ASTM D5403-93(2007)

Standard Test Methods for Volatile Content of Radiation Curable Materials

SIGNIFICANCE AND USE
These test methods are the procedures of choice for determining volatile content of materials designed to be cured by exposure to ultraviolet light or electron beam irradiation. These types of materials contain liquid reactants that react to become part of the film during cure, but, which under the test conditions of Test Method D 2369, will be erroneously measured as volatiles. The conditions of these test methods are similar to Test Method D 2369 with the inclusion of a step to cure the material prior to weight loss determination. Volatile content is determined as two separate components—processing volatiles and potential volatiles. Processing volatiles is a measure of volatile loss during the actual cure process. Potential volatiles is a measure of volatile loss that might occur during aging or under extreme storage conditions. These volatile content measurements are useful to the producer and user of a material and to environmental interests for determining emissions.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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.

General Information

• Status: Historical
• Publication Date: 31-May-2007
• ICS: 13.280 - Radiation protection
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.55 - Factory Applied Coatings on Preformed Products

Relations

• Replaces: ASTM D5403-93(2002) - Standard Test Methods for Volatile Content of Radiation Curable Materials
• Effective Date: 01-Jun-2007
• Referred By: ASTM D5201-05a(2020) - Standard Practice for Calculating Formulation Physical Constants of Paints and Coatings
• Effective Date: 01-Jun-2007
• Referred By: ASTM D2697-22 - Standard Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings
• Effective Date: 01-Jun-2007
• Referred By: ASTM D2369-20 - Standard Test Method for Volatile Content of Coatings
• Effective Date: 01-Jun-2007
• Referred By: ASTM D3960-05(2018) - Standard Practice for Determining Volatile Organic Compound (VOC) Content of Paints and Related Coatings
• Effective Date: 01-Jun-2007
• Referred By: ASTM D7188-05(2019) - Standard Terminology for Printing Inks, Materials, and Processes
• Effective Date: 01-Jun-2007
• Referred By: ASTM D7767-11(2018) - Standard Test Method to Measure Volatiles from Radiation Curable Acrylate Monomers, Oligomers, and Blends and Thin Coatings Made from Them
• Effective Date: 01-Jun-2007

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5403 − 93 (Reapproved2007)
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 E145 Specification for Gravity-Convection and Forced-
Ventilation Ovens
1.1 These test methods cover procedures for the determina-
E177 Practice for Use of the Terms Precision and Bias in
tion of weight percent volatile content of coatings, inks, and
ASTM Test Methods
adhesives designed to be cured by exposure to ultraviolet light
E691 Practice for Conducting an Interlaboratory Study to
or to a beam of accelerated electrons.
Determine the Precision of a Test Method
1.2 Test Method A is applicable to radiation curable mate-
3. Terminology
rials that are essentially 100 % reactive but may contain traces
(no more than 3 %) of volatile materials as impurities or
3.1 Definitions:
introduced by the inclusion of various additives.
3.1.1 cure, n—the condition of a coating after conversion to
1.3 Test Method B is applicable to all radiation curable the final state of cure as measured by tests generally related to
end use performance and mutually agreeable to supplier and
materials but must be used for materials that contain volatile
solvents intentionally introduced to control application viscos- purchaser.
ity and which are intended to be removed from the material
3.1.2 ultraviolet (UV) curing, n—conversion of a coating
prior to cure.
from its application state to its final use state by means of a
mechanism initiated by ultraviolet radiation generated by
1.4 These test methods may not be applicable to radiation
equipment designed for that purpose.
curable materials wherein the volatile material is water, and
other procedures may be substituted by mutual consent of the
3.1.3 electron beam (EB) curing, n—conversionofacoating
producer and user.
from its application state to its final use state by means of a
mechanism initiated by electron beam radiation generated by
1.5 The values stated in SI units are to be regarded as
equipment designed for that purpose.
standard. No other units of measurement are included in this
standard. 3.1.4 processingvolatiles,n—lossinspecimenweightunder
test conditions that are designed to simulate actual industrial
1.6 This standard does not purport to address all of the
cure processing conditions.
safety problems, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1.5 potential volatiles, n—loss in specimen weight upon
priate safety and health practices and determine the applica-
heating at 110°C for 60 min after radiation curing.
bility of regulatory limitations prior to use. A specific hazard 3.1.5.1 Discussion—This value is an estimation of volatile
statement is given in 15.7.
loss that may occur during aging or under extreme storage
conditions. Potential volatiles may also be referred to as
2. Referenced Documents
residual volatiles.
2.1 ASTM Standards: 3.1.6 total volatiles, n—sum of the processing volatiles and
D2369 Test Method for Volatile Content of Coatings the potential volatiles.
4. Summary of Test Methods
1 4.1 Adesignated quantity of material is weighed before and
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
after a cure step that simulates normal industrial processing.
responsibility of Subcommittee D01.55 on FactoryApplied Coatings on Preformed
The test specimen is weighed again after heating at 110 6 5°C
Products.
for 60 min.The percent volatile is calculated from the losses in
CurrenteditionapprovedJune1,2007.PublishedJuly2007.Originallyapproved
weight.
in 1993. Last previous edition approved in 2002 as D5403 - 93 (2002). DOI:
10.1520/D5403-93R07.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5. Significance and Use
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1 These test methods are the procedures of choice for
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. determining volatile content of materials designed to be cured
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5403 − 93 (2007)
by exposure to ultraviolet light or electron beam irradiation. 9.3 Apply a minimum of 0.2 g of test specimen to the
These types of materials contain liquid reactants that react to aluminum substrate and reweigh to 0.1 mg (B). Prepare a total
become part of the film during cure, but, which under the test of three test specimens.
conditions of Test Method D2369, will be erroneously mea-
NOTE1—Theelapsedtimebetweenapplicationandweighingshouldbe
sured as volatiles. The conditions of these test methods are
no greater than 30 s. If the sample to be tested contains any reactive
similar to Test Method D2369 with the inclusion of a step to
diluent with a vapor pressure at room temperature greater than 1.0 mm Hg
(forexample,styrene),theelapsedtimebetweenspecimenapplicationand
cure the material prior to weight loss determination. Volatile
weighing must be no greater than 15 s.
contentisdeterminedastwoseparatecomponents—processing
volatiles and potential volatiles. Processing volatiles is a 9.4 Cure the test specimen by exposure to UV or EB as
measure of volatile loss during the actual cure process. prescribed by the supplier of the material.
Potential volatiles is a measure of volatile loss that might occur
NOTE 2—If there is any doubt as to the adequacy of the exposure for
during aging or under extreme storage conditions. These
affecting proper cure (6.1), an additional sample can be tested utilizing
volatile content measurements are useful to the producer and
50 % additional exposure and the volatile content results compared. If the
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
measured volatiles, undercure may lead to erroneously high
NOTE 3—Materials that can react with atmospheric moisture during
values. Since various pieces of cure equipment may vary
post cure, that is, UV cationic-curable epoxy materials, may exhibit a
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
scheduleappropriatebothtothematerialtobetestedandtothe
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
305 mm) or heavy gage (0.05 mm minimum) foil. Test panels
Total volatiles 5 % Processing Volatiles1% Potential Volatiles
aremostconvenientandmaybecutintosmallerpiecesforease
where:
of weighing. Precondition the substrate for 30 min at 110 6
A = weight of aluminum substrate, g,
5°C and store in a desiccator prior to use.
B = weight of aluminum substrate plus test specimen, g,
8.2 Forced Draft Oven, Type IIAorType IIB as specified in
C = weight of aluminum substrate plus test specimen after
Specification E145.
cure, g, and
D = weight of aluminum substrate plus cured test specimen
8.3 Ultraviolet Light or Electron Beam Curing Equipment—
after heating.
There are several commercial suppliers of laboratory scale
equipment that simulates industrial curing processes.
11. Precision and Bias
9. Procedure
11.1 Interlaboratory Test Program—An interlaboratory
9.1 Mixthesample,ifnecessary,toensureuniformity.Hand study of volatile content of radiation cured materials (Test
MethodA) was conducted in accordance with Practice E691 in
stirringisrecommendedtoavoidtheentrapmentofairbubbles.
nine laboratories with three materials, with each laboratory
9.2 Weigh the preconditioned aluminum substrate, (8.1)to
obtaining three test results for each material.
0.1 mg (A). The size of the aluminum substrate must allow a
minimum of 0.2 g of material to be applied at the supplier’s
recommended film thickness
...