ASTM D5885-97
(Test Method)Standard Test Method for Oxidative Induction Time of Polyolefin Geosynthetics by High-Pressure Differential Scanning Calorimetry
Standard Test Method for Oxidative Induction Time of Polyolefin Geosynthetics by High-Pressure Differential Scanning Calorimetry
SCOPE
1.1 This test method covers a procedure for the determination of the oxidative induction time (OIT) of polyolefin geosynthetics using high pressure differential scanning calorimetry.
1.2 The focus of the test is on geomembranes, but geogrids, geonets, geotextiles, and other polyolefin-related geosynthetics are also suitable for such evaluation.
1.3 This test method measures the oxidative induction time associated with a given test specimen at a specified temperature and pressure.
1.4 This is an accelerated test for highly stabilized materials. It is applicable only to material whose OIT values under 3.4 MPa of oxygen is greater than 30 min at 150°C.
1.5 The values stated in SI units are to be regarded as the standard. The values stated in parentheses are provided for information only.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 8.
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Designation: D 5885 – 97
Standard Test Method for
Oxidative Induction Time of Polyolefin Geosynthetics by
High-Pressure Differential Scanning Calorimetry
This standard is issued under the fixed designation D 5885; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 4565 Test Methods for Physical and Environmental Per-
formance Properties of Insulations and Jackets for Tele-
1.1 This test method covers a procedure for the determina-
communications Wire and Cable
tion of the oxidative induction time (OIT) of polyolefin
D 4703 Practice for Compression Molding Thermoplastic
geosynthetics using high pressure differential scanning calo-
Materials into Test Specimens, Plaques, or Sheets
rimetry.
E 473 Terminology Relating to Thermal Analysis
1.2 The focus of the test is on geomembranes, but geogrids,
E 967 Practice for Temperature Calibration of Differential
geonets, geotextiles, and other polyolefin-related geosynthetics
Scanning Calorimeters and Differential Thermal Analyz-
are also suitable for such evaluation.
ers
1.3 This test method measures the oxidative induction time
E 691 Practice for Conducting an Interlaboratory Study to
associatedwithagiventestspecimenataspecifiedtemperature
Determine the Precision of a Test Method
and pressure.
G 88 Guide for Designing Systems for Oxygen Service
1.4 Thisisanacceleratedtestforhighlystabilizedmaterials.
It is applicable only to material whose OIT values under 3.4
3. Terminology
MPa of oxygen is greater than 30 min at 150°C.
3.1 Definitions:
1.5 The values stated in SI units are to be regarded as the
3.1.1 differential scanning calorimetry (DSC), n—a tech-
standard. The values stated in parentheses are provided for
nique in which the difference in heat flow inputs into a
information only.
substance and a reference material is measured as a function of
1.6 This standard does not purport to address all of the
temperatureortime,whilethesubstanceandreferencematerial
safety concerns, if any, associated with its use. It is the
are subjected to a controlled-temperature program. (See Ter-
responsibility of the user of this standard to establish appro-
minology E 473.)
priate safety and health practices and determine the applica-
3.1.2 geomembrane, n—an essentially impermeable geo-
bility of regulatory limitations prior to use. Specific precau-
synthetic composed of one or more synthetic sheets. (See
tionary statements are given in Section 8.
Terminology D 4439.)
2. Referenced Documents 3.1.2.1 Discussion—In this test method, essentially imper-
meable means that no measurable liquid flows through a
2.1 ASTM Standards:
geosynthetic when tested in accordance with Test Method
D 3417 TestMethodforHeatsofFusionandCrystallization
2 D 4491.
of Polymers by Thermal Analysis
3.1.3 geosynthetic, n—a planar product manufactured from
D 3895 Test Method for Oxidative-Induction Time of Poly-
2 polymeric material used with soil, rock, earth, or other geo-
olefins by Differential Scanning Calorimetry
technical engineering-related material as an integral part of a
D 4439 Terminology for Geosynthetics
man-made project, structure, or system. (See Terminology
D 4491 Test Methods for Water Permeability of Geotextiles
D 4439.)
by Permittivity
3.1.4 high-pressure differential scanning calorimetry (HP-
DSC), n—differential scanning calorimetry in which the sub-
1 stance and reference material are exposed to a controlled
This test method is under the jurisdiction of ASTM Committee D-35 on
Geosynthetics and is the direct responsibility of Subcommittee D35.02 on Endur- superambient atmosphere.
ance Properties.
Current edition approved Feb. 10, 1997. Published November 1997. Originally
published as D 5885 – 95. Last previous edition D 5885 – 95. Annual Book of ASTM Standards, Vol 10.02.
2 5
Annual Book of ASTM Standards, Vol 08.02. Annual Book of ASTM Standards, Vol 08.03.
3 6
Annual Book of ASTM Standards, Vol 04.13. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5885–97
3.1.5 index test, n—a test procedure that may be used to 5.5.1 The use of high test temperature, however, may have
establish an order for a set of specimens with respect to the deleterious effects. The first of these is the potential volatiliza-
property of interest. tion of additive packages used to stabilize the test materials.
3.1.6 oxidative induction time (OIT), n—the elapsed time The second is the potential for the influence of chemical
between first exposure to an oxidizing gas and the onset to mechanisms which are not significant at end-use operation
oxidation of a material under isothermal conditions. conditions.
5.5.2 This test method uses high oxygen pressure to accel-
3.1.6.1 Discussion—Oxidative induction time is an index
test parameter dependent upon a wide range of experimental erate the test period while making use of lower test tempera-
tures to protect additive packages.
conditions including temperature, pressure of oxygen, purge
gas flow rate, and the presence or absence of catalysts. 5.6 The results from this test method may or may not
correlate with those obtained by other OIT measurements such
4. Summary of Test Method as Test Method D 3895 or Test Methods D 4565.
4.1 The specimen to be tested and the corresponding refer-
6. Apparatus
ence material are heated from room temperature at a constant
6.1 Differential Scanning Calorimeter—Thermal analysis
rate in a non-purging, high-pressure oxygen environment at a
equipment capable of heating rates up to 20 6 1°C/min and of
defined pressure. When the specified temperature has been
automatically recording the differential heat flow between the
reached, the specimen is then held at that temperature until the
testsampleandareferencesampleisnecessary.Theequipment
oxidative reaction is displayed on the thermal curve. The OIT
must be capable of measuring sample temperature to 61°C
is the time interval from the start of the temperature program
while maintaining a set temperature to 60.5°C.
test to the onset of the oxidative reaction.
4.2 Inthisprocedure,anelevatedpressureofoxygenisused
NOTE 1—Modern computer-based instrumentation equipped with “iso-
to accelerate the reaction and to reduce analysis time.
track” modes provide adequate specimen temperature control.
4.3 Unless otherwise specified, the temperature used in this
6.2 Data Presentation Device—A printer, plotter, recorder,
test method shall be 150°C, and the chamber pressure is to be
or other recording output device capable of displaying heat
maintained at 3.4 MPa (500 psi) using a constant volume test
flow on the Y-axis versus time on the X-axis as output signals
condition.
from differential scanning calorimeters in 6.1.
6.3 High-Pressure DSC Cell—A unit capable of maintain-
5. Significance and Use
ing pressure up to 3.4 MPa (500 psig). The system shall be
5.1 The oxidative induction time is a characteristic of a
equipped with a pressure gage to monitor the internal pressure
compounded polyolefin product that is dependent not only on
of the cell to permit manual release of pressure to maintain
the type and amount of additives present, but also on the type
desired level.
of resin. In well-behaved systems, this test method can be used
NOTE 2—The gage shall be accurate to 2 % at 3.4 MPa (500 psig).
as a quality control measure to monitor the stabilization in
NOTE 3—All pressures in this test method are indicated relative to
geosynthetics as received from a supplier.
atmosphere pressure—that is, they are “gage” pressures.
5.2 When this test method is used to compare different
6.4 High-Pressure Oxygen Cylinder Regulator—Apressure
geomembrane formulations containing different antioxidant
regulator capable of regulating a pressure up to 5.5 MPa (800
packages, then those results shall be considered valid only at
psi). The outlet of the cylinder is to be linked to the high-
the temperature of test.
pressure cell using a clean stainless steel tube.
5.3 This test method is intended as an geosynthetic test. Use
6.5 Analytical Balance, 0.1-mg sensitivity.
of the OIT value to estimate the lifetime of the geomembrane
6.6 Specimen Holders, degreased aluminum pans, 6.0 to
fromwhichthetestspecimenistakenisnotaddressednorshall
7.0-mm diameter.
it be used for this purpose.
6.7 Core Hole Borer, cork borer or arch punch producing
5.3.1 The OIT measurement is an accelerated thermal aging
6.3-mm (0.25-in.) disks.
test and, as such, interpretation of resulting data may be
misleading if done by an inexperienced operator. Caution
7. Reagents and Materials
should be exercised in data interpretation since oxidation
7.1 All chemical reagents used in this test method shall be
reaction kinetics are a function of temperature and the proper-
analytical grade unless otherwise specified.
ties of the additives contained in the geosynthetic sample. For
7.2 Hexane or Acetone, for cleaning specimen pans and
example, OIT values are often used to select optimum resin
stainless steel tubing, see 8.2 and 8.3.
formulations. Certain antioxidants, however, may generate
7.3 Indium (99.999 % Purity), for calibration purposes, see
poor OIT results even though they may be adequate at their
9.1.
intended use temperature and vice versa.
7.4 Oxygen, purity >99.5 % for the test atmosphere.
5.4 This test method can be used for other purposes such as
manufacturing control and research and development.
8. Precautions
5.5 Oxidation induction time is strongly dependent upon
test temperature and the partial pressure of oxygen. The higher 8.1 Oxygen is a strong oxidizer that vigorously accelerates
the test temperature or the oxygen partial pressure, or both, the combustion. Keep oil and grease away from equipment using
shorter the oxidation induction time. or containing oxygen.
D5885–97
a temperature rise of no more than 5°C is observed
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