ASTM D2257-98(2012)
(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.
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 , Specification , and Test Method D1574.
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.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
General Information
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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 2012)
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 D541 Specification for Single Jute Yarn (Withdrawn 1996)
D681 Specification for Jute Rove and Plied Yarn for Elec-
1.1 This test method covers a procedure for determining the
trical and Packing Purposes (Withdrawn 2000)
extractable material on most fibers, yarns, and fabrics. Three
D1574 Test Method for Extractable Matter in Wool and
options are included. Option 1 uses heat and Soxhlet extraction
Other Animal Fibers
apparatus. Option 2 uses room temperature and extraction
D1909 Standard Table of Commercial Moisture Regains for
funnels. Option 3 uses either Option 1 or Option 2 extraction
Textile Fibers
but provides for calculation of extractable matter from the loss
D2258 Practice for Sampling Yarn for Testing
in mass of the material due to the extraction rather than the
D3333 Practice for Sampling Manufactured Staple Fibers,
extractable matter residue.
Sliver, or Tow for Testing
NOTE 1—Other standards for the determination of extractable matter in
D4920 Terminology Relating to Conditioning, Chemical,
textiles made of specific fibers include: Specification D541, Specification
and Thermal Properties
D681, and Test Method D1574.
2.2 Other Documents:
1.1.1 The solvents for use in this method are any solvents
IWTO 10-62(E) Method for Determination of the Dichlo-
that the party or parties concerned agreed on; such as,
romethane Soluble Matter in Combed Wool Sliver
Halogenated Hydrocarbon (HH) chloroform,
tetrachloroethane, alcohol.
3. Terminology
1.1.2 This test method may not extract cross-linked finishes
or resins which may be on the textile. 3.1 Definitions:
3.1.1 extractable matter, n—nonfibrous material in or on a
1.2 The values stated in SI units are to be regarded as
textile not including water, which is removable by a specified
standard. No other units of measurement are included in this
solvent or solvents as directed in a specified procedure.
standard.
3.1.1.1 Discussion—Nonfibrous material is usually oily,
1.3 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
(Option 1), or extraction funnel (Option 2) first with an agreed
solvent (Note 2). The solvents are evaporated and the residues
This test method is under the jurisdiction ofASTM Committee D13 on Textiles
and the specimens are dried and weighed separately. The
and is the direct responsibility of Subcommittee D13.51 on Conditioning and,
amounts of extracted matter are reported as percentages of
Chemical and Thermal Properties.
Current edition approved Feb. 1, 2012. Published February 2012. Originally
approved in 1989. Last previous edition approved in 1998 as D2257 – 98(2004).
DOI: 10.1520/D2257-98R12.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or The last approved version of this historical standard is referenced on
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM www.astm.org.
Standards volume information, refer to the standard’s Document Summary page on Available from International Wool Secretariat, Carlton Gardens, London S.W.
the ASTM website. 1, England.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2257 − 98 (2012)
either the oven-dried mass or of the oven-dried mass plus 6.4.2 To collect solvent from extractions, for Option 2.
commercial moisture regain for the textile.
NOTE 2—If metal containers are used, check to ensure that the
extracatable matter does not react with the metal if the residue is to be
4.2 Alternatively, in Option 3, the specimen is dried and
weighed.
weighed before and after extraction using Option 1 or Option
2. Extractable matter is calculated as the loss in mass reported 6.5 Oven
as percentages of the extracted oven-dried mass or this mass 6.5.1 Ventilated Forced-Draft Drying Oven, capable of
plus commercial moisture regain for the textile. maintaining a temperature of 105 6 3°C.
6.5.2 Vacuum Type, maintained at 65 6 2°C for use in
5. Significance and Use
Option 3 when low-boiling ingredients are present.
5.1 This test method may be used for acceptance testing of
6.6 Tray, to contain desiccant, with a screen to prevent
commercial shipments.
specimen or container contact with desiccant, for use in the
5.1.1 In case of a dispute arising from differences in
vacuum oven. If Phosphorus pentoxide (P 0 ) or sulfuric acid
2 5
reported test results using this test method for acceptance
(H SO ) is used, the screen must be acid resistant.
2 4
testing of commercial shipments, the purchaser and the sup-
6.7 Dessicator
plier should conduct comparative tests to determine if there is
a statistical bias between the laboratories. Competent statistical 6.8 Analytical Balance—sensitive to 0.0001 g.
assistance is recommended for the investigation of bias. As a
6.9 Nitrogen, to supply the vacuum oven.
minimum, the two parties should take a group of test speci-
6.10 Solvent—as agreed (see 1.1.1). (Warning—Various
mens which are as homogeneous as possible and which are
solvents have been used in the past, and are still used to some
from a lot of material of the type in question. The test
extent. Many of these solvents are flammable, toxic or have
specimens should then be randomly assigned in equal numbers
anesthetic effects, or unpleasant odors. As with all volatile
to each laboratory for testing.The average results from the two
solvents, the use of adequate ventilation under a hood is
laboratories should be compared using appropriate statistical
recommended when using this solvent.)
analysis and a probability level chosen by the two parties
before the testing begins. If a bias is found, either its cause
7. Hazards
must be found and corrected, or the purchaser and supplier
7.1 Refer to the manufacturer’s material safety data sheets
must agree to interpret future test results with consideration to
for specific information on chemicals used in this test.
the known bias.
7.2 After extraction with alcohol or other flammable or
5.2 This test method is used for the determination of the
toxic solvents, the specimens must be air-dried under a hood
amounts of naturally present oily or waxy impurities that have
until nearly all of the solvent has evaporated before they are
not been completely removed from textiles made from animal
dried in the oven. Otherwise there is a danger of building up a
fibers,andforthedeterminationoftheamountsofoilyorwaxy
dangerous concentration of explosive vapor in the oven. Oven
finishing materials applied to raw materials or textiles during
doors have been blown across the room by the force of an
manufacture. See 3.1.1, extractable matter.
explosion.
5.3 The test method may be used as a step in the determi-
7.3 Warning—Dichloromethane is toxic, and its use is
nation of the commercial weight of fiber, yarn, and textile
recommended only when necessary to conform to international
shipments.
specifications,andthenwithadequateventilationunderahood.
5.4 The International Wool Textile Organization specifies
the use of a halogenated hydrocarbon, dichloromethane, also
8. Sampling
called methylene chloride (CH Cl ) instead of the solvent
2 2
8.1 LotSample—Asalotsampleforacceptancetesting,take
specified in this test method (IWTO-10-62(E)).
at random the number of shipping containers directed in an
5.5 Extractables by mass loss is frequently used for textiles
applicable material specification or other agreement between
which have a relatively large amount of extractable material to
the purchaser and the supplier. Consider shipping containers to
effect a significant mass change.
be the primary sampling unit.
6. Apparatus and Reagents NOTE 3—An adequate specification or other agreement between the
purchaser and the supplier requires taking into account the variability
6.1 Extraction Apparatus
between shipping containers, within a shipping container, and between
6.1.1 Soxhlet Extraction Apparatus for Option 1 extraction
specimens taken from a single unit within a shipping container, so as to
provide a sampling plan with a meaningful producer’s risk, consumer’s
6.1.2 Extraction Funnels, wide-mouth, 125 or 150-mL ca-
risk, acceptable quality level, and limiting quality level.
pacity for Option 2 extraction.
8.2 Laboratory Sample—As a laboratory sample for accep-
6.2 Thimbles, fat-free cellulose or Alundum, for Option 1.
tance testing, proceed as follows:
6.3 Specimen Compressor, pestle or long forceps, for han-
8.2.1 Yarn on Packages—Take at random from each ship-
dling specimens in Option 2.
ping container in the lot sample the number of packages
6.4 Containers, directed in an applicable material specification or other agree-
6.4.1 To hold extractables and that will seal to prevent ment between the purchaser and the supplier, such as an
moisture changes, for example weighing bottles, for Option 1. agreement to use Practice D2258. Preferably, the same number
D2257 − 98 (2012)
of packages should be taken from each shipping case in the lot 10.2.3 Place the specimens in the thimbles, if used, and
sample. If differing numbers of packages are to be taken from transfer to the Soxhlet apparatus. Thimbles must be long
shipping cases in the lot sample, determine at random which enough to cover the opening of the siphon tube.
shipping cases are to have each number of packages drawn. 10.2.4 Add sufficient solvent to overflow plus about 25 %
8.2.2 Yarn on Beams—Take a laboratory sample from each
more to prevent the solvent from boiling dry.
of the beams in the lot sample as agreed between the purchaser
10.2.5 Adjust the heat for 3 to 5 siphonings per hour and
and the supplier.
extract the specimens for at least 20 siphonings. Maintain the
8.2.3 Fabrics—Take a full width swatch 1 m long from the
temperature of the solvent in the Soxhlet apparatus at a level
endofeachrolloffabricinthelotsample,afterfirstdiscarding
low enough to avoid interference with siphoning and in any
a minimum of 1 m of fabric from the very outside of the roll.
event, below 50°C. Be certain that the solvent is going through
8.2.4 Staple Fiber—Systematically take five laboratory
the thimble or filter paper during the extraction, and not
sample units from each bale in the lot sample as directed in
overflowing. In case there is evidence that 20 siphonings are
Practice D3333.
not sufficient, the purchaser and supplier should agree upon a
8.2.5 Tow, Sliver, or Top—Takefromtheleadendofastrand
suitable number of siphonings.
from each shipping container in the lot sample the first metre
10.2.6 Remove from the source of heat when the upper
of material that has a clean, uniform appearance. If the
chamber of the apparatus is nearly full and ready to siphon
shipping containers in the lot sample contain multiple
again. Pour off the nearly pure solvent from the extraction tube
packages, take a laboratory sample from one package drawn at
and save for reuse after suitable distillation.
random from each container.
10.2.7 Determine the mass of a weighing bottle to 0.001 g.
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
9. Conditioning
residue.
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
10. Procedure
for 30 min. Cool in a desiccator and weigh. Repeat the drying,
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).
10.1.1 Use the following procedure to determine the pres- 10.2.10 Record the final mass of the residue to the nearest
0.001 g.
ence of low boiling ingredients, that is, extractables that are
volatile at low temperatures.
NOTE 4—Solvent in weighing bottles may be recovered for subsequent
10.1.2 Extract one or more specimens of the material as
reuse by connecting the effluent stream of solvent and air to a suitable
directed in 10.2 or 10.3.
condenser.
10.1.3 Transfer the solvent quantitatively to a tared weigh-
10.2.11 Remove the remaining solvent from the Soxhlet
ing bottle and evaporate the solvent by blowing with a stream
apparatus, reinsert the thimble and specimen, and fill with the
of air at room temperature until there is a mass change of less
proper amount of alcohol. Extract through at least 12 siphon-
than 0.001 g in 10 min.
ings.
10.1.4 Heat the residue in an oven at 105 6 3°C for 30 min,
10.2.12 Determine the mass of a weighing bottle to 0.001 g.
cool, and weigh.
Transfer the alcohol from the flask to the weighing bottle,
10.1.5 If there is a mass loss greater than 0.001 g in the
evaporate the alcohol, dry, and weigh the residue to the nearest
residue (extractables) due to heating in the oven, the material
0.001 g.
contains extractable matter which volatilizes at low
10.2.13 Remove the specimen from the apparatus and air
temperatures, and the specimen solvent extract should not be
dry it. Continue as directed in 10.5.
heated in the oven.
10.1.6 If there is no detectable loss in residue mass (less 10.3 Option
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