ASTM D1574-2004 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: D 1574 04Standard Test Method forExtractable Matter in Wool and Other Animal Fibers1This standard is issued under the fixed designation D 1574; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision.

2、 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 amountof extractable matter in samples of all forms of wool, exceptgrease wool, th

3、at 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 1The determina

4、tion of extractable matter in yarns and in feltsis covered in Test Methods D 2257 and D 461. For the determination ofalcohol-extractable matter in oven-dry scoured wool, refer to Test Meth-ods D 584 and D 1334.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This standard does

5、 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 Documents2.1 A

6、STM Standards:2D 123 Terminology Relating to TextilesD 461 Test Methods for FeltD 584 Test Method for Wool Content of Raw WoolLaboratory ScaleD 1334 Test Method for Wool Content of Raw WoolCommercial ScaleD 1576 Test Method for Moisture in Wool by Oven DryingD 2257 Test Method for Extractable Matter

7、 in TextilesD 2462 Test Method for Moisture in Wool by Distillationwith TolueneD 4845 Terminology for 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 wool, refer to Terminology D 4

8、845.3.2 For definitions of other textile terms used in this testmethod, refer to Terminology D 123.4. Summary of Test Method4.1 The specimen is extracted in a Soxhlet apparatus with aspecified halogenated hydrocarbon solvent. The extract isfiltered, the solvent is evaporated, and both the residue an

9、d 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 Special procedures are provi

10、ded 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 D 1574 is considered satisfactory foracceptance testing since the method has been used extensivelyin the trade

11、for acceptance testing.5.1.1 In case of a dispute arising from differences inreported test results when using Test Method D 1574 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparative tests to determine ifthere is a statistical bias between their labo

12、ratories. 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 should then be randomly assigned

13、 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 test method is under the j

14、ursidiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.13 on Wool and Wool Felt .Current edition approved Nov. 1, 2004. Published December 2004. Originallypublished as D 1574 58 T. Last previous edition D 1574 87.2For referenced ASTM standards, visit the AS

15、TM 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 19428-2959, Unit

16、ed States.its cause must be found and corrected or the purchaser and thesupplier must agree to interpret future test results in the light ofthe known bias.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

17、quantity of lubricant added before cardingor remaining after carding, or the quantity of such materialsadded or removed in subsequent processing operations.5.3 The residues obtained in this test may be subjected tochemical analysis for identification and assay of the componentmaterials, if desired.5

18、.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 more closely theadded content of some extractables in wool such as oils. Whensuch materials are present and an estimate of their quantity isdesire

19、d, some other solvent or combination of solvents shouldbe used as specified in a material specification or by agreement.The information in theAnnex of this 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

20、 areundesirable, however, because of flammability, toxic or anes-thetic effects, or unpleasant odors. Trichlorotrifluoroethane isnonflammable, has a very low level of toxicity, and a highdegree of stability and is a good solvent for most fatty ormineral oils, greases, and waxes. The specified solven

21、t, underconditions of the test, was found in interlaboratory test not toextract wool protein.NOTE 2Since the specified solvent is primarily a solvent for oilsrather than soap, the extractable matter obtained in this procedure may beconsidered a measure of commercial oil content.NOTE 3Due to the haza

22、rdous nature of some of the solvents listed inTable A1.1, the user should refer to the manufacturers recommendationsfor use before using under the conditions of this test method.6. Apparatus and Reagents6.1 Soxhlet Extraction Apparatus, including an extractiontube, condenser, and flask. A large extr

23、action 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 satisfactory.6.2 Heater for Extraction Apparatus, preferably electric,thermostatically controlled, and of a design that avoids directheating of the

24、 flask above the lowest solution level.6.3 Drying Oven, ventilated either by natural convection orforced draft, thermostatically controlled and maintained at 1056 3C throughout the oven chamber.6.4 Filter Paper,3medium speed, retentive, in large sheets,580 by 580 mm (23 by 23 in.), or in circles lar

25、ge 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 metal if weighing ofthe specimen is to be performed in the drying enclosure; orcontainers that can be hermetically sealed (such as glassweighing bottl

26、es) if the specimen is to be cooled in a desiccatorbefore weighing in the ambient atmosphere.6.6 Balance, having a capacity adequate for weighing speci-mens, flasks, and containers and having a sensitivity of 0.001g.6.7 SolventEnsolv.47. Sampling7.1 Lot SampleAs a lot sample for acceptance testing,u

27、nless otherwise agreed upon between purchaser and supplier,take at random the number of packages of wool from a lot asdirected in Table 1. Consider packages of wool as the primarysampling unit.7.2 Laboratory SampleConsider the package of wool inthe lot sample as the laboratory sample.7.3 Test Specim

28、enFrom 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 extractables,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 extrac

29、tion.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 nearest 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 b

30、eidentical.8. Conditioning8.1 Neither preconditioning nor conditioning is necessary.9. Procedure9.1 Wrap the specimen in a single sheet of fresh filter paper(or place in an extraction thimble free of matter extractable bythe specified solvent) and insert the assemblage in the extrac-tion tube. Make

31、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 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 s

32、iphoning action. (If a thimble is used to hold the specimen,pour the solvent onto the specimen within the thimble). Whenthe 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

33、 sothat the total time taken for 20 siphon cycles is 100 6 10 min.3Whatman Filter Paper No. 2, or its equivalent, has been found satisfactory forthis test method.4This solvent is available from Enviro Tech International Inc., West LeMoyne,Melrose Park, IL 60160 ().TABLE 1 Sampling Schedule for Wool

34、in PackageNumber of Packagesin LotNumber of Packagesin Lot Sample1to3 all4to24 425 to 50 5more than 50 10% of the packageswith a maximumof 8D1574042NOTE 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 ensu

35、re the specified rate of siphoning.9.4 Following the twentieth cycle of siphoning, remove theflask and the extraction tube from the heater. Pull the 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 speci

36、men 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 the flask. Reconnect the flask, extraction tube, andcondenser and place back the flask on the heater to slowly boiloff the solvent (for recovery if desi

37、red) into the extraction tubeuntil the flask contains about 20 to 30 mL of solvent. Removethe flask from the assemblage and slowly evaporate thesolvent, in the flask, below the boiling point (care should betaken to avoid any loss of solvent and extractable matter byoverheating and sputtering); then

38、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 finishing agents may contain volatilecomponents that may be lost during evaporation of the solventand oven-drying. If the identification of the oil or finishinga

39、gent is known, a weighed specimen of the material may bedissolved in a fresh portion of the solvent, the solvent thenbeing evaporated as described 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 2an

40、d subsequently using the correction factor to determine themass of oven-dried matter corrected for the loss of volatilematerial for use in 10.1,Eq5: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 origina

41、l material dissolved in solvent,F = correction factor, andC = mass of oven-dried extracted matter corrected for lossof volatile material.9.5.2 If the oil or finishing agent is not known but is thoughtto contain volatile components, and if it is desirable todetermine the total quantity of extractable

42、s including thevolatile fraction, the following procedure may be used:9.5.2.1 Using the second test specimen intended for mois-ture testing (see 7.3.2), determine the true-moisture contentusing Test Method D 2462. This procedure determines mois-ture independent of volatile matter, which would be los

43、t in anoven-drying procedure.9.5.2.1.1 Test Method D 2462 is not applicable to materialknown to contain any steam distillable water-soluble matter. Ifit is suspected 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,

44、 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 RationaleExtractable matter, as calculated usingEq 4, consists of non-volatile matter only. When the percent oftrue-moisture, X, is determined as di

45、rected 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 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

46、 available experimentaldata (T, U, M, and W), the mass of the volatile extractablematter N can be calculated (Eq 8) and subsequently, the percentvolatile matter 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

47、 toconstant mass, defined as the absence of any progressivedecrease in mass in excess of 0.10 % of the average, asdetermined by three successive weighings 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 beobta

48、ined with the specimen inside the oven, perform theweighings with any forced-air circulation turned off. Continuereadings of mass until the conditions specified 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

49、 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 container and specimen in the oven, remove thecover, and dry. Repeat the cooling and weighing procedures.Continue this procedure until the conditions sp