ASTM D4565-20

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4565 − 20
Standard Test Methods for
Physical and Environmental Performance Properties of
Insulations and Jackets for Telecommunications Wire and
Cable
This standard is issued under the fixed designation D4565; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
Procedure Section(s)
Pressure Test (Air Core Wire and Cable Only) 40
1.1 These test methods cover procedures for the physical
Sheath Adherence Test 31
testing of thermoplastic insulations and jackets used on tele- Water Penetration Test (Filled Core Wire and Cable Only) 41
Wire and Cable Bending Test 34
communications wire and cable and the testing of physical
Wire breaking strength 37
characteristics and environmental performance properties of
1.3 Thevaluesstatedininch-poundunitsaretoberegarded
completed products. To determine the procedure to be used on
as standard. The values given in parentheses are mathematical
the particular insulation or jacket or on the completed wire or
conversions to SI units that are provided for information only
cable, make reference to the specification for that product.
andarenotconsideredstandard,exceptwhereonlySIunitsare
1.2 These test methods appear in the following sections of
given.
this standard:
1.4 This standard does not purport to address all of the
Test Method Section(s)
safety concerns, if any, associated with its use. It is the
Dimensional Measurements of Insulations, Jackets, Miscellaneous 4–9
Cable Components, and of Completed Cable responsibility of the user of this standard to establish appro-
Cross-sectional Areas 9
priate safety, health, and environmental practices and deter-
Diameters 6
mine the applicability of regulatory limitations prior to use.
Eccentricity 8
Thickness 7 For specific warning statement see 19.1.
Physical and Environmental Tests of Insulation and Jackets 10–25
1.5 This international standard was developed in accor-
Aging Test (Jackets Only) 24
dance with internationally recognized principles on standard-
Cold Bend (Insulation Only) 16
Environmental Stress Crack (Polyolefin Jackets Only) 21
ization established in the Decision on Principles for the
Heat Distortion (Jackets Only) 22
Development of International Standards, Guides and Recom-
Heat Shock (Jackets Only) 23
mendations issued by the World Trade Organization Technical
Insulation Adhesion 19
Insulation and Jacket Shrinkback (Oven Test) 14
Barriers to Trade (TBT) Committee.
Insulation Compression 20
Insulation Shrinkback (Solder Test) 15
2. Referenced Documents
Melt Flow Rate Change—Polyolefin Materials 12
Oil Immersion Test (Jackets Only) 25
2.1 ASTM Standards:
Oxygen Induction Time (Polyolefin Insulation Only) 17
D471Test Method for Rubber Property—Effect of Liquids
Oxygen Induction Time (Cable Filling Compound Only) 18
Tensile and Elongation Tests 13 D638Test Method for Tensile Properties of Plastics
Physical and Environmental Tests of Insulations and Jackets of 26–42
D1238Test Method for Melt Flow Rates of Thermoplastics
Completed Wire and Cable
by Extrusion Plastometer
Cable Torsion Test 38
Compound Flow Test (Filled Core Wire and Cable Only) 42 D1248Specification for Polyethylene Plastics Extrusion
Corrugation Extensibility Test 36
Materials for Wire and Cable
Cable Impact Test 33
D1693Test Method for Environmental Stress-Cracking of
Jacket Bonding Tests 29
Jacket Notch Test 32 Ethylene Plastics
Jacket Peel or Pull 28
D2633Test Methods for Thermoplastic Insulations and
Jacket Slip Strength Test 30
Jackets for Wire and Cable
D3032Test Methods for Hookup Wire Insulation
These test methods are under the jurisdiction of ASTM Committee D09 on
Electrical and Electronic Insulating Materials and are the direct responsibility of
Subcommittee D09.07 on Electrical Insulating Materials. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2020. Published November 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1986. Last previous edition approved in 2015 as D4565–15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4565-20. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4565 − 20
D4731 Specification for Hot-Application Filling Com- DIMENSIONAL MEASUREMENTS OF INSULATIONS,
pounds for Telecommunications Wire and Cable JACKETS, MISCELLANEOUS CABLE
D4732Specification for Cool-Application Filling Com- COMPONENTS, AND COMPLETED CABLES
pounds for Telecommunications Wire and Cable
4. Scope
E29Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
4.1 Dimensional measurements include, but are not limited
E171/E171MPracticeforConditioningandTestingFlexible
to,measurementsofinsulationandjacketthicknesses,tapeand
Barrier Packaging
armor thicknesses, conductor diameters, DODs, core
diameters, overall diameters, and so forth.
3. Terminology
5. Significance and Use
3.1 Abbreviations:
5.1 Dimensional measurements, properly interpreted, pro-
3.1.1 DOD—Diameter Over Dielectric. This is a short term
vide information with regard to the conductors, insulation, or
to refer to the overall diameter over an insulated conductor.
jacket. The dimensional measurements provide data for re-
3.2 Definitions of Terms Specific to This Standard:
search and development, engineering design, quality control,
3.2.1 air core—products in which the air spaces between
and acceptance or rejection under specifications.
cable core components (pairs, and so forth) remain in their
unfilled or natural state.
6. Diameters
3.2.2 armored wire or cable—a wire or cable in which the
6.1 Measure diameters of essentially round items (such as
shielded or jacketed or shielded and jacketed wire or cable is
insulatedoruninsulatedconductors)usinganytypeofmicrom-
completelyenclosedbyametalliccoveringdesignedtoprotect
eterreadingtoatleast0.001in.(0.025mm)witheachdivision
the underlying telecommunications elements from mechanical
of a width that facilitates estimation of each measurement to
damage.
0.0001 in. (0.0025 mm). Take a minimum of two readings,
3.2.2.1 Discussion—Select shielding or armoring, or both,
essentiallyatrightanglestoeachother,andaveragetheresults.
from a variety of materials (for example, aluminum, copper,
6.2 In case of dispute, optical methods as described in Test
steel). The armoring is applied in a variety of ways (for
Methods D3032 shall be used as the referee method.
example, helically wrapped, longitudinally applied, applied
corrugated or smooth).
NOTE 1—For insulated conductors with dual insulation (for example,
foam-skin),theDODoftheinnerlayermustbemeasuredusingtheoptical
3.2.3 cable, telecommunications—products of six or more
methods of Test Methods D3032.
pair.
6.3 Measure the approximate or effective diameters of
3.2.4 filled core—those products in which air spaces are
non-circular cross sections (such as irregular or oval cables or
filled with some materials intended to exclude air or moisture,
cable cores) by the use of strap gauges.
or both.
6.4 Precision and Bias—The precision and bias of this test
3.2.5 gopher-resistant—awireorcablethatresiststheattack
method for measuring diameters are in accordance with Test
of gophers when installed directly buried.
Methods D2633.
3.2.5.1 Discussion—Telecommunications wire and cable
products intended for direct burial in the earth are normally
7. Thicknesses
rated as either “gopher-resistant” or “non-gopher-resistant.”
7.1 Measureinsulationthicknessusingappropriatemethods
User selection of products for burial will depend upon the
specified in Test Methods D2633, except that the micrometer
anticipated gopher protection needed for the planned installa-
accuracy described in 6.1 is required. A pin gauge having the
tion site. The gopher-resistant rating is assigned based upon
accuracy of the micrometers as specified in 6.1 is acceptable
test evaluations (evaluations are commonly performed by the
for thickness measurements made on tubular sections of
Fish and Wildlife Service, US Department of the Interior,
insulation removed from conductors. Optical methods (as
Denver, CO).
specified in 6.2) are also permitted.
3.2.6 non-gopher-resistant—a wire or cable that is not
7.2 Measure jacket thickness using appropriate methods
designed to resist gopher attack (see 3.2.5).
specified in Test Methods D2633, except that the micrometer
3.2.7 pair—twoinsulatedconductorscombinedwithatwist.
accuracy specified in 6.1 is required. In determining the
3.2.8 sheath—thejacketandanyunderlyinglayersofshield, thickness of jackets applied over corrugated shields or armors,
armor,orotherintermediatematerialdowntobutnotincluding
measurements must be made in the corrugation impressions
the core wrap. (thinnestjacketspots).Opticalmethods(asspecifiedin6.2)are
also permitted.
3.2.9 shielded wire or cable—a wire or cable in which the
core (or inner jacket) is completely enclosed by a metallic 7.3 Precision and Bias—The precision and bias of this test
covering designed to shield the core from electrostatic or
method for measuring thickness are in accordance with Test
electromagnetic interference.
Methods D2633.
3.2.10 wire, telecommunications—products containing less
NOTE 2—For designated purposes (such as process control, and so
than six pair. forth), continuous uniformity thickness gauges or measuring devices are
D4565 − 20
employed during processing to provide running records of jacket thick-
particular reel of finished wire or cable; accordingly, average
nesses. Record charts are normally maintained for a minimum of six
raw materials values shall be established as necessary for an
months.
appropriatemanufacturingtimeframe,unlessotherwiseagreed
upon between the producer and the purchaser.
8. Eccentricity
12.2 Insulation Material—Perform tests on insulation re-
8.1 Calculate eccentricity using measured thickness values
moved from finished conductors. Note that thin wall and fine
for insulation or jacket, or both.
gauge insulations shall be handled carefully because of en-
8.2 Calculate absolute eccentricity, E , of insulation or
ab
trapped air. In the case of insulation in filled cable, the
jacket, or both as follows:
preferred method is to obtain insulating material from conduc-
E 5 ~maximum thickness! 2 ~minimumthickness! (1)
tors before they are exposed to the filling operation. If
ab
necessary, conductors obtained from completed filled cable
8.3 Calculate percent eccentricity, E , of insulation or
%
shall be wiped dry and free of grease or foreign material using
jacket, or both as follows:
a dry cloth (without solvent). Chop the insulation, stripped
~maximumthickness! 2 ~minimumthickness !
fromaconductor,asnecessarytoobtainspecimenssuitablefor
E 5 3100 % (2)
~ !
%
averagethickness
~ !
testing(approximately3gofmaterialisrequiredforeachtest).
8.4 Precision and Bias—The precision and bias of this test
TestthechoppedmaterialasrequiredbyTestMethodD1238to
method of measuring eccentricity are in accordance with Test
determine a melt flow rate. Run three tests and average the
Methods D2633.
results.Standardconditionsoftestshallbeasindicatedin12.1.
12.3 Jacket Material—Jacket material used for this test
9. Cross-Sectional Areas
must be free of filling or flooding compound. Soft filling or
9.1 When needed, determine cross-sectional areas (usually
flooding compounds shall be removed by thoroughly wiping
insulations or jackets only) using the methods outlined in Test
the jacket specimen using a clean dry cloth (without solvent);
Methods D2633, except that the dimensions used in the
harder filling or flooding compounds shall be removed by
calculations must be maintained to the accuracy specified in
cutting.Buffingispermittedtobeusedasafinishingoperation
6.1.
to ensure clean and dry specimens. Use jacketing material
removed from completed cable for performing tests. Chop the
9.2 Precision and Bias—The precision and bias of this test
method for measuring cross-section areas are as specified in jacket material removed from the cable as is necessary to
obtain specimens suitable for testing (approximately3gof
Test Methods D2633.
materialisrequiredforeachtest).Testthechoppedmaterialas
PHYSICAL AND ENVIRONMENTAL TESTS OF
required by Test Method D1238 to determine a melt flow rate.
INSULATIONS AND JACKETS
Run three tests and average the results. Standard conditions of
test shall be as indicated in 12.1.
10. Scope
12.4 Calculation—Calculate the percent increase in flow
10.1 Physical and environmental tests for insulations and
rate as follows:
jacketsinclude,butarenotlimitedto,determinationofsomeor
M 2 M
all of the properties covered in Sections12–25. 2 1
I 5 3100 (3)
M
11. Significance and Use
where:
11.1 Physical tests, properly interpreted, provide informa-
I = increase,%,
tion with regard to the physical properties of the insulation or
M = melt index of raw material, and
jacket. The physical test values give an approximation of how
M = melt index of material from the finished cable.
the insulation will physically perform in its service life.
12.5 Precision and Bias—Theprecisionandbiasofthistest
Physical tests provide data for research and development,
method for measuring melt-flow rate changes are basically in
engineeringdesign,qualitycontrol,andacceptanceorrejection
accordance with Test Method D1238.
under specifications.
13. Tensile and Elongation Tests
12. Melt Flow Rate Change—Polyolefin Materials
13.1 Insulation Material—Provide test specimens by re-
12.1 Raw Material Baseline—Melt flow rate for insulation
moving insulation from finished conductors. (See Test Speci-
and jacket materials obtained from finished cable must be
men section of Test Methods D2633 for methods of removing
compared with the flow rates for corresponding raw materials.
the conductor.) Perform tests in accordance with Test Method
Determine the flow rates for the basic insulating and jacketing
D638 to determine such properties as tensile strength
raw materials in accordance with the requirements of Test
(nominal), yield strength, and percentage elongation at break.
Method D1238. Standard conditions of test shall be as pre-
The speed of testing shall be as prescribed by the product
scribedbytheproductspecification.Ifpossible,obtainsamples
specifications.
ofrawmaterialsbeforeorduringtheextrusionprocess(but not
after heating). Since insulating and jacketing raw materials are 13.2 Jacket Material—Providetestspecimensbydiecutting
normally obtained and used in bulk, it is usually difficult if not jacket segments removed (cut) from finished cable. Perform
impossible to relate a particular lot of raw material with a testing in accordance with Test Method D638 to determine
D4565 − 20
suchpropertiesastensilestrength(nominal),yieldstrengthand result of the heat exposure. Shrinkback in inches (or millime-
percentageelongationatbreak.Thespeedoftestingshallbeas tres) is the total measured length of the bared conductor minus
prescribed in the product specifications. the original length of the bared conductor (0.5 in. (13 mm)).
13.3 Precision and Bias—The precision and bias of these 15.2 Precision and Bias—Nostatementismadeabouteither
testmethodsformeasuringtensileandelongationpropertiesof the precision or bias of this test method for measuring
insulations and jackets are in accordance with Test Method shrinkback since the result merely states whether there is
D638. conformance to the criteria for success specified in the product
specification.
14. Insulation and Jacket Shrinkback (Oven Test)
16. Cold Bend (Insulation Only)
14.1 Insulation Material—Perform tests on insulated con-
ductors. Unless otherwise specified, test a minimum of one
16.1 Preferably conduct the test in the cold chamber. Tests
sample of each color of insulation from a cable. Immediately
shall be performed on insulated conductors. The insulation
prior to testing, cut specimens 8 in. (200 mm) long from the
shall not show any cracks visible by normal or corrected-to-
center of a 5-ft (1.5m) length; then reduce them to 6 in.
normal vision, when a specimen of insulated conductor that
(150mm) by trimming each end of the specimen. Place these
was conditioned to the specified temperature for 1 h, and
specimens in a forced air type circulating oven or in a forced
wrappedaroundthemandrelinthecoolingchamberatleastsix
convection type circulating air oven for4hatthe temperature
adjacent turns.Test temperature and mandrel diameter shall be
prescribed. The specimens shall be placed on a layer of
as prescribed by the product specification. Bending shall be at
preheated talc or felt. At the end of the conditioning period,
anapproximatelyuniformratesothatthetimeconsumedisnot
cool the wire to room temperature and measure the shrinkback
more than 1 min.
oftheinsulation.Shrinkbackisdefinedasthetotalshrinkageof
16.2 When the mandrel is too large for the chamber, place
the insulation from both ends of the specimen in inches (or
the sample in the low temperature chamber for the specified
millimetres).
temperature for 1 h, and upon removal from the low tempera-
14.2 Jacket Material—Perform tests on slabs cut from the
ture chamber, immediately wind around the mandrel for the
cablejacket.Unlessotherwisespecified,cutaminimumoffour
specifiednumberofatleastsixadjacentturns.Testtemperature
test specimens, each 2 in. (51 mm) long, 0.25 in. (6.3 mm)
and mandrel diameter shall be as prescribed by the product
wide, and the same thickness as the jacket. Make the length-
specification. Bending shall be at an approximately uniform
wisecutsparalleltothelongitudinalaxisofthecablewitheach
rate so that the time consumed is not more than 1 min.
specimen spaced circumferentially in 90° increments around
16.3 Precision and Bias—The precision of these tests has
the cable periphery. For cables that are longitudinally shielded
not been determined. No statement can be made about the bias
orarmored,oneofthespecimensshallbecutfromaportionof
of this test method for insulation cold bend since a standard
thejacketlyingdirectlyovertheoutershieldorarmoroverlap.
material is not available.
Place these specimens on a layer of preheated talc or felt in a
forced-air type circulating oven or in a forced-convection type
17. Oxidative Induction Time (Polyolefin Insulation
circulatingairovenfor4hatthetemperatureprescribed.Atthe
Only)
end of the conditioning period, cool the specimens to room
17.1 Scope—This test method covers the determination of
temperatureandmeasuretheshrinkbackofthejacketmaterial.
an Oxidative Induction Time (OIT) value for polyolefin insu-
Shrinkback is defined as the total lengthwise shrinkage in
lation materials removed from completed wire or cable prod-
inches (or millimetres).
ucts. This OIT value is determined by a thermoanalytical
14.3 Precision and Bias—Nostatementismadeabouteither
measurement of the onset time for the exothermic oxidation of
the precision or bias of these methods for measuring shrink-
insulation in pure oxygen, at a specified temperature. For
back since the result merely states whether there is confor-
commentary and additional information on the background,
mance to the criteria for success specified in the product
development, and significant details of this test procedure, see
specification.
Appendix X1.
15. Insulation Shrinkback (Solder Test)
17.2 Summary of Test Method—This test method describes
15.1 Test specimens of finished insulated conductor for the instrument calibration procedures, sample preparation,
solder shrinkback. Unless otherwise specified, test a minimum experimentalprocedure,andcalculationmethodsfordetermin-
of one specimen of each insulation color. Immediately prior to ingOITvaluesforpolyolefininsulationmaterials.Aninsulated
testing, cut 8-in. (200mm) specimens from the center of a 5-ft wire sample is removed from a completed cable/wire product
(1.5m) length and then reduce each specimen to 6 in. and wiped to remove filling compounds that are present in the
(150mm) by trimming each end of the specimen. Using any completed cable/wire.Two types of insulation test samples are
convenient method, strip 0.5 in. (13 mm) of insulation from described:
one end of the specimen. Using a solder pot maintained at a 17.2.1 Type I—Insulation stripped from wire (no copper
temperature of approximately 320 °C, immerse the bared present), or
conductor to a depth of 0.25 in. (6 mm) into the molten solder 17.2.1.1 Use Type I samples to measure the intrinsic stabil-
and hold for a period of 20 s. Remove the specimen and ity of the material and the efficacy of thermal stabilizers such
measure the amount of insulation shrinkback occurring as a as antioxidants.
D4565 − 20
17.2.2 Type II—Insulation on the wire (insulation and cop- 17.4.4 Pans—Standard aluminum DSC pans (6 mm in
per conductor). diameter) are required to hold specimens during testing.
17.2.2.1 Use Type II samples to evaluate not only the
NOTE6—Donotusecopperpansbecausethevariableoxidationstateof
thermal stability, but alsothemetal deactivationefficacyof the
the copper leads to imprecision in determination of the OITvalue. Do not
additives.
use metal screens (for example stainless steel mesh) sincethey actaspro-
oranti-oxidantsandhavethepotentialtoreduceprecisionandaccuracyof
17.3 Significance and Use:
the OIT measurement.
17.3.1 The OIT value measures the oxidative thermal sta-
17.4.4.1 Degreasing—To degrease pans, wash in Reagent
bility of a material and is primarily dependent on:
Grade acetone for 1 min and dry in a stream of dry nitrogen.
17.3.1.1 The intrinsic thermal stability of the material,
Use sufficient acetone to thoroughly wash the pans, that is,
17.3.1.2 The type and concentration of antioxidants and
;200mL/100pans.Ultrasoniccleaningofthepansinacetone
other thermal stabilizers present,
is acceptable.
17.3.1.3 The type and concentration of metal deactivators
17.4.5 Temperature Standards—Use pure (>99.9%) indium
present, and
and tin as temperature calibration standards. See Table 1.
17.3.1.4 The test temperature.
17.4.6 Balance—An analytical balance to weigh specimens
17.3.1.5 Discussion—Potentially, other components in the
with a sensitivity of 60.1 mg or better.
insulation material cause secondary effects. The OIT value for
an insulation has the potential to be significantly altered by 17.5 Instrument Calibration:
17.5.1 Instrument Preparation—Clean instrument cells be-
additives such as pigments, fillers, and processing aids as well
as catalyst residues from the cable, wire, insulation, or resin tween testing of different material formulations. Follow the
instrument manual procedure for cleaning cells or hold the
manufacture. The OIT value increases or decreases depending
on whether these additives and residues act as oxidation cells at 530 °C for 10 min in oxygen.
17.5.2 Temperature Calibration—Follow the instrument
inhibitors or promoters at the test temperature. At typical test
temperatures(forexample,170to220°C),compoundspresent manual procedures for temperature calibration of the instru-
ment using the following heating programs and calibration
in the polyolefin material have the potential to decompose and
change the polyolefin oxidation mechanism and thereby the criteria.
17.5.2.1 Indium—Theexperimentalsequencefortheindium
OIT value. If the oxidation mechanism is so altered, then the
OITvalue will not necessarily correlate to aging at normal use calibration is:
(1)Equilibrate at 50 °C (in nitrogen).
temperatures. Before using the OIT value to predict field
performance and lifetimes, it is suggested that additional (2)Heat at 10 °C/min from 50 to 145 °C.
studies be undertaken to establish a correlation between the (3)Heat at 1 °C/min from 145 to 165 °C.
OIT value measured at high temperature and the performance (4)Cool specimen to below 50 °C.
of the polyolefin under typical field conditions. (5)Repeat steps (1) through (4).
17.3.2 The OIT value is useful as a product performance (6)Use melting temperatures and heat of fusion from
test, quality control parameter, or a research and development second scan for calibration purposes.
17.5.2.2 Tin—Theexperimentalsequenceforthetincalibra-
tool for polyolefin materials.
tion is:
17.4 Apparatus, Reagents and Materials:
(1)Equilibrate at 50 °C (in nitrogen).
17.4.1 Calorimeter—ThisOITTestisperformedusingcom-
(2)Heat at 10 °C/min from 50 to 220 °C.
mercialanalyzersknownasDifferentialScanningCalorimeters
(3)Heat at 1 °C/min from 220 to 240 °C.
(DSCs)(Note3)whichmeasureheatflowasafunctionoftime
(4)Cool specimen to below 50 °C.
and temperature.ADSC with isothermal control and specimen
(5)Repeat steps (1) through (4).
temperature precision of at least 60.1 °C is required.
(6)Use melting temperatures and heat of fusion from
NOTE 3—Perkin Elmer’s Differential Scanning Calorimeters and TA
second scan for calibration purposes.
Instruments Differential Thermal Analyzer with a DSC cell have been
17.5.2.3 Melting Temperature—For calibration purposes,
found to produce acceptable results. Equivalent equipment producing
define the melting temperature as the extrapolated onset of the
comparable results may be used.
melting peak, not the peak maximum (see Fig. 1).
NOTE 4—This test requires accurate temperature and atmosphere
control in the DSC specimen compartment. DSC manufacturers offer 17.5.3 Calibration Criteria—An instrument in calibration
choices in cell configuration and temperature control parameters that
will validate the melting temperatures of pure indium and pure
affect this required control. For example, in some power compensation
tin at 156.6 6 0.2 °C and 232.0 6 0.5 °C, respectively. In
DSCs, use of the two-hole platinum specimen holder lids with a special
“flow-through” swing-away block cover is required. Consult equipment-
specific literature and with the equipment manufacturer to optimize the
A
operation of individual DSCs for this test. TABLE 1 Literature Values for Calibration Standards
Melting Temperature, °C Heat of Fusion (J/g)
17.4.2 Nitrogen—Use cylinder nitrogen (99.9% purity or
Calibration Standard
T ∆H
m m
better) for purging of cells.
Indium (In) 156.61 28.7
Tin (Sn) 232.0 60.7
17.4.3 Oxygen—Use cylinder oxygen (99.9% purity or
A
better) during the oxidation stage.
Rossini, F. D., Applied Chemistry, Vol 22, 1970, p. 557; Gronwold, F., Acta
Chemica Scandinavica, Vol 21, 1967, p. 1695; Gronwold, F, Journal of Thermal
NOTE 5—Do not use house gases that are piped throughout buildings
Analysis, Vol 13, 1978, p. 419; Gronwold, F., Pure and Applied Chemistry, 1992.
since their purity varies significantly.
D4565 − 20
FIG. 2 Specimen/Pan Arrangement
17.6.5 Specimen Weight—Record the specimen weight to
FIG. 1 Indium Calibration
60.1 mg.
NOTE 9—To determine the insulation sample weight, strip a 100mm
section of the insulated wire and weigh the stripped insulation. Divide the
addition, the heat of fusion for indium and tin will be 28.7 6
insulation weight by the sample length to determine the insulation weight
0.8 J/g and 60.7 6 2.0 J/g, respectively. Check the instrument
per mm (W). Multiplying the specimen length (5 to 6 mm) by this factor
i
calibration every one to two months or more frequently since (W) will give the weight for the insulation specimen.
i
this test requires accurate temperature control. (See Note 4.)
17.7 Procedure:
17.5.4 Gas Flow Rate—Use an oxygen flow rate of 50 6
17.7.1 Load Specimens—Place the specimen (specimen and
5mL⁄min as measured with a bubble meter or calibrated
pan) in the specimen position and an empty aluminum pan in
rotameter. Other flow rates between 50 and 200 mL/min are
the reference position of the instrument.
permitted, but must be reported.
17.7.2 Initial Temperature—Equilibrate the specimen at or
below 60 °C.
NOTE 7—It is desirable that the tubing connecting the gas switching
point and the calorimeter cell have an inside volume less than 20 mL.
17.7.3 Flush Cell—Holdatthisinitialtemperaturefor5min
NOTE 8—The average OIT value at 100 mL/min was ;3% lower than
while the nitrogen purge flushes the cell at a flow rate of ;50
the OIT measured at 50 mL/min. OIT values determined at 100 mL/min
to 60 mL/min.
had ;5% improved precision over OIT values obtained at 50 mL/min.
17.7.4 Heat to Test Temperature—Heat at 20 °C/min to the
17.5.5 Test Temperature—If possible, run a blank specimen
test temperature (typically 200 °C) with nitrogen gas purging
to ensure that the instrument can maintain the test temperature
the DSC cell.
within 60.3 °C. Heat the cell to the desired test temperature
NOTE 10—The endothermic peak observed during this heating stage is
(typically 200 °C) and monitor the specimen temperature for
the melting transition of the polyolefin and can be used for identification
10min.Ifnecessary,referto17.7.6forproceduralstrategiesto
(for example, to distinguish between high-density polyethylene, low-
make the measured specimen temperature equal to the desired
density polyethylene, and polypropylenes).
test temperature.
17.7.5 Gas Switch—Hold at test temperature for 5 min to
17.6 Sample Preparation:
establish thermal equilibrium after which switch from the
17.6.1 Insulated Wire Sample—Remove the insulated wires
nitrogenpurgetopureoxygenataflowrateof50 65mL/min.
from completed wire or cable products by removing the outer
Definethisswitchtimeas T .MeasuretheOxidativeInduction
cable sheath, inner metallic shields, and any core wraps. Split
Time (OIT) from this time (T ).
theoutercablesheathlengthwise,andpeelopenthesheathand
17.7.6 Specimen Test Temperature—If possible, record the
any metallic shields to reveal the inner core with the insulated
specimen temperature 5 min after T with a precision of
wire pairs.
60.1 °C or better. The specimen temperature must be within
17.6.2 Sample Cleaning—Wipe the insulated wire sample
60.3 °C of the desired test temperature. If this temperature is
with a clean cotton cloth or paper towel to remove any filling
morethan 60.3°Cfromtherequiredtesttemperature,prepare
compound. Do not use solvents to clean the insulated wire.
anewspecimenandmodifythetemperatureprogramtoensure
17.6.3 Sample Type—Determine the OIT value for an insu-
OIT measurement is made at the required temperature.
lation using either:
NOTE 11—If 200.0 °C was the desired test temperature and the
17.6.3.1 Type I Sample—Insulationstrippedfromthecopper
temperature at T +5 min was 200.7 °C, then set the upper limit of the
wire (see 13.1), or
temperature program to 199.3 °C to correct for the overshoot of the
17.6.3.2 Type II Sample—Insulated wire (insulation and
instrument. Alternatively, monitor and adjust the specimen temperature
continuously during the experiment to maintain the desired temperature
copper wire).
within 60.3 °C.
17.6.4 Specimen/Pan Arrangements—Use a single 5 to
6mm long specimen of insulation (or insulated wire). The 17.7.7 Specimen Scan—Continue the test in pure oxygen
length is such that the specimen fits neatly into the pan. (See until the exothermic peak is observed (on the chart recorder or
Fig. 2). computer screen).
D4565 − 20
17.7.8 Data Collection—Plot the data normalized as heat
flow(W/g)versustime.Expandthe x-axisasmuchaspossible
to facilitate analysis. Vary the y-axis depending on the proce-
dure used to determine the OIT (see 17.8).
17.8 OIT Calculation—Use either of the following two
procedures to determine the Oxidative Induction Time (OIT)
values for the specimens.
NOTE 12—The OIT calculation uses a threshold measure to define the
incipient point for the polyolefin oxidation. The OIT calculation defines
the onset of the major exothermic reaction (that is, the autocatalytic
oxidation reaction).
17.8.1 Procedure 1—OIT (Offset Method):
17.8.1.1 Plot data with a full scale y-axis of 1.0 W/g (or
smaller). (See Fig. 3.)
FIG. 4 OIT Tangent Method
17.8.1.2 Expand the x-axis so that full scale on the x-axis
ranges from T −2 min to 5 to 10 min past the onset of the
oxidation exotherm. This expansion helps to assist in analysis
17.8.2.3 Draw a tangent (dashed line (d) in Fig. 4)atthe
by the offset procedure.
inflection point of the exothermic peak and extend this tangent
17.8.1.3 Draw an extension to the baseline extrapolating
to intersect the baseline (c).
anyinstrumentdrift.Foranexampleseedashedline(a)inFig.
3.
TABLE 2 Summary of Precision Data
17.8.1.4 Draw a second line parallel to baseline (a) at a
Reproducibility
distanceof0.05W/gabovethebaseline.Seedashedline(b)in Repeatability Within
Mean OIT
Laboratory-to-
A
Laboratory (σ )
Sample Value l
Fig. 3.
Laboratory (σ )
R
(min)
17.8.1.5 The intersection of the dashed line (b) with the
(min) (%) (min) (%)
signaltraceisdefinedastheonsetofoxidativedegradationand
HDPE Insulation
(stripped from wire)
is denoted as T .
OIT 121.6 4.5 3.7 7.3 6.0
17.8.1.6 The Oxidative Induction Time by the offset proce-
OIT 126.4 2.8 2.2 7.2 5.7
dure is defined as the time from oxygen introduction (T)to
HDPE Insulation
(with copper wire)
this onset:
OIT 62.6 6.2 10.0 10.0 16.0
OIT offset 5 T 2 T (4) OIT 69.5 3.6 5.2 8.6 12.3
~ !
1 1 0 2
A
Five specimens were run for each sample
17.8.2 Procedure 2—OIT (Tangent Method):
17.8.2.1 Plot data with a y-axis sufficient to show full
melting endotherm of the polyolefin and the oxidation endo-
17.8.2.4 The point of intersection is the onset of oxidative
therm. Fora5mg polyolefin specimen, a y-axis of 4 to 5 W/g
degradation by the tangent method. This onset time is denoted
is adequate.
as T .
17.8.2.2 Draw an extension to the baseline extrapolating
17.8.2.5 The Oxidative Induction Time by the tangent
any signal drift. For an example see dashed line (c) in Fig. 4.
procedure is defined as the time from oxygen introduction (T )
to this onset time.
OIT ~tangent! 5 T 2 T (5)
2 2 0
17.9 Report:
17.9.1 Report the following information:
17.9.1.1 Melting temperatures (°C) for indium and tin
together with the date of the last determination,
17.9.1.2 Heats of fusion (J/g) for indium and tin together
with the date of the last determination,
17.9.1.3 Gas flow rate (mL/min),
17.9.1.4 Parameters for each specimen (stripped insulation,
insulated wire, specimen mass, and so forth),
17.9.1.5 Specimen temperature 5 min after gas switch to
oxygen (T +5 min), and
17.9.1.6 OIT (offset) or OIT (tangent). (Unless otherwise
1 2
specified by the user, the reported OIT shall be OIT , tangent
method.)
17.9.1.7 If multiple specimens are tested, report average
FIG. 3 OIT Offset Method OIT values and standard deviations.
D4565 − 20
17.10 Precision and Bias: and isolate it from the cable or wires so as not to contaminate
17.10.1 Precision—The precision of this test method for the compound. Obtain all samples of filling compound by
measuring Oxidative InductionTime, usingType I andType II taking them from manufactured cable or wire rather than by
samples, is illustrated in Table 2. These statistics were deter- obtaining them in an unprocessed condition.
mined from round robin studies between thirteen laboratories
18.4 Instrument Preparation—Clean the instrument cells
using both heat-flux and power-compensated thermal analyz-
aftertheyhavebeenstandingovernightandbetweenthetesting
ers. All data and reports of the task force that developed this
of different material formulations. To clean the cells, bring
3,4
test method are on file at ASTM.
themuptotemperatureandholdthematapproximately400°C
17.10.2 Bias—The test for oxidative induction time has no
for a period of 10 min in nitrogen.
bias since it is defined in terms of this test method.
18.5 Instrument Calibration—Adjust temperature scales ac-
NOTE 13—This test method employs indium and tin as internal
cording to instrument manual instructions until the determined
standards for calibration of temperature and caloric sensing, and requires
melting point of pure indium metal is indicated as 156.6 °C at
strict control of the test conditions to increase precision and hopefully to
a heating rate of 5 °C/min.
reducethebiasintheOITmeasurement.However,asismentionedin17.3
and in Appendix X1, materials which are in the polyolefin have the
NOTE 15—This note on calibration is written specifically for the
potential to decompose at the high temperatures used, causing a shift of
instruments described in footnote 3. It is possible that other equipment is
the OIT from the value for the polyolefin. Such a shift is important in the
equally suitable but yields somewhat different results when testing
use of this test method for quality control of the polyolefin compound. It
identical specimens. For the Perkin-Elmer DSC, run several pure metal
isimportanttorecognizethatthesameshiftisabiaswhenthetestisused
standards (such as, indium, tin, lead, zinc) through their melting point at
to measure the OIT of the polyolefin.
a heating rate of 5 °C/min. Plot melting temperatures and interpolate to
find the required set point. Repeat calibrations require only adjustments
18. Oxygen Induction Time (Cable Filling Compound
for the indium melt temperature.
Only) FortheTAInstrumentsDTAwithaDSCCell,settheinstrumentinthe
isothermal mode and calibrate the starting-temperature dial according to
18.1 Scope—This test method covers a procedure for
the instrument manual.Alternately, set the dial to a reading that results in
determining, by thermal analysis, the oxidative induction time
a corrected thermocouple read-out of the required temperature.
of filling compound removed from completed wire or cable.
18.6 Preparation—Place 3 to 5 mg of the filling material to
NOTE 14—For additional information on wire and cable filling be tested into an aluminum pan and cover this with a clean
compounds, refer to Specifications D4731 and D4732.
stainlesssteelscreen.Crimpthepantoholdthescreeninplace.
18.2 Apparatus, Reagents, and Materials:
18.7 Placethepreparedspecimenpanintheinstrumentcell.
18.2.1 This test is normally performed using commercial
Flush the cell for 5 min using cylinder nitrogen at a flow rate
devices commonly referred to as Differential Scanning Calo-
of 200 6 25 cm /min. Following the nitrogen purge, increase
rimeters (DSC) or as Differential Thermal Analyzers (DTA).
the cell-specimen temperature (at a heating rate of 10 °C/min)
Use of another apparatus is permitted if it is demonstrated to
from the initial temperature to 190 6 2 °C. Once temperature
yieldcomparableresults.Thefollowingreagentsandmaterials
equilibrium of 190 °C has been reached (steady recorder
are also required to perform this test:
signal), switch to oxygen flow at the same flow rate and
18.2.1.1 Use commercial cylinder nitrogen for purging in-
simultaneously start the time base recording.
strument cells.
18.8 Recordthestartoftheoxygeninjectionastime“zero.”
18.2.1.2 Use oxygen in this test method equal to or better
Maintain the isothermal temperature of 190 °C in the pure dry
than 99.6% extra dry grade.
oxygen atmosphere until the oxidative reaction exotherm
18.2.1.3 Small specimen pans are required to hold the
appears on the thermogram (see Fig. 5). When the test is
specimens while in the instrument cells. Pans shall be alumi-
completed, turn off the recorder, switch the gas back to
num.
18.2.1.4 Use No. 316 stainless steel screen (40 mesh) to
cover specimens in the pans.
18.2.1.5 Use pure metal standards such as indium, tin, lead,
or zinc for instrument calibrations as recommended by the
instrument manufacturer.
18.3 Sample Preparation—Select at random a short-length
section, approximately 1 ft (300 mm) long, of completed wire
or cable. Remove the core from the wire or cable section;
accomplish this by pulling or pushing the core out without
cutting the jacket. Remove the filling compound from the core
Supporting data have been filed atASTM International Headquarters and may
beobtainedbyrequestingResearchReportRR:D09-1034.ContactASTMCustomer
Service at service@astm.org.
ThetaskforcesummarizeditsfindinginapaperbyV.J.Kuckpublishedinthe
Proceedings of the 6th International Conference on Plastics in Telecommunications FIG. 5 Evaluation of Oxidative Induction Time (OIT) From
(Pub. Plastics & Rubber Institute, London, England), September, 1992. Recorded-time-base Thermogram
D4565 − 20
nitrogen, and allow the cell temperature of the instrument to merely states whether there is conformance to the criteria for
cool to ambient temperature. Remove and discard the pan and success specified in the product specification.
specimen.
21. Environmental Stress Crack (Polyolefin Jackets
18.9 On the recorder chart, draw an extension to the
Only)
recorded base line beyond the oxidative reactive exotherm.
21.1 Perform tests on specimens die cut in the transverse
Extrapolate the slope of the oxidative reactive exotherm to
direction from cable jackets having an outside diameter of
intercept the extended base line. The oxidative induction time
1.125 in. (30 mm) and larger. Prepare these specimens and
(OIT) is measured to within 61 min from zero time to the
subject them to an environmental stress cracking test as
intercept point.
specified in Test Method D1693 except that the conditioning
18.10 Precision and Bias—This test method is based on the
requirementiswaived,thedepthofthecontrolledimperfection
exotherm obtained when the filling compound degrades. As
shall be proportional to the jacket thickness, and the stress
such, precision of the test method is strongly dependent on the
crackingreagentshallbea10%solution(byvolume)ofIgepal
extent to which the filling compound under test is degraded.
CO-630 (Antarox CO-630) surfactant.
Since no calculation of OITis possible, a comparison between
21.2 Precision and Bias—The precision of this test method
the measured and the true values cannot be achieved.
has not been determined. No statement can be made about the
bias of this test for environmental stress crack (jacket only)
19. Insulation Adhesion
since the result merely states whether there is conformance to
19.1 Test specimens of finished insulated conductor for
the criteria for success specified in the product specification.
insulation adhesion. Prepare specimens by first trimming
insulated wire specimens to 5 in. (130 mm) in length. Remove
22. Heat Distortion (Jackets Only)
the insulation (by progressively removing short sections) from
22.1 This test is for polyvinyl chloride (PVC) jacket mate-
one end of the wire until only a 1-in. (25mm) length of
rial only.
undisturbed insulation remains at the other end of the speci-
22.2 Prepareasampleapproximately8in.(200mm)longto
men. (Warning—Exercise great care in this step to avoid
have a thickness of 0.050 6 0.010 in. (1.27 6 0.25 mm) and
nicking the conductor while removing the insulation.) Pass the
smooth surfaces. From this sample, prepare test specimens
bared conductor through a die plate or orifice having an
1in. (25.4 mm) long and 0.56 6 0.063 in. (14.3 6 1.6 mm)
aperture measuring 0.003 to 0.005 in. (0.07 to 0.13 mm) larger
wide. Where the diameter of the cable does not permit the
than the conductor until the shoulder of insulation rests on the
preparation of a specimen 0.56 in. (14.3 mm) wide, use a
die plate. Apply tension between the conductor and the die
molded sheet of the same compound.
plate and measure the force required to strip the remaining
insulation from the wire. Compare results with the require-
22.3 Measure the thickness of the specimen, T , using a
ments specified in the product specification. The speed of the
Randall and Stickney gauge, or the equivalent, having a
moving head of the tensile testing machine shall be as
0.375-in. (9.5 mm) foot with no loading other than the
prescribed by the product specification.
85grams-force of the gauge.
19.2 Precision and Bias—The precision of this test has not 22.4 In 3 h, complete the following procedure: Place a
been determined. No statement can be made about the bias of Randall and Stickney gauge, or the equivalent, with a load of
this test for insulation adhesion since the result merely states 2000 g on the foot in an oven that is preheated to a specified
whether there is conformance to the criteria for succe
...