ASTM D3012-19

Standard Test Method for Thermal-Oxidative Stability of Polypropylene Using a Specimen Rotator Within an Oven

SIGNIFICANCE AND USE
5.1 Under the severe conditions of this test method, the specimens undergo degradation at a rate that is dependent upon the thermal endurance of the polypropylene material under examination.  
5.2 The thermal level of this test method is considered sufficiently severe to cause failure of commercial grades of heat-stable polypropylene within a reasonable period of time. If desired, lower temperatures can be applied to estimate the performance of polypropylene materials with lower heat stability.  
5.3 The technique of specimen rotation described in this test method provides an estimate of the life-temperature relationship of polypropylene. If this test method is conducted at different temperatures on the same material, a more reliable estimate of the life-temperature relationship of polypropylene is determined. This test method can be conducted at several temperatures and the data interpreted through use of the Arrhenius relation, by plotting the logarithms of times to failure against the reciprocals of the temperatures in kelvins (K). Temperatures in the range from 100 to 150°C, with intervals of 10°C, are suggested for this purpose.  
5.4 The stability as determined under the prescribed test method is not directly related to the suitability of the compound for a use where different conditions prevail.  
5.5 The specimen rotation technique of thermal aging increases the probability that all specimens will be exposed similarly and that the effect of temperature gradients in an oven will be minimized.
SCOPE
1.1 This test method provides a means for estimating the resistance of polypropylene, in molded form, to accelerated aging by heat in the presence of air using a forced draft oven.  
1.2 The stability determined by this test method is not directly related to the suitability of the material for use when different environmental conditions prevail and shall not be used to predict performance.  
Note 1: The specified thermal levels in this test method are considered sufficiently severe to cause failure of commercial grades of heat-stable polypropylene within a reasonable period of time. If desired, lower temperatures can be applied to estimate the performance of polypropylene with lower heat stabilities.  
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 2: This test method and ISO 4577–1983 are technically similar but different in preparation of test specimens, thickness of test specimen, measurement of the number of air flow changes in the ovens, and the number of air changes per hour required.  
1.5 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.

General Information

• Status: Published
• Publication Date: 31-Mar-2019
• ICS: 83.080.20 - Thermoplastic materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.15 - Thermoplastic Materials

Relations

• Refers: ASTM D4101-24 - Standard Classification System and Basis for Specification for Polypropylene Injection and Extrusion Materials
• Effective Date: 01-Feb-2024
• Refers: ASTM D883-24 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2024
• Refers: ASTM D883-23 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2023
• Refers: ASTM E456-13a(2022)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Apr-2022
• Refers: ASTM D883-20 - Standard Terminology Relating to Plastics
• Effective Date: 01-Jan-2020
• Refers: ASTM E644-11(2019) - Standard Test Methods for Testing Industrial Resistance Thermometers
• Effective Date: 01-Nov-2019
• Refers: ASTM D883-19c - Standard Terminology Relating to Plastics
• Effective Date: 01-Aug-2019
• Refers: ASTM D883-19a - Standard Terminology Relating to Plastics
• Effective Date: 15-Apr-2019
• Refers: ASTM D883-19 - Standard Terminology Relating to Plastics
• Effective Date: 01-Feb-2019
• Refers: ASTM D883-18a - Standard Terminology Relating to Plastics
• Effective Date: 01-Dec-2018
• Refers: ASTM D883-18 - Standard Terminology Relating to Plastics
• Effective Date: 01-Nov-2018
• Refers: ASTM E456-13A(2017)e3 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E456-13A(2017)e1 - Standard Terminology Relating to Quality and Statistics
• Effective Date: 01-Oct-2017
• Refers: ASTM E2935-17 - Standard Practice for Conducting Equivalence Testing in Laboratory Applications
• Effective Date: 01-Oct-2017
• Refers: ASTM D883-17 - Standard Terminology Relating to Plastics
• Effective Date: 15-Aug-2017

Overview

ASTM D3012-19 – Standard Test Method for Thermal-Oxidative Stability of Polypropylene Using a Specimen Rotator Within an Oven provides a widely recognized procedure for evaluating the resistance of molded polypropylene to accelerated thermal-oxidative aging. Utilizing a forced draft oven and a rotating specimen holder, this method simulates severe thermal exposure and oxidative conditions to assess the material’s endurance over time. ASTM D3012-19 is essential for quality control, material comparison, and research and development activities involving polypropylene used in rigorous thermal environments.

Key Topics

• Accelerated Aging by Heat and Air: The method subjects polypropylene specimens to elevated temperatures (typically 150°C) in the presence of air, allowing for rapid evaluation of material stability.
• Specimen Rotator Technology: Rotation ensures uniform exposure of all specimens, minimizing variability due to temperature gradients and airflow inconsistencies in the oven.
• Life-Temperature Relationship: By running the test at different temperatures (100-150°C suggested), it is possible to estimate the relationship between service life and temperature using the Arrhenius equation.
• Visual Failure Assessment: The test determines time to failure based on visual signs such as crazing, cracking, discoloration, or crumbling, which are indicative of oxidative degradation.
• Conditioning and Precision: The standard provides guidance on specimen preparation, conditioning, and measurement repeatability and reproducibility across laboratories.

Applications

• Material Comparison: Manufacturers and researchers use ASTM D3012-19 to compare the thermal-oxidative stability of different polypropylene grades and formulations under harsh conditions.
• Quality Assurance: Producers of polypropylene materials rely on this test to verify conformity with industry standards, monitor batch consistency, and validate improvements in thermal stability.
• Research & Development: Polymer scientists employ this method to evaluate the effectiveness of stabilizers, additives, and compositional changes in enhancing the heat resistance of polypropylene.
• Predictive Data: While the specific conditions are more severe than most end-use environments, results can be interpreted to estimate the relative longevity of polypropylene products in hot, oxidative settings such as automotive, electrical, or household appliance components.
• Process and Specification Control: ASTM D3012-19 helps in setting internal or customer specifications and controlling the processing variables that impact finished product durability.

Related Standards

• ASTM D618: Conditioning Plastics for Testing – essential for preparing specimens to a standard humidity and temperature before testing.
• ASTM D883: Terminology Relating to Plastics – reference for defining terms used throughout materials testing.
• ASTM D3641: Injection Molding Test Specimens – standard procedures for preparing test specimens from thermoplastic materials.
• ASTM D4101: Classification and Property Specifications for Polypropylene Injection and Extrusion Materials.
• ASTM D5374: Testing Ovens for Electrical Insulation – specifies requirements for laboratory ovens used in such tests.
• ISO 4577:1983: Polypropylene and Propylene Copolymers – Air-Oven Method for Thermal Oxidative Stability – an international equivalent with slight procedural differences (notably specimen preparation and air flow measurement).
• ISO 1873: Polypropylene Thermoplastics – Specification and Properties

Summary

ASTM D3012-19 is a critical standard for assessing the thermal-oxidative stability of polypropylene using a forced draft oven and specimen rotator. It serves manufacturers, quality control labs, and research institutions by ensuring consistent, repeatable data on polypropylene's performance under severe aging conditions. When used alongside related ASTM and ISO standards, it supports informed material selection, product development, and quality assurance in markets demanding reliable high-temperature polypropylene performance.

Standards Content (Sample)

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: D3012 − 19
Standard Test Method for
Thermal-Oxidative Stability of Polypropylene Using a
Specimen Rotator Within an Oven
This standard is issued under the fixed designation D3012; 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* 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method provides a means for estimating the
D618 Practice for Conditioning Plastics for Testing
resistance of polypropylene, in molded form, to accelerated
D883 Terminology Relating to Plastics
aging by heat in the presence of air using a forced draft oven.
D3641 Practice for Injection Molding Test Specimens of
1.2 The stability determined by this test method is not
Thermoplastic Molding and Extrusion Materials
directly related to the suitability of the material for use when
D4101 Classification System and Basis for Specification for
different environmental conditions prevail and shall not be
Polypropylene Injection and Extrusion Materials
used to predict performance.
D5374 Test Methods for Forced-Convection Laboratory Ov-
ens for Evaluation of Electrical Insulation
NOTE1—Thespecifiedthermallevelsinthistestmethodareconsidered
sufficiently severe to cause failure of commercial grades of heat-stable
E77 Test Method for Inspection and Verification of Ther-
polypropylene within a reasonable period of time. If desired, lower
mometers
temperatures can be applied to estimate the performance of polypropylene
E220 Test Method for Calibration of Thermocouples By
with lower heat stabilities.
Comparison Techniques
1.3 The values stated in SI units are to be regarded as the
E456 Terminology Relating to Quality and Statistics
standard. The values in parentheses are for information only.
E608/E608M Specification for Mineral-Insulated, Metal-
Sheathed Base Metal Thermocouples
1.4 This standard does not purport to address all of the
E644 Test Methods for Testing Industrial Resistance Ther-
safety concerns, if any, associated with its use. It is the
mometers
responsibility of the user of this standard to establish appro-
E691 Practice for Conducting an Interlaboratory Study to
priate safety, health, and environmental practices and deter-
Determine the Precision of a Test Method
mine the applicability of regulatory limitations prior to use.
E1137/E1137M Specification for Industrial Platinum Resis-
NOTE 2—This test method and ISO 4577–1983 are technically similar
tance Thermometers
but different in preparation of test specimens, thickness of test specimen,
E2251 Specification for Liquid-in-Glass ASTM Thermom-
measurement of the number of air flow changes in the ovens, and the
eters with Low-Hazard Precision Liquids
number of air changes per hour required.
E2935 Practice for Conducting Equivalence Testing in
1.5 This international standard was developed in accor-
Laboratory Applications
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
2.2 ISO Standard:
Development of International Standards, Guides and Recom- ISO 4577–1983 Plastics—Polypropylene and Propylene
mendations issued by the World Trade Organization Technical Copolymers—Determination of Thermal Oxidative Sta-
Barriers to Trade (TBT) Committee. bility in Air-Oven Method
1 2
This test method is under the jurisdiction ofASTM Committee D20 on Plastics For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi- contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
als. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2019. Published May 2019. Originally the ASTM website.
approved in 1972. Last previous edition approved in 2013 as D3012 - 13. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D3012-19. 4th Floor, New York, NY 10036, http://www.ansi.org.
*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
D3012 − 19
ISO 19069 Plastics—Polypropylene (PP) Moulding and Ex- 5.4 The stability as determined under the prescribed test
trusion Materials: methodisnotdirectlyrelatedtothesuitabilityofthecompound
Part 1: Designation System and Basis for Specifications for a use where different conditions prevail.
Part 2: Preparation of Test Specimens and Determination of
5.5 The specimen rotation technique of thermal aging in-
Properties
creases the probability that all specimens will be exposed
similarlyandthattheeffectoftemperaturegradientsinanoven
3. Terminology
will be minimized.
3.1 Definitions—Terms used in this standard are defined in
accordance with Terminology D883, unless otherwise speci-
6. Apparatus
fied. For terms relating to precision and bias and associated
issues,thetermsusedinthisstandardaredefinedinaccordance 6.1 Oven, mechanical convection type for controlled circu-
with Terminology E456. lation of air (for example, a forced draft type), with adjustable
3.1.1 repeatability—precision under repeatability condi- air intake and exhaust facilities, and designed for air velocities
tions. (E456) around 1000 6 250 mm/s (197 6 49 ft/min).
3.1.2 repeatability conditions, n—conditions where inde-
6.1.1 Theovenshallbeequippedwithatemperature-control
pendent test results are obtained with the same method on
system designed to maintain the test temperature range from
identicaltestitemsinthesamelaboratorybythesameoperator
150 6 1°C (302 6 1.8°F) and a device to prevent temperature
using the same equipment within short intervals of time.
override. With the oven adjusted to the nominal test tempera-
(E456)
ture of 150°C, the override shall be set at 154°C (309°F). A
3.1.3 reproducibility—precision under reproducibility con-
bimetallic-striptemperatureswitchhasbeenfoundsatisfactory.
ditions. (E456)
6.2 Oven Temperature Measurement System, consisting of a
3.1.4 reproducibility conditions, n—conditions where test
thermocouple, thermometer, or resistance thermometer as the
results are obtained with the same method on identical test
sensor, together with its associated conditions and readout
items in different laboratories with different operators using
instrumentation covering at least the temperature range from 0
different equipment. (E456)
to 200°C (32 to 372°F).
4. Summary of Test Method
6.2.1 The thermometer must cover the range in one-degree
subdivisions. It must be tested for bulb stability and
4.1 Aging is accelerated by exposing the specimens to an
standardized, in accordance with Test Method E77.
elevated temperature in a forced draft oven equipped with a
6.2.2 The secondary standard shall beASTM Thermometer
biaxial or uniaxial rotating specimen holder.
S67C–03 of Specification E2251.
4.2 Visual examination is used to determine the time to
6.2.3 Thermocouples shall comply with the requirements of
failure. The time to failure of the material is taken as the
Specification E608/E608M and shall be calibrated in accor-
numberofdaysafterwhichthespecimenshowstheinitialstart
dance with Method E220.
of any visual type of localized crazing, cracking, holes,
6.2.4 Resistance thermometers shall comply with the re-
crumbling, or discoloration, or a combination thereof.
quirements of Test Methods E644 and Specification E1137/
5. Significance and Use
E1137M, and be calibrated in accordance with NIST Special
5,6
Publication 250-22.
5.1 Under the severe conditions of this test method, the
specimensundergodegradationataratethatisdependentupon
6.3 Molding Press,designedtooperateat200 65°C(3926
the thermal endurance of the polypropylene material under
9°F).
examination.
6.4 Injection Molding Unit, meeting the requirements of
5.2 The thermal level of this test method is considered
Practice D3641.
sufficiently severe to cause failure of commercial grades of
6.5 Mold:
heat-stable polypropylene within a reasonable period of time.
6.5.1 Compression Mold, comprised of the following:
If desired, lower temperatures can be applied to estimate the
6.5.1.1 Compression Molding Chase, having a blanked-out
performance of polypropylene materials with lower heat sta-
areaofsuitablesize(Note3)andcapableofproducingaplaque
bility.
1.00 6 0.05 mm (0.039 6 0.002 in.) thick.
5.3 Thetechniqueofspecimenrotationdescribedinthistest
method provides an estimate of the life-temperature relation-
NOTE 3—A 152.4 by 152.4-mm (6 by 6-in.) blanked-out section has
been found satisfactory.
ship of polypropylene. If this test method is conducted at
different temperatures on the same material, a more reliable
estimate of the life-temperature relationship of polypropylene
is determined. This test method can be conducted at several 4
APrecision Scientific Freas Model 835 B, or Blue M POM-206C-1, are known
temperatures and the data interpreted through use of the
as acceptable ovens for this test, but other equivalent models meeting the
requirements in 6.1, 6.1.1, and Section 9 are allowed.
Arrhenius relation, by plotting the logarithms of times to
Mangum,B.W.,“PlatinumResistanceThermometerCalibration,”NBSSpecial
failure against the reciprocals of the temperatures in kelvins
Publication 250-22 (1987).
(K). Temperatures in the range from 100 to 150°C, with
Available from National Institute of Standards and Technology (NIST), 100
intervals of 10°C, are suggested for this purpose. Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
D3012 − 19
6.5.1.2 Backing Plates,largeenoughtocoverthischaseand
strong enough to resist warping or distortion, under the
molding conditions. Polished steel plates, 3 mm (0.1 in.) thick,
are satisfactory.
6.5.2 Injection Mold, designed using the guidelines speci-
fiedinPracticeD3641.Themoldshallbecapableofproducing
either a plaque having a thickness of 1.00 6 0.05 mm (0.039
6 0.002 in.) from which 50 by 10 by 1.00-mm (2 by 0.4 by
0.039-in.) specimens can be die cut, or mold a standard test
specimen, 50 by 10 by 1.00 mm.
6.6 Parting Sheets—Fluoropolymer, polyester, or other film
that will not affect the long-term thermal stability of
polypropylene, 0.05 to 0.20 mm (0.002 to 0.008 in.) thick.The
film must be free of wrinkles and foreign matter, such as
lubricants and oils.
6.7 Cutting Die, to produce 50 by 10-mm (2 by 0.4-in.)
specimens from either a compression-molded or injection-
molded plaque. The die must be sharp and free of nicks.
6.8 Specimen Holder—The specimen holder is either a
biaxiallyoruniaxiallyrotatedunit,capableofexposingthetest
specimens to a stream of air having a relative velocity about
1000 mm/s (197 ft/min) (see 9.3). Illustrations of suitable
apparatus for biaxially and uniaxially rotated specimen holders
are shown in Figs. 1 and 2, respectively. Biaxial rotation
increases the probability that all specimens will be exposed
similarly.Inthecaseofdispute,theuseofbiaxialrotationshall
be the reference method.
6.8.1 Biaxially Rotated Specimen Holder (see Fig. 1) . The
frequency of rotation about the horizontal and vertical axes
–1
shall be 1 to 3 min .
FIG. 2 Uniaxially Rotated Specimen Holder—Drum Rotator
6.8.2 Uniaxially Rotated Specimen Holder (see Fig. 2). The
drum peripheral velocity shall be such that the air stream
impinges on the flat section of the test specimens at about 1
6.9 Air Velocity Meter, nondirectional resistance wire type
m/s.
for measuring the air velocity in the oven.
6.10 Anemometer, with a circular vane, for determining the
StandardScientificSupplyCompany,ModelCS191,orequivalent,canbeused.
frequency of air changes in the oven.The anemometer shall be
positioned directly in front of the oven outlet. Based on the
design of the outlet and the anemometer, every effort shall be
made to position the anemometer’s electronics in a way as to
minimize the degree of exposure to the heated air exiting the
oven.
6.11 Metal Clips, lined with fluorocarbon film or other
materials that have no adverse effect on the oxidative thermal
stability of polypropylene.
7. Specimen Preparation
7.1 The test specimens shall be cut from either a compres-
sion–molded plaque or injection-molded plaque prepared from
powders,granules,pellets,etc.,orotherhomogeneousmolding
material. Plaques shall be prepared as follows:
7.2 Compression Molding:
7.2.1 Adjust the temperature of the platens to 200 6 5°C
(392 6 9°F).
7.2.2 Place a smooth, clean parting sheet on a backing plate
and center the chase on it. Put enough of the sample into the
FIG. 1 Biaxial Ferris-Wheel-Type Rotator cavity to fill it completely when molded. A slight excess of
D3012 − 19
material is desirable. Cover the loaded chase first with a clean 9. Oven Parameters
parting sheet and then a backing plate. Finally, put the
9.1 Unless otherwise specified, the oven temperature shall
assembled mold on the lower platen and close the press
be 150°C (302°F) and shall not vary more than 61°C,
carefully until both platens are in contact with the assembly.
measured at a single location within the oven, or more than
Whenthematerialhasmelted,applysufficientpressuretoform
61.5°C throughout the oven.
a void-free plaque in the 1.00 6 0.5 mm (0.039 6 0.002 in.)
9.1.1 To monitor temperature, the oven temperature mea-
thick and record this pressure. Leave the polypropylene in the
surement sensor should be conveniently located about 80 mm
heated press under pressure for 3 to 4 min at 200 6 5°C (392
(3 in.) from the top liner of the oven, in the vicinity of the
6 9°F). Flash cool the mold assembly by transferring to a
exhaust port.
water-cooled press or by water quenching.
9.2 In the event that the average time to failure at 150°C is
NOTE 4—For some polypropylene materials that do not provide a fully less than seven days, the test report shall indicate “less than
filled-
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D3012 − 13 D3012 − 19
Standard Test Method for
Thermal-Oxidative Stability of Polypropylene Using a
Specimen Rotator Within an Oven
This standard is issued under the fixed designation D3012; 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*
1.1 This test method provides a means for estimating the resistance of polypropylene, in molded form, to accelerated aging by
heat in the presence of air using a forced draft oven.
1.2 The stability determined by this test method is not directly related to the suitability of the material for use when different
environmental conditions prevail and shall not be used to predict performance.
NOTE 1—The specified thermal levels in this test method are considered sufficiently severe to cause failure of commercial grades of heat-stable
polypropylene within a reasonable period of time. If desired, lower temperatures can be applied to estimate the performance of polypropylene with lower
heat stabilities.
1.3 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.
1.4 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
NOTE 2—This test method and ISO 4577–1983 are technically similar but different in preparation of test specimens, thickness of test specimen,
measurement of the number of air flow changes in the ovens, and the number of air changes per hour required.
1.5 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.
2. Referenced Documents
2.1 ASTM Standards:
D618 Practice for Conditioning Plastics for Testing
D883 Terminology Relating to Plastics
D3641 Practice for Injection Molding Test Specimens of Thermoplastic Molding and Extrusion Materials
D4101 Classification System and Basis for Specification for Polypropylene Injection and Extrusion Materials
D5374 Test Methods for Forced-Convection Laboratory Ovens for Evaluation of Electrical Insulation
E77 Test Method for Inspection and Verification of Thermometers
E220 Test Method for Calibration of Thermocouples By Comparison Techniques
E456 Terminology Relating to Quality and Statistics
E608E608/E608M Specification for Mineral-Insulated, Metal-Sheathed Base Metal Thermocouples
E644 Test Methods for Testing Industrial Resistance Thermometers
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1137/E1137M Specification for Industrial Platinum Resistance Thermometers
E2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
E2935 Practice for Conducting Equivalence Testing in Laboratory Applications
2.2 ISO Standard:
ISO 4577–1983 Plastics—Polypropylene and Propylene Copolymers—Determination of Thermal Oxidative Stability in
Air-Oven Method
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
Current edition approved April 1, 2013April 1, 2019. Published April 2013May 2019. Originally approved in 1972. Last previous edition approved in 20072013 as
D3012 - 07.D3012 - 13. DOI: 10.1520/D3012-13.10.1520/D3012-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.10036, http://www.ansi.org.
*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
D3012 − 19
ISO 187319069 Plastics—Polypropylene and Propylene-Copolymer Thermoplastics:(PP) Moulding and Extrusion Materials:
Part 1: Designation System and Basis for Specifications
Part 2: Preparation of Test Specimens and Determination of Properties
3. Terminology
3.1 Definitions—The definitions of plastics Terms used in this test method standard are defined in accordance with Terminology
D883 unless otherwise indicated. , unless otherwise specified. For terms relating to precision and bias and associated issues, the
terms used in this standard are defined in accordance with Terminology E456.
3.1.1 repeatability—precision under repeatability conditions. (E456)
3.1.2 repeatability conditions, n—conditions where independent test results are obtained with the same method on identical test
items in the same laboratory by the same operator using the same equipment within short intervals of time. (E456)
3.1.3 reproducibility—precision under reproducibility conditions. (E456)
3.1.4 reproducibility conditions, n—conditions where test results are obtained with the same method on identical test items in
different laboratories with different operators using different equipment. (E456)
4. Summary of Test Method
4.1 Aging is accelerated by exposing the specimens to an elevated temperature in a forced draft oven equipped with a biaxial
or uniaxial rotating specimen holder.
4.2 Visual examination is used to determine the time to failure. The time to failure of the material is taken as the number of
days after which the specimen shows localized crazing, the initial start of any visual type of localized crazing, cracking, holes,
crumbling, or discoloration, or a combination thereof.
5. Significance and Use
5.1 Under the severe conditions of this test method, the specimens undergo degradation at a rate that is dependent upon the
thermal endurance of the polypropylene material under examination.
5.2 The thermal level of this test method is considered sufficiently severe to cause failure of commercial grades of heat-stable
polypropylene within a reasonable period of time. If desired, lower temperatures can be applied to estimate the performance of
polypropylene materials with lower heat stability.
5.3 The technique of specimen rotation described in this test method provides an estimate of the life-temperature relationship
of polypropylene. If this test method is conducted at different temperatures on the same material, a more reliable estimate of the
life-temperature relationship of polypropylene is determined. This test method can be conducted at several temperatures and the
data interpreted through use of the Arrhenius relation, by plotting the logarithms of times to failure against the reciprocals of the
temperatures in kelvins (K). Temperatures in the range from 100 to 150°C, with intervals of 10°C, are suggested for this purpose.
5.4 The stability as determined under the prescribed test method is not directly related to the suitability of the compound for
a use where different conditions prevail.
5.5 The specimen rotation technique of thermal aging increases the probability that all specimens will be exposed similarly and
that the effect of temperature gradients in an oven will be minimized.
6. Apparatus
6.1 Oven, mechanical convection type for controlled circulation of air, air (for example, a forced draft type), with adjustable air
intake and exhaust facilities, and designed for air velocities around 1000 6 250 mm/s (197 6 49 ft/min).
6.1.1 The oven shall be equipped with a temperature-control system designed to maintain the test temperature range from 150
6 1°C (302 6 1.8°F) and a device to prevent temperature override. With the oven adjusted to the nominal test temperature of
150°C, the override shall be set at 154°C (309°F). A bimetallic-strip temperature switch has been found satisfactory.
6.2 Oven Temperature Measurement System, consisting of a thermocouple, thermometer, or resistance thermometer as the
sensor, together with its associated conditions and readout instrumentation covering at least the temperature range from 0 to 200°C
(32 to 372°F).
6.2.1 The thermometer must cover the range in one-degree subdivisions. It must be tested for bulb stability and standardized,
in accordance with Test Method E77.
6.2.2 The secondary standard shall be ASTM Thermometer S67C–03 of Specification E2251.
6.2.3 Thermocouples shall comply with the requirements of Specification E608E608/E608M and shall be calibrated in
accordance with Method E220.
A Precision Scientific Freas Model 835 B, or Blue M POM-206C-1, or equivalent, can be used.are known as acceptable ovens for this test, but other equivalent models
meeting the requirements in 6.1, 6.1.1, and Section 9 are allowed.
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6.2.4 Resistance thermometers shall comply with the requirements of Test Methods E644 and Specification E1137/E1137M, and
5,6
be calibrated in accordance with NIST Special Publication 250-22.
6.3 Molding Press, designed to operate at 200 6 5°C (3926 9°F).
6.4 Injection Molding Unit, meeting the requirements of Practice D3641.
6.5 Mold:
6.5.1 Compression Mold, comprised of the following:
6.5.1.1 Compression Molding Chase, having a blanked-out area of suitable size (Note 3) and capable of producing a plaque 1.00
6 0.05 mm (0.039 6 0.002 in.) thick.
NOTE 3—A 152.4 by 152.4-mm (6 by 6-in.) blanked-out section has been found satisfactory.
6.5.1.2 Backing Plates, large enough to cover this chase and strong enough to resist warping or distortion, under the molding
conditions. Polished steel plates, 3 mm (0.1 in.) thick, are satisfactory.
6.5.2 Injection Mold, designed using the guidelines specified in Practice D3641. The mold shall be capable of producing either
a plaque having a thickness of 1.00 6 0.05 mm (0.039 6 0.002 in.) from which 50 by 10 by 1.00-mm (2 by 0.4 by 0.039-in.)
specimens can be die cut, or mold a standard test specimen, 50 by 10 by 1.00 mm.
6.6 Parting Sheets—Fluoropolymer, polyester, or other film that will not affect the long-term thermal stability of polypropylene,
0.05 to 0.20 mm (0.002 to 0.008 in.) thick. The film must be free of wrinkles and foreign matter, such as lubricants and oils.
6.7 Cutting Die, to produce 50 by 10-mm (2 by 0.4-in.) specimens from either a compression-molded or injection-molded
plaque. The die must be sharp and free of nicks.
6.8 Specimen Holder—The specimen holder can be biaxially rotated is either a biaxially or uniaxially rotated provided that unit,
capable of exposing the test specimens are in to a stream of air having a relative velocity about 1000 mm/s (197 ft/min). ft/min)
(see 9.3). Illustrations of suitable apparatus for biaxially and uniaxially rotated specimen holders are shown in Figs. 1 and 2,
respectively. Biaxial rotation increases the probability that all specimens will be exposed similarly. In the case of dispute, the use
of biaxial rotation shall be the reference method.
6.8.1 Biaxially Rotated Specimen Holder (see Fig. 1) . The frequency of rotation about the horizontal and vertical axes shall
–1
be 1 to 3 min .
6.8.2 Uniaxially Rotated Specimen Holder (see Fig. 2). The drum peripheral velocity shall be such that the air stream impinges
on the flat section of the test specimens at about 1 m/s.
6.9 Air Velocity Meter, nondirectional resistance wire type for measuring the air velocity in the oven.
FIG. 1 Biaxial Ferris-Wheel-Type Rotator
Mangum, B. W., “Platinum Resistance Thermometer Calibration,” NBS Special Publication 250-22 (1987).
Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
Standard Scientific Supply Company, Model CS191, or equivalent, can be used.
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FIG. 2 Uniaxially Rotated Specimen Holder—Drum Rotator
6.10 Anemometer, with a circular vane, for determining the frequency of air changes in the oven. The anemometer shall be
positioned directly in front of the oven outlet. Based on the design of the outlet and the anemometer, every effort shall be made
to position the anemometer’s electronics in a way as to minimize the degree of exposure to the heated air exiting the oven.
6.11 Metal Clips, lined with fluorocarbon film or other materials that have no adverse effect on the oxidative thermal stability
of polypropylene.
7. Specimen Preparation
7.1 The test specimens shall be cut from either a compression–molded plaque or injection-molded plaque prepared from
granules powders, granules, pellets, etc., or other homogeneous molding material. Plaques shall be prepared as follows:
7.2 Compression Molding:
7.2.1 Adjust the temperature of the platens to 200 6 5°C (392 6 9°F).
7.2.2 Place a smooth, clean parting sheet on a backing plate and center the chase on it. Put enough of the sample into the cavity
to fill it completely when molded. A slight excess of material is desirable. Cover the loaded chase first with a clean parting sheet
and then a backing plate. Finally, put the assembled mold on the lower platen and close the press carefully until both platens are
in contact with the assembly. When the material has melted, apply sufficient pressure to form a void-free plaque in the 1.00 6 0.5
mm (0.039 6 0.002 in.) thick and record this pressure. Leave the polypropylene in the heated press under pressure for 3 to 4 min
at 200 6 5°C (392 6 9°F). Flash cool the mold assembly by transferring to a water-cooled press or by water quenching.
NOTE 4—For some polypropylene materials that do not provide a fully filled-out and uniform compression molded plaque at the at the conditions in
7.2.2, alternative and adjustments to the temperature, pressure and/or molding times would need to be made to provide an acceptable molded specimen.
This changes shall be noted in the report 11.1.4.
7.3 Injection Molding:
7.3.1 Plaques or test specimens shall be injection-molded in accordance with the requirements of Specification D4101.
7.4 Prepare a minimum of five specimens per material sample by die-cutting specimens from the plaque or directly molding the
standard test specimen. The standard specimen shall be 10 mm wide, 50 mm long, and 1.00 6 0.05 mm thick. Edges shall be
smoothed, if necessary, to remove imperfections introduced by cutting.
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7.5 Test specimens prepared directly by injection molding without die cutting or specimens cut from polypropylene products
can be used as agreed upon between the interested parties. In all cases the referee method will be based on compression molded
die cut specimens.
NOTE 5—Failure test times for compression-molded and injection-molded specimens are not necessarily comparable due to the skin surface effect and
the distinctness or sharpness of th
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