ASTM D1574-2004(2013) Standard Test Method for Extractable Matter in Wool and Other Animal Fibers《羊毛和其它动物纤维中可萃取物的标准试验方法》.pdf

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1、Designation: D1574 04 (Reapproved 2013)Standard Test Method forExtractable Matter in Wool and Other Animal Fibers1This standard is issued under the fixed designation D1574; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year o

2、f 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 amountof extractable matter in samples of all forms of wool, except

3、grease wool, that is extractable with a non-flammable vapordegreasing and cleaning solvent.1.2 This test method does not cover the determination of theamounts of different components in the extracted matter northeir identification.1.3 This test method is suitable for use with other animalfibers.NOTE

4、 1The determination of extractable matter in yarns and in feltsis covered in Test Methods D2257 and D461. For the determination ofalcohol-extractable matter in oven-dry scoured wool, refer to Test Meth-ods D584 and D1334.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This st

5、andard does not purport to address the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use. See 5.4 and Note 3.2. Referenced Doc

6、uments2.1 ASTM Standards:2D123 Terminology Relating to TextilesD461 Test Methods for Felt (Withdrawn 2003)3D584 Test Method for Wool Content of Raw WoolLaboratory ScaleD1334 Test Method for Wool Content of Raw WoolCommercial ScaleD1576 Test Method for Moisture in Wool by Oven-DryingD2257 Test Method

7、 for Extractable Matter in TextilesD2462 Test Method for Moisture in Wool by DistillationWith TolueneD4845 Terminology Relating to Wool3. Terminology3.1 Definitions:3.1.1 For definitions of textile terms used in this testmethod: animal fiber, extractable matter, grease wool, recycledwool, wool and w

8、ool, refer to Terminology D4845.3.2 For definitions of other textile terms used in this testmethod, refer to Terminology D123.4. Summary of Test Method4.1 The specimen is extracted in a Soxhlet apparatus with aspecified halogenated hydrocarbon solvent. The extract isfiltered, the solvent is evaporat

9、ed, and both the residue and theextracted specimen are dried and weighed. The amount ofextractable matter is calculated and reported as a percentage ofthe oven-dry mass of the wool specimen, that is, the mass ofthe oven-dried extracted specimen plus the mass of theoven-dried extracted material.4.2 S

10、pecial procedures are provided to correct for errors indetermining the amount of extractable matter as summarized in4.1 if it is known or thought to contain volatile components.5. Significance and Use5.1 Test Method D1574 is considered satisfactory for ac-ceptance testing since the method has been u

11、sed extensively inthe trade for acceptance testing.5.1.1 In case of a dispute arising from differences inreported test results when using Test Method D1574 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparative tests to determine ifthere is a statisti

12、cal 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 the type in question. The testspecimens shoul

13、d 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 testing is begun. If a bias is found, either1This

14、 test method is under the jursidiction 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 September 2013. Originallyapproved in 1958. Last previous edition approved in 2008 as D1574 04(2008).DOI:

15、10.1520/D1574-04R13.2For 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.3The last approved version of this histor

16、ical standard is referenced onwww.astm.org.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 test results in the light ofthe known bia

17、s.5.2 This test method may be used to estimate the quantity ofoil, grease, and waxy materials remaining on or in wool fibersafter scouring, or the quantity of lubricant added before cardingor remaining after carding, or the quantity of such materialsadded or removed in subsequent processing operatio

18、ns.5.3 The residues obtained in this test may be subjected tochemical analysis for identification and assay of the componentmaterials, if desired.5.4 The specified solvent in this test method does notremove some materials, such as soaps, that may be present inwool and hence in some cases may reflect

19、 more closely theadded content of some extractables in wool such as oils. Whensuch materials are present and an estimate of their quantity isdesired, some other solvent or combination of solvents shouldbe used as specified in a material specification or by agreement.The information in theAnnex of th

20、is test method may be usefulfor this purpose. Various solvents have been used in the past,and are still used to some extent. Many of these solvents areundesirable, however, because of flammability, toxic or anes-thetic effects, or unpleasant odors. Trichlorotrifluoroethane isnonflammable, has a very

21、 low level of toxicity, and a highdegree of stability and is a good solvent for most fatty ormineral oils, greases, and waxes. The specified solvent, underconditions of the test, was found in interlaboratory test not toextract wool protein.NOTE 2Since the specified solvent is primarily a solvent for

22、 oils ratherthan soap, the extractable matter obtained in this procedure may beconsidered a measure of commercial oil content.NOTE 3Due to the hazardous nature of some of the solvents listed inTable A1.1, the user should refer to the manufacturers recommendationsfor use before using under the condit

23、ions of this test method.6. Apparatus and Reagents6.1 Soxhlet Extraction Apparatus, including an extractiontube, condenser, and flask. A large extraction tube having astandard-taper joints T55/50 and 24/40 and a 300-mL flask arerecommended, but any size capable of holding at least a 10-gspecimen is

24、satisfactory.6.2 Heater for Extraction Apparatus, preferably electric,thermostatically controlled, and of a design that avoids directheating of the flask above the lowest solution level.6.3 Drying Oven, ventilated either by natural convection orforced draft, thermostatically controlled and maintaine

25、d at 1056 3C throughout the oven chamber.6.4 Filter Paper,4medium speed, retentive, in large sheets,580 by 580 mm (23 by 23 in.), or in circles large enough toform a thimble of a size to fit the apparatus, or as an alternative,a cellulose extraction thimble.6.5 Weighing Containers, of perforated met

26、al if weighing ofthe specimen is to be performed in the drying enclosure; orcontainers that can be hermetically sealed (such as glassweighing bottles) if the specimen is to be cooled in a desiccatorbefore weighing in the ambient atmosphere.6.6 Balance, having a capacity adequate for weighingspecimen

27、s, flasks, and containers and having a sensitivity of0.001 g.6.7 SolventEnsolv.57. Sampling7.1 Lot SampleAs a lot sample for acceptance testing,unless otherwise agreed upon between purchaser and supplier,take at random the number of packages of wool from a lot asdirected in Table 1. Consider package

28、s of wool as the primarysampling unit.7.2 Laboratory SampleConsider the package of wool inthe lot sample as the laboratory sample.7.3 Test SpecimenFrom each package in the laboratorysample take at random two specimens each weighing 10 6 1g.7.3.1 If the determination of volatile matter in extractable

29、s,as described in 9.5.2, is to be undertaken, weigh the testspecimen to the nearest 0.001 g and record this mass as T. Thisspecimen is for extraction.7.3.2 For each test specimen taken for extraction, take asecond test specimen for moisture determination, weighingbetween 50 and 70 g. Weigh to the ne

30、arest 0.05 g the same timethe extraction test specimen is weighed so that the moisturecontent of the two specimens at the time of weighing will beidentical.8. Conditioning8.1 Neither preconditioning nor conditioning is necessary.9. Procedure9.1 Wrap the specimen in a single sheet of fresh filter pap

31、er(or place in an extraction thimble free of matter extractable bythe specified solvent) and insert the assemblage in the extrac-tion tube. Make certain that all open edges of the filter paper orthimble extend above the siphon tube.9.2 Attach to the extraction tube a 300-mL flask that haspreviously

32、been dried at 105 6 3C, cooled in a desiccator, andweighed to the nearest 1 mg.9.3 Slowly pour sufficient solvent over the specimen to startthe siphoning action. (If a thimble is used to hold the specimen,pour the solvent onto the specimen within the thimble). When4Whatman Filter Paper No. 2, or its

33、 equivalent, has been found satisfactory forthis test method.5This solvent is available from Enviro Tech International Inc., West LeMoyne,Melrose Park, IL 60160 ().TABLE 1 Sampling Schedule for Wool in PackageNumber of Packagesin LotNumber of Packagesin Lot Sample1to3 all4to24 425 to 50 5more than 5

34、0 10% of the packageswith a maximumof 8D1574 04 (2013)2the siphoning has stopped add another 20 mL of solvent.Connect the extraction tube to the condenser, place the flask onthe heater, and extract for 20 siphon cycles. Adjust the heat sothat the total time taken for 20 siphon cycles is 100 6 10 min

35、.NOTE 4The specified solvent, Ensolv, boils at 69 C at sea level.However, at higher elevations the boiling point is reduced and care mustbe taken to ensure the specified rate of siphoning.9.4 Following the twentieth cycle of siphoning, remove theflask and the extraction tube from the heater. Pull th

36、e specimenand filter paper (thimble) up to the mouth of the extraction tubeand allow to drain until a state of dripping only is observed.Remove the specimen and filter paper (thimble) from theextraction tube and treat as described in 9.6.9.5 Pour the solvent thus contained in the extraction tubeinto

37、 the flask. Reconnect the flask, extraction tube, andcondenser and place back the flask on the heater to slowly boiloff the solvent (for recovery if desired) into the extraction tubeuntil the flask contains about 20 to 30 mL of solvent. Removethe flask from the assemblage and slowly evaporate thesol

38、vent, in the flask, below the boiling point (care should betaken to avoid any loss of solvent and extractable matter byoverheating and sputtering); then dry to constant mass, byplacing the flask in an oven at 105 6 3C. Cool in a desiccatorand weigh to the nearest 1 mg.9.5.1 Certain oils and finishin

39、g agents may contain volatilecomponents that may be lost during evaporation of the solventand oven-drying. If the identification of the oil or finishingagent is known, a weighed specimen of the material may bedissolved in a fresh portion of the solvent, the solvent thenbeing evaporated as described

40、in 9.5, and the residue weighedto determine the volatility of the oil. A correction factorspecific for the known oil may be calculated using Eq 1 and 2and subsequently using the correction factor to determine themass of oven-dried matter corrected for the loss of volatilematerial for use in 10.1, Eq

41、 5:M 5 S 2 V (1)F 5 S/S 2 V! 5 S/M (2)C 5 MF (3)where:M = mass of oven-dried extracted matter,V = mass of original material volatilized,S = mass of original material dissolved in solvent,F = correction factor, andC = mass of oven-dried extracted matter corrected for lossof volatile material.9.5.2 If

42、 the oil or finishing agent is not known but is thoughtto contain volatile components, and if it is desirable todetermine the total quantity of extractables including thevolatile fraction, the following procedure may be used:9.5.2.1 Using the second test specimen intended for mois-ture testing (see

43、7.3.2), determine the true-moisture contentusing Test Method D2462. This procedure determines moistureindependent of volatile matter, which would be lost in anoven-drying procedure.(1) Test Method D2462 is not applicable to material knownto contain any steam distillable water-soluble matter. If it i

44、ssuspected that such matter is present, the method should beused with caution.9.5.2.2 Extract the first test specimen as described in Sec-tion 9, having determined the mass T of the test specimenbefore extraction (see 7.3.1), and the mass W of the oven-driedtest specimen after extraction.9.5.2.3 Rat

45、ionaleExtractable matter, as calculated usingEq 4, consists of non-volatile matter only. When the percent oftrue-moisture, X, is determined as directed in 9.5.2.1, thecorresponding mass of moisture, U, can be calculated. Whenthe weighed test specimen has been extracted and oven-dried,its mass, W, is

46、 determined. But W is also equal to T, less themoisture U, less the non-volatile extractables M, less thevolatile extractables N (Eq 7), from the available experimentaldata (T, U, M, and W), the mass of the volatile extractablematter N can be calculated (Eq 8) and subsequently, the percentvolatile m

47、atter Y, can be obtained (Eq 9).9.6 Air-dry the extracted specimen, then place the specimenin a suitable container and dry in an oven at 105 6 3C toconstant mass, defined as the absence of any progressivedecrease in mass in excess of 0.10 % of the average, asdetermined by three successive weighings

48、using the procedurein either 9.6.1 or 9.6.2 to obtain the oven-dry mass of thespecimen.9.6.1 If the weighings of the dried specimen are to beobtained with the specimen inside the oven, perform theweighings with any forced-air circulation turned off. Continuereadings of mass until the conditions spec

49、ified in 9.6 areachieved.9.6.2 If the weighings of the dried specimen are to beobtained outside the oven, dry the specimen in a containerprovided with a tight-fitting cover with this cover removedwhile in the oven. At the end of the drying period, cover thecontainer and remove it from the oven. Place the coveredcontainer in a desiccator, loosen the cover, and cool thespecimen and container to approximately room temperature.When cooling is completed, set the cover firmly on thecontainer and weigh the container, cover, and specimen.Replace the contain