1、Designation: F 331 05Standard Test Method forNonvolatile Residue of Solvent Extract from AerospaceComponents (Using Flash Evaporator)1This standard is issued under the fixed designation F 331; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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 determination of nonvolatilematter, that is, residue on evaporation
3、, in 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 F 303. In cases in whichanalysis of particulate contamination is also required, beforesubjecting the extract to the following me
4、thod, it should beprocessed in accordance with Practice F311(Note 1). Particlecount analysis should then be performed in accordance withTest Methods F 312.NOTE 1Membrane filters with a maximum extractable content of 0.5weight % should be used on samples to be processed by this test method.Convention
5、al 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 regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does
6、 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 use.2. Referenced Documents2.1 ASTM Stand
7、ards:2D 1193 Specification for Reagent WaterF 303 Practices for Sampling Aerospace Fluids from Com-ponentsF311 Practice for ProcessingAerospace Liquid Samples forParticulate Contamination Analysis Using Membrane Fil-tersF 312 Test Methods for Microscopical Sizing and CountingParticles from Aerospace
8、 Fluids on Membrane Filters2.2 IEST Standard:3IEST-STD-1246D Product Cleanliness Levels and Con-tamination Control Program3. Summary of Test Method3.1 A sample of fluid or the filtrate (Note 1) from a sampleof extract from components is evaporated as necessary toapproximately 20 mL in a flash evapor
9、ator. 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 beingevaporated.4.2 Analytical Balance, single pan or magneti
10、cally dampeddouble pan.NOTE 2Sensitivity shall be suitable to obtain the required precisionnoted in 9.1.4.3 Evaporator, flash, batch-type.4.4 Graduated Cylinder.4.5 Tongs, laboratory, for manipulating weighing foildishes.4.6 Desiccator, balance, to be placed in balance case.4.7 Desiccator, cooling w
11、ith plate.4.8 Weighing Vessels, aluminum foil weighing dishes.4.9 Pressure Source, capable of providing 85 KPa (25-in.Hg) for short interval.4.10 Bottles, sample.4.11 Distillation Apparatus, laboratory, all glass (requiredwhere solvents with sufficiently low residue are not available).Do not use gre
12、ase or oil to lubricate glass joints.5. 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 of the Commit-tee on Analytical Reagents of the American Chemical Soc
13、iety1This test method 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, 2005. Published November 2005. Originallyapproved in 1970. Last previ
14、ous edition approved in 2000 as F 331 00.2For 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 Stan
15、dardization Document Order Desk, Bldg. 4 Section D, 700Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.where such specifications are available.4Other grades may beused, provided
16、it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D 1193.5.3 Solvent for Ex
17、tracting and RinsingThe baseline NVRof the solvent shall not exceed 10 % of the requirement beingtested.5.4 Cleaning AgentLiquid surface-active agent.Approvedequivalent may be used, provided they can be adequatelyrinsed from the surface, leaving a negligible residue.5.5 Desiccant, silica gel, indica
18、ting.6. Preparation of Apparatus6.1 Wash the inner walls of the evaporator flask andgraduated cylinder thoroughly with a solution of liquid,surface-active cleaning agent in hot water and rinse with tapwater (Note 3). Dry thoroughly. Double rinse with test solvent.NOTE 3Distilled or deionized water s
19、hall 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. Dry theweighing vessels in the oven at 65C for 1 h. Place theweighing vessels in the desiccator for 30 min minimum. Do nottouch foil dishes with the f
20、ingers. Use laboratory tongs orforceps as applicable.7. Procedure7.1 Determine sample volume (Note 4) using 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.)
21、Fill the evaporation pan with water, turn on theimmersion heater, and adjust the temperature to approximately50C (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
22、at a pressure of 35 to 80 KPa (vacuum of 10- to 24-in.Hg) (Note 8). Continue until volume is reduced to 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 to
23、tal volume of 20 to 25 mL, which is to be addedto the sample.NOTE 6Use a temperature that is appropriate 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 con-denser is used instead of the cooling flask.NOTE
24、8Lower pressure ranges are recommended for solvents such astrichlorotrifluoroethane, heptane, acetone, and mixtures oftrichloroethane/ethanol or cyclohexane/isopropyl alcohol than for solventssuch as straight isopropyl alcohol or ethyl acetate/cyclohexane mixture.7.2 Release the vacuum and remove th
25、e 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 fr
26、om 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 the
27、 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 4.11.8. Calculation8.1 For ex
28、tracted 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.
29、 Precision and Bias9.1 RepeatabilityDuplicate results by the same operatorshould not be considered suspect unless they differ by morethan 0.4 mg.9.2 ReproducibilityThe averages of duplicate results bydifferent operators in different laboratories should not beconsidered suspect unless they differ by
30、more than 0.6 mg.10. Keywords10.1 extractable content; flash evaporator; molecular con-tamination; nonvolatile residue; NVR; solvent4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the Amer
31、ican 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.F331052ASTM International takes no position respecting the validity of any patent ri
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