Designation: D4974 − 04 (Reapproved 2016)

Standard Test Method for

Hot Air Thermal Shrinkage of Yarn and Cord Using a
Thermal Shrinkage Oven1
This standard is issued under the fixed designation D4974; 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.

1. Scope D1776 Practice for Conditioning and Testing Textiles

1.1 This test method covers the measurement of shrinkage D6477 Terminology Relating to Tire Cord, Bead Wire, Hose
of yarns and cords when exposed in a thermal shrinkage oven. Reinforcing Wire, and Fabrics
1.2 This test method is applicable to yarns and cords made 3. Terminology
of nylon, polyester, and other polymers not detrimentally
affected by the temperature used and with linear densities in the 3.1 Definitions:
range from 20 to 700 tex (180 to 6300 denier). 3.2 For definitions of terms relating to tire cord, bead wire,
1.2.1 Yarns or cords for testing may be taken from yarn or hose wire, and tire cord fabrics, refer to Terminology D6477.
cord packages or from fabrics. 3.2.1 The following terms are relevant to this standard:
1.3 This test method shows values in both SI and inch- greige cord, in tire cords, standard atmosphere for testing
pound units. SI is the technically correct name for the system textiles, thermal shrinkage, tire cord.
of units known as the International System of Units. Inch- 3.3 For definitions of other terms related to textiles, refer to
pound units is the technically correct name for the customary Terminology D123.
units used in the United States. The values stated in either 3.3.1 The following terms are relevant to this standard:
acceptable metric units or other units shall be regarded yarn.
separately as standard. The values expressed in each system
may not be exact equivalents; therefore, each system must be 4. Summary of Test Method
used independently of each other, without combining values in 4.1 A relaxed, conditioned specimen of yarn or cord is
any way. Referee decisions are to use SI units. subjected to dry heat for a specified time while under a
1.4 This standard does not purport to address all of the specified tension. The percent shrinkage is read directly from a
safety concerns, if any, associated with its use. It is the scale or display on the instrument while the specimen is still
responsibility of the user of this standard to establish appro- under tension and exposed to heat.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard 5. Significance and Use
statements are given in Section 8. 5.1 This test method may be used for the acceptance testing
of commercial shipments of yarns and cords. Caution is
2. Referenced Documents
advised because yarn and cord may contract in length over a
2.1 ASTM Standards:2 period of time due to room temperature retraction. Thermal
D123 Terminology Relating to Textiles shrinkage values are reduced proportionately by the amount of
D885 Test Methods for Tire Cords, Tire Cord Fabrics, and room temperature retraction.
Industrial Filament Yarns Made from Manufactured
Organic-Base Fibers NOTE 1—Experience, especially with nylon, shows that yarn retraction,
which may be observed directly as shortening of length (or indirectly as
denier increase), will occur in unrestrained yarn or cord that is not at
1 equilibrium (equilibrium in this case being defined as essentially zero
This test method is under the jurisdiction of ASTM Committee D13 on Textiles
and is the direct responsibility of Subcommittee D13.19 on Industrial Fibers and
thermal shrinkage yarn or fully relaxed yarn). Normally, retractive forces
Metallic Reinforcements. are present in most wound packages of yarn and cord; thus, unrestrained
Current edition approved July 1, 2016. Published August 2016. Originally yarn near the surface is likely, with time, to undergo some retraction. After
approved in 1999. Last previous edition approved in 2011 as D4974–04(2011). DOI: retraction, such yarns exhibit lower thermal shrinkage values than yarn or
10.1520/D4974-04R16. cord deeper within the package. The opposite condition of yarn on the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or surface exists with yarn or cord wound against or near a rigid package
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM core, such as a metal or hardwood wind-up spool. Such core yarn or cord
Standards volume information, refer to the standard’s Document Summary page on cannot move against this restraint, and thus, will exhibit thermal shrinkage
the ASTM website. values even several weeks later near to those which were measured

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D4974 − 04 (2016)
immediately from the surface of the freshly wound package. Elevated bias or determine the proper set point to give the specified
humidity will accelerate retraction of unrestrained yarn, but moisture specimen temperature.
content in itself will have little influence on thermal shrinkage. Exposure
of untensioned skeins of yarn or cord to 95 to 100 % relative humidity at 6.3 The degree of room temperature length retraction, (for
room temperature for two days and reconditioning under standard example, that which occurs in unrestrained skeins of yarn over
laboratory conditions will cause most of the room temperature retraction time in the testing laboratory), of the laboratory sample or
that is possible within a sample to occur.
specimen affects the measurement of thermal shrinkage. Un-
5.1.1 In case of differences of practical significance in relaxed nylon, for example, shrinks much more than relaxed
reported test results from two or more laboratories conduct nylon. The amount of relaxation (retraction) occurring prior to
comparative tests to determine if there is a statistical bias testing of thermal shrinkage can affect the result.
between them. Competent statistical assistance is recom-
6.4 Frictional forces against the pulley/indicator assembly
mended for the investigation of bias. As a minimum, the parties
cause measurement errors. Ensure that the indicator needle
should take a group of test specimens that are as homogeneous
does not rub against the scale. Maintain the pulley bearings in
as possible and that are from a lot of material of the type in
good condition. The pulley wheel must be centered in the
question. The test specimens then should be assigned randomly
bearings. A force of 10 mN or less, applied to the tip of the
in equal numbers to each laboratory for testing. The average
indicator needle, should cause pulley rotation when the tester is
results from the two laboratories should be compared using
in proper operating condition.
Student’s t-test for unpaired data and a probability level chosen
by the parties before the testing is begun. If a bias is found, 6.5 Thermal shrinkage increases as the exposure time in-
either its cause must be found and corrected, or future test creases. Check the exposure time with a stopwatch. Some
results must be adjusted in consideration of the known bias. thermal oven models have a timer installed. Compare this timer
to a stopwatch and calibrate as necessary.
5.2 Thermal shrinkage of nylon, polyester, and other fibers
is related to the polymer of origin and its manipulation in 6.6 Center the threadline between the heating plates of the
processing. Thermal shrinkage measurement can be used to oven to obtain a correct measurement.
control product uniformity. 6.7 Specimens that are spun, textured, or crimped (as those
5.3 The level of thermal shrinkage is critical in the user’s removed from a fabric) may allow filaments to come in contact
subsequent operations. For example it can affect the drumset with interior surfaces of the thermal shrinkage oven. Such
(original length of cord) required in tire building to produce a physical contact will cause inaccurate readings of thermal
finished, final tire of a particular size. shrinkage.
5.4 Thermal shrinkage is critical to final shape and size of 6.8 Yarn or cords that are sufficiently sticky or tacky to
fiber reinforced articles. For example, thermal shrinkage affects prevent their free release from the pulley surface as it rotates
final size of V-belts and their ability to maintain tension while will cause inaccurate readings of thermal shrinkage.
running.
7. Apparatus
5.5 This test method is similar to the procedures of Methods
D885 for the determination of thermal shrinkage of yarns and 7.1 Thermal Shrinkage Oven3, consisting of a specimen
cords. Shrinkage is measured while the specimen is within an heating cavity capable of heating up to 250°C (480°F), a means
oven and tensioned as specified in Methods D885;D885 of accurately controlling the temperature of the cavity 6 2°C
however, there are enough vagaries among different units of (6 4°F), and a means for measuring and displaying the amount
apparatus for measurement of thermal shrinkage that numerical of specimen shrinkage to the nearest 0.1 %. Fig. 1 shows the
equivalence between units of different design should not be principle of operation of commercial thermal shrinkage ovens.
assumed, even under the same nominal conditions. 7.2 Stopwatch or Timer.
6. Interferences 7.3 Clip-On Masses.
6.1 An effective draft shield on the thermal oven is critical. 7.4 Draft Shield, if the oven does not have one provided.
Because the chamber in which the specimen is heated is open
on three sides, air drafts can effectively shorten the length of 8. Safety Hazards
specimen experiencing the prescribed temperature environ- 8.1 The oven portion of the tester can reach temperatures
ment. Results obtained without a shield generally are lower over 200°C (390° F). Do not touch the oven.
than with a shield. 8.2 Do not leave oven unattended if a specimen is installed.
6.2 The accurate control of temperature at any prescribed
setting is of utmost importance. Bias between the set point 9. Sampling and Test Specimens
temperature and the temperature that the specimen sees is a 9.1 Primary Sampling Unit—Consider shipping containers
major cause of instrument bias. The temperature that the of cords or rolls of fabric to be the primary sampling unit, as
specimen sees may be checked by attaching a small calibrated applicable.
thermocouple to a piece of cord and suspending it in the
specimen position such that the tip of the thermocouple is in
the center of the oven cavity. The thermocouple must not touch 3
Commercial thermal shrinkage ovens are available. Clip-on masses also are
the oven walls. Either correct any set point/sample temperature available from the manufacturer.

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 D4974 − 04 (2016)

FIG. 1 Principle of Operation of a Thermal Shrinkage Oven

9.2 Laboratory Sampling Unit—As a laboratory sampling handling damage is available after conditioning (see 10.1). If
unit for acceptance testing, take material randomly from the the applicable material specification or other agreement be-
primary sampling unit as follows: tween the purchaser and the supplier specifies testing more
9.2.1 For cords, take spools or packages per carton using the than one specimen per laboratory sampling unit, an additional
applicable procedure in Practice D2258. two specimens above the number to be tested should be taken
9.2.2 For fabric, take from rolls at least one full-width piece from the laboratory sampling unit and conditioned.
of fabric that is at least 1 m (1 yd) along the selvage (machine
direction), after first discarding all fabric from the outside of 10. Conditioning Specimens and Preparation for Testing
the roll that contains creases, fold marks, disturbed weave, or 10.1 Conditioning:
contamination by foreign material. 10.1.1 Condition specimens as relaxed skeins or segments
9.3 Test Specimens: of untensioned fabric as directed in Practice D1776 using the
9.3.1 For yarns and cords, strip at least 15 m (16 yd) from atmosphere specified for industrial yarns (see Section 3).
the outside of each package in the laboratory sampling unit. Ensure that no change in yarn/cord twist occurs while carrying
Inspect the outside of the package after stripping off the yarn. out this procedure.
If there is visible damage, continue to strip off units of 15 m (16 10.1.2 Condition and relax yarn and greige cord specimens
yd) and reinspect until there is no visible damage. Take one 12 to 28 h.
specimen, 600 mm (24 in.) long, from each package in the 10.1.3 Condition and relax adhesive-treated cord samples
laboratory sampling unit. Discard and replace specimens that 16 to 28 h, unless immediate testing (5 to 20 min after
are visibly damaged. processing) is agreed upon between the buyer and the supplier.
9.3.2 For fabrics, remove a minimum of three lengths of Immediate testing must be reported as an exception to this
warp yarn or cord 600 mm (24 in.) long from each swatch in method (see Section 12).
the laboratory sampling unit, with the specimens being taken at 10.2 Preparation for Testing:
least 75 mm (3 in.) from the selvage of the swatch. For fabrics 10.2.1 With the draft shield in place, preheat the oven until
other than tire cord fabric, such as square-woven tire fabrics, the chamber has attained the specified temperature for a
also take from each swatch in the laboratory sampling unit a minimum of 5 min.
minimum of three lengths of filling yarn or cord 600 mm (24 10.2.2 Test in standard atmosphere for testing industrial
in.) long after discarding those portions within 75 mm (3 in.) of yarns (see Section 3).
the selvage of the swatch. In all cases, take warp specimens 10.2.3 Adjust the oven temperature controller set point to
that are free of filling material and filling specimens that are give a specimen temperature of 177 6 2 °C (350 6 4° F). (See
free of warp material. 6.2).
9.3.2.1 Instructions on the number of test specimens in 9.3.2 10.2.4 One may consult with the instrument vendor if
assume that a single valid thermal shrinkage result will calibration of the oven temperature is suspected to be in error.
adequately characterize the thermal shrinkage of the laboratory
sampling unit from which the specimens are taken. The extra 11. Procedure
two specimens are taken to assure that a specimen free of 11.1 Test Conditions (Table 1):

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 D4974 − 04 (2016)
TABLE 1 Test Conditions indicator to a shrinkage level in 11.4 sufficient to prevent the indicator
Time, s from going below zero. Record positive shrinkage as the interval between
Specimen with Linear Specimen with Linear the lowest and highest reading of the indicator during the test of that
Temperature Tension Load specimen. Note for the report (Section 12) the percent change in length
Mass up to 400 tex Mass Greater than
(3600 denier) 400 tex (3600 denier) due to crimp relaxation in the tester.
177 ± 2°C 5.0 ± 1.0 mN/tex 120 ± 10 240 ± 10
(350 ± 4°F) (or 0.05 ± 0.01 11.7 Lower the draft shield immediately after introducing
gf/den) the specimen.
11.8 Start the timer at the moment the draft shield is
lowered.
11.1.1 For yarns or cords possessing low levels of shrinkage
11.9 At the end of 120 6 10 s (240 6 10 s for specimens
force, a tension loading of 1.0 6 0.2 mN/tex (0.010 6 0.002
equal to or greater than 400 tex or 3600 denier), read the
gf/den) may be used. Use of this lower tension load should be
percent shrinkage as indicated on the instrument output to the
noted in the report.
nearest 0.1 %.
11.2 Install one end of the specimen in the fixed clamp.
11.10 Remove and discard the specimen.
11.3 Bring the other end of the specimen over the pulley.
12. Report
11.4 Set the indicator to zero and hold it on zero while
performing the next step. 12.1 State that the specimens have been tested as directed in
Test Method D4974. Describe the material(s) or product(s)
11.5 Attach a clip-on mass to the unclamped end of the
tested and the method of sampling used. Report the following
specimen so that twist is not lost. Use a mass that creates a
information:
tension load as specified in 11.1. Table 2 shows the total mass
12.1.1 Individual thermal shrinkage results as indicated on
needed to effect such tensions for typical yarns and cords.
the instrument output to the nearest tenth of a unit.
NOTE 2—If the specimen is likely to untwist in the portion below the 12.1.2 Mass, in g, used to apply tension force.
pulley, attach a toothpick or the equivalent (approximately 7.5 cm long) to 12.1.3 Measurements as “immediate testing” if not condi-
the mass or clamp, perpendicular to the vertical threadline, so it will bear
tioned for standard period (see 10.1.2 and 10.1.3).
against the instrument case and prevent rotation of the mass.
12.1.4 Measurements as “package testing” if specimens are
11.6 Load specimen(s) into the oven. The specimen is not removed from package and relaxed prior to testing.
centered automatically in the oven. 12.1.5 “Percent length increase prior to shrinkage” if such
NOTE 3—In the case of highly-crimped yarns, typically those removed occurred during testing (see Note 3).
from tightly woven fabric, the initial dimensional change that occurs is
usually growth, that is, an immediate elongating of the specimen as the 13. Precision and Bias
specimen loses crimp and straightens. If the instrument allows, set the
13.1 Interlaboratory Test Data—An interlaboratory test was
conducted in 2000 using commercially available testers from
TABLE 2 Tensioning MassesA,B Lawson-Hemphill, Lenzing, and Testrite. Six tire cord materi-
A. Single-Strand Yarns als were included in the study, varying in polymeric structure
d Tex Denier Tensioning Mass, g
(nylon and polyester), form (yarn, greige cord, and dipped
235 210 10
940 840 42 cord), and linear density. The type of materials chosen and their
1100 1000 50 processing conditions produced an intentional thermal shrink-
1170 1050 53
1400 1260 63
age among the specimens from less than 1 % to greater than 7
1440 1300 65 %. Thirteen laboratories participated in the study. Three of the
1870 1680 84 laboratories used two instruments for a total of sixteen instru-
2100 1890 95
B. Multiple Strands or Cords of Multiple Strands
ments. In each laboratory two operators made triplicate shrink-
Construction Tensioning Mass, g age measurements on each of four test occasions. Variance
940 × 2 840 × 2 84 components were computed for individual thermal shrinkage
1100 × 2 1000 × 2 100
1400 × 2 1260 × 2 126
determinations and are summarized in Table 3.
1440 × 2 1300 × 2 130 13.2 Precision—Repeatability and reproducibility deal with
1870 × 2 1680 × 2 168
2100 × 2 1890 × 2 189 the variability of test results obtained under specified labora-
A
For yarns or cords not shown in Table 2, calculate clip-on mass required by
tory conditions. Repeatability concerns the variability between
multiplying total d Tex of specimen by 0.50 mN or total denier by 0.05 gf (for independent test results obtained within a single laboratory in
specimens expected to have low shrinkage tensions, the factors are are 0.090 mN the shortest practical period. Those results are obtained by a
and 0.01 gf, respectively).
B
If yarns or cords outside the linear density specified in this test method are tested
single operator with a specific set of test apparatus using test
on this type equipment, it may be necessary to use more mass in tensioning light specimens (or test units) taken at random from a single quantity
yarns (to ensure sufficient friction to accurately move the pulley) or less mass in of homogeneous material obtained or prepared for the inter-
tensioning very heavy yarns or cords (to prevent overstressing of the pulley
bearings). In such an event, show, in addition to the mass in grams in 12.1.2, the laboratory study (ILS). Reproducibility deals with the variabil-
words modified procedure, immediately followed in parentheses by the calculated ity between single test results obtained in different laboratories,
tension per unit of linear density, such as millinewtons per denier or grams per each of which has applied the test method to test specimens (or
denier. For example, testing of a 10 000-denier cord with 100 g of tensioning mass
will be reported in 12.1.2 as “100-g modified procedure (0.01 gf/denier).” test units) taken at random from a single quantity of homoge-
neous material obtained or prepared for the ILS.

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 TABLE 3 Interlaboratory Study Variance Components
Average Variance Variance Variance Variance Total Within-Lab s s
Material Variance Lab s (within-lab)
Shrinkage Instrument Operator Occasion Determination Variance Variance (repeatability) (reproducibility)
Polyester Yarn 1400 5.2 0.043665 0.015556 -0.00076 0.003951 0.010685 0.073097 0.029432 0.10 0.17 0.27
dtex

5
Nylon Yarn 930 dtex 7.6 0.40272 0.002372 0.001638 0.010809 0.019147 0.436686 0.033966 0.14 0.18 0.66
Nylon Yarn 1880 dtex 6.5 0.167416 0.009564 0.001451 0.004993 0.014463 0.197887 0.030471 0.12 0.17 0.44
Polyester Cord 1400/ 0.94 0.004404 0.000046 -0.00011 0.002657 0.002752 0.009749 0.005345 0.05 0.07 0.10
1/2
Nylon Cord 930/1/2 7.7 0.580907 -0.00434 0.001816 0.030175 0.016896 0.625454 0.044547 0.13 0.21 0.79
Nylon Cord 1800/1/2 5.4 0.126382 0.006947 0.000544 0.010189 0.018177 0.162239 0.035857 0.13 0.19 0.40
D4974 − 04 (2016)
 D4974 − 04 (2016)
Method repeatability is defined as the “maximum difference” the single operator case (“repeatability”), within-laboratory
that can “reasonably” be expected between two test results case, and between-laboratory case (“reproducibility”). Two
obtained on the same material when the test results are values or averages of observed values are considered signifi-
obtained in the same laboratory. Repeatability standard devia- cantly different at the 95 % probability level if the difference
tion is taken to be the square root of the “determination” between them exceeds the appropriate critical difference in the
variance component, and represents within-operator precision. table.
Method reproducibility is defined as the “maximum difference”
that can “reasonably” be expected between two test results 13.3 Bias—The procedure in this test method produces a
obtained on the same material when the test results are test value that can be defined only in terms of a test method.
obtained from different laboratories. The total, or There is no independent referee method by which bias may be
reproducibility, standard deviation, is formed by taking the determined. This test method has no known bias.
square root of the sum of intra- and inter-laboratory variance
components. 14. Keywords
The values in Table 4 show maximum critical differences for 14.1 shrinkage; thermal; tire cord
single determinations specified averages of determinations for

6
 D4974 − 04 (2016)
TABLE 4 Maximum Critical Differences
Material Number of Observations Single Operator Precision Within-Laboratory Precision Between Laboratory Precision
Polyester Yarn 1400 dtex 1 0.287 0.476 0.749
2 0.203 0.336 0.530
4 0.143 0.238 0.375
8 0.101 0.168 0.265
16 0.072 0.119 0.187
Nylon Yarn 930 dtex 1 0.384 0.511 1.832
2 0.271 0.361 1.295
4 0.192 0.255 0.916
8 0.136 0.181 0.648
16 0.096 0.128 0.458
Nylon Yarn 1880 dtex 1 0.333 0.484 1.233
2 0.236 0.342 0.872
4 0.167 0.242 0.617
8 0.118 0.171 0.436
16 0.083 0.121 0.308
Polyester Cord 1400/1/2 1 0.145 0.203 0.274
2 0.103 0.143 0.194
4 0.073 0.101 0.137
8 0.051 0.072 0.097
16 0.036 0.051 0.068
Nylon Cord 930/1/2 1 0.360 0.585 2.192
2 0.255 0.414 1.550
4 0.180 0.293 1.096
8 0.127 0.207 0.775
16 0.090 0.146 0.548
Nylon Cord 1880/1/2 1 0.374 0.525 1.116
2 0.264 0.371 0.789
4 0.187 0.262 0.558
8 0.132 0.186 0.395
16 0.093 0.131 0.279

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