point of the solvent is also included. This apparatus isused in the procedure described in 11.3. A Sox
24、hlet 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 accuracy of 10 mg of better and sufficientcapacity to weigh the extraction beaker with the medicalcomponent and solvent combined.6.5
25、Glass Beaker and Extraction Vessel, large enough tohold sufficient solvent to cover the medical component in theextraction vessel. Additionally, metal beakers could be used.Plastic beakers should not be used as low molecular weightresidues could be extracted from the beakers.6.6 Desiccator.6.7 Pipet
26、s, for transferring liquid. Some solvents can leachextractable compounds from plastic pipets. Glass or metallicpipets are recommended for organic solvents.6.8 Aluminum Foil, degreased in extraction solvent.6.9 Forceps, Tweezers, or Tongs, cleaned with acetone orextraction solvent.6.10 Filtration App
27、aratus, containing a removable 0.2 mfilter medium that is non-soluble in the extraction solvent.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 resid
28、ue maybe present on the component.7.2 Spectroscopy or ACS-grade solvents should be used.8. Hazards8.1 Many organic solvents are toxic, flammable, or explo-sive and should be handled only with chemically protectivelaboratory gloves and used in a fume hood.8.2 If sonication is used, the user should ma
29、ke sure that thesolvent is not heated, directly or through sonication, to atemperature above the flash point of the solvent.9. Sampling, Test Specimens, and Test Units9.1 Metallic medical components should be taken in randomgroupings from different lots if available.9.2 It is up to the user to deter
30、mine 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 components should be tested for organic andaqueous extractions.9.5 If a lo
31、ng medical component is cut, it is recommendedthat the original length and the cut lengths be recorded beforethe final cleaning operation for validation purposes. IndividualFIG. 2 Sample Soxhlet Extractor AssemblyF2459053cut lengths may be separately extracted and the results com-bined to provide a
32、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 G 121. Limits of detection with the two techniquescan be assessed by placing known a
33、mounts of residues on thetest coupons, and performing the extraction and analysesdescribed in Section 11. The recovery efficiency of the selectedextraction technique should be determined by doping pre-cleaned medical components with known amounts of the targetresidue, then extracting and quantifying
34、 the target residue. Theextraction efficiency E is the ratio of the amount of recoveredresidue to the doped amount of residue.10.2 The user should adjust the extraction parameters in11.3.11 or 11.5.8, or select the appropriate solvent, or both, inorder to achieve an extraction efficiency of E 75%.11
35、. Procedure11.1 If more than one specimen is to be extracted collec-tively, record the number of specimens.11.2 If multiple specimens are to be extracted 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 orother approp
36、riate means prior to solvent cleaning.11.3.2 Clean the extraction equipment by rinsing at leastthree times with spectroscopy-grade hexane or another suitablesolvent. The extraction solvent may be used.11.3.3 Air dry all beakers and glassware at room tempera-ture in a fume hood and store in a dessica
37、tor 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 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
38、.6 Place the sample component in the extractor vesseland add a magnetic stirring bar or PTFE boiling stones toreduce 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 t
39、he extractor vessel with the component on abalance and record the weight m1.11.3.8 Charge the flask with enough solvent 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
40、tomaintain the solvent at a brisk boil with moderate constantstirring.11.3.11 Extract the component(s) for 4 h or for approxi-mately 10 cycles if using a Soxhlet extractor. The extractiontime or number of cycles can be adjusted by the user based oninternal validation of their target residue.11.3.12
41、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
42、.13 Weigh the extraction vessel, component, and sol-vent, 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 weight as m3. The beaker should be weighed toa resolution of at least 0.1 mg.11
43、.3.15 Allow the insoluble debris to settle in the extractionvessel for 1 h. Withdraw an aliquot of the extracted solutionthat comprises at least 90 % of the total extracted solution andplace in the aliquot beaker as described in 11.3.14, beingcareful not to withdraw any insoluble debris from the bot
44、tom ofthe extraction vessel. Weigh the solution with beaker and foiland record as m4.11.3.15.1 Allow the solvent to completely evaporate in afume hood at room temperature. See X1.1.3 for more details.11.3.15.2 Place the beaker, with residue, in a dessicator fora minimum of 2 h.11.3.15.3 Weigh the be
45、aker and foil again and record as m5.11.3.15.4 If the volume of the aliquot beaker is smaller thanthe aliquot, multiple aliquots can be removed from the extrac-tion vessel, weighing each aliquot, evaporating the solvent, andcollecting the next aliquot. The solution weight m4is the sumof the aliquot
46、weights plus the foil weight. The final beakerweight m5should be recorded as described in 11.3.15.3.11.4 Blank Run:11.4.1 Conduct test blank(s) using the same amount ofsolvent and rinses, but no component, for the completeextraction and analysis procedure. Record all weights as above.11.5 Sonication
47、 Extraction:11.5.1 Background information on sonication extraction canbe found in Practices G 131 and G 136.11.5.2 Glassware may need to be cleaned with nitric acid orother appropriate means prior to solvent cleaning.11.5.3 Clean the glassware by rinsing at least three timeswith spectroscopy-grade h
48、exane or another suitable solvent.The extraction solvent may be used.11.5.4 Air dry all beakers and glassware at room tempera-ture in a fume hood and store in a dessicator prior to use.11.5.5 Place the medical component in a beaker, cover withclean foil, and weigh. Record the weight as m1.11.5.6 Add
49、 enough solvent to completely cover the compo-nent.11.5.7 Cover the beaker with the clean aluminum foil, thenplace in a sonicator bath. The aluminum foil should not contactthe water in the sonicator bath.11.5.8 Start the sonicator bath, and extract the component(s)for a time period and temperature determined by the userpending internal validation of their extraction efficiency on thetarget residues. The extraction temperature should be below theboiling point of the solvent. More details on sonication timescan be found in X1.2.3.11.5.9 After the extraction period is complete, r
