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Designation: G 114 06

Standard Practices for


Evaluating the Age Resistance of Polymeric Materials Used
in Oxygen Service1
This standard is issued under the fixed designation G 114; 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 1.6 This standard does not purport to address all of the
1.1 These practices describe several procedures that are safety concerns, if any, associated with its use. It is the
used to determine the age resistance of plastic, thermosetting, responsibility of the user of this standard to establish appro-
and elastomeric materials exposed to oxygen-containing me- priate safety and health practices and determine the applica-
dia. bility of regulatory limitations prior to use. Specific precau-
1.2 These practices address both established methods that tionary statements are given in Section 10.
have a foundation of experience and potential methods that 2. Referenced Documents
have yet to be validated. The latter are included to promote
research and later elaboration in this practice as methods of the 2.1 ASTM Standards: 2
former type. D 395 Test Methods for Rubber PropertyCompression
1.3 The results of these practices may not give exact Set
correlation with service performance since service conditions D 412 Test Methods for Vulcanized Rubber and Thermo-
vary widely and may involve multiple factors. This practice plastic ElastomersTension
may be used to evaluate materials on a laboratory comparison D 573 Test Method for RubberDeterioration in an Air
basis. Oven
1.4 Three procedures are described for evaluating the age D 638 Test Method for Tensile Properties of Plastics
resistance of polymeric materials depending on application and D 1349 Practice for RubberStandard Temperatures for
information sought. Testing
1.4.1 Procedure A: Natural AgingThis procedure is used D 1708 Test Method for Tensile Properties of Plastics by
to simulate the effect(s) of one or more service stressors on a Use of Microtensile Specimens
materials oxygen resistance, and is suitable for evaluating D 2240 Test Method for Rubber PropertyDurometer
materials that experience continuous or intermittent exposure Hardness
to elevated temperature during service. D 2512 Test Method for Compatibility of Materials with
1.4.2 Procedure B: Accelerated Aging Comparative Oxygen Liquid Oxygen (Impact Sensitivity Threshold and Pass-
ResistanceThis procedure is suitable for evaluating materials Fail Techniques)
that are used in ambient temperature service, or at a tempera- D 3045 Practice for Heat Aging of Plastics Without Load
ture that is otherwise lower than the aging temperature, and is D 4809 Test Method for Heat of Combustion of Liquid
useful for developing oxygen compatibility rankings on a Hydrocarbon Fuels by Bomb Calorimeter (Precision
laboratory comparison basis. Method)
1.4.3 Procedure C: Accelerated Aging Lifetime D 5510 Practice for Heat Aging of Oxidatively Degradable
PredictionThis procedure is used to determine the relation- Plastics
ship between aging temperature and predefined level property G 63 Guide for Evaluating Nonmetallic Materials for Oxy-
change, thereby allowing predictions to be made about the gen Service
effect of prolonged service on oxidative degradation. G 72 Test Method for Autogenous Ignition Temperature of
1.5 The values stated in SI units are to be regarded as the Liquids and Solids in a High-Pressure Oxygen-Enriched
standard, however, all numerical values must also be cited in Environment
the systems in which they were actually measured. G 74 Test Method for Ignition Sensitivity of Materials to
Gaseous Fluid Impact

1
These practices are under the jurisdiction of ASTM Committee G04 on
2
Compatibility and Sensitivity of Materials in Oxygen Enriched Atmospheres and is For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the direct responsibility of Subcommittee G04.02 on Recommended Practices. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved June 15, 2006. Published August 2006. Originally Standards volume information, refer to the standards Document Summary page on
approved in 1993. Last previous edition approved in 1998 as G 114 98. the ASTM website.

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G 86 Test Method for Determining Ignition Sensitivity of 3.1.8 natural agingaging that occurs during normal ser-
Materials to Mechanical Impact in Ambient Liquid Oxy- vice which is a function of time after service installation and
gen and Pressurized Liquid and Gaseous Oxygen Environ- other stressors, including temperature, present during service.
ments 3.1.9 physical agingaging that occurs during normal stor-
G 125 Test Method for Measuring Liquid and Solid Mate- age which is a function of time after production.
rial Fire Limits in Gaseous Oxidants
2.2 Federal Standard: 4. Summary of Practice
Federal Specification BB-0-925 Oxygen, Technical, Gas 4.1 This practice can be used to evaluate systematically the
and Liquid3 effect of natural aging (Procedure A) or accelerated aging
2.3 Military Standard: (Procedures B and C) on oxygen resistance. To apply its
MIL-O-27210E Amendment 1Oxygen, Aviators Breath- principle, the user first characterizes the material, then subjects
ing, Liquid and Gas the material to an aging stressor or stressors, followed by
2.4 ISO Standard: re-characterizing the material. Caution must be taken in inter-
ISO 188:1998 Rubber, Vulcanized or Thermoplastic preting results because interactions occurring in service may be
Accelerated Ageing and Heat Resistance Tests different than those simulated during aging.
2.5 DIN Standard: 4.2 It is always more accurate, although not always practi-
DIN 53508 Accelerated Aging of Rubber cal, to determine the effect of natural aging (Procedure A)
without resorting to accelerated aging (Procedures B and C).
3. Terminology Accelerated aging procedures are more useful for determining
3.1 Definitions of Terms Specific to This Standard: material rankings (Procedure B) or for making lifetime predic-
3.1.1 agingthe exposure of a material to stressors includ- tions (Procedure C).
ing time, temperature, pressure, chemical exposure, humidity, 4.3 Summary of Practice for Evaluating the Effect of Aging
abrasion, ionizing radiation, light, impact with gas or particles, in Incident Studies:
mechanical load (static or dynamic), or any other stressor that 4.3.1 In incident studies, in which initial characterization
may be present during service. These stressors may be present data are not available, then historical or average-property data
individually or in combination. may be used to draw coarser conclusions about the effect of
3.1.2 accelerated aginga type of artificial aging whereby aging on oxygen resistance.
the effect of prolonged exposure during service is simulated by 4.4 Practices for Natural Aging (Procedure A) and Accel-
aging at elevated temperature. erated Aging for Comparative Oxygen Resistance (Procedure
3.1.3 artificial agingaging which is a function of com- B):
bined stressors lying outside the domain of normal storage and 4.4.1 The effect of aging is reported as positive or negative
service domains; or alternatively, aging in which exposure to depending upon whether the property used to evaluate oxygen
temperature is used to produce an effect that simulates that of resistance increases or decreases, and the magnitude of the
time. The degree of artificiality may vary considerably. An effect is reported as the degree to which the measured property
example of mild artificiality might be exposure of a material to changes relative to that of the unaged material.
a greater pressure than it experiences during service. An 4.5 Practice for Accelerated Aging for Lifetime Prediction
example of extreme artificiality would be the use of sand paper (Procedure C):
to increase a materials surface roughness to simulate particle- 4.5.1 The time necessary to produce a predetermined level
impact abrasion that occurs during service. A high degree of of property change is determined at a series of elevated aging
artificiality affects the strength of conclusion that can be drawn, temperatures, and the time necessary to produce the same level
because it may be difficult to relate the results to the use of property changed at some lower temperature is then deter-
condition. Artificial aging is preferred that accelerates natural mined by linear extrapolation.
aging but does not alter the underlying mechanism responsible 4.5.2 A practice for evaluating the effect of accelerated
aging-induced property changes. aging on physical and mechanical properties under conditions
3.1.4 oxidative degradationphysical or mechanical prop- of variable time and temperature has been validated for
erty changes occurring as a result of exposure to oxygen- significance and is described in detail. This practice is similar
containing media. to those given in Practices D 3045 and D 5510, but is specific
3.1.5 oxygen-containing mediaair, oxygen-enriched me- to aging in oxygen-containing media.
dia containing greater than 25 mole % oxygen, or pure oxygen. 4.5.3 A practice for evaluating the effect of accelerated
3.1.6 oxygen resistanceresistance of a material to ignite aging on ignition and combustion properties under conditions
spontaneously, propagate by sustained combustion, or undergo of variable time and temperature has not been validated for
oxidative degradation. significance, but may yield meaningful results. The practice
3.1.7 oxygen serviceapplications involving the produc- described is included to promote research and possible devel-
tion, storage, transportation, distribution, of use of oxygen- opment into an established method.
containing media. 4.5.4 There can be very large errors when accelerated aging
Arrhenius approaches are used to estimate the time necessary
to produce a fixed amount of property change at some lower
3
Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700 temperature. This estimated time to produce a fixed amount of
Robbins Ave., Philadelphia, PA 19111. property change or failure at the lower temperature is often

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called the service life. Because of the errors associated with 5.9 In terms of physical and mechanical properties, aging is
these calculations, this time should be considered to be the expected to have a greater influence on a polymers ultimate
maximum expected rather than typical. properties such as strength and elongation, than bulk properties
such as modulus.
5. Significance and Use 5.10 In terms of fire properties, aging is expected to have a
5.1 This practice allows the user to evaluate the effect of greater influence on a polymers ignition properties (for ex-
service or accelerating aging on the oxygen resistance of ample, autogenous ignition temperature (AIT), mechanical and
polymeric materials used in oxygen service. pneumatic impact) than its propagation properties (for ex-
5.2 The use of this practice presupposes that the properties ample, upward and downward flame propagation). To date, the
used to evaluate the effect of aging can be shown to relate to only background on aging influences is that of the Bundesan-
the intended use of the material, and are also sensitive to the stalt Fr Materialforschung und -Prfung (BAM) which has for
effect of aging. years assessed the effect of aging at elevated pressure and
5.3 Polymers aged in the presence of oxygen-containing temperature on a materials AIT. BAM has used the AIT test
media may undergo many types of reversible and irreversible results to establish maximum constraints on the use of mate-
physical and chemical property change. The severity of the rials at elevated pressure and temperature.4
aging conditions determines the extent and type of changes that
take place. Polymers may not necessarily be degraded by 6. Rationale for Aging Tests
aging, but may be unchanged or improved. For example, aging 6.1 The body of information on the effect of natural aging
may drive off volatile materials, thus raising the ignition on oxygen resistance under conditions of multiple stressors is
temperature without compromising mechanical properties. small, and so, this practice is intended to promote testing
However, aging under prolonged or severe conditions (for towards the goal of developing better practices to evaluate the
example, elevated oxygen concentration) will usually cause a competing effects of multiple stressors.
decrease in mechanical performance, while improving resis- 6.2 The body of information on the effect of accelerated
tance to ignition and combustion. aging on ignition and combustion is small, and so, this practice
5.4 Aging may result in reversible mass increase (phys- is intended to promote testing towards the goal of developing
isorption), irreversible mass increase (chemisorption), plastici- potential practices to evaluate the effect of accelerated aging on
zation, discoloration, loss of volatiles, embrittlement, softening ignition and combustion.
due to sorption of volatiles, cracking, relief of molding
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stresses, increased crystallinity, dimensional change, advance 7. Apparatus


of cure in thermosets and elastomers, chain scissioning, and 7.1 General Considerations:
crosslinking. 7.1.1 The apparatus used for aging can vary widely. When
5.5 After a period of service, a materials properties may be aging in ambient pressure air, gravity-convection ovens or
significantly different than those when new. For example, all forced-ventilation ovens may be used. When aging in pressur-
materials rated for oxygen service should remain resistant to ized oxygen-enriched media or pure oxygen, because of the
ignition and combustion (primary fire risk). Furthermore, all increased risk of ignition or combustion, pressure-rated cell-
materials rated for oxygen service should be resistant to type ovens or oxygen pressure chambers that provide a greater
oxidative degradation, hence retain relevant physical and margin of safety must be used.
mechanical properties during service, because part failure can 7.1.2 This practice focuses on small-scale aging methods
indirectly lead to an unacceptable ignition or combustion risk involving only a few specimens at most. The scale of the aging
(secondary fire risk). procedure can be increased in numerous ways, provided care is
5.6 In cases where aging makes a material more susceptible taken to ensure safety.
to fire or causes significant oxidative degradation, aging tests 7.1.3 A provision shall be made for suspending specimens
may be used to evaluate whether a material will become vertically without touching each other or the sides of the aging
unacceptable during service. In cases where aging makes a chamber. If possible, maintain at least a 5 cm (2 in.) separation
material less susceptible to fire, aging tests may be used to between specimens and the sides of the aging oven, cell, or
evaluate whether a material can be conditioned (artificially chamber.
aged) to prolong its service lifetime. 7.1.4 The temperature, and pressure if different than ambi-
5.7 Oxygen resistance as determined by this practice does ent, should be automatically recorded.
not constitute grounds for material acceptability in oxygen 7.1.5 Temperatures shall be measured in close proximity to
service. Determination of material acceptability must be per- the test piece.
formed within the broader context of review of system or 7.1.6 Uniform heating shall be accomplished by mechanical
component design, plausible ignition mechanisms, ignition agitation or forced circulation whenever possible or practical.
probability, post-ignition material properties, and reaction Baffles or other design features shall be used to insure uniform
effects such as are covered by Guide G 63.
5.8 The potential for personnel injury, facility damage,
product loss, or downtime occurring as a result of ignition, 4
Wegener, W., Binder, C., Hengstenberg, P., Herrmann, K. P., and Weinert, P.,
combustion, or catastrophic equipment failure will be least for Tests to Evaluate the Suitability of Materials for Oxygen Service, Flammability
systems or components using air and greatest for systems or and Sensitivity of Materials in Oxygen-Enriched Atmospheres: Third Volume, ASTM
components using pure oxygen. STP 986, D. W. Schroll, Ed. ASTM, 1988, pp. 268278.

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G 114 06
heating is obtained in all parts of the chamber and to prevent heat transfer medium surrounding the chamber shall be made
local overheating or dead spots. of materials that do not react with oxygen.
7.1.7 In cases where circulated air is used, increasing the air 7.5.1.1 The chamber shall be equipped with a burst disk to
flow rate, will improve temperature uniformity. However, prevent the maximum allowable water pressure (MAWP) for
while low air speed will promote accumulation of degradation the chamber from being exceeded in the case of an extreme
products and volatilized ingredients, as well as oxygen deple- reaction between the test material and oxygen. Additionally, an
tion, high air speed will promote increase the rate of deterio- engineering design safety factor can be used to further reduce
ration due to reduced oxygen depletion and increased volatil- the possibility of catastrophic over-pressurization.
ization of plasticizers and antioxidants. 7.5.1.2 The size of the chamber is optional, but shall be such
7.1.8 Specimen preparation for larger scale experiments or that (1) the total volume of the test specimens does not exceed
unique combinations of stressors that qualify as research may 10 percent of the free space in the chamber, and (2) the
utilize other hardware that allows safe aging. Safety must be maximum expected operating pressure (MEOP) produced by a
carefully evaluated for any aging arrangement. worst case combustion to form completely oxidized gaseous
by-products does not exceed eighty percent of the MAWP for
NOTE 1The effects of aging may be quite variable, especially when
specimens are aged for long intervals. Factors that may affect reproduc- the chamber. For example, in a typical isothermal combustion
ibility of data include temperature uniformity and control within the aging in 100 percent oxygen, and assuming oxygen is the limiting
apparatus and humidity. For example, materials susceptible to hydrolysis reactant (that is, all oxygen originally present is consumed), the
may undergo degradation not directly attributable to the effects of oxygen. MEOP can be estimated as:5
NOTE 2Aging apparatuses must be designed so that specimens, ngas R Tf
especially vulcanized elastomers, do not come in contact with copper or MEOP 5 Vc # 0.8 MAWP (1)
copper-containing alloys, which can accelerate aging.
7.2 Gravity-Convection Air Ovens: where:
7.2.1 Gravity convection ovens are recommended for film ngas = number of moles of gas produced by the combustion
specimens having a nominal thickness not greater than 0.25 (assumes all moles of gas originally present in the
mm (0.010 in.). In order to maintain a constant, evenly aging medium were consumed),
R = ideal gas constant, and
distributed temperature throughout the heating interval, auto-
Vc = pressure chamber volume.
matic temperature control by means of thermostatic regulation
And where Tf is the final temperature inside the chamber
shall be used. Aluminum chamber or cell walls will help
after 100 % combustion as determined by:
maintain temperature consistency. The air shall circulate at no
less than 3 and no more than 10 changes per hour.
7.3 Forced-Ventilation Air Ovens:
Tf 5 T i 1 S DHc msample
Cp mchamber D (2)

7.3.1 Forced ventilation ovens are recommended for speci- where:


mens having a nominal thickness greater than 0.25 mm (0.010 Ti = initial aging temperature,
in.). The source of heat is optional, but shall be located outside DHc = heat of combustion of the test specimen as
the aging chamber proper. The air shall be preheated to the determined under isothermal conditions per
target aging temperature. The air shall circulate at no less than Test Method D 4809,
3 and no more than 10 changes per hour, and the flow shall be mchamber = mass of the combusted specimens,
as laminar and uniform as possible. Specimens shall be placed Cp = heat capacity of the metal or metal alloy used
with the smallest surface facing the air flow so as to avoid to construct the pressure chamber, and
disturbing the air flow. mchamber = mass of pressure chamber.
NOTE 3During forced-ventilation air aging and in cases where a NOTE 4Warning: The pressure chamber shall be constructed of
motor driven fan is used, in order to avoid ozone contamination, the aging materials that are known to be resistant to ignition and combustion in the
media must not come into contact with the fan motor brush discharge. For aging medium used, and at the aging temperatures and pressures used.
this reason, it is not permissible to use motor-driven fans inside the oven. NOTE 5Warning: Precautions must be taken to insure the pressure
chamber is not overloaded, or aging temperatures and pressures used that
7.4 Cell-type Air Ovens: would cause the safety margins for the chamber to be exceeded.
7.4.1 Cell-type ovens shall consist of one or more uncon-
7.5.2 In cases where the effect of aging on ignition or
nected cylindrical cells having a minimum height of 300 mm
combustion properties is being examined, the vessel used to
(12 in.) in which the temperature can be kept constant and the
perform the ignition AIT reaction vessel, mechanical impact
air circulates at no less than 3 and no more than 10 changes per
test chamber, or pneumatic impact test chamber subassembly)
hour. Cells shall be surrounded by the good heat transfer
or combustion test (calorimeter bomb) may also serve as the
medium (aluminum block, liquid bath, or saturated vapor). The
apparatus for the aging step.
air passing through one cell shall not enter into other cells.
7.5.2.1 To examine the effect of aging on the autogenous
Cells are especially useful when aging dissimilar types of
ignition sensitivity, specimens would be placed into the AIT
polymers (see Note 6).
7.5 Pressure Chambers:
7.5.1 Pressure chambers shall consist of a vessel made of
stainless steel or other suitable material. When aging in 5
ASME, 2004, Boiler and Pressure Vessel Code, Section VIII, Division 1, New
oxygen-enriched media or oxygen, both the chamber and the York, New York.

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reaction vessel of Test Method G 72, and aged at the desired However, the form of test article shall be such that negligible
pressure(s) and temperature(s). heating due to machining to remove the softgood of interest
7.5.2.2 To examine the effect of aging on gaseous pneu- will be required after aging and prior to property evaluation.
matic impact ignition sensitivity, specimens would be placed 9.7 The method of specimen fabrication should be the same
into the test chamber subassembly of Test Method G 74, and as that of the intended application.
aged at the desired pressure(s) and temperature(s). 9.8 Use different specimens for physical property tests than
7.5.2.3 To examine the effect of aging on pressurized used for ignition tests, for example. Physical testing may
oxygen mechanical impact ignition sensitivity, specimens prestress, crack, or otherwise change the specimens in ways
would be placed into the test chamber of Test Method G 86, that would not occur in actual service, and therefore may bias
and aged at the desired pressure(s) and temperature(s). ignition test results.

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7.5.2.4 To examine the effect of aging on heat of combus- 9.9 Whenever possible, marking (such as application of
tion, specimens would be placed into the calorimeter bomb gage lines used for measuring elongation) shall be carried out
Test Method D 4809, and aged at the desired pressure(s) and after aging as inks can affect aging.
temperature(s). 9.10 Use the same cleaning methods as used in service.
7.6 Specimen Rack, of suitable design to allow ready Lubricants that would be used with the material should be
circulation around the specimens during aging. applied in similar amounts. If the material is used in intimate
7.7 Test Equipment, in accordance with appropriate ASTM contact with other materials, then it is preferable to age the
procedures to determine the selected property or properties. material in contact with these same materials.
8. Reagents NOTE 6If possible, it is recommended that only the following types of
polymers be aged together:
8.1 Gaseous OxygenConforming to MIL-O-27210E, (a) polymers of the same general type
Amendment 1, Type 2, Federal Specification BB-0-925, Type 1 (b) elastomers with similar amounts of sulfur
or oxygen of 99.5 % minimum purity is used. Oxygen of other (c) elastomers with similar sulfur:accelerant ratios
purities or in mixture with other materials may be necessary (d) polymers with similar types and loading of accelerants, antioxidants,
depending upon the intent of the study. peroxides, and plasticizers
8.2 GasesDiluent gases used to prepare atmospheres 10. Safety Precautions
other than pure oxygen should have a purity at least equal to
that specified for the oxygen. 10.1 Oxygen:
NOTE 7Warning: Gaseous oxygen vigorously accelerates combus-
9. Test Specimens, Test Articles, and Sampling tion. Adequate safety precautions are important when heating organic
9.1 The number and type of specimens required shall be in materials in oxygen under pressure, since the rate of oxidation may, in
accordance with the ASTM test method for the specific some cases, become very rapid, particularly if a large surface area of
material is aged.
property being determined. For example, for evaluation of the
Keep oil and grease away. Do not use oil or grease on regulators, gages
effect of oxygen aging on tensile properties, dumbbell-shaped or control equipment.
specimens prepared in accordance with Test Method D 412 Use only with equipment conditioned for oxygen service by carefully
shall be considered standard for elastomers. For plastics and cleaning to remove oil, grease and other combustibles.
thermosets, Type IV dogbones prepared in accordance with Keep combustibles away from oxygen and eliminate ignition sources.
Test Method D 638 shall be considered standard, or if limited Keep surfaces clean to prevent ignition or explosion, or both, on contact
amounts of material are available, microtensile specimens with oxygen.
Always use a pressure regulator. Release regulator tension before
prepared in accordance with Test Method D 1708 shall be
opening cylinder valve.
considered standard. All equipment and containers used must be suitable and recommended
9.2 The form of test specimens shall be such that no for oxygen service.
mechanical, chemical, or heat treatment will be required after Never attempt to transfer oxygen from cylinder in which it is received
aging. to any other cylinder.
9.3 Aging shall be carried out on materials conditioned Do not drop cylinder. Make sure cylinder is secured at all times.
accordance with the ASTM test for the specific property to be Keep cylinder valve closed when not in use.
Stand away from outlet when opening cylinder valve.
determined. Further provisions should be made to insure For technical use only. Do not use for inhalation purposes.
whenever possible that the specimen thickness should be Keep cylinder out of the sun and away from heat.
comparable to but no greater than the minimum thickness in Keep cylinder away from corrosive environment.
the intended application. Test specimens shall also be free of Do not use cylinder without label.
blemishes or other flaws. Do not use dented or damaged cylinders.
9.4 Comparison of results shall be limited to test specimens 10.1.1 See Compressed Gas Association Pamphlets G-4 and
having similar dimensions and having approximately the same G-4.16 for details on the safe use of oxygen.
exposed area. 10.2 Refer to the safety precautions sections of referenced
9.5 Comparison of results shall be limited to test specimens standards for further safety information applicable to the use of
having the comparable cure dates (elastomers and thermosets)
or mold dates (plastics).
9.6 Size permitting, aging of representative hardware or 6
Available from Compressed Gas Association, 1235 Jefferson Davis Highway,
components containing the softgood of interest is preferred. Arlington, VA.

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each standard and therefore applicable to this practice when 12.1.8 To do related mechanical property tests, it may be
used in conjunction with it. preferable to do them on different specimens than used for
ignition or combustion tests, since the mechanical testing may
11. Testing of Unaged Specimens abrade disrupt, crack or otherwise change the specimens in
11.1 To minimize repeatability errors, it is recommended ways that would not occur in actual service, thus altering
that properties of the unaged sample be determined within 96 results.
h of the start of the aging interval. Results on specimens which 12.2 Choosing Aging Conditions:
are found to be imperfect shall be discarded and retests shall be 12.2.1 The user must first identify the stressors most likely
made. to contribute to aging of the material (for example, time,
11.2 The material should be in the exact condition for use temperature, pressure, erosion due to flow friction, or chemical
prior to aging. Any cleaning should be consistent with cleaning exposure), and the test method that is most likely to measure
required for the application of interest. the property change.
11.3 Test the material as specified in the test method(s) 12.2.2 TimeTime may be the most elemental aging factor.
chosen: Test Methods D 395, D 412, D 638, D 1708, D 2240, Time alone may age a material (for example, physical aging of
D 2512, D 4809, G 72, G 74, G 86, G 125, or other. If time is elastomers and glassy polymers). It is always more accurate,
suspected to be a key aging parameter, retain some of the although not always practical, to determine the effect time
material in its original condition for later testing in concert with without resorting to accelerated aging. The effect of natural
the aged material. aging can be determined by testing materials that have been in
11.4 If desired, and to increase the data base obtained, the service or in storage and comparing results with data obtained
material may be further characterized prior to aging by on new material. Time may affect any properties, and hence
weighing it, recording dimensions, or checking other mechani- characterization by any of the test procedures described herein
cal properties related to application (Charpy or Izod mechani- may be worthwhile.
cal impact strength, tear resistance, flexibility, etc.).
12.2.3 TemperatureFor materials used in elevated tem-
12. Aging Procedures perature service, aging at the same elevated temperature will
12.1 General Considerations: simulate natural aging. In this case, the effect of temperature is
12.1.1 To evaluate accurately the effect of aging on oxygen determined directly. For materials used in ambient temperature
resistance, the property being evaluated must be relevant to the service, exposure to elevated temperatures will simulate accel-
service application. erated aging. In this case, an Arrhenius method is used to
12.1.2 Use a sufficient number of replicates of each material convert the effect of temperature to that of time, thereby
for each aging condition so that results can be compared by allowing predictions to be made about the effect of time
analysis of variance or similar statistical data analysis proce- (prolonged service) on a given property. Aging at elevated
dure. temperature often leads to an increased AIT as determined by
12.1.3 Use aging temperatures and times such that the Test Method G 72. Oxidation caused by chemisorption of
deterioration will not be so great as to prevent determination of oxygen may cause a decrease in the heat of combustion as
final properties. determined by Test Method D 4809, or may increase the
12.1.4 The minimum interval between curing (elastomers, oxygen index, see Test Method G 125. Aging may lead to a
thermosets) or molding (plastics) and the start of aging shall be cracking, loss of resiliency, and other physical and mechanical
24 h. property loss, see Test Methods D 395, D 412, D 638, D 1708,
12.1.5 The maximum interval between curing or molding D 2240. Aging may also lead to an increase in specific surface
and the start of aging shall also be controlled so that compari- area; that can produce easily ignitable edges, hence ambient
son of results is limited to materials with similar production temperature mechanical impact ignition tests per Test Method
dates. It is especially important to maintain a consistent D 2512 or Test Method G 86, or pneumatic impact ignition
production dateaging date interval when comparing like tests per Test Method G 74 may be worthwhile. If specific
materials, or when dealing with materials that are known to information about the effect of temperature up to 280C
undergo significant physical aging. If the production date of a (540F) on impact ignition properties is desired, heated gas-
material is unknown, aging shall begin within two months of eous oxygen mechanical impact ignition tests per Test Method
delivery to the customer. G 74, or heated gaseous oxygen pneumatic impact ignition
12.1.6 When conducting aging at a single temperature, it is tests per Test Method G 86 may be worthwhile.
usually desirable at age all materials at the same time in the NOTE 8Caution: For every 10C increase in temperature, the oxida-
same apparatus as long as mixing of polymers of dissimilar tion rate may be approximately double. When testing rapidly aging
type (see Note 6) can be avoided. materials, or materials containing or contaminated with oxidizing chemi-
12.1.7 Aging is most meaningful if done at conditions cals, or during aging of materials with a large surface area, the oxidation
replicating those of service. In this case, use the same cleaning rate may be catalyzed to such as extent as to become violent with
increasing temperature.
methods as intended for service. Lubricants that would be used
with the material should be applied in similar amounts. If the 12.2.4 PressurePressure may cause physisorption of oxy-
material is used in intimate contact with other materials, then it gen, which in the case of elastomers may cause swelling, and
is preferable to age the material in contact with these same in the case of rapid pressure cycling, fatigue and mechanical
materials. failure. Therefore, tests to ascertain dimensional changes and
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mechanical property retention may be of interest. Also, vari- neglected or accounted for, the effect of natural aging can also be
able pressure AIT tests run from 2.1 to 20.7 MPa (300 to 3000 estimated by testing materials removed from service and comparing
psi) per Test Method G 72, variable pressure gaseous oxygen results with data obtained on new material.
mechanical impact ignition tests run at 0 to 68.9 MPa (0 to 12.3.2 During natural aging, all aging conditions must
10 000 psi) per Test Method G 86, or pressurized gaseous approximate service conditions, for example, time, tempera-
oxygen pneumatic impact ignition tests run at 0 to 68.9 MPa (0 ture, pressure, loading, friction/erosion, and chemical expo-
to 10 000 psi) per Test Method G 74 may be worthwhile. sure.
NOTE 9Depending on component design and application, the ignition 12.3.3 Subject the material to the selected stressor(s). For
probability due to adiabatic compression may be greater than the ignition example, to effect time/pressure/temperature aging, place the
probability due to autogenous ignition. In such cases, pneumatic impact material in the pressure chamber, pressurize it as specified in
(adiabatic compression) ignition tests per Test Method G 74 may be more
Test Method G 72, raise the temperature to the level of interest,
appropriate than AIT tests per Test Method G 72.
NOTE 10If oxygen pressure or concentration is low during aging, and and allow it to soak for the chosen time. By using elements of
oxidation is rapid, oxygen may not diffuse into the specimen fast enough Test Method G 72 for this procedure, the safety measures of
to allow uniform oxidation. Conversely, higher oxygen pressure or Test Method G 72 and the historical experience adds confi-
concentration will promote rapid diffusion and more uniform oxidation. dence in the margin of safety present, provided the amount of
Care, however, must be exercised to insure the oxidation rates achieved material involved is not in excess of the amount the vessel of
during aging closely resemble the rates occurring in service.
Test Method G 72 is capable of containing in an inadvertent
12.2.5 LoadingThe effects of oxygen exposure may be ignition.
exacerbated by dynamic and static loading effects occurring 12.3.4 Specimens are placed in the aging apparatus only
during service. However duplication of these effects during test after it has been preheated to operating temperature. The aging
can be a challenge. In general, constructing mock fixtures, or interval starts when the specimens are placed in the aging
testing partially dissembled or intact components may be apparatus.
necessary.
12.2.6 Friction/ErosionFriction erosion tends to increase 12.4 Procedure B: Accelerated Aging for Comparative Oxy-
the specific surface area of smooth surfaces and decrease the gen Resistance:
specific surface area of rough surfaces. Increased surface area 12.4.1 This procedure is used to evaluate the relative
suggests AIT tests per Test Method G 72, or gaseous oxygen oxygen resistance of different materials and develop oxygen
mechanical impact ignition tests per Test Method D 2512 or compatibility rankings on a laboratory comparison basis.
Test Method G 86, or pneumatic impact ignition tests per Test 12.4.2 The procedure is suitable for evaluating materials
Method G 74, since increased surface roughness is currently that are used in ambient temperature service, or at a tempera-
thought to increase ignition sensitivity. Conversely, to the ture that is otherwise lower than the aging temperature. The
extent that surface erosion does not affect the bulk specimen or aging temperature may be any elevated standard temperature
bulk properties, the user would not expect to see great changes such as are given in Practice D 1349.
in the heat of combustion as determined by Test Method 12.4.3 The aging interval will depend on the rate of dete-
D 4809, or tensile strength as determined by Test Methods rioration of the particular material being tested. Intervals
D 412, D 638, or D 1708. frequently used are 3, 7, and 14 days.
12.2.7 Chemical ExposureIn addition to oxygen, aggres-
12.4.4 Unless otherwise indicated, the pressure of the aging
sive chemical media encountered during service (for example,
apparatus prior to heating will be 1 atmosphere (14.7 psi, 101
solvents and cleaning agents) can also cause aging. Aggressive
kPa).
chemical media may extract additives, can permeate into the
material, can attack the surface, can alter the specific surface 12.4.5 Specimens are placed in the aging apparatus only
area, can passivate the surface, or change a materials mechani- after it has been preheated to operating temperature. The aging
cal properties, turning it hard, gummy or otherwise. Surface interval starts when the specimens are placed in the aging
properties may be affected preferentially compared to bulk apparatus.
properties, and changes can either be reversible or irreversible. 12.5 Procedure C: Accelerated Aging for Lifetime Predic-
The wide assortment of prospects suggests that many of the test tion:
procedures described herein may be worthwhile. 12.5.1 When using this procedure, all aging conditions used
12.3 Procedure A: Natural Aging: must approximate service conditions, except for time, tempera-
12.3.1 This procedure is used to simulate the effect(s) of one ture, and pressure. For example, aging times and temperatures
or more service stressors on a materials oxygen resistance, and will be selected from Table 1 of Practice D 3045. Unless
is suitable for evaluating materials that experience continuous otherwise indicated, the pressure of the aging apparatus prior to
or intermittent exposure to elevated temperature during ser- heating will be 1 atmosphere (14.7 psi, 101 kPa).
vice. 12.5.2 This procedure is used to determine the relationship
NOTE 11As long as the properties of interest can be shown to be between aging temperature and predefined level property
invariant from lot to lot, and time-dependent physical aging can be change. When using this procedure, a minimum of four aging

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temperatures shall be used. When possible, follow the proce- P = percentage change in property,
dures given in Practice D 3045, Table 1 when selecting aging O = original value, and
times and temperatures (follow Schedules A, B, C, and D), A = value after aging.
namely: 13.1.2 For properties like hardness, the aging results shall
12.5.2.1 The lowest temperature (Schedule A) should pro- be expressed as an absolute change:
duce the desired level of property change or product failure in P5AO (4)
approximately nine to twelve months. The next highest tem-
perature (Schedule B) should produce the same level of 13.2 Procedure C: Accelerated Aging Lifetime Prediction:

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property change or product failure in approximately six 13.2.1 When materials are compared at a single tempera-
months. ture, use analysis of variance to compare the mean of the
measured property data for each material at each aging
NOTE 12The lowest temperature (Schedule A) is typically 15 to 25C
interval. Use the results from each replicate of each material
above the maximum expected service temperature, or alternatively, the
estimated limiting temperature as described in Practice D 3045. being compared for analysis of the variance. It is recommended
that the F statistic for 95 % confidence be used to determine
12.5.2.2 The third and fourth temperatures (Schedules C significance for the results from the analysis of variance
and D) should produce the same level of property change or calculations.
product failure in approximately three months and one month, 13.2.2 When materials are being compared using a series of
respectively. temperatures, use the following procedure to analyze the data
NOTE 13The use of high aging temperatures during accelerated aging and to estimate the aging time needed to produce a predeter-
may result in different degradation mechanisms than those occurring mined level of property change at some temperature lower than
during service, thus invalidating results. Also, avoid aging at known the actual test temperatures. This time can be used for general
transition temperatures since aging rates may change significantly.
ranking of material in terms of oxygen age resistance, or as an
12.5.3 The maximum expected service temperature or esti- estimate of the upper service limit at the temperature selected.
mated limiting temperature may be based on prior knowledge 13.2.3 Prepare plots of the measured property as a function
of similar material, and may subsequently amended on the of the aging interval for all the temperatures used. Plots should
basis of data acquired using Procedure B. be prepared in accordance with Figure 1 of Practice D 3045
12.5.4 It is often difficult to estimate the effect of acceler- (reproduced) where the x-axis is the logarithm of the aging
ated aging before obtaining test data. Therefore, it is usually time and the y-axis is the value of the measured property.
necessary to start only the short-term data at one or two 13.2.4 Use nonlinear regression analysis to determine the
temperatures (Schedules C and D) until data are obtained that relationship between the logarithm of the aging time and the
can be used as a basis for selecting the remaining aging measured property. Based on the nonlinear regression analysis
temperatures. results, determine the aging time necessary to produce a
NOTE 14Lifetime prediction studies have shown that because of predetermined level of property change. An acceptable regres-
diffusion limited (heterogeneous) oxidation, bulk properties such as sion equation must have an r2 of at least 80 %. A plot of
strength may not be amenable to Arrhenius approaches, while surface residuals (value of property retention predicted by regression
sensitive properties such as elongation are. equation minus actual value) versus aging time must show a
12.6 Re-characterizing the Aged Material: random distribution. The use of graphical interpretation to
12.6.1 At the end of the aging interval, remove the speci- estimate the exposure time necessary to produce the predeter-
mens from the aging apparatus, cool to room temperature, and mined level of property change is not recommended.
allow them to rest not less than 16 h nor more than 96 h before 13.2.5 Plot the logarithm of the calculated aging time to
determination of physical, mechanical, ignition, or combustion produce the predetermined level of property change as a
properties selected in 11.3. For specimens to be used in tensile function of the reciprocal temperature (1/T in K) for each aging
elongation tests, apply gage lines at this point. temperature used in accordance with Fig. 2 (Arrhenius plot) of
12.6.2 Following return to normal (or other chosen) condi- Practice D 3045 (reproduced). Use linear least squares regres-
tions perform the same characterization tests of Section 11. For sion analysis to determine the log time/reciprocal temperature
example, if the selected method is Test Method G 72 (AIT), relationship:
begin the temperature ramp immediately after the aging soak at Ea
temperature is complete. log t 5 log to RT (5)

An acceptable regression analysis must meet the require-


13. Calculation
ments described in 13.2.4.
13.1 Procedure A: Natural Aging, and Procedure B: Accel- 13.2.6 Using the values for log to and Ea/R determined in
erated Aging Comparative Oxygen Resistance: 13.2.5, calculate the time, t, to produce the predetermined level
13.1.1 For properties such as tensile strength and ultimate of property change at the temperature of interest, T, for
elongation, or tensile stress, the aging results shall be expressed example room temperature or another agreed-upon tempera-
as a percentage change for the given property: ture.
P 5 @~A O! / O# 3 100 (3) 13.2.7 Calculate the 95 % confidence interval for the time to
produce the defined property change using the standard error
where: from the regression analysis performed in 13.2.5. This 95 %

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FIG. 1 Heat Aging CurvesProperty Retention versus Aging Time

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FIG. 2 Arrhenius PlotTime of 50 % Property Retention versus Reciprocal of Absolute Temperature

confidence interval can be determined by taking the calculated 14.1.10.1 Plots analogous to Figs. 1 and 2,
time 6 (2 3 standard error for the estimated time). 14.1.10.2 Nonlinear regression equations to determine the
relationship between the logarithm of the aging time and the
14. Report
measured property for each aging temperature used,
14.1 In reporting the aging process, include the following 14.1.10.3 The linear regression (Arrhenius) equation used
data: for predicting the time to produce a predetermined level of
14.1.1 Type of material, manufacturer, composition, and property change as a function of reciprocal temperature,
batch/lot number, if known,
14.1.10.4 Estimated time to produce a predetermined level
14.1.2 Material preparation and cure and molding informa-
of property change at a selected temperature,
tion, if known,
14.1.10.5 95 % confidence intervals for times to produce a
14.1.3 Sample dimensions and condition,
predetermined level of property change, and
14.1.4 Observations of any visible changes,
14.1.5 Type of aging apparatus used, 14.1.10.6 The level of property change used in all calcula-
14.1.6 Aging temperature(s) used, and aging times at each tions.
aging temperature, 14.2 In reporting the change in flammability properties, use
14.1.7 Pre-aged and post-aged physical, ignition, and com- the following formats to cite the aging influence:
bustion properties and the percent change, 14.2.1 For use of Test Method G 72, the change in the AIT
14.1.8 Cross references to any original-or final condition should be reported, and a decrease in AIT shall be called a
flammability test reports that may be available, and degradation, an increase is called an enhancement.
14.1.9 Other applicable aging parameters: pressure, abra- 14.2.2 For use of Test Method G 74, the change in reactive
sion, chemical exposure, friction, etc. pressure should be reported, and a decrease in reactive pressure
14.1.10 When a series of temperatures are used to age should be called a degradation, an increase an enhancement.
materials the following shall be reported for each material 14.2.3 For use of Test Method G 86, the change in reactive
tested: threshold energy should be reported and a decrease in threshold

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should be called a degradation, and an increase should be 15.2 BiasThe procedure in this practice has no bias
called an enhancement. because the test conditions are defined only in terms of this
14.2.4 For use of Test Method G 125, the change in oxygen practice.
index should be reported and a decrease should be called a
degradation, and an increase should be called an enhancement. 16. Keywords
14.2.5 For use of Test Method D 4809, the change in heat of
combustion should be reported and an increase should be 16.1 aging; accelerated aging; combustion; enriched air;
called a degradation and a decrease should be called an flammability; ignition; lifetime prediction; natural aging; oxi-
enhancement. dative degradation; oxygen; oxygen compatibility

15. Precision and Bias


15.1 PrecisionIt is not practical to specify the precision of
this practice since the result will depend on the conditions
selected and the test method(s) chosen for evaluation.

ANNEX
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(Mandatory Information)

A1. EXAMPLE PROCEDURE FOR TIME/PRESSURE AGING

A1.1 Prepare specimens in as-used cleanliness. degradation is no longer observed, and the material should be
reported as having a degradation threshold equal to the highest
A1.2 Weigh, and examine specimens for appearance flex- temperature tested at which degradation did not occur.
ibility.
A1.5 At the end of the aging cycle, the vessel should be
A1.3 Test the specimens using Test Method G 72. vented, cooled, and the specimens should again be examined
for qualitative changes in appearance, flexibility, etc.
A1.4 Place in vessel of Test Method G 72, pressurize,
warm, and soak for 100 h, using the procedures and safety A1.6 Re-test the specimens in the aged condition.
precautions of Test Method G 72.
A1.7 Report the difference, in weight, physical changes,
A1.4.1 The initial soak temperature should be selected as and alteration of AIT.
100C below the autoignition temperature. If testing demon-
strates material degradation, then the test should be repeated at A1.8 This example procedure is based upon the method
progressively lower temperatures in increments of 25C until used at BAM.

APPENDIX

(Nonmandatory Information)

X1. ADDITIONAL LITERATURE

X1.1 Waller, J. M., Hornung, S. D., and Beeson, H. D., Sensitivity of Materials in Oxygen-Enriched Atmospheres,
Fuel Cell Elastomeric Materials Oxygen Compatibility Test- ASTM STP 1319, 1997.
ing: Effect of 450 and 6200 kPa Oxygen, Flammability and

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