1、Designation: D 1283 05Standard Test Method forAlkali-Solubility of Wools1This standard is issued under the fixed designation D 1283; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses
2、 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 a chemical procedure fordetermination of the amount of wool substance soluble in alkaliunder standard conditions and is applicable
3、to wool in scouredfiber form, or as fiber obtained from yarn or from woven ornonwoven fabric.1.2 The values stated in inch-pound are to be regarded asstandard. The values stated in SI units are provided forinformation only.NOTE 1This test method is applicable to other animal fibers althoughthe level
4、 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 does not purport to address all of thesafety concerns, if any, associated with its use. It is therespon
5、sibility 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 Standards:2D 123 Terminology Relating to TextilesD 1060 Practice for Core Sampling of Raw Wool in Pack-a
6、ges for Determination of Percentage of Clean Wool FiberPresentD 1193 Specification for Reagent WaterD 4845 Terminology Relating to WoolE1 Specification for ASTM ThermometersE11 Specification for Wire-Cloth Sieves for Testing Pur-poses3. Terminology3.1 For all terminology relating to D13.13, Wool and
7、 WoolFelt, refer to Terminology D 4845.3.1.1 The following terms are relevant to this standard:alkali-solubility, wool.3.2 For all other terminology related to textiles, see Termi-nology D 123.4. Summary of Test Method4.1 Specimens are maintained at a stipulated constant tem-perature in a caustic so
8、lution 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 the degree of dam-age to wool resulting from certain chemical treatments, par-ticularly when test results on t
9、he 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 solubility than coarse wool, because of greatersurface area per unit mass of fiber.5.2 This test method is not recom
10、mended 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 Although results in one laboratory cannot usually beverified in another laboratory, this test method is consid
11、eredsatisfactory 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 solubility procedure. Comparative tests as directed in5.3.1 are advisable before Test Method D 1283 is used fo
12、racceptance testing.5.3.1 In case of a dispute arising from differences inreported test results when using Test Method D 1283 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparative tests to determine ifthere is a statistical bias between their laborat
13、ories. 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 whichare from a lot of material of the type in question. The testspecimens should then be randomly assigned
14、in equal numbersto each laboratory for testing. The average result from the twolaboratories should be compared using Students t-test forunpaired data and an acceptable probability level chosen by thetwo parties before testing is begun. If a bias is found, either its1This test method is under the jur
15、isdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.13 on Wool and Wool Felt.Current edition approved Sept. 1, 2005. Published September 2005. Originallyapproved in 1953. Last previous edition approved in 2001 as D 1283 85(2001).2For referenced ASTM standa
16、rds, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
17、 19428-2959, United States.cause must be found and corrected or the purchaser and thesupplier must agree to interpret future test results in the light ofthe known bias.6. Apparatus6.1 Test TubesGlass test tubes 1.5 in. (38 mm) by 7.9 in.(200 mm) with cork stoppers.6.2 Constant-Temperature BathA bath
18、 equipped to main-tain a temperature of 65 6 0.5 C throughout.6.3 ThermometerASTM Aniline Point Thermometer,having a range from 25 to 105 C and conforming to therequirements for Thermometer 34C as prescribed in Specifi-cation E1.6.4 Weighing BottlesGlass bottles of approximately 30 to35-mL capacity,
19、 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 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
20、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 shall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society.4Other grade
21、s 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 WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D
22、 1193.7.3 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 Bicarbonate Solution (2.5 g/L)Dissolve 2.5 gof sodium bicarbonate (NaHCO3) in water and dilute to 1 L.7.6 Sodium Hydrox
23、ide, 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 dilute to 1 L.7.7 Working Reference Wool SamplesSamples of undam-aged scoured wool of known alkali-solubility.8. Sampling8
24、.1 Lot SampleAs a lot sample for acceptance testing,take at random the number of shipping containers directed inan applicable material specification or other agreement be-tween the purchaser and the supplier, such as an agreement touse Practice D 1060. Consider shipping containers to be theprimary s
25、ampling units.NOTE 2A realistic specification or other agreement between thepurchaser and the supplier requires taking into account the variabilitybetween shipping containers, between laboratory samples within a ship-ping container, and between specimens within a laboratory sample so as toprovide a
26、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 Laboratory SampleAs a laboratory sample for accep-tance testing, take the number of subsamples from eachpackage in the lot sa
27、mple as directed in an applicable materialspecification or other agreement between the purchaser and thesupplier, such as an agreement to use Practice D 1060 if baledor bagged wool is to be tested.8.3 Test SpecimensAs directed in Section 9, determine thenumber of specimens to be tested from each sub
28、sample in thelaboratory sample.9. Number of Specimens per Subsample9.1 Control or Non-Critical TestingFor routine controltesting or other non-critical purpose where acceptance testingis not involved, four specimens, randomly chosen from a lot,may be tested as directed in Sections 10 and 11.9.2 Accep
29、tance 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 thelaboratory sample is not more than 2.0 % above or below thetrue average of the subsample in the laboratory sampl
30、e (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 extensive past records for similarmaterials tested in the users laboratory as directed in themethod, calculate the require
31、d 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 number),v = reliable estimate of the coefficient of variation ofindividual observations on similar materials in theusers
32、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 associ-ated with the estimate of v, andA = 2.0 % of the average, the value of the allowablevariation.9.2.1.2 No Reliable Estimate of vWhen the
33、re is no reli-able estimate of v for the users laboratory, Eq 1 should not beused directly. Instead, specify the fixed number of 17 speci-mens per subsample in the laboratory sample. This number ofspecimens is calculated using v = 4.2 % of the average, whichis a somewhat larger value of v than is us
34、ually found inpractice. When a reliable estimate of v for the users laboratory3Detailed 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 list
35、ed bytheAmerican 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.D1283052becomes available, Eq 1 will usually require fewer than
36、 17specimens per subsample in the laboratory sample.10. Preparation of Specimens10.1 Fabric and Yarn:10.1.1 FabricTake the required number of 2-g sub-samples from different areas of the fabric lot. Cut eachsubsample into small squares and unravel the fabric to obtainthe yarn. Keep the subsamples sep
37、arate. Reduce the yarn soobtained, or an equal quantity of yarn originally available fortest, to fiber form by the use of a set of hand cards. Take careto retain all fibers; treat the fibers as prescribed in 10.3.10.1.2 YarnTake the required number of 2-g subsamplesfrom different areas of the yarn l
38、ot. 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 opening; treat thefibers as prescribed in 10.3.10.3 Extraction and CardingExtract the wool fibers withsuccessive portions
39、 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 fiber at room temperature or slightly above,preferably under forced draft. Hand card the wool. Removegross impurities,
40、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 the wool with HCl (1 + 120) at room tem-perature for 15 min, using 100 mL of solution per gram ofwool. Squeeze, rinse
41、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 solution per gram ofwool. Squeeze and rinse, with mild agitation, in two successiveportions of neutral water. Squeeze the
42、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 oven at 105 to 110 C.Transfer to a weighing bottle.11. Procedure11.1 From each of the subsamples, take one test specim
43、enwhich, 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 specimens longer than required to reach constant mass (nofurther decrease in mass of more than 0.2 % in 15 min ofadd
44、itional 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 constant temperature waterbath and bring to 65C.11.4 Immerse each dried and weighed specimen in the 65CNaOH solution
45、 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 the specimens inthe solution, pour the contents of each test tube throughseparate sieves. Rinse the tubes twice with
46、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 approximately 3 L/min.11.7 Place the sieves on blotting paper or toweling to absorbthe excess water and partially dry t
47、he 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 nearest 0.001 g, dryinguntil successive weighings show no further decrease in mass ofmore than 0.2 % in 15 min of addi
48、tional drying time.11.9 Test a reference sample of wool of known alkali-solubility with every twentieth test or every 6 months, which-ever comes first, along with the unknown, to verify theoperational procedure.12. Calculation12.1 Calculate the alkali-solubility, as a percentage of theoriginal mass,
49、 according to Eq 2:Alkali2solubility, % 5 M12 M2!/M13 100 (2)where:M1= mass of oven-dry specimen before sodium hydroxidetreatment, andTABLE 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 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 1.68
