ASTM D2257-98(2004)
(Test Method)Standard Test Method for Extractable Matter in Textiles
Standard Test Method for Extractable Matter in Textiles
SIGNIFICANCE AND USE
This test method may be used for acceptance testing of commercial shipments.
5.1.1 In case of a dispute arising from differences in reported test results using this test method for acceptance testing of commercial shipments, the purchaser and the supplier should conduct comparative tests to determine if there is a statistical bias between the laboratories. Competent statistical assistance is recommended for the investigation of bias. As a minimum, the two parties should take a group of test specimens which are as homogeneous as possible and which are from a lot of material of the type in question. The test specimens should then be randomly assigned in equal numbers to each laboratory for testing. The average results from the two laboratories should be compared using appropriate statistical analysis and a probability level chosen by the two parties before the testing begins. If a bias is found, either its cause must be found and corrected, or the purchaser and supplier must agree to interpret future test results with consideration to the known bias.
This test method is used for the determination of the amounts of naturally present oily or waxy impurities that have not been completely removed from textiles made from animal fibers, and for the determination of the amounts of oily or waxy finishing materials applied to raw materials or textiles during manufacture. See 3.1.1, extractable matter.
The test method may be used as a step in the determination of the commercial weight of fiber, yarn, and textile shipments.
The International Wool Textile Organization specifies the use of a halogenated hydrocarbon, dichloromethane, also called methylene chloride (CH2Cl2) instead of the solvent specified in this test method (IWTO-10-62(E)).
Extractables by mass loss is frequently used for textiles which have a relatively large amount of extractable material to effect a significant mass change.
SCOPE
1.1 This test method covers a procedure for determining the extractable material on most fibers, yarns, and fabrics. Three options are included. Option 1 uses heat and Soxhlet extraction apparatus. Option 2 uses room temperature and extraction funnels. Option 3 uses either Option 1 or Option 2 extraction but provides for calculation of extractable matter from the loss in mass of the material due to the extraction rather than the extractable matter residue.
Note 1
Other standards for the determination of extractable matter in textiles made of specific fibers include: Specification D 541, Specification D 681, and Test Method D 1574.
1.1.1 The solvents for use in this method are any solvents that the party or parties concerned agreed on; such as, Halogenated Hydrocarbon (HH) chloroform, tetrachloroethane, alcohol.
1.1.2 This test method may not extract cross-linked finishes or resins which may be on the textile.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. See Sections 6 and 7.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D2257–98 (Reapproved 2004)
Standard Test Method for
Extractable Matter in Textiles
This standard is issued under the fixed designation D2257; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D1574 Test Method for Extractable Matter in Wool and
Other Animal Fibers
1.1 This test method covers a procedure for determining the
D1909 StandardTable of Commercial Moisture Regains for
extractable material on most fibers, yarns, and fabrics. Three
Textile Fibers
options are included. Option 1 uses heat and Soxhlet extraction
D2258 Practice for Sampling Yarn for Testing
apparatus. Option 2 uses room temperature and extraction
D3333 Practice for Sampling Manufactured Staple Fibers,
funnels. Option 3 uses either Option 1 or Option 2 extraction
Sliver, or Tow for Testing
but provides for calculation of extractable matter from the loss
D4920 Terminology Relating to Conditioning, Chemical,
in mass of the material due to the extraction rather than the
and Thermal Properties
extractable matter residue.
2.2 Other Documents:
NOTE 1—Other standards for the determination of extractable matter in
IWTO 10-62(E) Method for Determination of the Dichlo-
textiles made of specific fibers include: Specification D541, Specification
romethane Soluble Matter in Combed Wool Sliver
D681, and Test Method D1574.
1.1.1 The solvents for use in this method are any solvents 3. Terminology
that the party or parties concerned agreed on; such as,
3.1 Definitions:
Halogenated Hydrocarbon (HH) chloroform, tetrachloroeth-
3.1.1 extractable matter, n—nonfibrous material in or on a
ane, alcohol.
textile not including water, which is removable by a specified
1.1.2 This test method may not extract cross-linked finishes
solvent or solvents as directed in a specified procedure.
or resins which may be on the textile.
3.1.1.1 Discussion—Nonfibrous material is usually oily,
1.2 This standard does not purport to address all of the
waxy, resinous, or polymeric in nature, but may also include
safety concerns, if any, associated with its use. It is the
other material, such as protein, particularly if ethyl alcohol is
responsibility of the user of this standard to establish appro-
used, or in, the extracting solvent.
priate safety and health practices and determine the applica-
3.1.2 For definitions of other moisture terms related to
bility of regulatory limitations prior to use. See Sections
textiles, refer to Terminology D4920. For definitions of other
6 and 7.
textile terms used in this test method refer to Terminology
D123.
2. Referenced Documents
2.1 ASTM Standards: 4. Summary of Test Method
D123 Terminology Relating to Textiles
4.1 The specimen is extracted either in Soxhlet apparatus
D541 Specification for Single Jute Yarn
(Option 1), or extraction funnel (Option 2) first with an agreed
D681 Specification for Jute Rove and Plied Yarn for Elec-
solvent (Note 2). The solvents are evaporated and the residues
3 3
trical and Packing Purposes
and the specimens are dried and weighed separately. The
amounts of extracted matter are reported as percentages of
either the oven-dried mass or of the oven-dried mass plus
commercial moisture regain for the textile.
This test method is under the jurisdiction ofASTM Committee D13 onTextiles
and is the direct responsibility of Subcommittee D13.51 on Conditioning and,
4.2 Alternatively, in Option 3, the specimen is dried and
Chemical and Thermal Properties.
weighed before and after extraction using Option 1 or Option
Current edition approved Oct. 1, 2004. Published November 2004. Originally
2. Extractable matter is calculated as the loss in mass reported
approved in 1989. Last previous edition approved in 1998 as D2257 – 98. DOI:
10.1520/D2257-98R04. as percentages of the extracted oven-dried mass or this mass
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
plus commercial moisture regain for the textile.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
3 4
Withdrawn. The last approved version of this historical standard is referenced Available from International Wool Secretariat, Carlton Gardens, London S.W.
on www.astm.org. 1, England.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2257–98 (2004)
5. Significance and Use 6.6 Tray, to contain desiccant, with a screen to prevent
specimen or container contact with desiccant, for use in the
5.1 This test method may be used for acceptance testing of
vacuum oven. If Phosphorus pentoxide (P 0 ) or sulfuric acid
2 5
commercial shipments.
(H SO ) is used, the screen must be acid resistant.
2 4
5.1.1 In case of a dispute arising from differences in
6.7 Dessicator
reported test results using this test method for acceptance
6.8 Analytical Balance—sensitive to 0.0001 g.
testing of commercial shipments, the purchaser and the sup-
6.9 Nitrogen, to supply the vacuum oven.
plier should conduct comparative tests to determine if there is
a statistical bias between the laboratories. Competent statistical 6.10 Solvent—as agreed (see 1.1.1). (Warning—Various
assistance is recommended for the investigation of bias. As a solvents have been used in the past, and are still used to some
minimum, the two parties should take a group of test speci- extent. Many of these solvents are flammable, toxic or have
mens which are as homogeneous as possible and which are anesthetic effects, or unpleasant odors. As with all volatile
from a lot of material of the type in question. The test solvents, the use of adequate ventilation under a hood is
specimens should then be randomly assigned in equal numbers recommended when using this solvent.)
to each laboratory for testing.The average results from the two
laboratories should be compared using appropriate statistical 7. Hazards
analysis and a probability level chosen by the two parties
7.1 Refer to the manufacturer’s material safety data sheets
before the testing begins. If a bias is found, either its cause
for specific information on chemicals used in this test.
must be found and corrected, or the purchaser and supplier
7.2 After extraction with alcohol or other flammable or
must agree to interpret future test results with consideration to
toxic solvents, the specimens must be air-dried under a hood
the known bias.
until nearly all of the solvent has evaporated before they are
5.2 This test method is used for the determination of the
dried in the oven. Otherwise there is a danger of building up a
amounts of naturally present oily or waxy impurities that have
dangerous concentration of explosive vapor in the oven. Oven
not been completely removed from textiles made from animal
doors have been blown across the room by the force of an
fibers,andforthedeterminationoftheamountsofoilyorwaxy
explosion.
finishing materials applied to raw materials or textiles during
7.3 Warning—Dichloromethane is toxic, and its use is
manufacture. See 3.1.1, extractable matter.
recommended only when necessary to conform to international
5.3 The test method may be used as a step in the determi-
specifications,andthenwithadequateventilationunderahood.
nation of the commercial weight of fiber, yarn, and textile
shipments.
8. Sampling
5.4 The International Wool Textile Organization specifies
8.1 Lot Sample—As a lot sample for acceptance testing,
the use of a halogenated hydrocarbon, dichloromethane, also
take at random the number of shipping containers directed in
called methylene chloride (CH Cl ) instead of the solvent
2 2
an applicable material specification or other agreement be-
specified in this test method (IWTO-10-62(E)).
tween the purchaser and the supplier. Consider shipping
5.5 Extractables by mass loss is frequently used for textiles
containers to be the primary sampling unit.
which have a relatively large amount of extractable material to
effect a significant mass change.
NOTE 3—An adequate specification or other agreement between the
purchaser and the supplier requires taking into account the variability
6. Apparatus and Reagents between shipping containers, within a shipping container, and between
specimens taken from a single unit within a shipping container, so as to
6.1 Extraction Apparatus
provide a sampling plan with a meaningful producer’s risk, consumer’s
6.1.1 Soxhlet Extraction Apparatus for Option 1 extraction
risk, acceptable quality level, and limiting quality level.
6.1.2 Extraction Funnels, wide-mouth, 125 or 150-mL ca-
8.2 Laboratory Sample—As a laboratory sample for accep-
pacity for Option 2 extraction.
tance testing, proceed as follows:
6.2 Thimbles, fat-free cellulose or Alundum, for Option 1.
8.2.1 Yarn on Packages—Take at random from each ship-
6.3 Specimen Compressor, pestle or long forceps, for han-
ping container in the lot sample the number of packages
dling specimens in Option 2.
directed in an applicable material specification or other agree-
6.4 Containers,
ment between the purchaser and the supplier, such as an
6.4.1 To hold extractables and that will seal to prevent
agreement to use Practice D2258. Preferably, the same number
moisture changes, for example weighing bottles, for Option 1.
of packages should be taken from each shipping case in the lot
6.4.2 To collect solvent from extractions, for Option 2.
sample. If differing numbers of packages are to be taken from
NOTE 2—If metal containers are used, check to ensure that the
shipping cases in the lot sample, determine at random which
extracatable matter does not react with the metal if the residue is to be
shipping cases are to have each number of packages drawn.
weighed.
8.2.2 Yarn on Beams—Take a laboratory sample from each
6.5 Oven of the beams in the lot sample as agreed between the purchaser
6.5.1 Ventilated Forced-Draft Drying Oven, capable of and the supplier.
maintaining a temperature of 105 6 3°C. 8.2.3 Fabrics—Take a full width swatch 1 m long from the
6.5.2 Vacuum Type, maintained at 65 6 2°C for use in endofeachrolloffabricinthelotsample,afterfirstdiscarding
Option 3 when low-boiling ingredients are present. a minimum of 1 m of fabric from the very outside of the roll.
D2257–98 (2004)
8.2.4 Staple Fiber—Systematically take five laboratory overflowing. In case there is evidence that 20 siphonings are
sample units from each bale in the lot sample as directed in not sufficient, the purchaser and supplier should agree upon a
Practice D3333. suitable number of siphonings.
8.2.5 Tow, Sliver, or Top—Take from the lead end of a 10.2.6 Remove from the source of heat when the upper
strand from each shipping container in the lot sample the first chamber of the apparatus is nearly full and ready to siphon
metre of material that has a clean, uniform appearance. If the again. Pour off the nearly pure solvent from the extraction tube
shipping containers in the lot sample contain multiple pack- and save for reuse after suitable distillation.
ages, take a laboratory sample from one package drawn at 10.2.7 Determine the mass of a weighing bottle to 0.001 g.
random from each container. Transfer the contents of the flask to the tared weighing bottle,
8.3 Test Specimens—Takea10 6 1-g specimen from each rinse with a small quantity of solvent, and add this to the
unit in the laboratory sample. If necessary, take an additional contents of the weighing bottle.
specimen from a random unit in the laboratory sample until 10.2.8 Iflowboilingingredientswerefound(10.1.5)evapo-
there is a total of ten specimens. rate the solvent as directed in 10.1.3 without oven drying the
residue.
9. Conditioning
10.2.9 Iflow-boilingingredientswerenotfound,evaporate
9.1 Neither preconditioning nor conditioning is necessary. the solvent and then dry the residue in an oven at 105 6 3°C
for 30 min. Cool in a desiccator and weigh. Repeat the drying,
10. Procedure
cooling, and weighing cycle until the difference in intervals of
10.1 Presence of boiling ingredients (extractable volatile at
30 min results in a mass change of less than 0.001 g.
low temperatures).
10.2.10 Record the final mass of the residue to the nearest
10.1.1 Use the following procedure to determine the pres-
0.001 g.
ence of low boiling ingredients, that is, extractables that are
NOTE 4—Solvent in weighing bottles may be recovered for subsequent
volatile at low temperatures.
reuse by connecting the effluent stream of solvent and air to a suitable
10.1.2 Extract one or more specimens of the material as
condenser.
directed in 10.2 or 10.3.
10.2.11 Remove the remaining solvent from the Soxhlet
10.1.3 Transfer the solvent quantitatively to a tared weigh-
apparatus, reinsert the thimble and specimen, and fill with the
ing bottle and evaporate the solvent by blowing with a stream
proper amount of alcohol. Extract through at least 12 siphon-
of air at room temperature until there is a mass change of less
ings.
than 0.001 g in 10 min.
10.2.12 Determine the mass of a weighing bottle to 0.001 g.
10.1.4 Heat the residue in an oven at 105 6 3°C for 30 min,
Transfer the alcohol from the flask to the weighing bottle,
cool, and weigh.
evaporate the alcohol, dry, and weigh the residue to the nearest
10.1.5 If there is a mass loss greater than 0.001 g in the
0.001 g.
residue (extractables) due to heating in the oven, the material
10.2.13 Remove the specimen from the apparatus and air
contains extractable matter which volatilizes at low tempera-
dry it. Continue as directed in 10.5.
tures, and the specimen solvent extract should not be heated in
10.3 Option 2, room temperature extraction:
the oven.
10.3.1 Place the specimen in an extraction funnel.
10.1.6 If there is no detectable loss in residue mass (less
10.3.2 Cover the specimen with solvent and let stand for
than 0.001 g) due to heating in the oven, the material does not
about 10 min with occasional stirring to facilitate specimen
contain low boiling ingredients and the extracted residue is
surface and solvent contact.
dried in the oven before final weighing.
10.3.3 Open the funnel stopcock and drain off the solvent
10.2 Option 1, Soxlet Extraction,
into a weighed container. Compress the specimen to force out
10.2.1 Extract fat-free cellulose or Alundum thimbles for
the excess solvent from the specimen.
each specimen in the solvents to be used, in the Soxhlet
10.3.4 Repeat 10.3.2 and 10.3.3 at least once more (Note 5).
chamber
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