ASTM D1283-2005(2013) Standard Test Method for Alkali-Solubility of Wools《羊毛碱溶性的标准试验方法》.pdf

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1、Designation: D1283 05 (Reapproved 2013)Standard Test Method forAlkali-Solubility of Wools1This standard is issued under the fixed designation D1283; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numbe

2、r in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a chemical procedure fordetermination of the amount of wool substance soluble in alkaliunder standard conditions and

3、 is applicable to wool in scouredfiber form, or as fiber obtained from yarn or from woven ornonwoven fabric.1.2 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are n

4、ot considered standard.NOTE 1This test method is applicable to other animal fibers althoughthe level of alkali-solubility may be different from wool. With individualanimal fibers, undamaged solubility should be determined before attempt-ing to assess damage on an unknown sample.1.3 This standard doe

5、s 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 Stan

6、dards:2D123 Terminology Relating to TextilesD1060 Practice for Core Sampling of Raw Wool in Packagesfor Determination of Percentage of Clean Wool FiberPresentD1193 Specification for Reagent WaterD4845 Terminology Relating to WoolE1 Specification for ASTM Liquid-in-Glass ThermometersE11 Specification

7、 for Woven Wire Test Sieve Cloth and TestSieves3. Terminology3.1 For all terminology relating to D13.13, Wool and WoolFelt, refer to Terminology D4845.3.1.1 The following terms are relevant to this standard:alkali-solubility, wool.3.2 For all other terminology related to textiles, see Termi-nology D

8、123.4. Summary of Test Method4.1 Specimens are maintained at a stipulated constant tem-perature in a caustic solution for a specified period of time. Thepercentage of alkali-solubility is calculated from the loss inmass of the specimen.5. Significance and Use5.1 Alkali-solubility is an indication of

9、 the degree of dam-age to wool resulting from certain chemical treatments, par-ticularly when test results on the same wool, before suchtreatment, are available.5.1.1 Undamaged scoured wool has typical alkali-solubilityin the range of 9 to 15 %. Fine, undamaged wool normally willexhibit higher solub

10、ility than coarse wool, because of greatersurface area per unit mass of fiber.5.2 This test method is not recommended for use on woolknown to have sustained alkali damage.5.2.1 Alkali-damaged wool has had material solubilized thatordinarily would be included in the alkali-solubility test results.5.3

11、 Although results in one laboratory cannot usually beverified in another laboratory, this test method is consideredsatisfactory for acceptance testing because it has been usedextensively in the trade for this purpose and because it is theonly available method for assessing damage to wool by analkali

12、 solubility procedure. Comparative tests as directed in5.3.1 are advisable before Test Method D1283 is used foracceptance testing.5.3.1 In case of a dispute arising from differences inreported test results when using Test Method D1283 foracceptance testing of commercial shipments, the purchaser andt

13、he supplier should conduct comparative tests to determine ifthere is a statistical bias between their laboratories. Competentstatistical assistance is recommended for the investigation ofbias. As a minimum, the two parties should take a group of testspecimens which are as homogeneous as possible and

14、 whichare from a lot of material of the type in question. The testspecimens should then be randomly assigned in equal numbersto each laboratory for testing. The average result from the two1This test method is under the jurisdiction of ASTM Committee D13 on Textilesand is the direct responsibility of

15、 Subcommittee D13.13 on Wool and Felt.Current edition approved Jan. 1, 2013. Published January 2013. Originallyapproved in 1953. Last previous edition approved in 2005 as D1283 05. DOI:10.1520/D1283-05R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer S

16、ervice at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1laboratories should be compared using Stud

17、ents t-test forunpaired data and an acceptable probability level chosen by thetwo parties before testing is begun. If a bias is found, either itscause must be found and corrected or the purchaser and thesupplier must agree to interpret future test results in the light ofthe known bias.6. Apparatus6.

18、1 Test TubesGlass test tubes 1.5 in. (38 mm) by 7.9 in.(200 mm) with cork stoppers.6.2 Constant-Temperature BathA bath equipped to main-tain a temperature of 65 6 0.5 C throughout.6.3 ThermometerASTMAniline Point Thermometer, hav-ing a range from 25 to 105 C and conforming to therequirements for The

19、rmometer 34C as prescribed in Specifi-cation E1.6.4 Weighing BottlesGlass bottles of approximately 30 to35-mL capacity, fitted with ground glass covers.6.5 Constant-Temperature Drying Oven, to be maintained at105 to 110 C, preferably employing a forced draft.6.6 Sieves3No. 100 (150-m) approximately

20、1.75 in. (45mm) in diameter and 1.75 in. (45 mm) high.6.7 Hand Cards.6.8 Analytical BalanceThe balance must be capable ofweighing to 0.001 g.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents s

21、hall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society.4Other grades may be used, provided it is first ascertained thatthe reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.7.2 Purity of Wat

22、erUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193.7.3 1,1,2 Trichloro-1,2,2 Trifluoroethane57.4 Hydrochloric Acid (1 + 120)Mix 1 volume of concen-trated hydrochloric acid (HCl, sp gr 1.19) with 120 volumes ofwater.7.5 Sodium B

23、icarbonate Solution (2.5 g/L)Dissolve 2.5 gof sodium bicarbonate (NaHCO3) in water and dilute to 1 L.7.6 Sodium Hydroxide, Standard Solution (0.100 N)Prepare and standardize a 0.100 N solution of sodium hydrox-ide (NaOH) in carbon dioxide-free water, kept free from accessby CO2from the air, and dilu

24、te to 1 L.7.7 Working Reference Wool SamplesSamples of undam-aged scoured wool of known alkali-solubility.8. Sampling8.1 Lot SampleAs a lot sample for acceptance testing, takeat random the number of shipping containers directed in anapplicable material specification or other agreement betweenthe pur

25、chaser and the supplier, such as an agreement to usePractice D1060. Consider shipping containers to be the pri-mary sampling units.NOTE 2A realistic specification or other agreement between thepurchaser and the supplier requires taking into account the variabilitybetween shipping containers, between

26、 laboratory samples within a ship-ping container, and between specimens within a laboratory sample so as toprovide a sampling plan which at the specified level of the property ofinterest has a meaningful producers risk, consumers risk, acceptablequality level, and limiting quality level.8.2 Laborato

27、ry SampleAs a laboratory sample for accep-tance testing, take the number of subsamples from eachpackage in the lot sample as directed in an applicable materialspecification or other agreement between the purchaser and thesupplier, such as an agreement to use Practice D1060 if baledor bagged wool is

28、to be tested.8.3 Test SpecimensAs directed in Section 9, determine thenumber of specimens to be tested from each subsample in thelaboratory sample.9. Number of Specimens per Subsample9.1 Control or Non-Critical TestingFor routine controltesting or other non-critical purpose where acceptance testingi

29、s not involved, four specimens, randomly chosen from a lot,may be tested as directed in Sections 10 and 11.9.2 Acceptance Testing:9.2.1 Take a number of specimens per subsample in thelaboratory sample, such that the user may expect at the 95 %probability level that the test result for a subsample in

30、 thelaboratory sample is not more than 2.0 % above or below thetrue average of the subsample in the laboratory sample (seeTable 1). Determine the number of specimens per subsample inthe laboratory sample as follows:9.2.1.1 Reliable Estimate of vWhen there is a reliableestimate of v based upon extens

31、ive past records for similarmaterials tested in the users laboratory as directed in themethod, calculate the required number of specimens persubsample in the laboratory sample using Eq 1:n 5 tv/A!2(1)where:n = number of specimens per subsample in the laboratorysample (rounded upward to a whole numbe

32、r),v = reliable estimate of the coefficient of variation ofindividual observations on similar materials in theusers laboratory under conditions of single-operatorprecision,t = the value of Students t for two-sided limits, a 95 %probability level, and the degrees of freedom associatedwith the estimat

33、e of v, andA = 2.0 % of the average, the value of the allowablevariation.3Detailed requirements for these sieves are given in Specification E11.4“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by

34、theAmerican Chemical Society, see “Reagent Chemicals and Standards,” by JosephRosin, D. Van Nostrand Co., Inc., New York, NY and the “United StatesPharmacopeia.”5This solvent is available under various trademarks as Refrigerant-113.D1283 05 (2013)29.2.1.2 No Reliable Estimate of vWhen there is no re

35、liableestimate of v for the users laboratory, Eq 1 should not be useddirectly. Instead, specify the fixed number of 17 specimens persubsample in the laboratory sample. This number of specimensis calculated using v = 4.2 % of the average, which is asomewhat larger value of v than is usually found in

36、practice.When a reliable estimate of v for the users laboratory becomesavailable, Eq 1 will usually require fewer than 17 specimensper subsample in the laboratory sample.10. Preparation of Specimens10.1 Fabric and Yarn:10.1.1 FabricTake the required number of 2-g subsamplesfrom different areas of th

37、e fabric lot. Cut each subsample intosmall squares and unravel the fabric to obtain the yarn. Keepthe subsamples separate. Reduce the yarn so obtained, or anequal quantity of yarn originally available for test, to fiber formby the use of a set of hand cards. Take care to retain all fibers;treat the

38、fibers as prescribed in 10.3.10.1.2 YarnTake the required number of 2-g subsamplesfrom different areas of the yarn lot. Keep the subsamplesseparate. Reduce the yarn to fiber as instructed in 10.1.1.10.2 FiberLoose scoured or processed wool, card sliveror wool top may be used without additional openi

39、ng; treat thefibers as prescribed in 10.3.10.3 Extraction and CardingExtract the wool fibers withsuccessive portions of residue-free 1,1,2 trichloro-1,2,2 trifluo-roethane at room temperature until evaporation of a 2-mLportion of the extract leaves no visible residue on a watchglass. Air-dry the fib

40、er at room temperature or slightly above,preferably under forced draft. Hand card the wool. Removegross impurities, such as pieces of skin, burrs, etc., by hand, ifpresent.10.4 Lime-Pulled WoolLime-pulled wool requires specialtreatment. Remove as much lime as possible by physicalseparation. Treat th

41、e wool with HCl (1 + 120) at room tem-perature for 15 min, using 100 mL of solution per gram ofwool. Squeeze, rinse in water, and squeeze again.10.5 Buffer TreatmentTreat the wool to be tested with abuffer solution consisting of NaHCO3(2.5 g/L) at room tem-perature for 15 min, using 100 mL of soluti

42、on per gram ofwool. Squeeze and rinse, with mild agitation, in two successiveportions of neutral water. Squeeze the wool again and partiallydry at a temperature not exceeding 105 C. Cut the carded woolwith scissors into12 to34-in. (10 to 15-mm) lengths, and drythe approximate required mass in the ov

43、en at 105 to 110 C.Transfer to a weighing bottle.11. Procedure11.1 From each of the subsamples, take one test specimenwhich, after oven drying, will weigh 1.0 6 0.1 g. Oven-drythose specimens at 105 to 110C to constant mass, determinedto the nearest 0.001 g and test them separately. Avoid dryingthe

44、specimens longer than required to reach constant mass (nofurther decrease in mass of more than 0.2 % in 15 min ofadditional drying).11.2 Use a separate test tube for each specimen to be tested.Into each test tube pour 100 mL of 0.100 N NaOH solution andloosely stopper.11.3 Put the test tubes in the

45、constant temperature waterbath and bring to 65C.11.4 Immerse each dried and weighed specimen in the 65CNaOH solution in the test tubes.11.5 Stir each specimen once as soon as it is placed in thesolution, and again 10 min later, to ensure complete wetting-out.11.6 After 60 6 0.1 min of immersion of t

46、he specimens inthe solution, pour the contents of each test tube throughseparate sieves. Rinse the tubes twice with tap water to removeany adhering particles and to deposit them on the sieves. Rinsethe material collected on the sieves for 5 min by means of astream of ambient tap water running at app

47、roximately 3 L/min.11.7 Place the sieves on blotting paper or toweling to absorbthe excess water and partially dry the specimens in the oven.When most of the moisture has been removed, return thespecimens to their respective weighing bottles and dry toconstant mass.11.8 Weigh each specimen to the ne

48、arest 0.001 g, dryinguntil successive weighings show no further decrease in mass ofmore than 0.2 % in 15 min of additional drying time.TABLE 1 Values of Students t for One-Sided and Two-Sided Limits and the 95 % ProbabilityAdf One-Sided Two-Sided df One-Sided Two-Sided df One-Sided Two-Sided1 6.314

49、12.706 11 1.796 2.201 22 1.717 2.0742 2.920 4.303 12 1.782 2.179 24 1.711 2.0643 2.353 3.182 13 1.771 2.160 26 1.706 2.0564 2.132 2.776 14 1.761 2.145 28 1.701 2.0485 2.015 2.571 15 1.753 2.131 30 1.697 2.0426 1.943 2.447 16 1.746 2.120 40 1.684 2.0217 1.895 2.365 17 1.740 2.110 50 1.676 2.0098 1.860 2.306 18 1.734 2.101 60 1.671 2.0009 1.833 2.262 19 1.729 2.093 120 1.658 1.98010 1.812 2.228 20 1.725 2.086 1.645 1.960AValues in this table were calculated using Hewlett Packard HP 67/97 Users Library Programs 03848D, “One-Sided and Tw