ASTM D2257-1998(2004) Standard Test Method for Extractable Matter in Textiles《纺织材料中可萃取物的试验方法》.pdf

1、Designation: D 2257 98 (Reapproved 2004)Standard Test Method forExtractable Matter in Textiles1This standard is issued under the fixed designation D 2257; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A

2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This test method covers a procedure for determining

3、theextractable material on most fibers, yarns, and fabrics. Threeoptions are included. Option 1 uses heat and Soxhlet extractionapparatus. Option 2 uses room temperature and extractionfunnels. Option 3 uses either Option 1 or Option 2 extractionbut provides for calculation of extractable matter from

4、 the lossin mass of the material due to the extraction rather than theextractable matter residue.NOTE 1Other standards for the determination of extractable matter intextiles made of specific fibers include: Specification D 541, SpecificationD 681, and Test Method D 1574.1.1.1 The solvents for use in

5、 this method are any solventsthat the party or parties concerned agreed on; such as,Halogenated Hydrocarbon (HH) chloroform, tetrachloroet-hane, alcohol.1.1.2 This test method may not extract cross-linked finishesor resins which may be on the textile.1.2 This standard does not purport to address all

6、 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. See Sections6 and 7.2. Referenced Documents2.1 ASTM Standards:2

7、D 123 Terminology Relating to TextilesD 541 Specification for Single Jute Yarn3D 681 Specification for Jute Rove and Plied Yarn forElectrical and Packing Purposes3D 1574 Test Method for Extractable Matter in Wool andOther Animal Fibers3D 1909 Table of Commercial Moisture Regains for TextileFibersD 2

8、258 Practice for Sampling Yarn for TestingD 3333 Practice for Sampling Manufactured Staple Fibers,Sliver, or Tow for TestingD 4920 Terminology Relating to Moisture in Textiles2.2 Other Documents:IWTO 10-62(E) Method for Determination of the Dichlo-romethane Soluble Matter in Combed Wool Sliver43. Te

9、rminology3.1 Definitions:3.1.1 extractable matter, nnonfibrous material in or on atextile not including water, which is removable by a specifiedsolvent or solvents as directed in a specified procedure.3.1.1.1 DiscussionNonfibrous material is usually oily,waxy, resinous, or polymeric in nature, but m

10、ay also includeother material, such as protein, particularly if ethyl alcohol isused, or in, the extracting solvent.3.1.2 For definitions of other moisture terms related totextiles, refer to Terminology D 4920. For definitions of othertextile terms used in this test method refer to TerminologyD 123.

11、4. Summary of Test Method4.1 The specimen is extracted either in Soxhlet apparatus(Option 1), or extraction funnel (Option 2) first with an agreedsolvent (Note 2). The solvents are evaporated and the residuesand the specimens are dried and weighed separately. Theamounts of extracted matter are repor

12、ted as percentages ofeither the oven-dried mass or of the oven-dried mass pluscommercial moisture regain for the textile.4.2 Alternatively, in Option 3, the specimen is dried andweighed before and after extraction using Option 1 or Option2. Extractable matter is calculated as the loss in mass report

13、ed1This test method is under the jurisdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.51 on Conditioning and,Chemical and Thermal Properties.Current edition approved Oct. 1, 2004. Published November 2004. Originallyapproved in 1989. Last previous edition

14、 approved in 1998 as D 2257 98.2For 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.3Withdrawn.4Available from Int

15、ernational Wool Secretariat, Carlton Gardens, London S.W.1, England.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.as percentages of the extracted oven-dried mass or this massplus commercial moisture regain for the textile.5. Signif

16、icance and Use5.1 This test method may be used for acceptance testing ofcommercial shipments.5.1.1 In case of a dispute arising from differences inreported test results using this test method for acceptancetesting of commercial shipments, the purchaser and the sup-plier should conduct comparative te

17、sts to determine if there isa statistical bias between the laboratories. Competent statisticalassistance is recommended for the investigation of bias. As aminimum, the two parties should take a group of test speci-mens which are as homogeneous as possible and which arefrom a lot of material of the t

18、ype in question. The testspecimens should then be randomly assigned in equal numbersto each laboratory for testing. The average results from the twolaboratories should be compared using appropriate statisticalanalysis and a probability level chosen by the two partiesbefore the testing begins. If a b

19、ias is found, either its causemust be found and corrected, or the purchaser and suppliermust agree to interpret future test results with consideration tothe known bias.5.2 This test method is used for the determination of theamounts of naturally present oily or waxy impurities that havenot been comp

20、letely removed from textiles made from animalfibers, and for the determination of the amounts of oily or waxyfinishing materials applied to raw materials or textiles duringmanufacture. See 3.1.1, extractable matter.5.3 The test method may be used as a step in the determi-nation of the commercial wei

21、ght of fiber, yarn, and textileshipments.5.4 The International Wool Textile Organization specifiesthe use of a halogenated hydrocarbon, dichloromethane, alsocalled methylene chloride (CH2Cl2) instead of the solventspecified in this test method (IWTO-10-62(E).5.5 Extractables by mass loss is frequent

22、ly used for textileswhich have a relatively large amount of extractable material toeffect a significant mass change.6. Apparatus and Reagents6.1 Extraction Apparatus6.1.1 Soxhlet Extraction Apparatus for Option 1 extraction6.1.2 Extraction Funnels, wide-mouth, 125 or 150-mL ca-pacity for Option 2 ex

23、traction.6.2 Thimbles, fat-free cellulose or Alundum, for Option 1.6.3 Specimen Compressor, pestle or long forceps, for han-dling specimens in Option 2.6.4 Containers,6.4.1 To hold extractables and that will seal to preventmoisture changes, for example weighing bottles, for Option 1.6.4.2 To collect

24、 solvent from extractions, for Option 2.NOTE 2If metal containers are used, check to ensure that theextracatable matter does not react with the metal if the residue is to beweighed.6.5 Oven6.5.1 Ventilated Forced-Draft Drying Oven, capable ofmaintaining a temperature of 105 6 3C.6.5.2 Vacuum Type, m

25、aintained at 65 6 2C for use inOption 3 when low-boiling ingredients are present.6.6 Tray, to contain desiccant, with a screen to preventspecimen or container contact with desiccant, for use in thevacuum oven. If Phosphorus pentoxide (P205) or sulfuric acid(H2SO4) is used, the screen must be acid re

26、sistant.6.7 Dessicator6.8 Analytical Balancesensitive to 0.0001 g.6.9 Nitrogen, to supply the vacuum oven.6.10 Solventas agreed (see 1.1.1). (WarningVarioussolvents have been used in the past, and are still used to someextent. Many of these solvents are flammable, toxic or haveanesthetic effects, or

27、 unpleasant odors. As with all volatilesolvents, the use of adequate ventilation under a hood isrecommended when using this solvent.)7. Hazards7.1 Refer to the manufacturers material safety data sheetsfor specific information on chemicals used in this test.7.2 After extraction with alcohol or other

28、flammable ortoxic solvents, the specimens must be air-dried under a hooduntil nearly all of the solvent has evaporated before they aredried in the oven. Otherwise there is a danger of building up adangerous concentration of explosive vapor in the oven. Ovendoors have been blown across the room by th

29、e force of anexplosion.7.3 WarningDichloromethane is toxic, and its use isrecommended only when necessary to conform to internationalspecifications, and then with adequate ventilation under a hood.8. Sampling8.1 Lot SampleAs a lot sample for acceptance testing,take at random the number of shipping c

30、ontainers directed inan applicable material specification or other agreement be-tween the purchaser and the supplier. Consider shippingcontainers to be the primary sampling unit.NOTE 3An adequate specification or other agreement between thepurchaser and the supplier requires taking into account the

31、variabilitybetween shipping containers, within a shipping container, and betweenspecimens taken from a single unit within a shipping container, so as toprovide a sampling plan with a meaningful producers risk, consumersrisk, acceptable quality level, and limiting quality level.8.2 Laboratory SampleA

32、s a laboratory sample for accep-tance testing, proceed as follows:8.2.1 Yarn on PackagesTake at random from each ship-ping container in the lot sample the number of packagesdirected in an applicable material specification or other agree-ment between the purchaser and the supplier, such as anagreemen

33、t to use Practice D 2258. Preferably, the same numberof packages should be taken from each shipping case in the lotsample. If differing numbers of packages are to be taken fromshipping cases in the lot sample, determine at random whichshipping cases are to have each number of packages drawn.8.2.2 Ya

34、rn on BeamsTake a laboratory sample from eachof the beams in the lot sample as agreed between the purchaserand the supplier.8.2.3 FabricsTake a full width swatch 1 m long from theend of each roll of fabric in the lot sample, after first discardinga minimum of 1 m of fabric from the very outside of t

35、he roll.D 2257 98 (2004)28.2.4 Staple FiberSystematically take five laboratorysample units from each bale in the lot sample as directed inPractice D 3333.8.2.5 Tow, Sliver, or TopTake from the lead end of astrand from each shipping container in the lot sample the firstmetre of material that has a cl

36、ean, uniform appearance. If theshipping containers in the lot sample contain multiple pack-ages, take a laboratory sample from one package drawn atrandom from each container.8.3 Test SpecimensTakea106 1-g specimen from eachunit in the laboratory sample. If necessary, take an additionalspecimen from

37、a random unit in the laboratory sample untilthere is a total of ten specimens.9. Conditioning9.1 Neither preconditioning nor conditioning is necessary.10. Procedure10.1 Presence of boiling ingredients (extractable volatile atlow temperatures).10.1.1 Use the following procedure to determine the pres-

38、ence of low boiling ingredients, that is, extractables that arevolatile at low temperatures.10.1.2 Extract one or more specimens of the material asdirected in 10.2 or 10.3.10.1.3 Transfer the solvent quantitatively to a tared weigh-ing bottle and evaporate the solvent by blowing with a streamof air

39、at room temperature until there is a mass change of lessthan 0.001 g in 10 min.10.1.4 Heat the residue in an oven at 105 6 3C for 30 min,cool, and weigh.10.1.5 If there is a mass loss greater than 0.001 g in theresidue (extractables) due to heating in the oven, the materialcontains extractable matte

40、r which volatilizes at low tempera-tures, and the specimen solvent extract should not be heated inthe oven.10.1.6 If there is no detectable loss in residue mass (lessthan 0.001 g) due to heating in the oven, the material does notcontain low boiling ingredients and the extracted residue isdried in th

41、e oven before final weighing.10.2 Option 1, Soxlet Extraction,10.2.1 Extract fat-free cellulose or Alundum thimbles foreach specimen in the solvents to be used, in the Soxhletchamber.Asuitably folded qualitative grade filter paper may beused in place of the thimble. Thimbles are not needed for fabri

42、cyarn or thread specimens.10.2.2 Weigh 10 6 1 g of each specimen to the nearest0.010 g.10.2.3 Place the specimens in the thimbles, if used, andtransfer to the Soxhlet apparatus. Thimbles must be longenough to cover the opening of the siphon tube.10.2.4 Add sufficient solvent to overflow plus about 2

43、5 %more to prevent the solvent from boiling dry.10.2.5 Adjust the heat for 3 to 5 siphonings per hour andextract the specimens for at least 20 siphonings. Maintain thetemperature of the solvent in the Soxhlet apparatus at a levellow enough to avoid interference with siphoning and in anyevent, below

44、50C. Be certain that the solvent is going throughthe thimble or filter paper during the extraction, and notoverflowing. In case there is evidence that 20 siphonings arenot sufficient, the purchaser and supplier should agree upon asuitable number of siphonings.10.2.6 Remove from the source of heat wh

45、en the upperchamber of the apparatus is nearly full and ready to siphonagain. Pour off the nearly pure solvent from the extraction tubeand save for reuse after suitable distillation.10.2.7 Determine the mass of a weighing bottle to 0.001 g.Transfer the contents of the flask to the tared weighing bot

46、tle,rinse with a small quantity of solvent, and add this to thecontents of the weighing bottle.10.2.8 If low boiling ingredients were found (10.1.5) evapo-rate the solvent as directed in 10.1.3 without oven drying theresidue.10.2.9 If low - boiling ingredients were not found, evaporatethe solvent an

47、d then dry the residue in an oven at 105 6 3Cfor 30 min. Cool in a desiccator and weigh. Repeat the drying,cooling, and weighing cycle until the difference in intervals of30 min results in a mass change of less than 0.001 g.10.2.10 Record the final mass of the residue to the nearest0.001 g.NOTE 4Sol

48、vent in weighing bottles may be recovered for subsequentreuse by connecting the effluent stream of solvent and air to a suitablecondenser.10.2.11 Remove the remaining solvent from the Soxhletapparatus, reinsert the thimble and specimen, and fill with theproper amount of alcohol. Extract through at l

49、east 12 siphon-ings.10.2.12 Determine the mass of a weighing bottle to 0.001 g.Transfer the alcohol from the flask to the weighing bottle,evaporate the alcohol, dry, and weigh the residue to the nearest0.001 g.10.2.13 Remove the specimen from the apparatus and airdry it. Continue as directed in 10.5.10.3 Option 2, room temperature extraction:10.3.1 Place the specimen in an extraction funnel.10.3.2 Cover the specimen with solvent and let stand forabout 10 min with occasional stirring to facilitate specimensurface and solvent contact.10.3.3 Open the funnel st