1、Designation: D2257 98 (Reapproved 2012)Standard Test Method forExtractable Matter in Textiles1This standard is issued under the fixed designation D2257; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A n
2、umber in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 the
3、extractable 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 th
4、e 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 D541, SpecificationD681, and Test Method D1574.1.1.1 The solvents for use in this
5、method are any solventsthat the party or parties concerned agreed on; such as,Halogenated Hydrocarbon (HH) chloroform, tetrachloroeth-ane, alcohol.1.1.2 This test method may not extract cross-linked finishesor resins which may be on the textile.1.2 The values stated in SI units are to be regarded as
6、standard. No other units of measurement are included in thisstandard.1.3 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
7、applica-bility of regulatory limitations prior to use. See Sections6 and 7.2. Referenced Documents2.1 ASTM Standards:2D123 Terminology Relating to TextilesD541 Specification for Single Jute Yarn3D681 Specification for Jute Rove and Plied Yarn for Elec-trical and Packing Purposes3 3D1574 Test Method
8、for Extractable Matter in Wool andOther Animal FibersD1909 Standard Table of Commercial Moisture Regains forTextile FibersD2258 Practice for Sampling Yarn for TestingD3333 Practice for Sampling Manufactured Staple Fibers,Sliver, or Tow for TestingD4920 Terminology Relating to Conditioning, Chemical,
9、and Thermal Properties2.2 Other Documents:IWTO 10-62(E) Method for Determination of the Dichlo-romethane Soluble Matter in Combed Wool Sliver43. Terminology3.1 Definitions:3.1.1 extractable matter, nnonfibrous material in or on atextile not including water, which is removable by a specifiedsolvent o
10、r solvents as directed in a specified procedure.3.1.1.1 DiscussionNonfibrous material is usually oily,waxy, resinous, or polymeric in nature, but may also includeother material, such as protein, particularly if ethyl alcohol isused, or in, the extracting solvent.3.1.2 For definitions of other moistu
11、re terms related totextiles, refer to Terminology D4920. For definitions of othertextile terms used in this test method refer to TerminologyD123.4. Summary of Test Method4.1 The specimen is extracted either in Soxhlet apparatus(Option 1), or extraction funnel (Option 2) first with an agreedsolvent (
12、Note 2). The solvents are evaporated and the residuesand the specimens are dried and weighed separately. Theamounts of extracted matter are reported as percentages ofeither the oven-dried mass or of the oven-dried mass pluscommercial moisture regain for the textile.1This test method is under the jur
13、isdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.51 on Conditioning and,Chemical and Thermal Properties.Current edition approved Feb. 1, 2012. Published February 2012. Originallyapproved in 1989. Last previous edition approved in 1998 as D2257 98(2004).
14、DOI: 10.1520/D2257-98R12.2For 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. The last approved versio
15、n of this historical standard is referencedon www.astm.org.4Available from International 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.4.2 Alternatively, in Option 3, the spe
16、cimen is dried andweighed before and after extraction using Option 1 or Option2. Extractable matter is calculated as the loss in mass reportedas percentages of the extracted oven-dried mass or this massplus commercial moisture regain for the textile.5. Significance and Use5.1 This test method may be
17、 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 tests to determine if there isa statistical
18、 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 type in question. The testspecimens should
19、 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 bias is found, either its causemust be fou
20、nd 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 completely removed from textiles made from an
21、imalfibers, 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 weight of fiber, yarn, and textileshipments.
22、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 frequently used for textileswhich have a relative
23、ly 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 extraction.6.2 Thimbles, fat-free cellulose
24、 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 solvent from extractions, for Option 2.N
25、OTE 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, maintained at 65 6 2C for use inOption 3 w
26、hen 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 resistant.6.7 Dessicator6.8 Analytical Bala
27、ncesensitive 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 unpleasant odors. As with all volatileso
28、lvents, 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 flammable ortoxic solvents, the specimens
29、 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 the force of anexplosion.7.3 WarningDichlor
30、omethane 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 containers directed inan applicable materi
31、al 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 variabilitybetween shipping containers, w
32、ithin 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 SampleAs a laboratory sample for accep-tance tes
33、ting, 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 anagreement to use Practice D2258. Preferably, the
34、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 Yarn on BeamsTake a laboratory sample from e
35、achof the beams in the lot sample as agreed between the purchaserand the supplier.D2257 98 (2012)28.2.3 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 the roll.8.2.4 Staple Fiber
36、Systematically take five laboratorysample units from each bale in the lot sample as directed inPractice D3333.8.2.5 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 clean, uniform appearance. If theshipping cont
37、ainers 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 a random unit in the laboratory sample until
38、there 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-ence of low boiling ingredients, that is, ex
39、tractables 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 at room temperature until there is a mass ch
40、ange 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 matter which volatilizes at low tempera-tures, an
41、d 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 the oven before final weighing.10.2 Option 1,
42、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 fabricyarn or thread specimens.10.2.2 Weigh 10 6
43、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 25 %more to prevent the solvent from boiling
44、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 50C. Be certain that the solvent is going th
45、roughthe 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 when the upperchamber of the apparatus is near
46、ly 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 bottle,rinse with a small quantity of solvent,
47、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 and then dry the residue in an oven at 105 6 3
48、Cfor 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 4Solvent in weighing bottles may be recovered fo
49、r 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 least 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
