1、Designation: E1731 11Standard Test Method forGravimetric Determination of Nonvolatile Residue fromCleanroom Gloves1This standard is issued under the fixed designation E1731; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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 determination of solventextractable nonvolatile residue (NVR) from gloves used incleanr
3、ooms where spacecraft are assembled, cleaned, or tested.1.2 The NVR of interest is that which can be extracted fromgloves using a specified solvent that has been selected for itsextracting qualities, or because it is representative of solventsused in the particular facility.Alternative solvents may
4、be used,but since their use may result in different values beinggenerated, they must be identified in the procedure data sheet.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all
5、 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 practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification f
6、or Reagent WaterE2217 Practice for Design and Construction of AerospaceCleanrooms and Contamination Controlled AreasF50 Practice for Continuous Sizing and Counting of Air-borne Particles in Dust-Controlled Areas and Clean RoomsUsing Instruments Capable of Detecting Single Sub-Micrometre and Larger P
7、articlesG120 Practice for Determination of Soluble Residual Con-tamination by Soxhlet Extraction2.2 Federal Standards3:Fed Std 209E Airborne Particulate Cleanliness Classes inCleanrooms and Clean Zones42.3 Other Documents:IEST-RP-CC001 HEPA and ULPA Filters5IEST-RP-CC005 Gloves and Finger Cots Used
8、in Clean-rooms and Other Controlled Environments5Industrial Ventilation, A Manual of Recommended Prac-tice6ISO 14644-1 Cleanrooms and Associated Controlled Envi-ronments, Classification of air cleanliness7ISO 14644-2 Cleanrooms and Associated Controlled Envi-ronments, Specifications for testing and
9、monitoring toprove continued compliance with ISO 14644-173. Terminology3.1 Definitions:3.1.1 contaminant, nunwanted molecular or particulatematter that could affect or degrade the performance of thecomponents upon which they are deposited.3.1.2 contamination, na process of contaminant transportor ac
10、cretion, or both.3.1.3 environmentally controlled area, ncleanrooms,clean facilities, controlled work areas, and other enclosures thatare designed to protect hardware from contamination. SeeIndustrial Ventilation, A Manual of Recommended Practice forsuggestions on facility operation. Cleanliness is
11、achieved bycontrolling airborne particulate matter, temperature, relativehumidity, materials, garments, and personnel activities. Guide-lines for controlled areas can be found in Practice E2217.3.1.4 high effciency particulate air (HEPA), na termdescribing filters having an efficiency of 99.97 % for
12、 removalof 0.3-m and larger particles. For this application, filters shallmeet the requirements of IEST-RP-CC001 (2.3 and 6.1 of thistest method).1This test method is under the jurisdiction of ASTM Committee E21 on SpaceSimulation and Applications of Space Technology and is the direct responsibility
13、 ofSubcommittee E21.05 on Contamination.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 1995. Last previous edition approved in 2006 as E1731 06. DOI:10.1520/E1731-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Servic
14、e at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:/dodssp.daps.dla.mil.4Fed-St
15、d-209E has been replaced by ISO 14644-1 and -2, but may continue tobe used by mutual agreement.5Available from the Institute of Environmental Sciences and Technology, 2340South Arlington Heights Road, Suite 100, Arlington Heights, IL 60005- 4516,http:/www.iest.org.6Available from Committee on Indust
16、rial Ventilation, American Conference ofGovernmental Industrial Hygienists, 1330 Kemper Meadow Dr., Suite 600, Cincin-nati, OH 45240. http:/www.acgih.org/about/committees/c_indvnt.htm.7Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/ww
17、w.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.5 molecular contaminant (nonparticulate), nmay bein a gaseous, liquid, or solid state. It may be uniformly ornonuniformly distributed or be in the form of droplets. Mo-le
18、cular contaminants account for most of the NVR.3.1.6 NVR, nthat quantity of molecular matter remainingafter the filtration of a solvent containing contaminants, andevaporation of the solvent at a specified temperature.3.1.7 particle (particulate contaminant), na piece of mat-ter in a solid state, wi
19、th observable length, width, and thick-ness. The size of a particle is defined by its greatest dimensionand is expressed in micrometres.4. Summary of Test Method4.1 A glove to be tested is cut into several standard-sizedpieces. The pieces are placed in a clean blanked container anda measured volume
20、of solvent is added to the container. (SeeNote 1.)4.2 The container is placed in a heated ultrasonic cleaner, ora heated water bath, and heated (and agitated if in an ultrasonicbath) for a specific length of time, after which the pieces ofglove are removed from the container.4.3 The solvent in the c
21、ontainer is filtered into another cleancontainer and allowed to evaporate to a low volume.4.4 The solvent is transferred to a clean preweighed weigh-ing dish and evaporated to a constant weight.4.5 The results are expressed in mg/cm2of glove surfacearea or in mg/unit mass of glove sections.4.6 A con
22、trolled blank shall be run on all solvents, filtrationcomponents, and all other equipment associated with theanalysis. In the event that more than one determination is runthe same day, additional blanks will not be necessary, but willrely on the value from the first test.4.7 NVR samples thus obtaine
23、d may be used for analysissuch as IR or FTIR to identify contaminant species if required.NOTE 1Some cleanroom gloves are of a coated or layered construc-tion or have different textures applied to the inside and outsid e surfaces.Because the inside and outside surfaces of these gloves may releasediff
24、erent quantities of nonvolatile residue, results using this method maynot reflect the actual potential for transfer of contamination from this typeof glove to hardware surfaces.5. Significance and Use5.1 The NVR obtained by this test method is that amountwhich is available for release by the gloves
25、onto handledsurfaces.5.2 Evaporation of solvent at the stated temperature is toquantify the NVR that can be expected to exist at roomtemperature, since the slight difference between room tempera-ture and the test temperature is not likely to result in significantvariances.5.3 This method may be more
26、 aggressive than necessary todetermine the suitability of cleanroom gloves that are restrictedto dry operations only.5.4 Various other methods exist for determining NVR, forexample Practice G120 and IES-RP-CC005. This test is notintended to replace test methods used for other purposes.6. Apparatus a
27、nd Materials6.1 Unidirectional Airflow Work Station, 100 % exhaust, forhandling solvents. Must meet the particulate air cleanlinessClass 5 (100) or better in accordance with ISO 14644-1 andISO 14644-2 (Fed-Std-209). HEPA filters in the work stationmust not have been tested with Di-Octyl Phthlate (DO
28、P) at anytime. Filters should conform to IEST-RP-CC001 HEPA andULPA Filters. See Practice F50 for information on airborneparticle counting methods. Temperature shall be controlledwithin a range of 20 to 25C and relative humidity to less than60 %.6.2 Solvent, Acetone, Reagent grade A.C.S.6.3 Analytic
29、al Balance, 0.01-mg readability, 0.1-mg preci-sion. Capacity to be determined by the user.6.4 Vacuum Filtration System, 25-mm diameter, consistingof a membrane filter funnel and vacuum pump that will providea pressure of 250 torr (20 in. Hg vac.). Other size filtrationsystems may be used as needed.
30、All items that will come incontact with solvents during analysis shall be made of glass,stainless steel, or other materials that will not affect theanalysis via induced contamination.Any house vacuum systemmay be used.6.5 Solvent-Resistant Membrane Filters, Fluorocarbon,25-mm diameter, 0.2-m nominal
31、 pore size. The use ofsupported membrane filters is not recommended because ofpossible adverse effects of the solvent on support media.6.6 Teflon-Coated Tweezers, or Hemostat, unserrated tips.6.7 Beakers, low form glass, 500 mL.6.8 Laboratory Detergent, liquid.6.9 Methanol, Reagent grade, A.C.S.6.10
32、 Deionized Water, organic free, Type II per Specifica-tion D1193, with a minimum resistivity of 1.0 megohm-cm.6.11 Gloves, barrier type, low particle-generating, low out-gassing, per IEST-RP-CC005.6.12 NVR Solvent, acetone or other solvent. (See Note 2.)Must be verified to contain no more than 0.35-
33、mg NVR per300-mL solvent (0.12 mg/100 mL) when tested in accordancewith Section 8 of this test method (See Note 3).NOTE 2Other solvents may be used if they are more representative ofservice conditions, but the actual solvent used must be reported perSection 11 of this test method.NOTE 3In the event
34、that the solvent does not meet the required puritylevel, it may be necessary to triple distill it, keeping the temperature of thevapor phase of the distillate no more than 0.2C higher than the boilingpoint of the solvent. Higher temperatures will result in the “carryover” ofheavier fractions in the
35、vapor phase, which will cause the solvent to failthe required purity tests.6.13 Ultrasonic Tank, 5.7-L capacity nominal, with heatercapable of maintaining a temperature of 35 6 2C, and coverto position beakers in tank. Other sizes may be used.6.14 Evaporating Dishes, aluminum foil, 43-mm diameter,or
36、 acceptable equivalent.6.15 Drying Oven (desiccator), stainless steel interior.7. Preparation of Equipment7.1 All operation shall be performed in the work station per6.1.7.2 Wash all glassware, filter funnels, weighing dishes, andthe associated tools (see Note 4). Rinse with deionized waterfor a per
37、iod of 1 minute followed by rinsing with acetone orE1731 112methanol, then with the NVR solvent as described in 6.12. Dryin a cleaned oven for1hat35to40C, remove and store in adesiccator until used.7.3 All items, such as glassware, funnels, and so forth, thatwill come in contact with the NVR solvent
38、 during analysis,will be blanked per Section 8 of this test method before use.NOTE 4A3 % solution of liquid detergent in deionized water has beenfound to be effective.8. NVR and System Blank8.1 The NVR of the solvent, and all glassware and otheritems that will come in contact with the solvent during
39、 theanalysis, shall be determined before use. The only exception iswhen several tests are to be run consecutively, in which case,the blank only needs to be determined once for a batch. It mustbe remembered that the solvent may absorb moisture from theatmosphere, so it should be kept covered and smal
40、l quantitiesprocessed at one time.8.1.1 Pour 300 mL of solvent into a 500-mL beaker cleanedper 7.2.8.1.2 Perform analysis per Section 9.8.1.3 NVR system blank shall be less than 0.35 mg/300 mL.8.1.4 Record results of blank analysis on the test data sheet.8.1.5 Solvents that do not meet the NVR requi
41、rements maybe redistilled and retested.8.1.6 Only verified clean, non-contaminating metals, glass,or fluorocarbon containers are acceptable for storage ofblanked solvent.9. Procedure9.1 All operations shall be performed in a work station per6.1.9.2 Assemble filtration assembly according to manufactu
42、r-ers instructions.9.3 Cut and place in a beaker at least two sections 5 by 5 cmfrom each glove, preferably from the palm and the back of theglove. Cut up at least two gloves, or enough surface area for200 cm2, minimum, counting both sides of the glove, in aprecleaned 500-mL beaker. Test the gloves
43、as received fromthe supplier. When reporting results on the basis of mg/unitmass, weigh the cut sections of gloves to an accuracy of 0.01mg. Place in 500-mL beaker as above.9.4 Add 300 mL of blanked NVR solvent to beaker. Coverbeaker with a watchglass to minimize sample contaminationfrom fallout.9.5
44、 Place beaker in ultrasonic tank that has been filled withultrasonic tank fluid heated to 35 6 2C and install tank coverto position the beaker in the tank. Typical fluid used is D.I.water, but other fluids are allowed.9.6 Ultrasonic agitate for 15 min. This agitation is necessaryto assure that all a
45、vailable NVR is contacted by the solvent andremoved from the glove segments being tested.9.7 Remove beaker from tank and extract glove sectionsusing precleaned tongs. Hold the glove segments over thebeaker until dripping ceases. Note any discoloration, deterio-ration, or hardening of the glove segme
46、nts in the commentssection of the test data sheet. Place the damp glove segmentson a tray or rack to dry. When they are dry, as determined bylack of solvent odors, either discard, or store in a clean nylonbag, at the option of the analyst. No further analysis isperformed on these samples.9.8 Place t
47、he vessel in HEPA-filtered airflow at ambienttemperature. Position the beaker near or directly under theairflow. Allow evaporation to approximately 10 mL. It may benecessary to cover the vessel partly with a watchglass toprotect against fallout during evaporation.9.9 Transfer solvent to a clean, pre
48、weighed weighing dish.Rinse beaker with 10 mL of solvent and add the wash solventto the weighing dish. Repeat this three times. Total rinsevolume shall not exceed 30 mL.9.10 Allow to evaporate in the laminar flow bench until novisible solvent remains.9.11 Place the weighing dish in the oven at 35 6
49、2C for 30min.9.12 Remove the dish from the drying oven, protect con-tents from contamination, and allow to equilibrate to roomambient conditions.9.13 Weigh the dish and contents. Record this weight.9.14 Return dish to oven for 30 min.9.15 Reweigh the dish. Continue equilibrating and reweigh-ing until weight stabilizes (weights vary by 0.1 mg or less).Record the results in the test data sheet,9.16 Retain NVR if further analysis (as by infrared spec-troscopy) is necessary to identify the contaminants.9.17 Calculate as shown below and record results on the test
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