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Astm D5229 - 2020
Astm D5229 - 2020
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5229/D5229M − 20
INTRODUCTION
Consistent evaluation and comparison of the response of polymer matrix composites to moisture
absorption can only be performed when the material has been brought to a uniform through-the-
thickness moisture profile. The procedures described in Test Method D570 and Practice D618 do not
guarantee moisture equilibrium of the material. A similar, but more rigorous, procedure for
conditioning to equilibrium is described by this test method, which can also be used with fluid
moisture other than water, and which, additionally, can provide the moisture absorption properties
necessary for the analysis of single-phase Fickian moisture diffusion within such materials.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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1.6.1 Within the text, the inch-pound units are shown in to analytical dimensions when used within square brackets, as
brackets. the symbols may have other definitions when used without the
1.7 This standard does not purport to address all of the brackets.
safety concerns, if any, associated with its use. It is the 3.2.2 accuracy criterion, n—the maximum amount of
responsibility of the user of this standard to establish appro- change in average moisture content for a test coupon, over the
priate safety, health, and environmental practices and deter- span of the reference time period, which is allowable for the
mine the applicability of regulatory limitations prior to use. establishment of effective moisture equilibrium. (See also
1.8 This international standard was developed in accor- average moisture content, moisture equilibrium, and reference
dance with internationally recognized principles on standard- time period.)
ization established in the Decision on Principles for the 3.2.3 average moisture content, M (%), n—the average
Development of International Standards, Guides and Recom- amount of absorbed moisture in a material, taken as the ratio of
mendations issued by the World Trade Organization Technical the mass of the moisture in the material to the mass of the
Barriers to Trade (TBT) Committee. oven-dry material and expressed as a percentage, as follows:
2. Referenced Documents Wi 2 Wo
M, % 5 3 100 (1)
2.1 ASTM Standards:3 Wo
D570 Test Method for Water Absorption of Plastics
where:
D618 Practice for Conditioning Plastics for Testing
D792 Test Methods for Density and Specific Gravity (Rela- Wi = current specimen mass, g, and
tive Density) of Plastics by Displacement Wo = oven-dry specimen mass, g.
D883 Terminology Relating to Plastics (See also oven-dry.)
D2344/D2344M Test Method for Short-Beam Strength of 3.2.4 Fickian diffusion, n—a model of material moisture
Polymer Matrix Composite Materials and Their Laminates absorption and desorption that follows Fick’s second law, as
D2584 Test Method for Ignition Loss of Cured Reinforced follows in one-dimension:
Resins
D2734 Test Methods for Void Content of Reinforced Plastics
]c ] 2c
D3171 Test Methods for Constituent Content of Composite 5 Dz 2
]t ]z
Materials
D3878 Terminology for Composite Materials 3.2.5 glass transition temperature, Tg[Θ], n—the approxi-
E691 Practice for Conducting an Interlaboratory Study to mate midpoint of the temperature range over which a reversible
Determine the Precision of a Test Method change takes place between a viscous or rubbery condition and
a hard, relatively brittle condition, in an amorphous polymer, or
2.2 Military Standard:4 in amorphous regions of a partially crystalline polymer.
MIL-B-131 Barrier Materials, Water Vapor-Proof, Grease- 3.2.5.1 Discussion—The glass transition temperature of
Proof, Flexible, Heat-Sealable many polymer matrix composites is lowered by the presence of
absorbed moisture.
3. Terminology
3.2.6 moisture, n—liquid (water, jet fuel, salt water, or any
3.1 Definitions: other liquid) that is either diffused in relatively small quantity
3.1.1 Terminology D3878 defines terms relating to high- and dispersed through a gas as a vapor, condensed on a surface
modulus fibers and their composites. Terminology D883 de- as visible dew, or present in quantity sufficient for immersion
fines terms relating to plastics. In the event of a conflict of an object.
between terms, Terminology D3878 shall have precedence 3.2.6.1 Discussion—The dictionary definition of moisture
over the other terminology standards. for this test method is extended to include not only the vapor
3.2 Definitions of Terms Specific to This Standard: of a liquid and its condensate, but the liquid itself in large
3.2.1 If the term represents a physical quantity, its analytical quantities, as for immersion.
dimensions are stated immediately following the term (or letter
3.2.7 moisture concentration, c [ML−3], n—the absolute
symbol) in fundamental dimension form, using the following
amount of absorbed moisture in a material expressed as the
ASTM standard symbology for fundamental dimensions,
mass of moisture per unit volume.
shown within square brackets: [M] for mass, [L] for length, [T]
for time, [Θ] for thermodynamic temperature, and [nd] for 3.2.8 moisture diffusivity constant, Dz [L2T−1], n—the prop-
non-dimensional quantities. Use of these symbols is restricted erty of a material that describes the rate at which the material
absorbs or desorbs moisture.
3.2.8.1 Discussion—In Fickian materials, this property is
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or relatively independent of the moisture exposure level (and thus
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM the moisture equilibrium content material property). However,
Standards volume information, refer to the standard’s Document Summary page on the moisture diffusivity constant is strongly influenced by
the ASTM website.
4
Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
temperature. Moisture diffusivity can be anisotropic; the sub-
Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:// script z indicates the value in the through-the-thickness direc-
dodssp.daps.dla.mil. tion for anisotropic diffusion behavior.
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3.2.9 moisture equilibrium, n—the condition reached by a to be a standard laboratory environment) in accordance with
material when there is essentially no further change in its Procedure C of this test method.
average moisture content with the surrounding environment. 3.2.17 standard laboratory atmosphere, n—an atmosphere
3.2.9.1 Discussion—Moisture equilibrium can be either ab- (environment) having a temperature of 23 6 2 °C
solute or effective. Absolute moisture equilibrium requires no [73.4 6 3.6 °F] and a relative humidity of 50 6 10 %.
measurable change in moisture content, while effective mois-
3.2.18 test temperature, n—the environmental temperature
ture equilibrium allows a specified small change in the average
used in Procedures A-E, Y, and Z.
moisture content of a material (the accuracy criterion) over a
3.2.18.1 Discussion—This is distinguished, for the purposes
specified time span (the reference time period). (See also
of this test method, from the environmental temperature used
accuracy criterion, average moisture content, and reference
during any subsequent material evaluation testing.
time period.) Effective moisture equilibrium is a satisfactory
definition for most engineering applications. Unless otherwise 3.2.19 traveler coupon, n—a surrogate coupon of the same
specified, references to moisture equilibrium in this test material and thickness, and of appropriate size (but without
method mean effective moisture equilibrium, as quantified in tabs) that is used in a conditioning procedure to determine
10.2. Moisture equilibrium can also be either static, when there moisture content for specimen configurations (such as a tabbed
is no moisture transport at all across the surfaces, or dynamic, mechanical coupon, or a coupon that does not meet the
when moisture transport exists, but the net sum for the material minimum mass requirement) that cannot otherwise be properly
is zero. This test method is not capable of discerning between measured by this test method.
these two types of moisture equilibrium. 3.3 Symbols:
3.2.10 moisture equilibrium content, Mm (%), n—the maxi- 3.3.1 c—moisture concentration.
mum amount of absorbed moisture that a material can contain 3.3.2 Dz—moisture diffusivity constant in the through-the-
at moisture equilibrium for a given moisture exposure level, thickness direction.
expressed as a percent of dry material mass. (See also moisture
3.3.3 G(T,t)—moisture absorption or desorption function for
saturation content.)
materials that follow Fickian diffusion.
3.2.10.1 Discussion—In polymer matrix composites, this
property is relatively independent of temperature (and thus the 3.3.4 h—thickness of a material panel or plate in the
moisture diffusivity constant material property), but it is a through-the-thickness direction for double-sided moisture ex-
function of the moisture exposure level. For the purposes of posure.
this test method, Mm is assumed to be equivalent to the average 3.3.5 M—average moisture content of a material. The fol-
moisture content at effective moisture equilibrium, Mf. lowing subscripts denote the average moisture content for
3.2.11 moisture exposure level, n—a measure or description specific conditions:
of the severity of a conditioning environment in terms of the Mb, the average moisture content at a baseline time;
amount of liquid or vapor present. (See also moisture and Me, the average moisture content at establishment of effec-
relative vapor level.) tive moisture equilibrium;
Med, the average moisture content at establishment of
3.2.12 moisture saturation content, n—the moisture equilib-
effective moisture equilibrium as a delta from the average
rium content at the maximum possible moisture exposure level,
moisture content at a baseline time;
wherein the material contains the greatest possible amount of
Met, the average moisture content at establishment of effec-
absorbed moisture. (See also moisture equilibrium content.)
tive moisture equilibrium as a total value from the condition of
3.2.13 oven-dry, n—the condition of a material that has been zero moisture content;
dried in accordance with Procedure D of this test method until Mf, the final moisture content at the end of conditioning for
moisture equilibrium is achieved. a fixed time;
3.2.14 reference time period, n—the time interval for mass Mi, the average moisture content at a given time;
measurement used to define effective moisture equilibrium in a Mi − 1, the average moisture content at the previous time;
material. (See also accuracy criterion, average moisture ML, the moisture loss from the state of effective equilibrium
content, and moisture equilibrium.) due to subsequent heating; and
3.2.14.1 Discussion—A small change in the average mois- Mm, the moisture equilibrium content that is reached when a
ture content (the accuracy criterion) for a material during the uniform through-the-thickness moisture profile occurs for a
reference time period indicates effective moisture equilibrium. given temperature and moisture exposure level.
3.2.15 relative vapor level (%), n—the ratio of the pressure 3.3.5.1 Discussion—Procedures A-H of this test method
of a vapor present to the pressure of the saturated vapor, at the condition specimens to Me. Except for the use of a thin
same temperature, expressed as a percent. specimen in Procedure A, conditioning specimens to Mm is
3.2.15.1 Discussion—Applicable only to the gaseous form generally not practical. See also the discussion in Appendix
of a fluid. When the vapor is water vapor, the term is called X2.
relative humidity. (See also moisture exposure level.) 3.3.6 t—time.
3.2.16 standard conditioned specimen, n—the material con- 3.3.7 tm—the maximum time required for a material to reach
dition of a test coupon that has reached effective moisture moisture equilibrium under specified conditions of temperature
equilibrium at a nominal relative humidity of 50 % (considered and initial moisture content.
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3.3.8 Tg—glass transition temperature. 4.3 In Procedure B, a general test coupon (not necessarily
3.3.9 w—the width of a nominally square moisture absorp- the coupon of Procedure A) is maintained, similarly to Proce-
tion test coupon. dure A, in a steady-state environment at specified temperature
and environmental exposure levels until the material reaches
3.3.10 W—the mass of a test coupon. The following sub- effective moisture equilibrium.
scripts are used to denote the mass of a test coupon for specific
conditions: 4.4 In Procedure C, a general test coupon is maintained in a
Wb, the mass at the baseline time; steady-state environment at a specified temperature and a
Wi, the mass at a given time; and relative humidity of 50 % until the material reaches effective
Wi − 1, the mass at the previous time. moisture equilibrium.
3.3.11 z—the coordinate axis in the through-the-thickness 4.5 In Procedure D, a general test coupon is maintained in
direction for a plate or panel. an air-circulating oven at a prescribed elevated temperature
environment until effective moisture equilibrium is reached.
4. Summary of Test Method 4.6 In Procedure E, a general test coupon is conditioned in
two or more sequential non-ambient steady-state environ-
4.1 This is a gravimetric test method that monitors the
ments.
change over time to the average moisture content of a material
specimen by measuring the total mass change of coupons that 4.7 In Procedure Y, a general test coupon is first conditioned
are exposed on two sides to a specified environment. There are to equilibrium using Procedure B, then is exposed to room
a number of test procedures described by this test method. temperature ambient followed by an elevated temperature for
4.1.1 Procedure A covers the determination of the two defined times, then again conditioned to equilibrium.
Fickian moisture diffusion material properties, the moisture 4.8 In Procedure Z, a general test coupon is first conditioned
diffusivity constant and the moisture equilibrium content. The to equilibrium using Procedure B, then is exposed to the same
other procedures cover material conditioning to a specific testing environment (nominal ramp and soak time and an
moisture environment. additional hold time to mimic the test time) as the specimens it
4.1.2 Procedure B covers non-ambient moisture condition- represents.
ing of material coupons at a prescribed constant conditioning
environment prior to other types of testing. Sub-procedure 5. Significance and Use
codes are used to specify the conditioning environment, 5.1 Procedure A is designed to produce moisture diffusion
conditioning time, and mass change monitoring procedure. material property data that may be used as follows:
4.1.3 Procedure C covers the ambient conditioning of ma- 5.1.1 To determine approximate exposure times for coupon
terial coupons to a nominal relative humidity level of 50 %, conditioning in Procedures B-E, Y, and Z;
prior to other types of testing. 5.1.2 As input to moisture prediction analysis computer
4.1.4 Procedure D covers the conditioning (drying) of codes; or
material coupons to an essentially moisture-free condition. 5.1.3 For making qualitative decisions on material selection
4.1.5 Procedure E covers conditioning in two or more or performance under environmental exposure to various forms
sequential steps using Procedure Bxxx. of moisture.
4.1.6 Procedure Y covers the determination of the amount of 5.2 Procedures B-E are designed to condition test coupons
moisture loss in conditioned material coupons when removed to a specified environmental condition or equilibrium state
from the conditioning environment (such as due to heating prior to other material property testing (including, but not
during cure of strain gauges). limited to, mechanical testing).
4.1.7 Procedure Z covers the determination of the amount of
moisture loss in conditioned material coupons due to heating to 5.3 Procedures Y-Z are designed to determine the loss of
the mechanical test temperature and holding at the test tem- moisture content due to removal of a test coupon from the
perature for the duration of the mechanical test. conditioning chamber (such as for strain gauge bonding) or due
to heating of the test coupon prior to and during mechanical
4.2 In Procedure A, the percent moisture mass gain versus loading.
time is monitored for thin material specimen(s) that are
maintained in a steady-state environment at a known tempera- 5.4 A single pair of tests on thin and thick specimens using
ture and moisture exposure level until the material reaches Procedure A provides the moisture diffusivity constant, Dz, and
effective moisture equilibrium, and thick material specimen(s) the moisture equilibrium content, Mm, at the given moisture
that are maintained in a steady-state environment at a known exposure level and temperature. Multiple tests at differing
temperature and moisture exposure level until the material is temperatures are required to establish the dependence of Dz on
conditioned past the point of linear moisture gain. From the temperature. Multiple tests at differing moisture exposure
data obtained from these two specimen thicknesses, the mois- levels are required to establish the dependence of Mm on
ture equilibrium content, Mm, and the one-dimensional mois- moisture exposure level.
NOTE 1—For many polymer matrix composites, the moisture diffusivity
ture absorption rate of the coupon may be determined and the is usually only weakly related to relative humidity and is often assumed to
through-the-thickness moisture diffusivity constant, Dz, calcu- be a function only of temperature, usually following an Arrhenius-type
lated. exponential relation with inverse absolute temperature. For many of these
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materials, moisture equilibrium content is only weakly related to tempera- 6.3.2 Materials with a significant amount of surface crack-
ture and is usually assumed to be a function only of relative humidity (1). ing;
5.5 Vapor-exposure testing shall be used to condition the 6.3.3 Material systems that have been shown to behave in a
specimen when the in-service environmental condition is a non-Fickian manner, or that have multi-phase moisture diffu-
vapor such as humid air. Immersion in a liquid bath should be sion mechanisms as discussed by Bonniau and Bunsell (5);
used to simulate vapor exposure only when apparent absorp- 6.3.4 Material systems that are known to have a moisture
tion properties are desired for qualitative purposes. Properties diffusivity constant that is strongly dependent upon moisture
determined in the latter manner shall be reported as apparent concentration;
properties.
6.3.5 Material systems that are known to have a moisture
NOTE 2—For many polymer matrix composites, the moisture absorp- diffusivity constant that is significantly time-dependent;
tion properties under atmospheric humid conditions are generally not
equivalent to exposure either to liquid immersion or to pressurized steam. 6.3.6 Material systems that are known to have a moisture
These latter environments may have different material diffusion charac- diffusivity constant that is significantly stress-dependent, and
teristics. that are used in a laminate containing significant amounts of
residual stress;
6. Interferences 6.3.7 Material systems containing an abnormal amount of
6.1 The calculation of the through-the-thickness moisture voids (porosity), or with a non-uniform void distribution, as
diffusivity constant in Procedure A assumes a single-phase discussed by Harper et al. (6). Moisture (in liquid or gaseous
Fickian material that possesses constant moisture diffusivity form) can fill the voids, resulting in an incorrect measurement
properties through the thickness of the specimen. The validity of the amount of moisture absorbed into the material, and can
of Procedure A for evaluating the moisture diffusivity constant result in removal of specimens from the conditioning environ-
in a material of previously unknown moisture absorption ment at a premature time;
behavior will be uncertain prior to the test, as the test results 6.3.8 Test apparatus that produces a significant temperature
themselves determine whether the material follows the single- gradient in the specimen, either through-the-thickness or in-
phase Fickian diffusion model. As discussed by Shirrell (2), plane, as the material moisture diffusion constant is generally a
previous investigators have shown that for diffusion to be strong function of temperature;
rigorously classified as Fickian, it must satisfy the following 6.3.9 Testing above the glass transition temperature of any
three conditions: constituent or phase-component within the composite material,
6.1.1 Both absorption and desorption curves must be essen- which generally results in non-Fickian or multiphase moisture
tially linear up to 60 % of Mm;
diffusion behavior, or both;
6.1.2 Beyond the initially linear portion, both absorption
and desorption curves must be concave to the abscissa axis 6.3.10 Materials that lose mass during moisture condition-
until Mm is reached; and ing (for example, materials that have water or fluid soluble
6.1.3 For the same environmental exposures, absorption components); or
curves resulting from different specimen thicknesses of the 6.3.11 Materials that advance their cure state during expo-
same material must be essentially super-imposable if each sure to water or water vapor (for example, some phenolic
curve is plotted in the form of a normalized sorption curve in resins).
which the abscissa is ~ =time! ⁄h, instead of =time. 6.4 For materials with a very high moisture diffusion rate, a
6.2 These conditions are rigorous, and may not be fully met low moisture equilibrium content, or both, the time scales
by many engineering materials. In fact, these conditions may required for periodic weighings may be very short (on the order
be difficult to experimentally verify for certain materials, and of minutes or hours), and extreme care must be taken with the
for this reason, the decision on how rigorously these conditions mass measurements and with the calibration and control of the
must be met for a given test material is left to the user. For environmental chamber, in order to avoid large measurement
example, a severe complete absorption/desorption cycle may errors. The most convenient solution for reducing the test
cause damage to a given material, causing cracking and sensitivity of these materials is to simply increase the thickness
providing a non-Fickian diffusion path, making evaluation of of the test specimen.
these conditions impossible. 6.5 The definition of effective equilibrium allows for a small
6.3 However, there are a number of material forms or test continual increase in moisture absorption at test termination.
conditions that are known to have the potential to violate one Consequently, the moisture content of the conditioned coupons
or more of the assumptions used by this test method, or to may not be truly representative of the effects of long term
potentially cause non-Fickian material behavior. Many of these exposure. Examples of materials that may exhibit significant
issues are discussed by several of the papers in ASTM STP 658 continual moisture uptake after effective equilibrium include
(3) or in the paper by Blikstad et al. (4). They include: those with excessive porosity, concentrated resin pockets, and
6.3.1 Materials with fibers that are distributed in three wrinkled fibers. If prolonged exposure is a concern, condition-
dimensions, and that affect the moisture diffusion mechanism ing to a real world exposure lifetime is recommended, or at
by means such as wicking along the fiber/matrix interface, such least moisture uptake should be interrogated in a timeframe
as: materials stitched through-the-thickness, or some injection- significantly after reaching effective equilibrium, as defined in
molded materials; this standard.
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7. Apparatus For typical specimen geometries, an instrument with an accu-
7.1 Balance—An analytical balance is required that shall be racy of 60.0025 mm [60.0001 in.] is adequate for the thick-
capable of the appropriate accuracy shown in Table 1. ness measurement, while an instrument with an accuracy of
60.025 mm [60.001 in.] is adequate for the width and length
NOTE 3—These accuracy requirements are derived from the definition measurements.
of effective moisture equilibrium (Eq 6) and the specimen mass of 8.2.2,
as discussed in X2.10. 7.5 Desiccator—A clean, dry desiccator in which specimens
7.2 Oven or Vacuum Drying Chamber—An air-circulating being oven-dried shall be brought to laboratory temperature
oven is required that shall be capable of maintaining the following removal of the specimens from the oven.
required temperatures to within 63 °C [65 °F]. A vacuum 7.6 Specimen Bag—A sealable, flexible, moisture-proof bag
drying chamber or a vacuum oven may also be used. (or other suitable sealable container) made of material suitable
7.3 Conditioning Chamber—A conditioning chamber is re- for exposure to specimens that have been removed from the
quired that shall be capable of maintaining the required conditioning chamber for cooling prior to weighing. Bags that
temperature to within 63 °C [65 °F]. The chamber shall be meet the requirements of MIL-B-131 have been found satis-
monitored either on an automated continuous basis or on a factory for use in standard applications.
manual basis at regular intervals. The chamber shall consist of 7.7 Absorbent Cloth—Clean, non-linting absorbent cloth for
either of the following: use in wiping exuded or condensed moisture from test speci-
7.3.1 For Absorption by Vapor Exposure—A temperature mens.
and vapor-level controlled vapor exposure chamber that is
capable of maintaining the required relative vapor level to 7.8 Gloves—Clean, non-linting gloves for use when han-
within 63 %, or dling specimens.
7.3.2 For Absorption by Liquid Immersion—A temperature-
controlled liquid bath. 8. Test Specimen
NOTE 4—While many newer models have solid-state controls, a great 8.1 Sampling of Test Specimens:
many environmental chambers control the chamber humidity via moni- 8.1.1 Procedure A—Test a minimum of one "thin" coupon
toring of “dry-bulb” (actual) and “wet-bulb” (moisture depressed)
temperatures, which are converted to equivalent relative humidity via a and one "thick" coupon. Testing of three (3) replicates of each
table or algorithm supplied by the manufacturer. The ability of these coupon thickness is recommended when sufficient material is
chambers to control relative humidity is dependent on the accuracy of the available.
thermometer readings. Particularly important in these chambers is regular 8.1.2 Procedures B-E—When a group of test specimens of
cleaning of the water reservoir, replacement of the wick, and maintenance
of a proper contact between the wick and the wet-bulb thermometer. the same material and thickness for subsequent material
Chambers that control the dry-bulb temperature and the differential evaluation are to be conditioned at the same time, and periodic
between the dry-bulb and wet-bulb temperatures generally have improved weighing of the specimens is required by the procedure, a
control of chamber relative humidity over those that control the dry-bulb minimum of three (3) specimens or three traveler coupons from
and wet-bulb temperatures. the group shall be weighed. See 8.2.5 for a discussion of when
NOTE 5—Since loss of the water supply to a humidity chamber results
in the conditioning environment changing to a drying condition with often traveler coupons should be used. If the group of test specimens
a significant delay to the desired moisture conditioning, the use of a real are not "dried" prior to moisture conditioning, the initial
time power and water supply monitoring and alarm system for the moisture content, Mb, of the material prior to conditioning may
chamber is recommended. The alarm system should be able to contact be determined by either (a) drying the traveler coupons using
off-site lab personnel in the event of an anomaly. A further recommenda-
tion is to use a system to shut off the chamber heat when a water supply
Procedure D after moisture conditioning has been completed,
or humidity fault is detected. (b) drying using Procedure D an additional three traveler
coupons, or (c) if the material diffusivity constant and effective
7.4 Micrometers and Calipers—A micrometer with a 4 to
moisture equilibrium content are known, by using the proce-
7 mm [0.16 to 0.28 in.] nominal diameter ball interface shall be
dures in Appendix X3.
used to measure the specimen thickness when at least one
surface is irregular (such as the bag-side of a laminate). A NOTE 6—In some cases, the "dry" weight prior to moisture conditioning
micrometer with a 4 to 7 mm [0.16 to 0.28 in.] nominal to equilibrium may not be equal to the "dry" weight when subsequently
diameter ball interface or with a flat anvil interface shall be dried after moisture conditioning (see Section 6), in which case (a) and (b)
above may not be equivalent. If this situation is suspected and determi-
used to measure the specimen thickness when both surfaces are nation of an accurate initial moisture content is required, then tests using
smooth (such as tooled surfaces). A micrometer or caliper, with both approaches are recommended.
a flat anvil interface, shall be used to measure the width and
length of the specimen. The accuracy of the instruments shall 8.1.3 Procedure Y—In cases where specimens are required
be suitable for reading to within 1% of the sample dimensions. to be removed from the conditioning environment prior to
testing (such as the case where elevated temperature testing
requires the use of high temperature cures (190 °C [375 °F])
TABLE 1 Balance Accuracy
for the strain gauge adhesive and the strain gauges are bonded
after moisture conditioning), the loss of moisture during the
Specimen Mass, g Balance Accuracy Requirement, mg
time out of the conditioning environment should be quantified
$5 but <50 0.1
$50 1.0 by a minimum of three (3) "moisture loss" specimens that
represent each material and laminate thickness. Mechanical
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test specimens should be re-conditioned for the re-conditioning A minimum laminate thickness of 10 times the nominal fiber diameter is
time duration determined by the "moisture loss" specimens. recommended.
8.1.4 Procedure Z—The moisture loss during testing at 8.2.4 Specimen Size and Shape For Use With Procedure A:
elevated temperatures should be quantified by a minimum of 8.2.4.1 Thin Specimen—Since the purpose of the "thin" test
three (3) “moisture loss” specimens that represent each: specimen is only for moisture equilibrium content
material, laminate thickness, hot/wet specimen geometry determination, there is no size requirement other than the
(width and length), and test temperature. Separate moisture minimum mass in accordance with 8.2.2.
loss specimens shall be used for fixtured and non-fixtured
8.2.4.2 Thick Specimen—As edge effects must be mini-
specimens with the same dimensions. Moisture loss specimens
mized in materials with anisotropic moisture diffusivity con-
are not required to be tabbed or notched, even if the specimens
stants in order to accurately determine the through-thickness
they represent are tabbed or notched. When simulating tabbed
diffusion constant, the "thick" test specimen shall consist of
specimens, the moisture loss specimens may be gripped using
either 8.2.4.2 (1) or 8.2.4.2 (2) below. The "thick" test speci-
un-bonded, simulated tabs to prevent specimen damage and
men for moisture diffusivity constant determination shall be
mimic heat transfer through tabs into grips.
thick enough such that achieving a moisture content of
8.2 Test Specimen Geometry: approximately 70 % of the moisture equilibrium content for the
8.2.1 Summary—The following requirements are summa- same exposure conditions shall require a minimum of 35 days
rized in Table 2 for ease of reference. of exposure (if less time is required, then a repeat of the test
8.2.2 Specimen Mass Requirement—Specimens (including with a thicker specimen is recommended).
travelers) shall have a mass of at least 5.0 g (see X2.10). (1) A nominally square plate or curved panel with dimen-
Specimen mass affects the balance accuracy requirement es- sions that satisfy the relation:
tablished in 7.1.
8.2.3 Specimen Thickness—The specimen thickness shall
w
not vary by more than 65 % over the surface of the specimen $ 100 (2)
h
and shall comply with 8.2.2 and Eq 2, as applicable.
where:
NOTE 7—No minimum specimen thickness is required. However, the
specimen thickness has a profound effect on the total time required to w = nominal length of one side, mm [in.], and
reach equilibrium, as well as on the reference time period of 10.1.7.1. h = nominal thickness, mm [in.].
Also, when designing a coupon, consideration should be given to the (2) A 100 6 10 mm [4.0 6 0.5 in.] square plate with
macrostructure of the composite material in the through-the-thickness stainless steel foil bonded to the edges such that moisture
direction. If the moisture absorption coupon is substantially thinner than
the material in the end-use form, there should be sufficient number of absorption through the edges is essentially eliminated. When
fibers through the thickness that the absorption properties of the material this specimen is prepared, care shall be taken to weigh the
coupon can be considered equivalent to the absorption properties of the coupon both before and after bonding of the foil in order to
same material in a much thicker form, under the same environmental obtain the mass increase due to the foil and the adhesive. The
conditions. A thin (even one-ply) laminate, if reinforced by a significant
number of fibers that are small in diameter relative to the thickness, could
adhesive used shall be incapable of absorbing sufficient mois-
be acceptable if it met the other specimen geometry requirements of 8.2. ture to affect the results.
However, a substantially thicker multi-ply laminate, reinforced by fibers NOTE 8—A typical "thin" specimen for the carbon/epoxy material
having a diameter on the order of the ply thickness, may not be acceptable. described in X2.2 having dimensions of 1 mm [0.040 in.] thick by 100 mm
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[4 in.] square would have a mass of approximately 18 g. If conditioned at 10.1.1 The procedure to be used (A-Z), the sub-procedure
74 °C [170 °F] and 90 % relative humidity, use of Eq X1.7 (using an codes Bxxx when using Procedure B (listed in Table 3), the
accuracy criteria of 0.02 % and a maximum difference between Mm and Mf
of 0.02 %) predicts that this specimen would reach equilibrium in
sequential Procedure B sub-procedure codes when using Pro-
approximately 57 days. The minimum reference time period used to test cedure E, and whether the specimens shall be dried using
equilibrium is established by 10.1.7.1 as the greater of 0.04 h2/Dz (equal Procedure D prior to moisture conditioning. Procedure B
to 44 h) or 24 h; rounding to a practical even time gives a reference period sub-procedure codes for some common conditioning methods
of 2 days. A typical "thick" specimen for the carbon/epoxy material are listed in Table 4. If Procedure B is specified without a
described in X2.2 may have dimensions of 3.0 mm [0.120 in.] thick by
100 mm [4 in.] square with sealed edges, satisfying 8.2.4.2 (2). If sub-procedure code, then conditioning shall be performed per
conditioned at 74 °C [170 °F] and 90 % relative humidity, use of Eq X1.7 code BHEE.
(using the same criteria) predicts that this specimen would reach 70 % of
NOTE 10—If a drying step is included, whether as an initial step prior
the effective moisture equilibrium in approximately 38 days.
to moisture conditioning, or as part of an oven-dry experiment, care
8.2.5 Specimen Size and Shape For Use With Procedures should be taken to avoid excessively high drying temperatures and high
B-Z—The specimen size and shape requirement for Procedure thermal excursions that may induce thermal cracking, oxidation, or mass
loss, or combinations of the three in the material.
A (8.2.4) is not a requirement for the conditioning procedures
(B-Z) of this test method. The coupon size and shape used in 10.1.2 The density and fiber volume sampling method
Procedures B-Z is normally that required for subsequent (required only for Procedure A), coupon geometry, and test
material evaluation following conditioning, as long as the method (see Note 11 for guidance).
coupon meets the mass and thickness requirements of 8.2.2 and NOTE 11—For many polymer matrix composites, the volume percent
8.2.3. When the coupon is of such type or geometry that the reinforcement can be determined by one of the matrix digestion proce-
moisture change in the material cannot be properly measured dures of Test Methods D3171, or, for certain reinforcement materials such
by weighing the specimen itself, traveler coupon(s) of the as glass and ceramics, by the matrix burn-off technique of Test Method
D2584. Test Methods D2734 describe the limitations and use of the
same material and thickness, and of appropriate size (but calculations required to approximate the void content in the composite.
without tabs, if present) shall be used to determine moisture The void content equations of Test Methods D2734 are applicable to both
equilibrium for the specimens being conditioned. Material Test Methods D2584 and D3171. Test Methods D792 can be used to
evaluation tests that require traveler moisture conditioning determine specific gravity.
coupons include mechanical tests using tabbed coupons, speci- 10.1.3 The moisture absorption specimen sampling method,
mens containing fasteners, specimens with strain gauges, and type, and geometry (and travelers, if required), from 8.1.
test methods using coupons that do not meet the minimum 10.1.4 The balance measurement accuracy, 1.0 mg or
mass requirement for this test method, such as commonly used 0.1 mg, from 7.1.
in thermo-mechanical analysis methods. 10.1.5 Conditioning chamber test temperature (for both the
8.2.6 Preparation—In specimens cut from plates, precau- initial drying step, if required, and for the moisture condition-
tions shall be taken to avoid notches, undercuts, rough or ing step(s)).
uneven surfaces, or delaminations due to inappropriate ma-
NOTE 12—Maximum test temperatures are recommended for all Pro-
chining methods. Final dimensions should be obtained by cedures in Table 5. Keep the test temperature for any material not listed in
water lubricated precision milling or grinding, or both, or the the table at least 25 °C [45 °F] below the wet Tg of the material.
use of a wet diamond saw. The procedure used shall be 10.1.6 Moisture type (water vapor, liquid water, specified
reported. fluid, or specified gas) and moisture exposure level (in terms of
8.2.7 Labeling—Label the specimen coupons so as to be relative humidity for water vapor exposure). For gas exposures,
distinct from each other in a manner that will both be the gas components, concentrations, and the pressure level for
unaffected by the test and not influence the test. The coupon the conditioning chamber.
must be weighed prior to adding the label (see 10.3.5) when
using a marking method that adds mass to the coupon. NOTE 13—CMH-17 Rev G (1) notes that a worst-case aircraft service
water vapor environment is generally considered to be 85 % relative
Examples of various marking methods include coded wire humidity. Two-step accelerated conditioning schemes consisting of 95 to
overwrap and edge marking. 98 % relative humidity exposure for a period of time followed by
additional exposure time at a lower relative humidity level can be used to
NOTE 9—A coded-wire overwrap is a wire, of a material (such as reduce the conditioning time, as long as equilibrium is reached at the final
stainless steel) that is substantially unaffected by the pending environmen- humidity level. Refs (7) and (8) discuss methods of accelerated condi-
tal exposure. The wire is wrapped around the specimen tightly enough to tioning. Also note that exposure to liquid immersion is not generally
prevent loss of the wire, but loosely enough that it does not interfere with equivalent to exposure to an environment of 100 % relative humidity.
the absorption process. The wire is coded by various means, including, but
not limited to, tags, notches, knots, or color.
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TABLE 4 Procedure B Sub-Procedure Codes for Common Conditioning Methods
Procedure Code Conditioning Method
Procedure BHEP Non-ambient moisture conditioning in a humidity chamber at a prescribed constant conditioning
environment to equilibrium; periodic coupon weighing is required. The default conditioning environment
is 70 °C [160 °F], 85 % RH.
Procedure E (BHVP + BHEP) Non-ambient moisture conditioning in a humidity chamber for two prescribed constant conditioning
environment steps; in step one, the conditioning is continued until a specified percentage of equilibrium
is reached, then the step conditioning is continued to equilibrium; periodic coupon weighing is required.
The default conditioning environment is 70 °C [160 °F], 95 % RH for step 1 and 70 °C [160 °F], 85 %
RH for step 2.
Procedure BHEE Non-ambient moisture conditioning in a humidity chamber at a prescribed constant conditioning
environment to equilibrium; periodic coupon weighing is not required. The default conditioning
environment is 70 °C [160 °F], 85 % RH.
Procedure BHFF Non-ambient moisture conditioning in a humidity chamber at a prescribed constant conditioning
environment for a fixed time period; only initial and final weighing are required. The default conditioning
environment is 70 °C [160 °F], 85 % RH.
Procedure BWEP Non-ambient moisture conditioning in a water immersion tank at a prescribed constant temperature to
equilibrium; periodic coupon weighing is required. The default conditioning environment is 70 °C
[160 °F].
Procedure BWFF Non-ambient moisture conditioning in a water immersion tank at a prescribed constant temperature for
a fixed time period; only initial and final weighing are required. The default conditioning environment is
70 °C [160 °F].
Procedure BBFF Non-ambient moisture conditioning in a boiling water immersion tank for a fixed time period; only initial
and final weighing are required.
Procedure BFEP Non-ambient moisture conditioning in a fluid (other than water) immersion tank at a prescribed constant
temperature to equilibrium; periodic coupon weighing is required.
Procedure BFFF Non-ambient moisture conditioning in a fluid (other than water) immersion tank at a prescribed constant
temperature for a fixed time period; only initial and final weighing are required.
Procedure BGFF Non-ambient conditioning in a chamber with a specified gas composition environment for a fixed time
period; only initial and final weighing are required.
TABLE 5 Maximum Recommended Test Temperatures match a reasonable human time schedule for weighing, then a
Polymer Matrix Material Maximum Recommended Test Temperature, °C [°F] more regular time interval may be adopted and the mass
121 °C [250°F] cure epoxies 70 [158] change requirement (less than 0.02 % mass change over the
177 °C [350 °F] cure epoxies 80 [176] reference time period in accordance with 10.2) shall be
Other 25 [45] less than wet Tg
prorated to the adjusted time interval. For example, if a
required reference time period for equilibrium is determined to
be 115 000 s (32 h), the coupons may be weighed at either 24 h
10.1.7 Time interval between weighings. Procedure A re- intervals or 48 h intervals, with the mass change requirement
quires repeated weighings for the determination of the diffu- adjusted from 0.020 % to either 0.015 % (24⁄32 × 0.020) or
sivity constant, which shall be performed within 61 % of the 0.030 % (48⁄32 × 0.020), respectively.
nominal time interval. Procedure BxxP requires periodic 10.1.8 The average moisture content change percentage for
weighings at specified intervals. Procedures BxxE, BxxP, C, D, effective equilibrium if different from the standard value of
Y, and Z require a final set of three weighings spaced apart by 0.020 % in 10.2. If a different value is specified, then the
the reference time period. Procedure BxxF only requires a final coefficient in the first row of Table 2 and Table 6 must be
weighing. recalculated in accordance with X2.4 – X2.7.
10.1.7.1 Determine the reference time period from Table 6. 10.1.9 For Procedure Y, the environmental conditions for
If the moisture diffusivity constant, Dz, is known, or if a the specimen when out of the conditioning chamber (in the
reasonable value for Dz can be assumed from past experience, case of strain gauge bonding, specify the room temperature
previous testing, data from the literature, or similarity to other hold time, elevated temperature cure time, and the strain gauge
known materials, then the minimum length of the reference cure temperature). Also specify one of Procedures Bxxx, C, or
time period shall be established by use of the YES value from E as the preconditioning step.
Table 6. If Dz is unknown, then the NO value from Table 6 10.1.10 For Procedure Z, the ramp time, soak time, test
shall be used. If this required reference time period does not duration time, and the test temperature for the elevated
temperature mechanical property tests. Also specify one of
TABLE 6 Establishing the Reference Time Period Procedures Bxxx, C, or E as the preconditioning step.
Is Dz Known? Reference Time Period 10.2 Definition of Effective Moisture Equilibrium—For the
Yes (0.04 · h2/Dz) seconds purposes of this test method, if not otherwise specified by the
the greater of h or test requestor, a material shall be defined to be in a state of
86 400 seconds (1 day)
where:
effective moisture equilibrium when the average moisture
Dz = through-the-thickness moisture content of the material changes by less than 0.020 % over each
diffusivity constant, mm2/s [in.2/s] of two consecutive reference time period spans, AND exami-
h = thickness, mm [in.]
No 604 000 seconds (7 days) nation of the moisture content versus =time plot supports the
percent change criteria that effective equilibrium is reached
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(see Note 25). This criteria for change in moisture content over dimensions, a measurement to the nearest 0.01 mm [0.0005 in.]
a reference time period can be expressed in several equivalent is adequate. Measure the nominal plate side dimensions to the
ways; four equivalent expressions are shown below: nearest 1.0 mm [0.050 in.] and report these. Report as "dry"
dimensions.
10.4.2 Moisture Absorption:
? M 2 M ? ,0.020 %
i i21 (3)
10.4.2.1 Record the oven-dry “thin” specimen mass as the
or baseline mass, Wbn, for moisture absorption. Record the initial
"thick" specimen mass, Wbk. Place the specimens in the
U W i 2 W b W i21 2 W b
Wb
2
Wb
U
3 100 , 0.020 % (4) conditioning chamber, which has previously reached the speci-
fied steady-state environment.
or 10.4.2.2 At the end of each specified weighing time interval
(if not otherwise specified by the test requestor, the weighing
U W i 2 W b W i21 2 W b
Wb
2
Wb
,0.00020 U (5) time interval shall be 24 h), remove the specimens from the
conditioning chamber, and place the specimens in the specimen
or bag. Close or seal the bag and allow the specimens to come to
U W i 2 W i21
Wb
U
,0.00020 (6)
an acceptable temperature for laboratory handling. Remove
each specimen from the bag (resealing the bag if other
specimens remain within) and wipe the specimen free of
where: surface moisture with an absorbent lint-free towel. Immedi-
M = specimen average moisture content, %, ately weigh each specimen to the required precision. Record
W = specimen mass, g, and the subscripts indicate: each measurement as Wi, along with the corresponding total
i = value at current time, elapsed time and the time interval since the previous weighing,
i−1 = value at previous time, and and return the specimens to either the specimen bag or the
b = value at baseline time.
conditioning chamber. The specimen shall not be out of the
NOTE 14—The above criterion has been found to provide acceptable
conditioning for many polymer composite materials which have moisture conditioning chamber for more than 30 min/weighing and shall
equilibrium values of at least 0.5 %. For materials with lower moisture not be out of the specimen bag for more than 5 min/weighing.
equilibrium values, a tighter moisture content change criteria may be
NOTE 15—Minimizing the specimen time out of the conditioning
necessary, along with more accurate mass measurements, to obtain
chamber, and especially time out of the specimen bag, is critical to getting
accurate and repeatable conditioning.
a smooth and accurate moisture absorption curve. The maximum allow-
10.3 General Instructions: able times of 10.4.2.2 may need to be shortened for some specimen/
10.3.1 Report any inadvertent deviations from the proce- material combinations, particularly early in the moisture absorption test.
dure. 10.4.2.3 Calculate and record the percent mass change at
10.3.2 Shield the balance from air drafts and isolate it from each time interval by Eq 7. For the "thin" specimen, monitor
vibrations that could affect its accuracy. the absorption of moisture until effective moisture equilibrium
10.3.3 Wear clean, non-linting gloves when handling speci- is reached as determined by 10.2 using the reference time
mens. period from 10.1.7.1. Record the last value of percent mass
10.3.4 Expose both surfaces of the specimen to the test change as the moisture equilibrium content, Mm. For the
environment. Specimens shall be individually spaced apart to "thick" specimen, monitor the absorption of moisture until at
provide adequate air or vapor circulation in drying or vapor least 70 % of the effective moisture equilibrium is reached.
exposure environments, and adequate fluid circulation in an NOTE 16—It is recommended to leave the Procedure A specimens in the
immersion bath. conditioning chamber for a significantly longer period of time after
10.3.5 Remember to subtract the mass of any additional reaching the effective moisture equilibrium in order to ensure that the
material such as wire overwrap label or edge sealant from the material moisture absorption follows a single phase Fickian behavior and
that the effective moisture equilibrium value is sufficiently close to the
mass of the specimen at each time interval weighing. actual moisture equilibrium value.
10.4 Procedure A—Moisture Absorption Property Determi- 10.4.2.4 Measure and report, as post-test observations, the
nation: thickness and plate side dimensions again. Report as "condi-
10.4.1 Specimen Preconditioning: tioned" dimensions.
10.4.1.1 Perform Procedure D as a preconditioning step on 10.4.3 Moisture Desorption Following Absorption—If the
the "thin" coupons to be used to determine the moisture material is known to contain, or is suspected to contain, any
equilibrium content. Drying of the "thick" coupons to be used appreciable amount of moisture-soluble ingredients, the “thin”
to determine the moisture diffusivity constant is not required; specimen (following moisture absorption) shall be dried in an
however, if the specimen is suspected to have significant initial oven in accordance with Procedure D to a state of essentially
moisture, then drying is recommended. moisture-free equilibrium. This may also be done using either
10.4.1.2 Perform and report representative material density specimen thickness for evaluation of the moisture desorption
and fiber volume tests. characteristics of the material.
10.4.1.3 Measure the specimen thickness in a minimum of 10.4.3.1 If the post-test oven-dry equilibrium mass is lower
three locations and report the average measurement with an than the preconditioned mass (as established in 10.4.1), the
accuracy of 1 % of the thickness or better. For typical coupon difference shall be considered soluble matter lost during the
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testing process, as calculated by Eq 9. For such materials, the each specimen from the bag (resealing the bag if other
effective moisture equilibrium content shall be calculated by specimens remain within) and wipe the specimen free of
adding the mass of the moisture-soluble matter (Wb − Wp) to surface moisture with an absorbent lint-free towel. Immedi-
the mass of the coupon at establishment of effective moisture ately weigh each specimen to the required precision. Record
equilibrium from 10.4.2.3. This corrected moisture equilibrium each measurement as Wi, along with the corresponding total
mass shall be used in Eq 7 to calculate the percent mass elapsed time and the time interval since the previous weighing,
change, and the resulting value shall be recorded as the and return the specimens to either the specimen bag or the
moisture equilibrium content, Me. conditioning chamber or fluid bath. The specimen shall not be
NOTE 17—If specimen mass loss due to solvent degradation or physical out of the conditioning chamber or fluid bath for more than
handling is detected, then the calculated moisture diffusion properties may 30 min ⁄weighing and shall not be out of the specimen bag for
be in error. more than 5 min ⁄weighing.
10.4.3.2 Measure and report, as post-test observations, the 10.5.5 Mass Change—Calculate and record the percent
thickness and plate side dimensions again. Report as "postcon- mass change at each time interval by Eq 7.
ditioned dry" dimensions. 10.5.6 Conditioning Time—Condition the specimen for the
10.5 Procedure B—Non-Ambient Specimen Conditioning: time period corresponding to one of the following subproce-
10.5.1 Specimen Preconditioning—Not required for sub- dures:
procedures BHxx, BWxx, and BBxx but may be specified. 10.5.6.1 Procedure BxEx—Effective Equilibrium—Monitor
Required for sub-procedures BFxx and BGxx. If specified or the absorption of moisture until effective moisture equilibrium
required, perform Procedure D as a preconditioning step. is reached as determined by 10.2 using the reference time
NOTE 18—If this step is skipped, then the increase in moisture measured
period from 10.1.7.1. Record the last value of percent mass
during conditioning will, in general, not be equal to the effective moisture change as the moisture equilibrium content, Me. A minimum of
equilibrium content, due to the presence of initial moisture. The initial four weighings are necessary to ensure effective moisture
moisture content, Mb, of the material prior to conditioning may be equilibrium; the pretest weighing, and three final weighings.
determined by either (a) drying the traveler coupons using Procedure D However, additional conditioning time and weighings may be
after moisture conditioning has been completed, (b) drying using Proce-
dure D on additional traveler coupons, or (c) if the material diffusivity required to establish effective moisture equilibrium. Previous
constant and effective moisture equilibrium content are known, by using experience (such as a curve showing equilibrium time versus
the procedures in Appendix X3. thickness), or analytical estimation using techniques such as
10.5.2 Initial Weighing—Record the initial specimen mass those described in the Appendixes, together with data obtained
(after any preconditioning) as the baseline mass, Wb. from Procedure A, can provide an approximate total elapsed
10.5.3 Conditioning—Place the specimen in one of the conditioning time and minimize the required number of weigh-
following conditioning environments. ings. Record the last value of percent mass change as the total
10.5.3.1 Procedure BHxx—Humidity Chamber moisture equilibrium content, Met, if the specimens were
Conditioning—Place the specimen in the conditioning preconditioned by drying, or as the delta moisture equilibrium
chamber, which has previously reached the specified steady- content, Med, if the specimens were not preconditioned.
state environment. If the conditioning temperature is not NOTE 19—While similar to Procedure F of Practice D618, this
specified, condition at 70 °C [160 °F]. If the conditioning procedure requires quantified moisture equilibrium instead of the fixed
relative humidity is not specified, condition at 85 % RH. conditioning time period used by Procedure F of Practice D618.
10.5.3.2 Procedure BWxx—Water Immersion
10.5.6.2 Procedure BxFx—Fixed Time—Condition for the
Conditioning—Place the specimen in the water bath, which has
specified fixed time period. Record the value of percent mass
previously reached the specified steady-state temperature. If
change as the final (non-equilibrium) moisture content, Mf.
the conditioning temperature is not specified, condition at
70 °C [160 °F]. 10.5.6.3 Procedure BxVx—Variable Time—Monitor the ab-
10.5.3.3 Procedure BBxx—Boiling Water Immersion sorption of moisture until reaching a specified moisture content
Conditioning—Place the specimen in the water bath, which has level. Record the value of percent mass change as the final
previously reached a steady-state boiling temperature. Record (non-equilibrium) moisture content, Mf.
the temperature of the water. 10.5.7 Conditioning Monitoring—Monitor the specimen
10.5.3.4 Procedure BFxx—Fluid Immersion Conditioning— mass change using one of the following sub-procedures:
Place the specimen in the specified fluid bath, which has 10.5.7.1 Procedure BxxE—Initial + Three Final
previously reached the specified steady-state temperature. Weighings—After conditioning for the specific time or the time
10.5.3.5 Procedure BGxx—Gas Environment anticipated where effective equilibrium is reached, perform
Conditioning—Place the specimen in the chamber with the three weighings of the specimen spaced apart by the reference
specified gas concentration and pressure. time period from 10.1.7.1. This sub-procedure is typically used
10.5.4 Weighing—At the end of each specified weighing with the Equilibrium conditioning time (BxEx) sub-procedure;
time interval, remove the specimens from the conditioning if Effective Equilibrium in accordance with 10.2 is reached,
chamber or fluid bath and place the specimens in the specimen then stop the specimen conditioning; if Effective Equilibrium is
bag. Close or seal the bag and allow the specimens to come to not reached, then continue conditioning and weighing at the
an acceptable temperature for laboratory handling. Remove reference time period intervals.
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10.5.7.2 Procedure BxxF—Initial + Final Weighings— within) and wipe the specimen free of surface moisture with an
Perform a final specimen weighing after the specified condi- absorbent lint-free towel. Immediately weigh the specimen to
tioning time. This sub-procedure is typically used with the the required precision. Record each measurement as Wi, along
Fixed conditioning time (BxFx) sub-procedure. with the corresponding total elapsed time and the time interval
10.5.7.3 Procedure BxxP—Periodic Weighings—Perform since the previous weighing, and return the specimen to either
periodic weighing of the specimen at the specified time interval the specimen bag or the conditioning chamber. The specimen
or reference time period from 10.1.7.1. This sub-procedure is shall not be out of the conditioning chamber for more than
typically used with the Equilibrium or Variable conditioning 30 min ⁄weighing and shall not be out of the specimen bag for
time (BxEx or BxVx) sub-procedures; continue conditioning more than 5 min ⁄weighing.
and weighing at the specified or reference time period intervals 10.6.3 Calculate and record the percent mass change at each
until Effective Equilibrium (BxEx) or the specified moisture time interval by the use of Eq 7. Monitor the specimen mass
content (BxVx) is reached. until effective moisture equilibrium is reached as determined
10.5.8 Specimen Storage After Conditioning: by 10.2. Record the last value of percent mass change as the
10.5.8.1 Procedure BxEx—Effective Equilibrium—Once the moisture equilibrium content, Med. Periodic weighing of the
specimen has reached effective equilibrium, the specimen may specimen is not required. A minimum of four weighings are
remain in the conditioning chamber for a maximum of two necessary to ensure effective moisture equilibrium; the pretest
weeks before testing (or for a maximum time specified by the weighing, and three final weighings. However, additional
test requestor). Weight gain shall continue to be monitored conditioning time and weighings may be required to establish
until the specimen is mechanically tested. Alternately, the effective moisture equilibrium.
specimen may be stored in a sealed MIL-PRF-131 bag for a 10.6.4 Following establishment of moisture equilibrium,
maximum of two weeks before testing (or for a maximum time store the material at the standard laboratory atmosphere until
specified by the test requestor). Unless otherwise specified by required for subsequent material testing.
the test requestor, it is acceptable, but not mandatory, to place NOTE 20—While similar to Procedure A of Practice D618, this
moist cloths in the sealed bags, provided the cloths are not in procedure requires quantified moisture equilibrium instead of the fixed
direct contact with the specimen. conditioning time period used by Procedure A of Practice D618. This
10.5.8.2 Procedure BxFx—Fixed Time—Once the specimen procedure also allows for elevated temperature conditioning to accelerate
has reached the specified conditioning time, the specimen may the process.
remain in the conditioning chamber for a maximum of three 10.7 Procedure D—Oven-Dry Specimen Conditioning:
days before testing (or for a maximum time specified by the 10.7.1 Initially weigh the specimen to the required precision
test requestor). Alternately, the specimen may be stored in a and record this value as the baseline mass, Wb, for oven drying.
sealed MIL-PRF-131 bag for a maximum of two weeks before Heat the oven to the specified drying temperature. Place the
testing (or for a maximum time specified by the test requestor). specimen in the oven, which is located, for the purpose of
Unless otherwise specified by the test requestor, it is humidity control, in a facility that has a standard laboratory
acceptable, but not mandatory, to place moist cloths in the atmosphere.
sealed bags, provided the cloths are not in direct contact with
NOTE 21—A vacuum drying chamber or a vacuum oven may be used in
the specimen. place of a standard oven. Such equipment can provide a substantial
10.5.8.3 Procedure BxVx—Variable Time—Once the speci- reduction in the time required to reach equilibrium.
men has reached the specified moisture content, the specimen 10.7.2 At the end of each specified weighing time interval,
shall be removed from the conditioning chamber and stored in remove the specimen from the oven and place the specimen in
a sealed bag for a maximum of two weeks before testing (or for a desiccator to cool to laboratory temperature. After the
a maximum time specified by the test requestor). Unless specimen has cooled to an acceptable temperature for labora-
otherwise specified by the test requestor, it is acceptable, but tory handling, remove the specimen from the desiccator and
not mandatory, to place moist cloths in the sealed bags, wipe the specimen free of surface moisture with an absorbent
provided the cloths are not in direct contact with the specimen. lint-free towel. Immediately weigh the specimen to the re-
10.6 Procedure C—Standard 50 % Humidity Chamber quired precision. Record each measurement as Wi, along with
Specimen Conditioning: the corresponding total elapsed time and the time interval since
10.6.1 Initially weigh the specimen to the required precision the previous weighing, and return the specimen to either the
and record this value as the baseline mass, W b, for condition- oven or the desiccator. The specimen shall not be out of the
ing. Place the specimen in the conditioning chamber, which has oven for a total of more than 30 min/weighing and shall not be
previously reached a steady-state environment at the specified out of the desiccator for a total of more than 5 min/weighing.
temperature and a relative humidity level of 50 %. If the 10.7.3 Calculate and record the percent mass change at each
conditioning temperature is not specified, condition at 70 °C time interval by the use of Eq 7. Monitor the desorption of
[160 °F]. moisture until effective moisture equilibrium is reached as
10.6.2 At the end of each specified weighing time interval, determined by 10.2. Calculate and record the original moisture
remove the specimen from the conditioning chamber and place content, Mb, of the material in accordance with Eq 8.
the specimen in the specimen bag to cool to an acceptable 10.7.4 Following establishment of oven-dry equilibrium,
temperature for laboratory handling. Remove the specimen cool the specimen in a desiccator and store in a desiccator until
from the bag (resealing the bag if other specimens remain final use.
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NOTE 22—While similar to Procedure B of Practice D618, this 10.10 Procedure Z—Moisture Loss During Specimen Test-
procedure requires quantified moisture equilibrium instead of the fixed ing:
conditioning time period used by Procedure B of Practice D618.
10.10.1 Specimen Preconditioning—Perform the specified
10.8 Procedure E—Multiple Step Conditioning: Procedure B, C, or E as a preconditioning step.
10.8.1 Specimen Preconditioning—Not required, but may 10.10.2 Conditioning—Remove the "moisture loss" speci-
be specified. If specified, perform Procedure D as a precondi- men from the conditioning chamber, and place into the test
tioning step. See Note 18. machine. Set up the moisture loss specimen in the same way as
10.8.2 Conditioning—This procedure can be used to accel- the mechanical test specimens that it represents, including any
erate the specimen conditioning time. fixtures if required. Heat the specimen and fixture using the
10.8.2.1 Step 1—Perform conditioning using procedure same nominal ramp rate and soak time that will be applied to
BxVP and the first specified environment to the specified the test specimens followed by an additional specified hold
moisture content level. If the moisture content level is not time, after the soak, to mimic the duration of test loading. Once
specified, condition to 80 % 6 5 % of the expected effective the ramp, soak, and hold are complete, return the moisture loss
equilibrium for the final specified environment. specimen to room temperature. Immediately weigh each speci-
NOTE 23—In some situations, the 80 % of equilibrium level may be too men to the required precision. Record the measurement as Wi.
high, leading to a long conditioning time in the subsequent step. Moisture Calculate and record the percent mass change (loss), ML,
diffusion and content data for each environment can be used in a moisture relative to the equilibrium moisture content.
gain simulation to determine the optimum conditioning time for the initial
step. 11. Calculation
10.8.2.2 Step 2—(Optional) Perform conditioning using 11.1 Absorption/Desorption Rate—For all procedures
procedure BxVP and the second specified environment to the where periodic weighings are performed, plot and examine the
second specified moisture content level. Repeat this step for
percent mass change (as calculated by Eq 7) versus =time
any additional intermediate conditioning environments.
curve as illustrated by Fig. 1.
10.8.2.3 Step N—Perform conditioning using procedure
BxEP using the final specified environment to effective equi-
librium.
NOTE 24—While certain two-step, accelerated conditioning cycles can
be considered acceptable, such as use of an initial high-humidity step (95
+ % RH) to speed up moisture gain, followed by completion to
equilibrium at a lower final humidity level (85 % RH), one must be careful
not to select an accelerating environment that changes the material, alters
the physics of diffusion, or both. Long exposures to high temperatures
combined with moisture may alter the chemistry of the material. While an
initial high relative humidity step is acceptable, the extreme cases of
exposure to pressurized steam or immersion in hot/boiling water are not
accepted methods of accelerating humidity absorption, as they have been
found to produce different results from that of 100 % humidity.
10.9 Procedure Y—Moisture Loss During Time Out of
Conditioning Environment:
10.9.1 Specimen Preconditioning—Perform the specified
Procedure B, C, or E as a preconditioning step.
10.9.2 Conditioning—Remove the "moisture loss" specimen
from the conditioning chamber and place in the room tempera- FIG. 1 Moisture Absorption of Carbon/Epoxy (0,45,–45,0)s
ture ambient environment (do not cover or place in bags). After Eight-Ply Laminates at 120 °F (7)
the specified time at room temperature (such as simulating the
time to prepare and strain gauge a test specimen), place the
specimen into an oven at the specified temperature (such as for NOTE 25—It is important to plot and examine the mass change versus
strain gauge adhesive cure) for the specified time. Remove the =time curve prior to deciding that the specimen has reached effective
specimens from the oven and allow to cool to room tempera- moisture equilibrium. Often the mass change criteria in 10.2 can indicate
ture. Immediately weigh each specimen to the required preci- reaching effective moisture equilibrium when the plot obviously shows
that equilibrium has not been reached. Use of the plot to determine
sion. Record the measurement as Wi. Calculate and record the whether or not effective equilibrium has been reached requires engineer-
percent mass change (loss), ML, relative to the equilibrium ing judgment and typically some knowledge of the material’s moisture
moisture content. gain behavior; test labs should not make decisions about reaching effective
10.9.3 Re-Conditioning—Perform the specified Procedure moisture equilibrium without concurrence from the test requestor.
B, C, or E as a re-conditioning step to return the "moisture 11.2 Absorption/Desorption Percent Mass Change—
loss" specimen to moisture equilibrium. Record the time Calculate the percent change in mass for moisture absorption
required to return to effective equilibrium. This re-conditioning or desorption to three (3) decimal places as follows:
time should be used to re-condition mechanical test specimens
which have been removed from the conditioning environment
for such purposes as strain gauge bonding. ∆M 5 Mass change, % 5 U Wi 2 Wb
Wb
U3 100 (7)
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where: 12.1.5 Identification of the material tested, including: type,
Wi = current specimen mass, g, and source, manufacturer’s lot or batch number, previous history,
Wb = baseline specimen mass, g. filament diameter, tow or yarn filament count and twist, sizing,
form or weave, fiber areal weight, polymer matrix type,
11.3 Initial (Baseline) Moisture Content—Calculate the av-
precursor polymer content, and prepreg volatiles content.
erage moisture present in the material prior to conditioning to
12.1.6 Description of the fabrication method used in prepar-
three (3) decimal places as follows:
ing the material including: cure cycle, consolidation method,
and a description of the equipment used.
W ar 2 W od 12.1.7 Ply orientation stacking sequence of the laminate.
M b 5 Initial Moisture Content, % 5 3 100 (8)
W od 12.1.8 For Procedure A, density, volume percent
where: reinforcement, void content, and average ply thickness of the
material.
War = as-received specimen mass, g, and
12.1.9 Results of nondestructive evaluation tests.
Wod = oven-dry specimen mass, g.
12.1.10 Method of preparing the test specimen.
11.4 Percent Mass Lost—Calculate the percent mass lost to 12.1.11 Calibration dates and methods for all measurement
three (3) decimal places, if determined, as follows: and test equipment.
12.1.12 Results of preconditioning.
W ab 2 W p 12.1.13 For Procedure A, dimensions of the specimen fol-
Mass lost, % 5 3 100 (9) lowing preconditioning prior to moisture conditioning and at
W ab
the completion of the test procedure.
where: 12.1.14 Type of test chamber used, the moisture used for the
Wab = absorption baseline specimen mass, g, and test, the nominal and actual test temperatures, moisture expo-
Wp = post-desorption oven-dry specimen mass, g. sure levels, and the measurement time interval.
11.5 Moisture Equilibrium Content—For Procedure A, the 12.1.15 Relative humidity and temperature of the testing
last value of percent mass change from the "thin" specimen is laboratory.
the moisture equilibrium content, Mm. 12.1.16 Specimen mass at each time interval.
12.1.17 Plots of percent mass change versus =time, calcu-
11.6 Diffusivity—For Procedure A, calculate the diffusivity, lated by Eq 7, with mass change reported to three (3) decimal
Dz, as follows using the data from the "thick" specimen: places.
12.1.18 Material effective moisture equilibrium content, or
Dz 5 π
h
S D S=
4M m
2
M2 2 M1
t 2 2 =t 1
D 2
(10) final moisture content, or moisture loss (in mass percent)
depending on the procedure used, with moisture content or loss
where: reported to three (3) decimal places.
12.1.19 Moisture diffusivity constant, as calculated by Eq
h = average specimen thickness, mm [in.], 10.
Mm = effective moisture equilibrium content, %,
12.1.20 Percent of soluble matter lost calculated by Eq 9.
M2 – M1 = slope of moisture absorption plot in the initial,
12.1.21 Any unusual test observations such as warping,
and
cracking, or change of appearance, or combination thereof, of
=t 2 2 =t 1 = linear portion of the curve, =seconds 21 .
the test specimen.
12.1.22 Average, standard deviation, and coefficient of
NOTE 26—Time units must be converted from those time units used variation of the moisture properties for sample populations of
during testing to those time units desired for the moisture diffusivity three or more (having the same nominal reinforcement content
constant (for example, days to seconds). and subjected to the same conditioning environment).
NOTE 27—If there is no discernible initial linear portion of the moisture 12.1.23 Moisture desorption data shall be reported in the
absorption versus =time plot, then the assumption of single-phase same manner as the absorption data.
Fickian moisture absorption (and the calculated moisture diffusivity
constant) may be invalid. 12.2 For material evaluation test specimens which are or are
not conditioned in accordance with one of the procedures of
12. Report this test method, the pretest specimen conditioning shall be
reported as one of the following standard descriptions:
12.1 Report the following information, or references point- 12.2.1 As Fabricated and Desiccated—A condition in
ing to documentation containing this information, to the which a specimen (including the material it is fabricated from)
maximum extent applicable: is stored in a desiccated container following material fabrica-
12.1.1 The date of issue of this test method and the tion and between test specimen preparation steps, and for
procedure and sub-procedure used. which the moisture content is assumed to be low, but has not
12.1.2 The date(s) and location(s) of the test. been explicitly measured.
12.1.3 The name(s) of the test operator(s). 12.2.2 Unknown Moisture Content—If a controlled moisture
12.1.4 Any variations to this test method, anomalies noticed content is not established during pretest conditioning, the
during testing, or equipment problems occurring during testing. pretest moisture content shall be reported as “unknown.” This
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includes “as fabricated” or “ambient” condition specimens that TABLE 7 2018 Round-Robin Data
have not been stored in a controlled low-humidity environment Lab %Moisture
prior to test. This also includes fixed-time, non-equilibrium Lab Individual Lab Average Lab Std Dev
2 1.571
exposures in which the specimen weight change is not mea- 3 1.469
sured (the pretest conditioning environment and time of 4a 1.134
exposure shall be reported). 4b 1.198 1.165 0.032
4c 1.162
12.2.3 Non-Equilibrium Moisture Content—A condition of 5a 1.368 1.341
non-equilibrium moisture conditioning resulting in a specific 5b 1.314
reported moisture content, and established by a documented 8 1.509
10 1.389
procedure that is reported in sufficient detail to allow duplica- 12 1.406
tion of the conditioning result by an independent party. 13 1.308
N 8
12.2.4 Non-Equilibrium Moisture Profile—A condition of Mean 1.395
non-equilibrium moisture conditioning resulting in a specific StdDev 0.127
reported moisture content and a through-thickness moisture CV (%) 9.11
SR 0.127
profile determined analytically, and established by a docu-
mented procedure that is reported in sufficient detail to allow Between laboratory reproducibility limit, R = 2.8 × SR = 0.36 %Moisture
duplication of the conditioning result by an independent party.
12.2.5 Effective Moisture Equilibrium—Moisture content
equilibrium of the specimen as established by this test method; 13.2 Precision:
the pretest moisture content shall be reported as moisture 13.2.1 The precision is defined as a 95 % confidence
content at a stated pretest conditioning relative humidity (or interval, which can be expressed two ways. Practice E691
immersion) and temperature. suggests that for this degree of confidence, the maximum
12.2.6 The moisture content reported under 12.2.3 – 12.2.5 difference between an individual observation and the average
above shall be reported as the “total” moisture content, Met, if should be within 2.0 standard deviations, while the maximum
the specimen is dried prior to conditioning, or shall be reported difference between any two observations should be within 2.8
as “delta” moisture content, Med, if the initial moisture content standard deviations. For brevity, only the magnitude of the
prior to pretest conditioning is not determined. In the latter latter is reported; the former can be derived from the latter.
case, an analytically determined "initial" moisture content, in Only between-laboratory reproducibility is reported, as only a
accordance with Appendix X3, may also be reported, along single result is available from most of the labs participating in
with the "total" moisture content which shall be the sum of the this study. The within-laboratory standard deviation for the one
"initial" and "delta" moisture contents. lab which tested 3 traveler specimens is used for the repeat-
ability standard deviation to calculate SR.
13. Precision and Bias 13.2.2 It should be noted that Practice E691 recommends a
13.1 Round-Robin Results—An exploratory round robin minimum of six materials be included in an interlaboratory
conditioning program as part of the Test Method D2344/ screening study to develop a broadly applicable precision
D2344M SBS round robin testing was conducted in 2017- statement.
2018. Nine laboratories participated in the program. The test 13.3 Bias—Bias cannot be determined for this test method
laminate configuration was [0]30, and was composed of a as no acceptable reference standard exists.
carbon/epoxy grade 203 CSW fabric, with total thickness of
6.32 mm [0.249 in.]. Each laboratory was instructed to 14. Keywords
condition the SBS specimens per Procedure BHEP. The effec- 14.1 conditioning; moisture absorption; moisture desorp-
tive equilibrium moisture content results for each laboratory tion; moisture diffusivity; moisture equilibrium; polymer ma-
are listed in Table 7. trix composite materials
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APPENDIXES
(Nonmandatory Information)
where: 8 ` F
exp 2 ~ 2j11 ! 2 π 2 S D z~ T ! t
h2 DG
c = specimen moisture concentration, g/mm3 [lbm/in.3],
G ~ T,t ! 5 1 2 2(
π j50 ~ 2j11 ! 2 (X1.5)
t = time, s,
∂c⁄∂t = time rate of change of moisture concentration, X1.3 The function of Eq X1.5 may be approximated by:
g/mm3/s [lbm/in.3/s],
Dz = Fickian material diffusion constant through-the-
thickness of the material, mm2/s [in.2/s], and F S
G ~ T,t ! 5 1 2 exp 27.3
D z~ T ! t
h2 D G
0.75
(X1.6)
z = through-the-thickness direction, mm [in.].
X1.4 The moisture equilibrium content, Mm, of a material is
X1.1.2 The boundary and initial conditions are:
a function only of the ambient moisture exposure level (such as
relative humidity). However, the speed at which this moisture
c 5 ci 0 , z , h t # 0 (X1.2) equilibrium content is attained is a function of the ambient
c 5 ca x 5 0; x5h t . 0 (X1.3) temperature, due to the temperature dependence of the mois-
ture diffusivity constant. The time necessary to reach a given
X1.1.3 Temperature and moisture diffusion are uncoupled
moisture content for fixed temperature and moisture exposure
(there is generally a six-order-of-magnitude difference between
level is (from Eq X1.6):
the two differing diffusion speeds, which makes this a reason-
able assumption);
X1.1.4 No variation in moisture diffusivity properties
through the thickness of the material; and
t5 F S
h 2 21
D z 7.3
ln 1 2
M~t! 2 Mb
Mm 2 Mb DG 4/3
(X1.7)
X1.1.5 Limited to one-dimensional, steady-state problems. X1.5 Thus, the time necessary for a completely oven-dry
specimen to reach 99.9 % of material moisture equilibrium at
X1.2 Given the above assumptions, the moisture content in a given temperature, regardless of the ambient moisture expo-
the material for a given moisture exposure level is given as sure level, is approximately:
follows:
0.93h 2
t max~ T ! 5 (X1.8)
M ~ T,t ! 5 M b 1G ~ T,t !~ M m 2 M b ! (X1.4) D z~ T !
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X2.1 The principal test parameters for evaluation of the TABLE X2.2 Specimen Aspect Ratio Versus Error
material moisture properties are tightly coupled. The values of w/h Dz/Da Error, %
these parameters selected by this test method are believed to 10 0.694 44.1
produce acceptable results within the current range of appli- 25 0.857 16.7
40 0.907 10.3
cable engineering materials. The rationale for their selection is 100 0.961 4.1
described as follows by an illustration of the check of critical 200 0.980 2.0
test parameters, using a common polymer matrix composite 1000 0.998 0.2
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X2.6 Redefining Eq X1.4 in terms of the final two weigh- thickness, reference time period, and accuracy criterion on a
ings and Mm allows the calculation of a value of G(T,t) that test series. The results, shown in Table X2.1, predict values
satisfies the requirement for bounded error while using a given of Me for carbon/epoxy material at 74 °C [170 °F] and 90 %
relative humidity for various specimen thicknesses, reference
accuracy criterion: time periods, and accuracy criteria.
X2.9 Specimen size for moisture diffusivity property mea-
M e 5 M e21 1G ~ T,t !~ M m 2 M e21 ! (X2.1)
surement on coupons without sealed edges is established from
or a 100:1 aspect ratio requirement for a square specimen.
Rationale for the 100:1 aspect ratio comes from Springer’s
M e 2 M e21
G ~ T,t ! 5 derivation (from 1-D theory) of correction factors accounting
M m 2 M e21
for moisture ingress through the edges of a rectangular
M e 2 M e21 specimen. While the correction factor is extremely complicated
5
~ M m 2 M e ! 1 ~ M e 2 M e21 ! for laminated anisotropic materials, the point is illustrated by
accuracy evaluating the width-to-thickness aspect ratio for a square
5 (X2.2)
absolute_tolerance1accuracy specimen versus edge effect error for a nominally isotropic
or material. For this case, the correction factor is:
0.02 0.02
G ~ T,t ! 5 5 5 0.50 (X2.3)
0.0210.02 0.04 1
Dz 5 Da (X2.5)
X2.7 G(T,t) is the multiplier of the difference between the
moisture content at the beginning of a time span and the
S 11
2h
w D 2
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X3.1 The relative moisture content as a function of time laminate thickness of 3.76 mm [0.148 in]. Some dummy test
from a given exposure condition can be estimated using the data for a specimen which was not preconditioned to the dry
following equation (combining Eq X1.4 and Eq X1.6): state is plotted in the figure; interpolating between the curves,
the baseline moisture content for this specimen can be esti-
H
~ M ~ T,t ! 2 M b ! 5 ~ M m 2 M b ! 1 2 exp 27.3 F S D z~ T ! t
h2 D GJ
0.75
mated as 0.3 %.
(X3.1)
REFERENCES
(1) Composite Materials Handbook, CMH-17 Rev G, Polymer Matrix Composite Materials, Vol 15, May 1981, p. 272.
Composites, Volume 1-Guidelines, Chapter 2, 2011. (6) Harper, B. D., Staab, G. H., and Chen, R. S., “A Note on the Effects
(2) Shirrell, C. D.,“Diffusion of Water Vapor in Graphite/Epoxy of Voids Upon the Hygral and Mechanical Properties of AS4/3502
Composites,” Advanced Composite Materials—Environmental Graphite/Epoxy ,” Journal of Composite Materials, Vol 21, March
Effects, ASTM STP 658, J. R. Vinson, Ed., ASTM International, 1978, 1987, pp. 280–289.
pp. 21–42. (7) Life Assurance of Composite Structures, Vol 1, General Dynamics/
(3) Advanced Composite Materials—Environmental Effects, ASTM STP Fort Worth, U.S. Air Force Materials Laboratory Contractor Report
658, J. R. Vinson, Ed., ASTM International, 1978. AFML-TR-75-51, May 1975.
(4) Blikstad, M., Sjöblom, P., and Johannesson, T., “Long-Term Moisture (8) Ciriscioli, P. R., Lee, W. I., Peterson, D. G., Springer, G. S., and Tang,
Absorption in Graphite/Epoxy Angle-Ply Laminates,” Journal of J., “Accelerated Environmental Testing of Composites,” Journal of
Composite Materials, Vol 18, June 1984, pp. 32–46. Composite Materials, Vol 21, March 1987, pp. 225–242.
(5) Bonniau, P., and Bunsell, A. R., “A Comparative Study of Water (9) Environmental Effects on Composite Materials, George S. Springer,
Absorption Theories Applied to Glass Epoxy Composites,” Journal of Ed., Technomic Publishing Co., 1981.
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