1、Designation: D 1113 90a (Reapproved 2001)Standard Test Method forVegetable Matter and Other Alkali-Insoluble Impurities inScoured Wool1This standard is issued under the fixed designation D 1113; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f revision, the year of last revision. A number in parentheses 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 the determination of the contentof oven-dried, ash-free, alcohol extr
3、active-free vegetable 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 D 5
4、84, the determination of clean woolfiber present on a commercial scale is covered in Test Method D 1334, andthe calculation of commercial weight and yield of various commercialcompositions (formerly covered in Appendix to Test Method D 584) iscovered in Practice D 2720.1.2 This standard does not pur
5、port 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. For specific safetyhazard statements, see Se
6、ction 8.2. Referenced Documents2.1 ASTM Standards:D 123 Terminology Relating to Textiles2D 584 Test Method for Wool Content of Raw WoolLaboratory Scale2D 1334 Test Method for Wool Content of Raw WoolCommercial Scale2D 2720 Practice for Calculation of Commercial Weight andYield of Scoured Wool, Top,
7、and Noil for Various Com-mercial Compositions23. Terminology3.1 Definitions:3.1.1 other alkali-insoluble impurities, n in scoured wool,the oven-dried, ash-free, alcohol-extractives-free, alkali-insoluble substances other than vegetable matter base, such asskin, cotton or other fibers, paper string,
8、tag (dung) pieces, andpaint pieces, etc.3.1.2 oven-dried, adjthe condition of a material that hasbeen heated under prescribed conditions of temperature andhumidity until there is no further significant change in its mass.3.1.2.1 DiscussionAn oven-dried material will retain asmall amount of moisture
9、that is dependent on the temperatureand relative humidity of the atmosphere in contact with thematerial during the drying process. An oven-dried material willonly be moisture-free when the air supplied to the drying ovenhas been previously desiccated.3.1.2.2 DiscussionThe term “mass” in the above de
10、fini-tion is the correct designation for what is commonly designated“weight”.3.1.3 vegetable matter base, n in raw wool, oven-driedscoured burrs, seeds, twigs, leaves, and grasses, free of mineralmatter and alcohol-extractable matter.3.1.4 For the definition of wool and other textile terms usedin th
11、is method, refer to Terminology D 123.4. 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-dried components of the undissolved
12、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 D 1113 is considered satisfactory for ac-ceptance testing of commercial shipments, and the procedurehas been used exte
13、nsively in the trade for this purpose,particularly in connection with the determination of clean woolfiber present by Test Method D 584. The procedure in TestMethod D 1113 is used by the U.S. Customs Service for thedetermination of the vegetable matter in importations of rawwool on which the allowan
14、ce for loss of wool during commer-cial cleaning is based in part.35.1.1 In case of a dispute arising from differences inreported test results when using Test Method D 1113 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparative tests to determine ifthe
15、re is a statistical bias between their laboratories. Competentstatistical assistance is recommended for the investigation of1This test method is under the jurisdiction of ASTM Committee D13 on Textiles,and is the direct responsibility of Subcommittee D13.13 on Wool and Wool Felt.Current edition appr
16、oved Dec. 31, 1990. Published March 1991. Originallypublished as D111350T. Last previous edition D111378 (1983).2Annual Book of ASTM Standards, Vol 07.01.3Tariff Schedules of the United States, Schedule 3, Part 1, Subpart C, Headnote1(c).1Copyright ASTM, 100 Barr Harbor Drive, West Conshohocken, PA
17、19428-2959, United States.bias. 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 the type in question. The testspecimens should then be randomly assigned in equal numbersto each laboratory for testing. The av
18、erage results from the twolaboratories should be compared using Students t-test forunpaired data and an acceptable probability level chosen by thetwo parties before the testing is begun. If a bias is found, eitherits cause must be found and corrected or the purchaser and thesupplier must agree to in
19、terpret future test 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
20、 62C.6.3 Muffle Furnace, thermostatically controlled in the rangeof 700 6 25C.6.4 BeakersHeat resistant glass or stainless steel, of2-litre capacity.7. Reagents and Materials7.1 Sodium Hydroxide Solution (NaOH), 3 % by weight.7.2 Sodium Hydroxide Solution, 10 % by weight.7.3 Sodium Hypochlorite Solu
21、tion (NaOCl), 5 % byweight.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,take
22、at random the number of shipping containers directed inan applicable material specification or other agreement be-tween the purchaser and the supplier. Consider shippingcontainers to be the lot sampling unit.NOTE 2An adequate specification or other agreement between thepurchaser and the supplier req
23、uires taking into 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 li
24、miting quality level.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 MethodsD 584 and D 1334, prepare a portion of scoured and dried woolfrom each lot sampling unit of the lot sample described in 9.1.Make sure
25、 that each portion is 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 anotherrepl
26、icate, that is, a second laboratory sample unit.9.2.2 For tests on samples of scoured wool not obtained inconnection with Test Methods D 584 and D 1334 take replicatesample units as directed in 9.2.1.9.3 Test SpecimensAs test specimens, prepare two testspecimens from each laboratory sampling unit by
27、 combiningten or more 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 D 584.10.2 Weigh specimens taken as directed in 9.2 in thecondition as received, in the oven-dry cond
28、ition, or afterexposure 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, brin
29、g 1 L of 3 % NaOH solution 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
30、. Remove the beaker from 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
31、 such wools the alternative 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 D 584.11.1.1 Alternative Method (Note 2)In a 2-L heat-resistantglass or stain
32、less steel beaker, bring 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
33、through the 40-meshfilter, 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
34、 filter. Sprinkle about 15 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 o
35、n the filter. Estimate the 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 there
36、sidue as directed in 11.4 and use the appropriate calculations.NOTE 5For clean wool fiber determination (Test Method D 584), takecare to exclude or correct for components emanating from the original orD 11132sample package wrapper or container.11.4 Drying and AshingTransfer the rinsed material fromt
37、he filter into a tared porcelain 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).12. Calculation of Results12.1 Vegetable Matter BaseUsing Eq 1 and the appropri-ate values in Table 1, calculate the co
38、rrection factor forconverting 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 f1v11 f2v21 . (1)V 5 100FvW12 A!/W2(2)where:Fv= correction factor for vegetable
39、 matter only,V = vegetable matter base expressed as a percent ofthe weight of the original specimen,f1f2= weight (mass) fractions of the individual typesof vegetable matter in the recovered alkali-insoluble impurities,v1v2= factors for the individual types of vegetablematter (from Table 1),W1= weigh
40、t (mass) of oven-dried recovered 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
41、forconverting the weight (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 Fv1 fcc 1 fpp 1 fss
42、1 ftt 1 fxx (3)T 5 100FTW12 A!/W2(4)where:Fv, W1, W2and A have the meanings given in 12.1, andFT= average correction factor for total alkali-insoluble impurities,T = percentage oven-dried, ash-free,extractives-free total alkali-insoluble im-purities,fc,fp,fs,ft,fx= weight fractions of cotton and oth
43、er fi-bers, paint, skin, tag material, and paperstring, respectively, in the recoveredalkali-insoluble impurities, andc, p, s, t, x = factors for cotton and other fibers, paint,skin, tag material, and paper string, re-spectively (from Table 1).13. Report13.1 State that the tests were made as directe
44、d in ASTM TestMethod D 1113. Describe the 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 percent
45、ages: oven-driedweight, as-received weight, 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 t
46、hree subsamples randomlydrawn from the same core sample of a grease wool, using theprocedures prescribed in Test Method D 584. In each labora-tory two 40-g specimens were taken from each oven-driedscoured subsample and tested by one operator for total alkali-insoluble impurities, using 3 % NaOH solu
47、tion and visuallyestimating the fractions of the impurity components. Thisprocedure was repeated on core samples from two additionalgreasy wools. The vegetable matter base content for all threescoured wools was less than 1 percentage point. Under theseconditions the components of variance for the pe
48、rcentage oftotal alkali-insoluble impurities expressed as standard devia-tions were found 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 alkal
49、i-insolubleimpurities in scoured wool should be considered significantlydifferent at the 95 % probability level if the difference equals orexceeds the following critical differences (Note 6):4ASTM Research Report No. D13-1012. A copy is available from ASTMHeadquarters, 100 Barr Harbor Drive, West Conshohocken, PA 194282959, UnitedStates.TABLE 1 Correction Factors for Alkali-Insoluble ImpuritiesNOTE 1Average value of the ratio of scoured, oven-dry ash-free,extractive-free weight of vegetable matter and other alkali-insolublematter to the correspondin
