1、Designation: D1113 13Standard Test Method forVegetable Matter and Other Alkali-Insoluble Impurities inScoured Wool1This standard is issued under the fixed designation D1113; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number 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 the determination of the contentof oven-dried, ash-free, alcohol extractive-free vegetable
3、mat-ter and other alkali-insoluble impurities present in scouredwool. It is also applicable to “related fibers” such as the hairfrom the goat, camel, alpaca, and other animals.NOTE 1The determination of clean wool fiber present on a laboratoryscale is covered in Test Method D584, the determination o
4、f clean woolfiber present on a commercial scale is covered in Test Method D1334, andthe calculation of commercial weight and yield of various commercialcompositions (formerly covered in Appendix to Test Method D584)iscovered in Practice D2720.1.2 This standard does not purport to address all of thes
5、afety 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. For specific safetyhazard statements, see Section 8.2. Referenced Docum
6、ents2.1 ASTM Standards:2D123 Terminology Relating to TextilesD584 Test Method for Wool Content of Raw WoolLaboratory ScaleD1334 Test Method for Wool Content of Raw WoolCommercial ScaleD2720 Practice for Calculation of Commercial Weight andYield of Scoured Wool, Top, and Noil for Various Com-mercial
7、CompositionsD4845 Terminology Relating to Wool3. 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:other alkali-insoluble impurities, oven-dried, vegetable matterbase.3.1.2 For definitions of o
8、ther textile terms used in this testmethod, refer to Terminology D123.4. Summary of Test Method4.1 The wool, or other animal fiber, is dissolved in a boiling3% sodium hydroxide solution or a hot 10% sodium hydroxidesolution under specified controlled conditions. The weights ofthe ash-free, oven-drie
9、d components of the undissolved residueare converted by means of tabulated factors to the correspond-ing weights of vegetable matter base and other alkali-insolubleimpurities.5. Significance and Use5.1 Test Method D1113 is considered satisfactory for accep-tance testing of commercial shipments, and
10、the procedure hasbeen used extensively in the trade for this purpose, particularlyin connection with the determination of clean wool fiberpresent by Test Method D584. The procedure in Test MethodD1113 is used by the U.S. Customs Service for the determi-nation of the vegetable matter in importations
11、of raw wool onwhich the allowance for loss of wool during commercialcleaning is based in part.35.1.1 In case of a dispute arising from differences inreported test results when using Test Method D1113 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparat
12、ive 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 that are as homogeneous as possible and that arefrom a lot of material of t
13、he type 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 Students t-test forunpaired data and an acceptable probability level chosen by thetwo parties before the testi
14、ng is begun. If a bias is found, either1This test method is under the jurisdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.13 on Wool and Felt.Current edition approved July 1, 2013. Published August 2013. Originallyapproved in 1950. Last previous edition
15、 approved in 2008 as D111390a (2008).DOI: 10.1520/D1113-13.2For 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.3T
16、ariff Schedules of the United States, Schedule 3, Part 1, Subpart C, Headnote1(c).Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1its cause must be found and corrected or the purchaser and thesupplier must agree to interpret future te
17、st results in light of theknown bias.6. Apparatus6.1 Filter, 40-mesh sieve (U. S. Sieve Series, opening0.0165 in. (0.42 mm) or metal screen, or cheese cloth havingcomparable openings.6.2 OvenA forced-draft oven designed to supply clean airat a desired temperature with a tolerance of 62C.6.3 Muffle F
18、urnace, thermostatically controlled in the rangeof 700 6 25C.6.4 BeakersHeat resistant glass or stainless steel, of 2-litrecapacity.7. Reagents and Materials7.1 Sodium Hydroxide Solution (NaOH), 3 % by weight.7.2 Sodium Hydroxide Solution, 10 % by weight.7.3 Sodium Hypochlorite Solution (NaOCl), 5 %
19、 by weight.8. Hazards8.1 Sodium hydroxide is extremely corrosive, and care mustbe exercised to avoid contact with the eyes, skin, or clothing.8.2 Operators should wear eye protection while handlingcaustic solutions.9. Sampling9.1 Lot SampleAs a lot sample for acceptance testing, takeat random the nu
20、mber of shipping containers directed in anapplicable material specification or other agreement betweenthe purchaser and the supplier. Consider shipping containers tobe the lot sampling unit.NOTE 2An adequate specification or other agreement between thepurchaser and the supplier requires taking into
21、account the variabilitybetween shipping containers, between laboratory sampling units within ashipping container, and between test specimens within a laboratorysampling unit to produce a sampling plan with a meaningful producersrisk, consumers risk, acceptable quality level, and limiting quality lev
22、el.9.2 Laboratory SampleAs a laboratory sample for accep-tance testing, proceed as follows:9.2.1 For tests to be made in connection with Test MethodsD584 and D1334, prepare a portion of scoured and dried woolfrom each lot sampling unit of the lot sample described in 9.1.Make sure that each portion i
23、s approximately 100 g, which willbecome a laboratory sampling unit. Note that these portions areto be obtained from random locations in the wool mass. If thescoured wool is judged to contain over 5 % of vegetable matterand sufficient scoured wool is available, prepare anotherreplicate, that is, a se
24、cond laboratory sample unit.9.2.2 For tests on samples of scoured wool not obtained inconnection with Test Methods D584 and D1334 take replicatesample units as directed in 9.2.1.9.3 Test SpecimensAs test specimens, prepare two testspecimens from each laboratory sampling unit by combiningten or more
25、pinches of fiber into a bundle having a mass of 406 1g.10. Conditioning10.1 Dry specimens taken as directed in 9.1 under theconditions for oven drying prescribed in Test Method D584.10.2 Weigh specimens taken as directed in 9.2 in thecondition as received, in the oven-dry condition, or afterexposure
26、 in the standard atmosphere for testing textiles,depending upon the directions or requirements of the interestedparties.10.3 Weigh specimens (10.1 or 10.2) to the nearest 0.01 g.(W2).11. Procedure11.1 Preferred MethodIn a 2-L heat-resistant glass orstainless steel beaker, bring 1 Lof 3 % NaOH soluti
27、on to a boil.With the solution at a boil, carefully add the entire weighedspecimen. Quickly immerse the wool in the NaOH solutionwith the aid of a stirring rod, and adjust the heat to resumeboiling of the solution. Boil the solution gently with continuousstirring for 90 6 2 s. Remove the beaker from
28、 the heat and add500 ml of tap water, stir, then allow to settle.NOTE 3The preferred method uses 3 % sodium hydroxide solution, inwhich most wools are soluble when treated as directed. However, certaincoarse, dry carpet wools do not dissolve completely in the 3 % solution.For such wools the alternat
29、ive method (11.1.1), in which 10 % sodiumhydroxide solution is used, is necessary.NOTE 4Keep depilatory in pulled wool specimens to a minimum bytreating the sample as directed in 10.3 of Test Method D584.11.1.1 Alternative Method (Note 2)In a 2-L heat-resistantglass or stainless steel beaker, bring
30、600 cm2(mL) of 10 %NaOH solution to a boil. Remove the beaker from the heat,place on a dry wooden or asbestos mat, and immediately addthe weighed specimen. Stir continuously for 3 min 6 5s,add1000 mL of tap water, stir, and allow to settle.11.2 FiltrationDecant the solution through the 40-meshfilter
31、, using a stirring rod or a jet of water to assist filtration byagitation of the solution on the filter. Wash all the remainingvegetable matter and other alkali-insoluble impurities in thebeaker onto the filter. Discard any sand or depilatory (Note 3)in the beaker and on the filter. Sprinkle about 1
32、5 mL of 5 %sodium hypochlorite solution over the residue on the filter, thenrinse with a moderate spray of water at 35 to 40C for 3 to 4min or until the residue is neutral as indicated by litmus paper.11.3 Components of Alkali-Insoluble ImpuritiesObservethe rinsed material on the filter. Estimate th
33、e fraction of thetotal dry weight corresponding to each type of burr and othervegetable matter, as well as non-wool fibers, skin, paint, andtag material present (Note 5).11.3.1 More Accurate Determination of ComponentsSeparate and treat each of the component types from theresidue as directed in 11.4
34、 and use the appropriate calculations.NOTE 5For clean wool fiber determination (Test Method D584), takecare to exclude or correct for components emanating from the original orsample package wrapper or container.11.4 Drying and AshingTransfer the rinsed material fromthe filter into a tared porcelain
35、crucible or dish. Dry at 10562C to constant weight (W1). Ignite in a muffle furnace at 7006 25C to a white ash, cool in a desiccator, and weigh (A).D1113 13212. Calculation of Results12.1 Vegetable Matter BaseUsing Eq 1 and the appropri-ate values in Table 1, calculate the correction factor forconve
36、rting the weight of recovered oven-dried, ash-free, alkali-insoluble material to the weight of vegetable matter base in thespecimen. Calculate the percentage of vegetable matter baseusing Eq 2.Fv5 f1v11f2v21. (1)V 5 100FvW12 A!/W2(2)where:Fv= correction factor for vegetable matter only,V = vegetable
37、 matter base expressed as a percent ofthe weight of the original specimen,f1f2= weight (mass) fractions of the individual types ofvegetable matter in the recovered alkali-insolubleimpurities,v1v2= factors for the individual types of vegetablematter (from Table 1),W1= weight (mass) of oven-dried reco
38、vered alkali-insoluble impurities,W2= weight (mass) of specimen used for the test, andA = weight (mass) of ash from recovered alkali-insoluble impurities.12.2 Total Alkali-Insoluble Impurities Using Eq 3 and theappropriate values in Table 1, calculate the correction factor forconverting the weight (
39、mass) of recovered oven-dried, ash-free, alkali-insoluble material to the original weight of totaloven-dried, ash-free, extractives-free alkali-insoluble impuri-ties in the specimen. Calculate the percentage of such totalimpurities according to Eq 4.FT5 Fv1fcc1fpp1fss1ftt1fxx (3)T 5 100FTW12 A!/W2(4
40、)where:Fv,W1,W2and A = have the meanings given in 12.1, andFT= average correction factor for totalalkali-insoluble impurities,T = percentage oven-dried, ash-free,extractives-free total alkali-insolubleimpurities,fc,fp,fs,ft,fx= weight fractions of cotton and otherfibers, paint, skin, tag material, a
41、ndpaper string, respectively, in the recov-ered alkali-insoluble impurities, andc, p, s, t, x = factors for cotton and other fibers,paint, skin, tag material, and paperstring, respectively (from Table 1).13. Report13.1 State that the tests were made as directed inASTM TestMethod D1113. Describe the
42、material or product sampled andthe method of sampling used.13.2 Report the following information:13.2.1 Percentages of vegetable matter base and total alkali-insoluble impurities to the nearest 0.1 percentage point.13.2.2 The basis for the calculated percentages: oven-driedweight, as-received weight
43、, or conditioned weight of thesample.13.2.3 State whether 3 % or 10 % NaOH was used.14. Precision and Bias14.1 Interlaboratory Test Data4The first of a plannedseries of interlaboratory tests was run in 1970, in which fourlaboratories each scoured and dried three subsamples randomlydrawn from the sam
44、e core sample of a grease wool, using theprocedures prescribed in Test Method D584. In each laboratorytwo 40-g specimens were taken from each oven-dried scouredsubsample and tested by one operator for total alkali-insolubleimpurities, using 3 % NaOH solution and visually estimatingthe fractions of t
45、he impurity components. This procedure wasrepeated on core samples from two additional greasy wools.The vegetable matter base content for all three scoured woolswas less than 1 percentage point. Under these conditions thecomponents of variance for the percentage of total alkali-insoluble impurities
46、expressed as standard deviations werefound to be:Single-operator component 0.151 percentage pointBetween-laboratory component 0.042 percentage point14.2 PrecisionFor the components of variance listed in14.1, two averages of observed percentages of alkali-insolubleimpurities in scoured wool should be
47、 considered significantlydifferent at the 95 % probability level if the difference equals orexceeds the following critical differences (Note 6):Critical Difference, Percentage Points, forthe Conditions NotedANumber of Observationsin Each AverageSingle-OpratorPrecisionBetween LaboratoryPrecision1 0.4
48、2 0.432 0.30 0.323 0.24 0.274Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D13-1012.TABLE 1 Correction Factors for Alkali-Insoluble ImpuritiesNOTE 1Average value of the ratio of scoured, oven-dry ash-free,extractive-free weight
49、 of vegetable matter and other alkali-insolublematter to the corresponding weight of oven-dry, ash-free material recov-ered by this method.Type of Alkali-InsolubleImpuritiesCorrection Factor forPreferred Method(3 % NaOH Solution)Correction Factor forAlternative Method(10 % NaOHSolution)Cockle burrA1.1 1.1Sand burrA1.1 1.2Spiral burrA1.2 1.3Bean burrA1.0 1.1ShivesAand similar vegetablematter1.3 1.6Cotton and other fibers 1.1 1.1Skin 2.0 2.0String (paper) 1.1 1.1Hard tag pieces 1.4 1.4Paint piecesB. .ASee Fig. 1.BThe correction factor for paint pieces w
