ASTM D5403-93(2002)
(Test Method)Standard Test Methods for Volatile Content of Radiation Curable Materials
Standard Test Methods for Volatile Content of Radiation Curable Materials
SCOPE
1.1 These test methods cover procedures for the determination of weight percent volatile content of coatings, inks, and adhesives designed to be cured by exposure to ultraviolet light or to a beam of accelerated electrons.
1.2 Test Method A is applicable to radiation curable materials that are essentially 100 % reactive but may contain traces (no more than 3 %) of volatile materials as impurities or introduced by the inclusion of various additives.
1.3 Test Method B is applicable to all radiation curable materials but must be used for materials that contain volatile solvents intentionally introduced to control application viscosity and which are intended to be removed from the material prior to cure.
1.4 These test methods may not be applicable to radiation curable materials wherein the volatile material is water, and other procedures may be substituted by mutual consent of the producer and user.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. A specific hazard statement is given in 15.7.
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Designation:D5403–93(Reapproved2002)
Standard Test Methods for
Volatile Content of Radiation Curable Materials
This standard is issued under the fixed designation D 5403; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3.1.1 cure—the condition of a coating after conversion to
the final state of cure as measured by tests generally related to
1.1 These test methods cover procedures for the determina-
end use performance and mutually agreeable to supplier and
tion of weight percent volatile content of coatings, inks, and
purchaser.
adhesives designed to be cured by exposure to ultraviolet light
3.1.2 ultraviolet (UV) curing—conversion of a coating from
or to a beam of accelerated electrons.
its application state to its final use state by means of a
1.2 Test Method A is applicable to radiation curable mate-
mechanism initiated by ultraviolet radiation generated by
rials that are essentially 100 % reactive but may contain traces
equipment designed for that purpose.
(no more than 3 %) of volatile materials as impurities or
3.1.3 electron beam (EB) curing—conversion of a coating
introduced by the inclusion of various additives.
from its application state to its final use state by means of a
1.3 Test Method B is applicable to all radiation curable
mechanism initiated by electron beam radiation generated by
materials but must be used for materials that contain volatile
equipment designed for that purpose.
solvents intentionally introduced to control application viscos-
3.1.4 processing volatiles—loss in specimen weight under
ity and which are intended to be removed from the material
test conditions that are designed to simulate actual industrial
prior to cure.
cure processing conditions.
1.4 These test methods may not be applicable to radiation
3.1.5 potential volatiles—loss in specimen weight upon
curable materials wherein the volatile material is water, and
heating at 110°C for 60 min after radiation curing.
other procedures may be substituted by mutual consent of the
3.1.5.1 Discussion—This value is an estimation of volatile
producer and user.
loss that may occur during aging or under extreme storage
1.5 This standard does not purport to address all of the
conditions. Potential volatiles may also be referred to as
safety problems, if any, associated with its use. It is the
residual volatiles.
responsibility of the user of this standard to establish appro-
3.1.6 total volatiles—sum of the processing volatiles and
priate safety and health practices and determine the applica-
the potential volatiles.
bility of regulatory limitations prior to use. A specific hazard
statement is given in 15.7.
4. Summary of Test Methods
2. Referenced Documents 4.1 Adesignated quantity of material is weighed before and
after a cure step that simulates normal industrial processing.
2.1 ASTM Standards:
2 The test specimen is weighed again after heating at 110 6 5°C
D 2369 Test Method for Volatile Content of Coatings
for 60 min.The percent volatile is calculated from the losses in
E 145 Specification for Gravity–Convection and Forced–
3 weight.
Ventilation Ovens
E 177 Practice for Use of the Terms Precision and Bias in
5. Significance and Use
ASTM Methods
5.1 These test methods are the procedures of choice for
E 691 Practice for Conducting an Interlaboratory Study to
determining volatile content of materials designed to be cured
Determine the Precision of a Test Method
by exposure to ultraviolet light or electron beam irradiation.
3. Terminology These types of materials contain liquid reactants that react to
become part of the film during cure, but, which under the test
3.1 Definitions:
conditions of Test Method D 2369, will be erroneously mea-
sured as volatiles. The conditions of these test methods are
These test methods are under the jurisdiction of ASTM Committee D01 on
similar to Test Method D 2369 with the inclusion of a step to
Paint and Related Coatings, Materials, and Applications and is the direct responsi-
cure the material prior to weight loss determination. Volatile
bility of Subcommittee D01.55 on Factory Applied Coatings on Preformed
Products. contentisdeterminedastwoseparatecomponents—processing
Current edition approved May 15, 1993. Published July 1993.
volatiles and potential volatiles. Processing volatiles is a
Annual Book of ASTM Standards, Vol 06.01.
measure of volatile loss during the actual cure process.
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5403
NOTE 2—If there is any doubt as to the adequacy of the exposure for
Potential volatiles is a measure of volatile loss that might occur
affecting proper cure (6.1), an additional sample can be tested utilizing
during aging or under extreme storage conditions. These
50 % additional exposure and the volatile content results compared. If the
volatile content measurements are useful to the producer and
original exposure was adequate, there should be no difference in the
user of a material and to environmental interests for determin-
results within the precision of the test method. If the results are different,
ing emissions.
the supplier of the material must be contacted and a revised cure schedule
established.
6. Interferences
9.5 Allow the test specimen to cool 15 min at room
6.1 The degree to which the results of these procedures
temperature and reweigh to 0.1 mg (C).
accurately measure the volatiles emitted during actual use is
9.6 Heatthetestspecimeninaforceddraftoven(8.2)for60
absolutely dependent upon proper cure during the test proce-
min at 110 6 5°C.
dure. Although overcure will have little or no effect upon
NOTE 3—Materials that can react with atmospheric moisture during
measured volatiles, undercure may lead to erroneously high
post cure, that is, UV cationic-curable epoxy materials, may exhibit a
values. Since various pieces of cure equipment may vary
weight gain during procedure in 9.6. If this occurs, the sample should be
widely in efficiency, it is essential that dialogue between
retested and allowed to post cure at room temperature for 48 h after
material manufacturer and testing laboratory establish a cure
procedurein9.5,andthenreweighedpriortoprocedurein9.6.Theweight
schedule appropriate both to the material to be tested and to the
after post cure should then be used as Weight C in the calculation of
cure equipment to be used in the procedure.
percent potential volatiles in 10.1.
9.7 Allow the test specimen to cool to room temperature in
TEST METHOD A
a desiccator and reweigh to 0.1 mg, (D).
7. Scope
10. Calculations
7.1 This test method is applicable to radiation curable
10.1 Calculate the weight percent volatiles as follows:
materials with solvent content less than or equal to 3 %.
Processing Volatiles 5 100 @~B 2 C!/~B 2 A!# (1)
8. Apparatus
Potential Volatiles 5 100 @~C 2 D!/~B 2 A!# (2)
8.1 Aluminum Substrate, standard test panels (102 mm by
Total volatiles 5 % Processing Volatiles 1 % Potential Volatiles
305 mm) or heavy gage (0.05 mm minimum) foil. Test panels
aremostconvenientandmaybecutintosmallerpiecesforease where:
of weighing. Precondition the substrate for 30 min at 110 6 A = weight of aluminum substrate, g,
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 E 145.
D = weight of aluminum substrate plus cured test speci-
8.3 Ultraviolet Light or Electron Beam Curing
men after heating.
Equipment—There are several commercial suppliers of labo-
ratory scale equipment that simulates industrial curing pro-
11. Precision and Bias
cesses.
11.1 Interlaboratory Test Program—An interlaboratory
9. Procedure
study of volatile content of radiation cured materials (Test
MethodA)wasconductedinaccordancewithPracticeE 691in
9.1 Mixthesample,ifnecessary,toensureuniformity.Hand
nine laboratories with three materials, with each laboratory
stirringisrecommendedtoavoidtheentrapmentofairbubbles.
obtaining three test results for each material.
9.2 Weigh the preconditioned aluminum substrate, (8.1) to
11.2 Test Result—The precision information given below
0.1 mg (A). The size of the aluminum substrate must allow a
for volatile content in weight percent is for the comparison of
minimum of 0.2 g of material to be applied at the supplier’s
two test results, each of which is the average of three test
recommended film thickness. Use rubber gloves or tongs, or
determinations.
both, to handle samples.
11.3 Precision:
9.3 Apply a minimum of 0.2 g of test specimen to the
aluminum substrate and reweigh to 0.1 mg (B). Prepare a total
Percent
of three test specimens.
Processing Volatiles
NOTE 1—Theelapsedtimebetweenapplicationandweighingshouldbe 95 % repeatability limit (within laboratory) 0.9
95 % reproducibility limit (between laboratories) 1.6
no greater than 30 s. If the sample to be tested conta
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