ASTM E1559-09(2022)
(Test Method)Standard Test Method for Contamination Outgassing Characteristics of Spacecraft Materials
Standard Test Method for Contamination Outgassing Characteristics of Spacecraft Materials
ABSTRACT
This test method covers a technique for generating data to characterize the kinetics of the release of outgassing products from spacecraft materials. This technique will determine both the total mass flux evolved by a material when exposed to a vacuum environment and the deposition of this flux on surfaces held at various specified temperatures. The quartz crystal microbalances used in this test method provide a sensitive technique for measuring very small quantities of deposited mass. There are two test methods in this standard: Test Method A and Test Method B. The test apparatus shall consists of four main subsystems: a vacuum chamber, a temperature control system, internal configuration, and a data acquisition system. A test procedure for collecting data and a test method for processing and presenting the collected data are included.
SCOPE
1.1 This test method covers a technique for generating data to characterize the kinetics of the release of outgassing products from materials. This technique will determine both the total mass flux evolved by a material when exposed to a vacuum environment and the deposition of this flux on surfaces held at various specified temperatures.
1.2 This test method describes the test apparatus and related operating procedures for evaluating the total mass flux that is evolved from a material being subjected to temperatures that are between 298 and 398 K. Pressures external to the sample effusion cell are less than 7 × 10−3 Pa (5 × 10−5 torr). Deposition rates are measured during material outgassing tests. A test procedure for collecting data and a test method for processing and presenting the collected data are included.
1.3 This test method can be used to produce the data necessary to support mathematical models used for the prediction of molecular contaminant generation, migration, and deposition.
1.4 All types of organic, polymeric, and inorganic materials can be tested. These include polymer potting compounds, foams, elastomers, films, tapes, insulations, shrink tubing, adhesives, coatings, fabrics, tie cords, and lubricants.
1.5 There are two test methods in this standard. Test Method A uses standardized specimen and collector temperatures. Test Method B allows the flexibility of user-specified specimen and collector temperatures, material and test geometry, and user-specified QCMs.
1.6 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1559 − 09 (Reapproved 2022)
Standard Test Method for
Contamination Outgassing Characteristics of Spacecraft
Materials
This standard is issued under the fixed designation E1559; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This test method covers a technique for generating data
1.8 This international standard was developed in accor-
to characterize the kinetics of the release of outgassing
dance with internationally recognized principles on standard-
products from materials. This technique will determine both
ization established in the Decision on Principles for the
the total mass flux evolved by a material when exposed to a
Development of International Standards, Guides and Recom-
vacuumenvironmentandthedepositionofthisfluxonsurfaces
mendations issued by the World Trade Organization Technical
held at various specified temperatures.
Barriers to Trade (TBT) Committee.
1.2 Thistestmethoddescribesthetestapparatusandrelated
operating procedures for evaluating the total mass flux that is
2. Referenced Documents
evolved from a material being subjected to temperatures that
2.1 ASTM Standards:
are between 298 and 398 K. Pressures external to the sample
E595Test Method for Total Mass Loss and Collected Vola-
−3 −5
effusion cell are less than7×10 Pa (5 × 10 torr).
tile Condensable Materials from Outgassing in a Vacuum
Depositionratesaremeasuredduringmaterialoutgassingtests.
Environment
A test procedure for collecting data and a test method for
2.2 Military Standard:
processing and presenting the collected data are included.
MIL-P-27401DPropellant Pressurizing Agent, Nitrogen
1.3 This test method can be used to produce the data
2.3 Other Standard:
necessary to support mathematical models used for the predic-
SMC-TR-95–28 Non-Volatile Residue Solvent
tion of molecular contaminant generation, migration, and
Replacement, Report No. TR95 (5448)-1
deposition.
1.4 All types of organic, polymeric, and inorganic materials
3. Terminology
can be tested. These include polymer potting compounds,
3.1 Definitions:
foams, elastomers, films, tapes, insulations, shrink tubing,
3.1.1 AT cut crystal, n—a quartz crystal orientation that
adhesives, coatings, fabrics, tie cords, and lubricants.
minimizes the temperature coefficient (frequency change ver-
1.5 Therearetwotestmethodsinthisstandard.TestMethod
sus temperature) over a wide range of temperature.
Auses standardized specimen and collector temperatures. Test
3.1.2 azeotropic mixture, n—a solution of two or more
Method B allows the flexibility of user-specified specimen and
liquids, the composition of which does not change upon
collector temperatures, material and test geometry, and user-
distillation. Also known as azeotrope.
specified QCMs.
3.1.3 collected volatile condensable material, CVCM,
1.6 The values stated in SI units are to be regarded as the
n—(fromTestMethodE595).Thequantityofoutgassedmatter
standard. The values given in parentheses are for information
from a test specimen that condenses on a collector maintained
only.
at a specific constant temperature for a specified time and
1.7 This standard does not purport to address all of the
measured before and after the test outside the chamber.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method is under the jurisdiction of ASTM Committee E21 on Space Standards volume information, refer to the standard’s Document Summary page on
Simulation andApplications of SpaceTechnology and is the direct responsibility of the ASTM website.
Subcommittee E21.05 on Contamination. AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Current edition approved April 1, 2022. Published May 2022. Originally Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
approved in 1993. Last previous edition approved in 2016 as E1559–09(2016). Available fromTheAerospace Corporation, P.O. Box 92957, LosAngeles, CA
DOI: 10.1520/E1559-09R22. 90009–2957, http://www.aero.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1559 − 09 (2022)
3.1.3.1 Discussion—CVCMisspecifictoTestMethodE595 3.1.14 total mass loss, TML, n—total mass of material
and is calculated from the condensate mass determined from outgassedfromatestspecimenthatismaintainedataspecified
thedifferenceinmassofthecollectorplatebeforeandafterthe constant temperature and operating pressure for a specified
test in a controlled laboratory environment. CVCM is ex- time and measured within the test chamber. TMLis expressed
pressed as a percentage of the initial specimen mass.The view as a percentage of the initial specimen mass. In addition,TML
factor is not considered; so all the VCM outgassing from the can be normalized with respect to the sample surface area and
sample may not be collected. Care should be used in compar- be expresed as µg/cm .
ing the CVCM from Test Method E595 with VCM from this
3.1.14.1 in-situ TML, n—calculated from the mass depos-
test method.
ited on a cryogenically cooled QCM and the view factor from
3.1.4 differential scanning calorimetry, DSC, n—a tech-
the effusion cell orifice to the QCM.
nique in which the difference in energy inputs into a substance
3.1.14.2 Discussion—In-situ TML is a function of the out-
and a reference material is measured as a function of tempera-
gassing test time and is expressed as a percentage of the initial
turewhilethesubstanceandreferencematerialaresubjectedto
specimen mass. This is not necessarily the same as the TML
a controlled-temperature program.
determined by Test Method E595.
3.1.5 effusion cell, n—a container, placed in a vacuum, in
3.1.14.3 ex-situ TML, n—total mass of material outgassed
which a sample of material can be placed and heated to some
from a test specimen that is maintained at a specified constant
specified temperature.
temperature and operating pressure for a specified time and
measured outside the test chamber.
3.1.5.1 Discussion—The container has a cylindrical orifice
at one end so that evolving gases exit the cell in a controlled
3.1.14.4 Discussion—Ex-situ TML is calculated from the
manner. The effusion cell dimensions and orifice size are
mass of the specimen as measured before and after the test in
specified such that there is free molecular flow of the evolving
a controlled laboratory environment and is expressed as a
gasses and a predictable molecular flux from the orifice.
percentage of the initial specimen mass. (From Test Method
3.1.6 mass flux, n—the mass of molecular flux.
E595.)
−2 −1
3.1.7 molecular flux (molecules·cm ·s ), n—the number 3.1.15 total outgassing rate, n—the net rate of mass loss
ofgasmoleculescrossingaspecifiedplaneinunittimeperunit
from a material sample as a result of outgassing. Total
area. outgassing rate can be normalized per unit sample surface area
−2 −1
and expressed as g·cm ·s or it can be normalized per unit
3.1.8 nonvolatile residue, NVR, n—the quantity of residual
−1 −1
initial sample mass and expressed as g·g ·s .
molecular and particulate matter remaining following the
3.1.16 volatile condensable material, VCM, n—the matter
filtration of a solvent containing contaminants and evaporation
of the solvent at a specified temperature. that outgasses from a material and condenses on a collector
surface that is at a specified temperature.
3.1.9 outgassing, n—the evolution of gas from a material,
usually in a vacuum. Outgassing also occurs in a higher
3.1.16.1 Discussion—For this test method, this is the quan-
pressure environment.
tityofoutgassedmatterfromatestspecimenthatcondenseson
surfaces maintained at QT2 or QT3. The VCM is calculated
3.1.10 quartz crystal microbalance, QCM, n—a device for
from the mass deposited on QCM2 or QCM3 and the view
measuring small quantities of mass using the properties of a
factor from the effusion cell orifice to the QCMs. VCM is a
quartz crystal oscillator.
function of the outgassing test time and is expressed as a
3.1.10.1 Discussion—The resonant frequency of a quartz
percentage of the initial specimen mass. In addition,VCM can
crystal oscillator is inversely proportional to the thickness of
be normalized with respect to the sample surface area and be
the crystal. When the mass of a uniform deposit is small 2
expressed as µg/cm . This is not the same as CVCM as
relative to the mass of the crystal, the change in frequency is
determined by Test Method E595 (see 3.1.3).
proportional to the mass of the deposit.
3.2 Acronyms:
3.1.11 QCM thermogravimetric analysis, QTGA, n—a tech-
3.2.1 GN,n—gaseous nitrogen.
nique in which a QCM is heated at a constant rate to remove
3.2.2 LN,n—liquid nitrogen.
a collected deposit.
3.2.3 MAPTIS, n—Materials and Process Technical Infor-
3.1.11.1 Discussion—This is performed to determine the
mation Service.
evaporation characteristics of the species in the deposit. The
3.3 Definitions of Terms Specific to This Standard:
mass of the deposit on the QCM is recorded as a function of
3.3.1 QCM1—the QCM that is operating at the temperature
time or temperature.
TQ1 (cryogenic) for measuring the total outgassing rate.
3.1.12 residual gas analyzer, RGA, n—a mass spectrometer
3.3.2 QCM2 and QCM3—the QCMs that are operating at
mounted inside or attached to a vacuum chamber.
temperatures TQ2 and TQ3 for the measurement of the
3.1.12.1 Discussion—RGA can be used for identifying
deposition of outgassing matter.
gases in the vacuum chamber.
−2 −1
4. Summary of Test Method
3.1.13 totalmassflux(g·cm ·s ),n—thesummationofthe
mass from all molecular species crossing a specified plane in 4.1 The test apparatus described in this test method is
unit time per unit area. designed to measure outgassing rate data that can be used to
E1559 − 09 (2022)
develop kinetic expressions for use in models that predict the 4.7 It is critical to the posttest analysis that the material
evolution of molecular contaminants and the migration and sample be completely described and specified, so that the
deposition of these contaminants on spacecraft surfaces. Ma- outgassing characteristics can be applied to the material when
terialsthatcontainvolatilespeciesthatwillbeoutgassedunder used on a spacecraft. It is also necessary so that any material
sample can be properly compared with that of other samples.
the temperature and vacuum conditions of this test method can
be characterized.The quartz crystal microbalances used in this The outgassing rate of the material will, in general, be
determined by its composition, processing history, and envi-
test method provide a sensitive technique for measuring very
small quantities of deposited mass. In addition to providing ronmentalconditioningbeforethetest.Alltestsampleprocess-
ingshouldberepresentativeofnormalmaterialprocessingand
data for kinetic expressions, the reduced data can be used to
usage.All materials are environmentally conditioned to speci-
compare the outgassing behavior of different materials for
fied conditions. However, samples may be subjected to envi-
material selection purposes.
ronmental conditions that are expected during actual use. Test
4.2 Therearetwotestmethodsinthisstandard.TestMethod
sampleprocessingandconditioninghistoryshallbeincludedin
Aisthestandardprocedureusingprescribedconfigurationsand
the test report.
temperatures. Test Method B allows for the use of spacecraft
4.8 Because outgassing of all materials is, to some extent,
systemspecifictemperatures,configurations,andQCMcollec-
diffusion rate controlled, the outgassing rate of a test sample
tor surface finishes.
depends on the distance from the sample interior to a free
4.3 The measurements are made by placing the material
surface. Hence, the geometry of a test sample must be
sample in an effusion cell so that the outgassing flux leaving
controlled in a specified manner to permit meaningful inter-
thecellorificewillimpingeonthreeQCMswhicharearranged
pretation of the data. When possible, the sample geometry
toviewtheorifice.AfourthQCMisoptional.Theeffusioncell
should be in the specified configuration to simplify modeling.
is held at a constant temperature in the high vacuum chamber
However, the material sample can be made with the same
and has a small orifice directed at the QCMs. The QCMs are
geometry as it would have in an actual application.
controlledtoselectedtemperatures.Thetotaloutgassingrateis
5. Test Apparatus
determined from the collection rate on a cryocooled QCM.At
5.1 Description—The test apparatus consists of four main
the end of the isothermal test, the QCMs are heated in a
subsystems: a vacuum chamber, a temperature control system,
controlled manner to determine the evaporation characteristics
internal configuration, and a data acquisition system. Fig. 1 is
of the deposits.
a schematic of the systems, and Fig. 2 shows the vacuum
4.4 The effusion cell is loaded from the vacuum interlock
chamber and internal configuration.
chamber to the main test chamber and is positioned at a fixed
5.2 Vacuum Chamber—The principal components of the
distance and angle with respect to the QCM surfaces. The
vacuum chamber are the main test chamber, the vacuum
effusion cell is temperature controlled to provide constant and
interlock chamber, and cryogenic shrouds (for example, LN ).
uniform heating of the sample.The vacuum interlock chamber
A high-vacuum gate valve is used to isolate the main test
is a device that enables the expedient introduction of the test
chamber from the interlock chamber. This allows the effusion
sample into the high vacuum of the main test chamber. Use of
celltobewithdrawnorinsertedintothemainchamberwithout
theinterlockchambertoloadandunloadsamplespreventsloss
the loss of high vacuum in the main chamber. High-vacuum
of vacuum in the main chamber and diminishes the need to
electrical and mechanical feedthroughs are used to access the
pump it down before each test.
interior of the chamber.
4.5 The QCM collection method for measuring the total
5.3 Internal Configuration—Three quartz crystal microbal-
outgassing rate from
...
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