1、Designation: E 1560 06Standard Test Method forGravimetric Determination of Nonvolatile Residue FromCleanroom Wipers1This standard is issued under the fixed designation E 1560; 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 wipers used inass
3、embly, cleaning, or testing of spacecraft, but not from thoseused for analytical surface sampling of hardware.1.2 The values stated in SI units are to be regarded as thestandard. No other units of measurement are included in thisstandard.1.3 The NVR of interest is that which can be extracted fromcle
4、anroom wipers using a specified solvent that has beenselected for its extractive qualities.Alternative solvents may beselected, 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
5、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:2D 1193 Specification for
6、Reagent WaterF24 Test Method for Measuring and Counting ParticulateContamination on SurfacesF50 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 Particles2.2 Military Sta
7、ndards:Air Force T.O. 00-25-203 Contamination Control of Aero-space Facilities, U.S. Air Force3MIL-F-51068F Filters, Particulate (High Efficiency, FireResistant)3,4MIL-STD-1916 Acceptance on Zero Sampling Inspection32.3 Federal Standards:Fed Spec. O-E-00760 Ethyl Alcohol, Reagent Grade3Fed Spec. O-T
8、-620 1,1,1-Trichloroethane, Technical, Inhib-ited (Methyl Chloroform)3Fed. Std. 209E Airborne Particulate Classes for Clean-rooms and Clean Zones3,52.4 Other Documents:ISO/DIS 14644-1 Cleanrooms and Associated ControlledEnvironments, Classification of air cleanliness6ISO/DIS 14644-2 Cleanrooms and A
9、ssociated ControlledEnvironments, Specifications for testing and monitoring toprove continued compliance with ISO 14644-163. Terminology3.1 Definitions:3.1.1 contaminantunwanted molecular or particulate mat-ter that could affect or degrade the performance of thecomponents on which they are deposited
10、.3.1.2 contaminationa process of contaminant transport oraccretion or both.3.1.3 environmentally controlled areacleanrooms, cleanfacilities, controlled work areas, and other enclosures that aredesigned to protect hardware from contamination. Cleanlinessis achieved by controlling airborne particulate
11、 matter, tempera-ture, relative humidity, materials, garments, and personnelactivities. Guidelines for controlled areas can be found in Table3-1 of Air Force T.O. 00-25-203.3.1.4 high effciency particulate air (HEPA)a term de-scribing filters having an efficiency of 99.97 % for removal of1This speci
12、fication is under the jurisdiction of ASTM Committee E21 on SpaceSimulation and Applications of Space Technology and is the direct responsibility ofSubcommittee E21.05 on Contamination.Current edition approved Nov. 1, 2006. Published December 2006. Originallyapproved in 1993. Last previous edition a
13、pproved in 2001 as E 1560 95 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, 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 Standardi
14、zation Documents Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5098, Attn: NPODS.4The use of Di Octyl Phthalate (DOP) in leak testing of filters or filterinstallation is not acceptable.5Fed-Std-209E has been replaced by ISO/DIS 14644-1 and -2, but may continueto be used by m
15、utual agreement.6Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.0.3-m and larger particles. For this appli
16、cation, filters shallmeet the requirements of MIL-F-51068F (2.2) and 6.1 of thistest method.3.1.5 molecular contaminant (nonparticulate)may be in agaseous, liquid, or solid state. It may be uniformly or nonuni-formly distributed or be in the form of droplets. Molecularcontaminants account for most o
17、f the NVR.3.1.6 NVRthat 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)a piece of matterin a solid state, with observable length, width, and thickness.The
18、 size of a particle is defined by its greatest dimensions andis expressed in m.4. Summary of Test Method4.1 A wiper to be tested is placed in a clean blankedcontainer and a measured volume of solvent is added to thecontainer.4.2 The container is placed in a heated ultrasonic cleanerand agitated by u
19、ltrasonic action for a specified period of timeand the wiper is 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 weigh-ing dish and evaporated to constant
20、weight.4.5 The results are expressed in milligrams/0.1 squaremetres of wiper surface area or in mg/unit mass of wiper.4.6 A control 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 s
21、ame day, additional blanks will not be necessary, but willrely on the blank value from the first test.4.7 NVR samples thus obtained will be saved for analysis toidentify contaminant species if a more complete analysis isnecessary.5. Significance and Use5.1 The NVR obtained by this test method is tha
22、t amountwhich is available for release by wipers in normal use.5.2 Evaporation of the 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 test temperature has not been shown to result insi
23、gnificant variances.5.3 Numerous other methods are being used to determineNVR. This test method is not intended to replace test methodsused for other applications.6. Apparatus and Materials6.1 Unidirectional airflow work station, 100 % exhaust forhandling solvents. Must meet the particulate air clea
24、nlinessClass 2 (100), or better in accordance with ISO/DIS 14644-1and ISO/DIS 14644-2(Fed-Std-209), latest revision whentested per Practice F50. HEPA filters in the work station mustnot have been tested with Di-Octyl Phthalate (DOP) at anytime. Temperature shall be controlled within a range of 20 to
25、25C and relative humidity to less than 50 %.6.2 Solvent, 1,1,1-Trichloroethane per Fed Spec. O-T-620.6.3 Solvent, Ethanol, per Fed Spec.O-E-00760.6.4 Analytical balance, 0.1-mg readability, 0.1-mg preci-sion.7Capacity to be determined by user.6.5 Vacuum filtration system, 25-mm diameter, consisting
26、ofa membrane filter funnel and vacuum pump that will provide apressure of 250 Torr (20-in. Hg vac.). See Fig. 1. Other sizefilters may be used as needed. All items that will come incontact with solvents during analysis shall be of glass, stainlesssteel, or other material that will not affect the ana
27、lysis viainduced contaminants.6.6 Solvent resistant membrane filters, Fluorocarbon,25-mm diameter, 0.2-m nominal pore size.8The use ofsupported membrane filters is not recommended because ofpossible adverse effects of the solvent on the support media.6.7 Teflon-coated tweezers, or hemostat, unserrat
28、ed tips.6.8 Beakers, low form glass, 500 ml.6.9 Laboratory detergent, liquid.96.10 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 MV/cm.6.13 Gloves,10Barrier-type, low particle-
29、generating, lowoutgassing, per I.E.S. Recommended Practice RP-CC-005-88.6.14 NVR solvent, consisting of three parts 1,1,1-Trichloroethane and one part ethanol v/v. Must be verified tocontain no more than 0.35-mg NVR per 300-mL solvent (0.12mg per 100 mL) when tested in accordance with Section 8 ofth
30、is test method.NOTE 1In the event 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 “carr
31、yover” ofheavier fractions in the vapor phase, which will cause the solvent to failthe required purity tests.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 sizes may be used.6.16 Evaporating dishes
32、, aluminum foil, 43-mm diameter.116.17 Drying oven,12cleanroom compatible, stainless steelinterior.7Analytical Balance, capable of measuring to 0.01 mg.8Nuclepore Corp. PTFE Filinert membrane filter, P/N 130606, and MilliporeCorp. Fluoropore filter, P/N 02500 have been found to be satisfactory. Othe
33、requivalent, solvent-resistant filters may be used. Larger diameter filters to fit largerfilter assemblies are acceptable.The sole source of supply of the apparatus known to the committee at this timeis Nuclepore Corp. If you are aware of alternative suppliers, please provide thisinformation to ASTM
34、 International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.9A 3 % solution of liquid detergent.10Gloves are necessary to protect the analyst from exposure to NVR solvent andto minimize the possibility of intro
35、ducing any artifacts from the analyst into thesample. Must be solvent resistant and provide a firm grip on items being grasped bythe gloves.11Evaporating dishes.12Drying oven, stainless steel interior.E15600627. Preparation of Equipment7.1 All operations shall be performed in a work station per6.1.7
36、.2 Wash all glassware, filter funnels, weighing dishes, andassociated tools in a 3 % solution of liquid detergent indeionized water. Rinse with deionized water for a period of 1min, followed by rinsing with acetone or methanol, then withthe NVR solvent described in 6.12. Dry in a cleaned oven for1 h
37、 at 35C, remove, and store in a desiccator 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.8. NVR and System Blank8.1 The NVR of the solvent, and all glasswa
38、re or other itemsthat will come in contact with the solvent during the analysis,shall be determined before use. The only exception is whenseveral tests are to be run consecutively, in which case, theblank only needs to be determined once for a batch. It must beremembered that this solvent will absor
39、b moisture from theatmosphere every time the storage container is opened, so largequantities should not be processed 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 blank shall be less than 0.35 mg per 300 mL.8.1.4 Record re
40、sults of blank analysis in laboratory logbook.8.1.5 Solvents that do not meet the NVR requirements shalleither be redistilled and retested or can be appropriatelymarked and set aside for other uses, including cleaningpurposes.8.1.6 Only verified clean, noncontaminating metals, glass,or fluorocarbon
41、containers are acceptable for storage ofblanked solvent.9. Procedure9.1 All operations shall be performed in a work station per6.1.9.2 Assemble the filtration assembly according to manufac-turers instructions.9.3 When reporting results on the basis of mg per unit area,place enough wipers to provide
42、a combined surface area of 0.1m2, minimum, in a precleaned 500-mL beaker.13For example,a wiper measuring 6 by 6 in. will have a surface area of 36 in.2,thus requiring four wipers to provide the necessary surfacearea. Do not cut wipers to simplify calculations or for any otherpurpose. The wipers must
43、 be tested as received from thesupplier. (No attempt shall be made to determine the surfacearea of each individual fiber in a woven product.) Whenreporting results on the basis of mg per unit mass, weigh asample of the wipers to be tested (similar to above sample size)to an accuracy of 0.1 mg. Place
44、 in beaker as above.13It is assumed that selection of samples from a shipment has been made inaccordance with MIL-STD-1916 to provide a truly representative sample.TEST REPORTING FORMNVR DATA SHEETSAMPLE IDENTIFICATIONMATERIAL TYPESIZE, COLOR, ETC.SPECIFICATIONDATE RECEIVED DATE TESTEDREQUESTER DEPT
45、 TEL. NO.TYPE OF SOLVENT USED PER 6.14 OTHERRESULTS PER UNIT AREA:MASS OF DISH AND RESIDUE (A) _ MGMASS OF WEIGHING DISH (B) _ MGBLANK OF SOLVENT (C) _ MGSURFACE AREA (D) _ MGNVR EXTRACTED FROM SAMPLE _ MG/0.1 m2TO SPEC YES _NO _RESULTS PER UNIT MASS:MASS OF DISH AND RESIDUE (E) _ MGMASS OF WEIGHING
46、 DISH (F) _ MGMASS OF SOLVENT (G) _ MGMASS OF WIPER (H) _ MGNVR EXTRACTED FROM WIPER _ MG/GRAMTO SPEC YES _NO _COMMENTS (use additional sheets if necessary)ANALYZED BYPRINT NAMESIGNATUREFIG. 1 Test Reporting FormNVR Data SheetE15600639.4 Add 300-mL blanked NVR solvent to beaker. Coverbeaker with a w
47、atchglass to minimize contamination of sampleby fallout.NOTE 2Wipers larger than 0.1 m2will require 500 mL of solvent toensure complete wetting of the sample.9.5 Place beaker in ultrasonic tank that has been filled withfluid heated to 35 6 2C and install tank cover to position thebeaker in the tank.
48、 Typically, the fluid used is D.I. water.9.6 Agitate for 30 min. This agitation is necessary to ensurethat all available NVR is contacted by solvent and removedfrom the wiper being tested.9.7 Remove beaker from tank and extract wiper(s) usingprecleaned tongs. Hold wipers over the beaker until drippi
49、ngceases. Place damp wiper on a tray or rack to dry. When theitem is dry, as determined by a lack of solvent odors, it will beplaced in a clean Nylon plastic envelope, and saved for futurereference, or discarded at the option of the analyst. No furtheranalysis will be performed on this sample.9.8 Filter the solvent into a precleaned and blanked beakerthat has been instal
