1、Designation: F331 13Standard Test Method forNonvolatile Residue of Solvent Extract from AerospaceComponents (Using Flash Evaporator)1This standard is issued under the fixed designation F331; the number immediately following the designation indicates the year of originaladoption or, in the case of re
2、vision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of nonvolatilematter, that is, residue on evaporation, i
3、n solvent extract fromaerospace components, using a rotary flash evaporator.1.2 The procedure for extraction from components is de-scribed in practices such as Practice F303. Before subjectingthe extract to the following method, it should be processed toremove the insoluble particulate in accordance
4、 with PracticeF311 (Note 1). Particle count analysis of the removed particu-late may then be performed in accordance with Test MethodF312. If particulate is not removed from the extract prior toperforming this method, this should be noted on the test report.NOTE 1Membrane filters with a maximum extr
5、actable content of 0.5weight % should be used on samples to be processed by this test method.Conventional membranes contain 5 to 10 % extractables. For obtainingvery low background levels, consideration should be given to usingmembranes without grid marks.1.3 The values stated in SI units are to be
6、regarded asstandard.1.4 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 practices and determine the applica-bility of regulatory limitations prior to
7、 use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterF303 Practices for Sampling for Particles in AerospaceFluids and ComponentsF311 Practice for Processing Aerospace Liquid Samples forParticulate Contamination Analysis Using Membrane Fil-tersF312 Test Methods for Mic
8、roscopical Sizing and CountingParticles from Aerospace Fluids on Membrane Filters2.2 IEST Standard:3IEST-STD-1246D Product Cleanliness Levels and Contami-nation Control Program3. Summary of Test Method3.1 A sample of fluid or the filtrate (Note 1) from a sampleof extract from components is evaporate
9、d as necessary toapproximately 20 mL in a flash evaporator. The residue is thentransferred to a foil dish and the evaporation completed byheating to a constant weight.4. Apparatus4.1 Oven, gravity convection provided with suitable ther-mometer and a temperature range suitable for the solvent beingev
10、aporated.4.2 Analytical Balance, single pan or magnetically dampeddouble pan.NOTE 2Sensitivity shall be suitable to obtain the required precisionnoted in 10.1.4.3 Evaporator, flash, batch-type.4.4 Graduated Cylinder.4.5 Tongs or forceps, laboratory, for manipulating weighingfoil dishes.4.6 Desiccato
11、r, balance, to be placed in balance case.4.7 Desiccator, cooling with plate.4.8 Weighing Vessels, aluminum foil weighing dishes. Thesemay be purchased pre-formed dishes or may be constructedfrom clean aluminum foil.4.9 Pressure Source, capable of providing 85 KPa (25-in.Hg) for short interval.4.10 D
12、istillation Apparatus, laboratory, all glass (requiredwhere solvents with sufficiently low residue are not available).Do not use grease or oil to lubricate glass joints.1This test method is under the jurisdiction of ASTM Committee E21 on SpaceSimulation and Applications of Space Technology and is th
13、e direct responsibility ofSubcommittee E21.05 on Contamination.Current edition approved June 1, 2013. Published July 2013. Originally approvedin 1970. Last previous edition approved in 2005 as F331 05. DOI: 10.1520/F0331-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcont
14、act 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 Standardization Document Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.Copyrig
15、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications
16、 of the Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity
17、of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193.5.3 Solvent for Extracting and RinsingThe baseline NVRof the solvent shall not exceed 10 % of the requirement beingtested.5.4 Cleaning AgentLiquid surface-active agent. A
18、pprovedequivalent may be used, provided they can be adequatelyrinsed from the surface, leaving a negligible residue.5.5 Desiccant, silica gel, indicating.6. Preparation of Apparatus6.1 Wash the inner walls of the evaporator flask andgraduated cylinder thoroughly with a solution of liquid,surface-act
19、ive cleaning agent in hot water and rinse with tapwater (Note 3). Dry thoroughly. Double rinse with test solvent.NOTE 3Distilled or deionized water shall be used in areas in whichhardness or contamination increase the blank over the allowable level.6.2 Soak the weighing vessels in solvent for 1 h. D
20、ry theweighing vessels in the oven at 65C or 3C above theevaporation point of the solvent for 1 h. Place the weighingvessels in the desiccator for 30 min minimum. Do not touchfoil dishes with the fingers. Use laboratory tongs or forceps asapplicable.7. Procedure7.1 Determine sample volume (Note 4) u
21、sing a cleangraduated cylinder. Transfer (Note 5) the sample to a cleanflash evaporator flask.Assemble the apparatus. (WarningDoNOT use stopcock grease on the glass joints of the evaporatorflask.) Fill the evaporation pan with water, turn on theimmersion heater, and adjust the temperature to approxi
22、mately50C (Note 6). Turn on the cold water supply and adjust thefeed so that running water covers the entire outer surface of thecooling flask (Note 7). Start the flash evaporator motor andoperate at a pressure of 35 to 80 KPa (vacuum of 10- to 24-in.Hg) (Note 8). Continue until volume is reduced to
23、 10 to 20 mL.NOTE 4The solvent used for testing should be recorded with thecollected data for each sample.NOTE 5All transfers should be accomplished with a double-rinse,using three aliquots of a total volume of 20 to 25 mL, which is to be addedto the sample.NOTE 6Use a temperature that is appropriat
24、e for the solvent used, butdo not exceed the weighing vessel drying temperature in 6.2.NOTE 7In some models of flash evaporators a water-cooled condenseris used instead of the cooling flask.NOTE 8Lower pressure ranges are recommended for solvents such asheptane, acetone, and mixtures of cyclohexane/
25、isopropyl alcohol than forsolvents such as straight isopropyl alcohol or ethyl acetate/cyclohexanemixture. Laboratories that have supplies of trichlorotriflouroethane ortrichloroethane/ethanol may use those solvents if they are legally allowedin their jurisdiction.7.2 Release the vacuum and remove t
26、he flask. Using cleantongs, preweigh a foil dish from the desiccator (Note 9).Transfer (Note 5) the sample from the flask to the preweighedfoil dish.NOTE 9The cover shall be kept securely on the desiccator exceptwhen inserting or removing weighing vessels. Desiccant must be replacedwhen it changes f
27、rom blue to pink.7.3 Place the foil dish in the oven until thoroughly dry.Remove and place in the desiccator to cool for 30 min. Removeand weigh to the nearest 0.2 mg.7.4 If results are in excess of the allowable limits, repeat 7.3,except place the dish in the oven for an additional 30 min.7.5 If th
28、e blank exceeds 10 % of requirement limit, repeat7.1-7.4, using a minimum of 500-mL solvent for blank analysis(Note 10). If the blank exceeds 10 % again, the solvent qualityis suspect.NOTE 10Purity of solvents can be improved by distilling it usingapparatus called out in 4.10.8. Calculation8.1 For e
29、xtracted samples, report the weight in mg/unitextent in accordance with IEST-STD-1246D or equivalent.8.2 For solvents and reagents used in this test method,calculate the nonvolatile residue (NVR) in mg/unit volume:NVR 5 A/V! x1000 mL1L(1)where:A = weight of residue, mg, andV = volume of sample, mL.9
30、. Reporting9.1 NVR results will vary depending on the solvent used forsampling of the contaminant. When reporting test results, thetest report must report the solvent used for sampling.9.2 The surface area of hardware sampled versus the totalsurface area of the hardware being evaluated will impact t
31、hestatistical reliability of this test method. When the full surfacearea of a component is not sampled, the actual or approximatesurface area sampled shall be reported. When multiple samplesare taken from different locations on a large surface area toprovide a more accurate measure of the NVR presen
32、t, all NVRmeasurements shall be reported. If a sufficient number ofsamples are taken, as when qualifying a new cleaning process,statistical deviation shall also be reported.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the
33、testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc., (USPC), Rockville,MD.F331 1329.3 The report shall note whether p
34、articulate was filtered outprior to the measurement of NVR.9.4 NVR residue remaining after the completion of this testmethod may be further analyzed by infrared spectroscopy orother methods if qualitative identification of the contaminantconstituents is desired.10. Precision and Bias10.1 Repeatabili
35、tyDuplicate results by the same operatorshould not be considered suspect unless they differ by morethan 0.4 mg.10.2 ReproducibilityThe averages of duplicate results bydifferent operators in different laboratories should not beconsidered suspect unless they differ by more than 0.6 mg.11. Keywords11.1
36、 extractable content; flash evaporator; molecular con-tamination; nonvolatile residue; NVR; solventASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that deter
37、mination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or
38、withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that
39、 your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (
40、single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).F331 133
