ASTM D5403-93(2021)

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: D5403 − 93 (Reapproved 2021)
Standard Test Methods for
Volatile Content of Radiation Curable Materials
This standard is issued under the fixed designation D5403; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 These test methods cover procedures for the determina-
D2369 Test Method for Volatile Content of Coatings
tion of weight percent volatile content of coatings, inks, and
E145 Specification for Gravity-Convection and Forced-
adhesives designed to be cured by exposure to ultraviolet light
Ventilation Ovens
or to a beam of accelerated electrons.
E177 Practice for Use of the Terms Precision and Bias in
1.2 Test Method A is applicable to radiation curable mate-
ASTM Test Methods
rials that are essentially 100 % reactive but may contain traces
E691 Practice for Conducting an Interlaboratory Study to
(no more than 3 %) of volatile materials as impurities or
Determine the Precision of a Test Method
introduced by the inclusion of various additives.
3. Terminology
1.3 Test Method B is applicable to all radiation curable
3.1 Definitions:
materials but must be used for materials that contain volatile
3.1.1 cure, n—the condition of a coating after conversion to
solvents intentionally introduced to control application viscos-
the final state of cure as measured by tests generally related to
ity and which are intended to be removed from the material
end use performance and mutually agreeable to supplier and
prior to cure.
purchaser.
1.4 These test methods may not be applicable to radiation
3.1.2 ultraviolet (UV) curing, n—conversion of a coating
curable materials wherein the volatile material is water, and
from its application state to its final use state by means of a
other procedures may be substituted by mutual consent of the
mechanism initiated by ultraviolet radiation generated by
producer and user.
equipment designed for that purpose.
3.1.3 electron beam (EB) curing, n—conversionofacoating
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this from its application state to its final use state by means of a
mechanism initiated by electron beam radiation generated by
standard.
equipment designed for that purpose.
1.6 This standard does not purport to address all of the
3.1.4 processingvolatiles,n—lossinspecimenweightunder
safety problems, if any, associated with its use. It is the
test conditions that are designed to simulate actual industrial
responsibility of the user of this standard to establish appro-
cure processing conditions.
priate safety, health, and environmental practices and deter-
3.1.5 potential volatiles, n—loss in specimen weight upon
mine the applicability of regulatory limitations prior to use. A
heating at 110 °C for 60 min after radiation curing.
specific hazard statement is given in 15.7.
3.1.5.1 Discussion—This value is an estimation of volatile
1.7 This international standard was developed in accor-
loss that may occur during aging or under extreme storage
dance with internationally recognized principles on standard-
conditions. Potential volatiles may also be referred to as
ization established in the Decision on Principles for the
residual volatiles.
Development of International Standards, Guides and Recom-
3.1.6 total volatiles, n—sum of the processing volatiles and
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. the potential volatiles.
4. Summary of Test Methods
4.1 Adesignated quantity of material is weighed before and
These test methods are under the jurisdiction of ASTM Committee D01 on
after a cure step that simulates normal industrial processing.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.55 on FactoryApplied Coatings on Preformed
Products. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2021. Published August 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2013 as D5403 – 93 (2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D5403-93R21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5403 − 93 (2021)
The test specimen is weighed again after heating at 110 °C 6 9.2 Weigh the preconditioned aluminum substrate, (8.1)to
5 °C for 60 min. The percent volatile is calculated from the 0.1 mg (A). The size of the aluminum substrate must allow a
losses in weight. minimum of 0.2 g of material to be applied at the supplier’s
recommended film thickness. Use rubber gloves or tongs, or
5. Significance and Use
both, to handle samples.
5.1 These test methods are the procedures of choice for
9.3 Apply a minimum of 0.2 g of test specimen to the
determining volatile content of materials designed to be cured
aluminum substrate and reweigh to 0.1 mg (B). Prepare a total
by exposure to ultraviolet light or electron beam irradiation.
of three test specimens.
These types of materials contain liquid reactants that react to
NOTE1—Theelapsedtimebetweenapplicationandweighingshouldbe
become part of the film during cure, but, which under the test
no greater than 30 s. If the sample to be tested contains any reactive
conditions of Test Method D2369, will be erroneously mea-
diluent with a vapor pressure at room temperature greater than 1.0 mm Hg
sured as volatiles. The conditions of these test methods are
(forexample,styrene),theelapsedtimebetweenspecimenapplicationand
similar to Test Method D2369 with the inclusion of a step to
weighing must be no greater than 15 s.
cure the material prior to weight loss determination. Volatile
9.4 Cure the test specimen by exposure to UV or EB as
contentisdeterminedastwoseparatecomponents—processing
prescribed by the supplier of the material.
volatiles and potential volatiles. Processing volatiles is a
NOTE 2—If there is any doubt as to the adequacy of the exposure for
measure of volatile loss during the actual cure process.
affecting proper cure (6.1), an additional sample can be tested utilizing
Potential volatiles is a measure of volatile loss that might occur
50 % additional exposure and the volatile content results compared. If the
during aging or under extreme storage conditions. These
original exposure was adequate, there should be no difference in the
volatile content measurements are useful to the producer and
results within the precision of the test method. If the results are different,
user of a material and to environmental interests for determin- the supplier of the material must be contacted and a revised cure schedule
established.
ing emissions.
9.5 Allow the test specimen to cool 15 min at room
6. Interferences
temperature and reweigh to 0.1 mg (C).
6.1 The degree to which the results of these procedures
9.6 Heat the test specimen in a forced draft oven (8.2) for
accurately measure the volatiles emitted during actual use is
60 min at 110 °C 6 5 °C.
absolutely dependent upon proper cure during the test proce-
dure. Although overcure will have little or no effect upon NOTE 3—Materials that can react with atmospheric moisture during
post cure, that is, UV cationic-curable epoxy materials, may exhibit a
measured volatiles, undercure may lead to erroneously high
weight gain during procedure in 9.6. If this occurs, the sample should be
values. Since various pieces of cure equipment may vary
retested and allowed to post cure at room temperature for 48 h after
widely in efficiency, it is essential that dialogue between
procedurein9.5,andthenreweighedpriortoprocedurein9.6.Theweight
material manufacturer and testing laboratory establish a cure
after post cure should then be used as Weight C in the calculation of
percent potential volatiles in 10.1.
scheduleappropriatebothtothematerialtobetestedandtothe
cure equipment to be used in the procedure.
9.7 Allow the test specimen to cool to room temperature in
a desiccator and reweigh to 0.1 mg, (D).
TEST METHOD A
10. Calculations
7. Scope
10.1 Calculate the weight percent volatiles as follows:
7.1 This test method is applicable to radiation curable
Processing Volatiles 5 100 @~B 2 C!/~B 2 A!# (1)
materials with solvent content less than or equal to 3 %.
Potential Volatiles 5 100 C 2 D / B 2 A (2)
@~ ! ~ !#
8. Apparatus
8.1 Aluminum Substrate, standard test panels (102 mm by Total volatiles 5 % Processing Volatiles1% Potential Volatiles
305 mm) or heavy gage (0.05 mm minimum) foil. Test panels
where:
aremostconvenientandmaybecutintosmallerpiecesforease
A = weight of aluminum substrate, g,
of weighing. Precondition the substrate for 30 min at 110 °C 6
B = weight of aluminum substrate plus test specimen, g,
5 °C and store in a desiccator prior to use.
C = weight of aluminum substrate plus test specimen after
8.2 Forced Draft Oven, Type IIAorType IIB as specified in
cure, g, and
Specification E145.
D = weight of aluminum substrate plus cured test specimen
after heating.
8.3 Ultraviolet Light or Electron Beam Curing Equipment—
There are several commercial suppliers of laboratory scale
11. Precision and Bias
equipment that simulates industrial curing processes.
11.1 Interlaboratory Test Program—An interlaboratory
9. Procedure
study of volatile content of radiation cured materials (Test
MethodA) was conducted in accordance with P
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