1、Designation: E 1731 06Standard Test Method forGravimetric Determination of Nonvolatile Residue fromCleanroom Gloves1This standard is issued under the fixed designation E 1731; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 determination of solventextractable nonvolatile residue (NVR) from gloves used incle
3、anrooms where spacecraft are assembled, cleaned, or tested.1.2 The values stated in SI units are to be regarded asstandard.1.3 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 o
4、f solventsused in the particular facility.Alternative solvents may be used,but since their use may result in different values beinggenerated, they must be identified in the procedure data sheet.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use.
5、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:2D 1193 Specification for Reagent WaterF50 Practice for Continuous Sizing and C
6、ounting of Air-borne Particles in Dust-Controlled Areas and Clean RoomsUsing Instruments Capable of Detecting Single Sub-Micrometre and Larger ParticlesG 120 Practice for Determination of Soluble Residual Con-tamination by Soxhlet Extraction2.2 Military Standards3:Air Force T.O. 00-25-203 Contaminat
7、ion Control of Aero-space FacilitiesMIL-F-51068F Filters, Particulate (High Efficiency, FireResistant)2.3 Federal Standards3:Fed Spec O-E-00760 Ethyl AlcoholFed Std 209E Airborne Particulate Classes for Cleanroomsand Clean Zones4ISO/DIS 14644-1 Cleanrooms and Associated ControlledEnvironments, Class
8、ification of air cleanliness5ISO/DIS 14644-2 Cleanrooms and Associated ControlledEnvironments, Specifications for testing and monitoring toprove continued compliance with ISO 14644-152.4 Other Documents:IES-RP-CC005.2 Gloves and Finger Cots Used in Clean-rooms and Other Controlled Environments6Indus
9、trial Ventilation, A Manual of Recommended Prac-tice73. Terminology3.1 Definitions:3.1.1 contamination, 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 accr
10、etion, 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 ac
11、hieved bycontrolling airborne particulate matter, temperature, relativehumidity, materials, garments, and personnel activities. Guide-lines for controlled areas can be found in Air Force T.O.00-25-203 Table 3-1.3.1.4 high effciency particulate air (HEPA), na termdescribing filters having an efficien
12、cy of 99.97 % for removalof 0.3-m and larger particles. For this application, filters shallmeet the requirements of 2.3 and 6.1 of this test method.1This test method is under the jurisdiction of ASTM Committee E21 on SpaceSimulation and Applications of Space Technology and is the direct responsibili
13、ty ofSubcommittee E21.05 on Contamination.Current edition approved Nov. 1, 2006. Published December 2006. Originallyapproved in 1995. Last previous edition approved in 2001 as D 1731 95(2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at ser
14、viceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5098, Attn: NPODS.4Fed-Std-209E has been replaced by ISO
15、/DIS 14644-1 and -2, but may continueto be used by mutual agreement.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.6Available from the Institute of Environmental Sciences, 940 E. NorthwestHwy., Mount Prospect, IL 60056.7
16、Available from Committee on Industrial Ventilation, American Conference ofGovernmental Industrial Hygienists, 1330 Kemper Meadow Dr., Suite 600, Cincin-nati, OH 45240.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.5 molecular co
17、ntaminant (nonparticulate), nmay bein a gaseous, liquid, or solid state. It may be uniformly ornonuniformly distributed or be in the form of droplets. Mo-lecular contaminants account for most of the NVR.3.1.6 NVR, nthat quantity of molecular matter remainingafter the filtration of a solvent containi
18、ng contaminants, andevaporation of the solvent at a specified temperature.3.1.7 particle (particulate contaminant), na piece of mat-ter in a solid state, with observable length, width, and thick-ness. The size of a particle is defined by its greatest dimensionand is expressed in micrometres.4. Summa
19、ry 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 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
20、(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 container is filtered into another cleancontainer and allowed to evaporate to a low volume.4.4 The solvent is transferred to a clean preweighed w
21、eigh-ing dish and evaporated to a constant weight.4.5 The results are expressed in mg/sq cm of glove surfacearea or in mg/unit mass of glove sections.4.6 A controlled blank shall be run on all solvents, filtrationcomponents, and all other equipment associated with theanalysis. In the event that more
22、 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 obtained may be used for analysissuch as IR or FTIR if required.NOTE 1Some cleanroom gloves are of a coated or layered construc-tion or have differe
23、nt textures applied to the inside and outside surfaces.Because the inside and outside surfaces of these gloves may releasedifferent quantities of nonvolatile residue, results using this method maynot reflect the actual potential or transfer of contamination from this typeof glove to hardware surface
24、s.5. Significance and Use5.1 The NVR obtained by this test method is that amountwhich is available for release by the gloves 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 b
25、etween room tempera-ture and the test temperature is not likely to result in significantvariances.5.3 Various other methods exist for determining NVR, forexample Practice G 120 and IES-RP-CC005.2. This test is notintended to replace test methods used for other purposes.6. Apparatus and Materials6.1
26、Unidirectional Airflow Work Station, 100 % exhaust, forhandling solvents. Must meet the particulate air cleanlinessclass 2 (100) or better in accordance with ISO/DIS 14644-1and ISO/DIS 14644-2(Fed-Std-209). HEPA filters in the workstation must not have been tested with Di-Octly Phthlate(DOP) at any
27、time. Filters should conform to MIL-F-51068FFilters, Particulate (High Efficiency, Fire Resistant). See Prac-tice F50for information on airborne particle counting meth-ods. Temperature shall be controlled within a range of 20 to25C and relative humidity to less than 60 %.6.2 Solvent, Acetone.6.3 Sol
28、vent, Ethanol per Fed Spec O-E-00760.6.4 Analytical Balance, 0.01-mg readability, 0.1-mg preci-sion. Capacity to be determined by the user.6.5 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.). Oth
29、er size filters may beused as needed. All items that will come in contact withsolvents during analysis shall be made of glass, stainless steel,or other materials that will not affect the analysis via inducedcontamination. Any house vacuum system may be used.6.6 Solvent-Resistant Membrane Filters, Fl
30、uorocarbon,25-mm diameter, 0.2-m nominal pore size. The use ofsupported membrane filters is not recommended because ofpossible adverse effects of the solvent on support media.6.7 Teflon-Coated Tweezers, or Hemostat, unserrated tips.6.8 Beakers, low form glass, 500 mL.6.9 Laboratory Detergent, liquid
31、.6.10 Methanol, Reagent grade, A.C.S.6.11 Acetone, Reagent grade, A.C.S.6.12 Deionized Water, organic free, Type II per Specifica-tion D 1193, with a minimum resistivity of 1.0 megohm-cm.6.13 Gloves, barrier type, low particle-generating, low out-gassing, per IES-RP-CC005.2.6.14 NVR Solvent, acetone
32、. Must be verified to contain nomore than 0.35-mg NVR per 300-mL solvent (0.12 mg/100mL) when tested in accordance with Section 8 of this testmethod.NOTE 2Other solvents may be used if they are more representative ofservice conditions, but the actual solvent used must be reported perSection 11 of th
33、is test method.6.15 Ultrasonic Tank, 5.7-L capacity nominal, with heatercapable of maintaining a temperature of 35 6 2C, and coverto position beakers in tank. Other convenient sizes may beused.6.16 Evaporating Dishes, aluminum foil, 43-mm diameter.6.17 Drying Oven, stainless steel interior.7. Prepar
34、ation 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 3). Rinse with deionized waterfor a period of 1 min followed by rinsing with acetone ormethanol, then with acetone (or other NV
35、R solvent) asdescribed in 6.14. Dry in a cleaned oven for1hat35to40C,remove and store in a dessicator until used.7.3 All items, such as glassware, funnels, and so forth, thatwill come in contact with the NVR solvent during analysis,will be blanked per Section 8 of this test method before use.NOTE 3A
36、3 % solution of liquid detergent in deionized water has beenfound to be effective.E17310628. NVR and System Blank8.1 The NVR of the solvent, and all glassware and otheritems that will come in contact with the solvent during theanalysis, shall be determined before use. The only exception iswhen sever
37、al tests are to be run consecutively, in which case,the blank only needs to be determined once for a batch. It mustbe remembered that this solvent may absorb moisture from theatmosphere, so it should be kept covered and small quantitiesprocessed at one time.8.1.1 Pour 300 mL of solvent into a 500-mL
38、 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 in log book.8.1.5 Solvents that do not meet the NVR requirements shalleither be redistilled and retested or marked and set aside forother uses,
39、including cleaning purposes.8.1.6 Only verified clean, noncontaminating 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 manufactur-ers instru
40、ctions.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 for0.2 m, minimum, counting both sides of the glove, in aprecleaned 500-mL beaker. Test the gloves as received fr
41、omthe supplier. When reporting results on the basis of mg/unitmass, weigh a sample of cut sections of gloves to an accuracyof 0.01 mg. 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 Place
42、 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 availab
43、le 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. Place the damp glove segmentson a tray or rack to dry. When they are dry, as
44、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 the vessel in HEPA-filtered airflow at ambienttemperature. Position the beaker near or directly under theairflow. Allow evaporati
45、on 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, preweighed weighing dish.Rinse beaker with 10 mL of solvent and add the wash solventto the weighing dish. Repeat this three times.
46、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 2C for 30min.9.12 Remove the dish from the oven, protect contents fromcontamination, and allow to equilibrate to room ambientcon
47、ditions.9.13 Weigh the dish and contents. Record weight in logbook.9.14 Return dish to dessicator for 30 min.9.15 Reweigh the dish. Continue equilibrating and reweigh-ing until weight stabilizes (weights vary by 0.1 mg or less).9.16 Retain NVR if further analysis as by infrared (IR)spectroscopy is n
48、ecessary to identify the contaminants.9.17 Record results in log book.10. Calculation of NVR10.1 NVR in mg/0.1 m2.NVR 5 A*2!20*B 1 C!D(1)where:A = mass of sample dish and residue, mg;B = mass of weighing dish, mg;C = mass of solvent, mg; andD = surface area of glove sections in m2.10.2 NVR in mg/uni
49、t massNVR 5E 2 F 1 G!H(2)where:E = mass of sample and weighing dish, mg;F = mass of weighing dish, mg;G = mass of solvent, mg; andH = mass of glove sections.11. Reporting Results11.1 The report shall use the Test Reporting Form, Fig. 1.11.2 The estimated accuracy of the NVR determinationshall be noted. This is based upon the accuracy and precisionof the balance, NVR background from the solvent and blanksamples, and any other factors observed during the testoperations. Explanation, if required, shall be included undercomments.12. Precision and Bias12.1 Precision
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