ASTM D5403-93(1998)

Designation: D 5403 – 93 (Reapproved l998)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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 end use performance and mutually agreeable to supplier and
purchaser.
1.1 These test methods cover procedures for the determina-
3.1.2 ultraviolet (UV) curing—conversion of a coating from
tion of weight percent volatile content of coatings, inks, and
its application state to its final use state by means of a
adhesives designed to be cured by exposure to ultraviolet light
mechanism initiated by ultraviolet radiation generated by
or to a beam of accelerated electrons.
equipment designed for that purpose.
1.2 Test Method A is applicable to radiation curable mate-
3.1.3 electron beam (EB) curing—conversion of a coating
rials that are essentially 100 % reactive but may contain traces
from its application state to its final use state by means of a
(no more than 3 %) of volatile materials as impurities or
mechanism initiated by electron beam radiation generated by
introduced by the inclusion of various additives.
equipment designed for that purpose.
1.3 Test Method B is applicable to all radiation curable
3.1.4 processing volatiles—loss in specimen weight under
materials but must be used for materials that contain volatile
test conditions that are designed to simulate actual industrial
solvents intentionally introduced to control application viscos-
cure processing conditions.
ity and which are intended to be removed from the material
3.1.5 potential volatiles—loss in specimen weight upon
prior to cure.
heating at 110°C for 60 min after radiation curing.
1.4 These test methods may not be applicable to radiation
3.1.5.1 Discussion—This value is an estimation of volatile
curable materials wherein the volatile material is water, and
loss that may occur during aging or under extreme storage
other procedures may be substituted by mutual consent of the
conditions. Potential volatiles may also be referred to as
producer and user.
residual volatiles.
1.5 This standard does not purport to address all of the
3.1.6 total volatiles—sum of the processing volatiles and
safety problems, if any, associated with its use. It is the
the potential volatiles.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Methods
bility of regulatory limitations prior to use. A specific hazard
4.1 A designated quantity of material is weighed before and
statement is given in Note 9.
after a cure step that simulates normal industrial processing.
2. Referenced Documents The test specimen is weighed again after heating at 110 6 5°C
for 60 min. The percent volatile is calculated from the losses in
2.1 ASTM Standards:
2 weight.
D 2369 Test Method for Volatile Content of Coatings
E 145 Specification for Gravity–Convection and Forced–
5. Significance and Use
Ventilation Ovens
5.1 These test methods are the procedures of choice for
E 177 Practice for Use of the Terms Precision and Bias in
3 determining volatile content of materials designed to be cured
ASTM Methods
by exposure to ultraviolet light or electron beam irradiation.
E 691 Practice for Conducting an Interlaboratory Study to
3 These types of materials contain liquid reactants that react to
Determine the Precision of a Test Method
become part of the film during cure, but, which under the test
3. Terminology conditions of Test Method D 2369, will be erroneously mea-
sured as volatiles. The conditions of these test methods are
3.1 Definitions:
similar to Test Method D 2369 with the inclusion of a step to
3.1.1 cure—the condition of a coating after conversion to
cure the material prior to weight loss determination. Volatile
the final state of cure as measured by tests generally related to
content is determined as two separate components—processing
volatiles and potential volatiles. Processing volatiles is a
These test methods are under the jurisdiction of ASTM Committee D-1 on Paint
measure of volatile loss during the actual cure process.
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.55 on Factory-Applied Coatings on Preformed Products. Potential volatiles is a measure of volatile loss that might occur
Current edition approved May 15, 1993. Published July 1993.
during aging or under extreme storage conditions. These
Annual Book of ASTM Standards, Vol 06.01.
volatile content measurements are useful to the producer and
Annual Book of ASTM Standards, Vol 14.02.
D 5403
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 Heat the test specimen in a forced draft oven (8.2) for 60
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
widely in efficiency, it is essential that dialogue between weight gain during procedure in 9.6. If this occurs, the sample should be
retested and allowed to post cure at room temperature for 48 h after
material manufacturer and testing laboratory establish a cure
procedure in 9.5, and then reweighed prior to procedure in 9.6. The weight
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.
TEST METHOD A 9.7 Allow the test specimen to cool to room temperature in
a desiccator and reweigh to 0.1 mg, (D).
7. Scope
10. Calculations
7.1 This test method is applicable to radiation curable
materials with solvent content less than or equal to 3 %.
10.1 Calculate the weight percent volatiles as follows:
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
are most convenient and may be cut into smaller pieces for ease
where:
of weighing. Precondition the substrate for 30 min at 110 6
A 5 weight of aluminum substrate, g,
5°C and store in a desiccator prior to use.
B 5 weight of aluminum substrate plus test specimen, g,
8.2 Forced Draft Oven, Type IIA or Type IIB as specified in
C 5 weight of aluminum substrate plus test specimen after
Specification E 145.
cure, g, and
8.3 Ultraviolet Light or Electron Beam Curing
D 5 weight of aluminum substrate plus cured test
Equipment—There are several commercial suppliers of labo-
specimen after heating.
ratory scale equipment that simulates industrial curing pro-
cesses.
11. Precision and Bias
11.1 Interlaboratory Test Program—An interlaboratory
9. Procedure
study of volatile content of radiation cured materials (Test
9.1 Mix the sample, if necessary, to ensure uniformity. Hand
Method A) was conducted in accordance with Practice E 691 in
stirring is recommended to avoid the entrapment of air bubbles.
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
11.2 Test Result—The precision information given below
minimum of 0.2 g of material to be applied at the supplier’s
for volatile content in weight percent is for the comparison of
recommended film thickness. Use rubber gloves or tongs, or
two test results, each of which is the average of three test
both, to handle samples.
determinations.
9.3 Apply a minimum of 0.2 g of test specimen to the
11.3 Precision:
aluminum substrate and reweigh to 0.1 mg (B). Prepare a total
Percent
of three test specimens.
Processing Volatiles
95 % repeatability limit (within laboratory) 0.9
NOTE 1—The elapsed time between application and weighing should be
95 % reproducibility limit (between laboratories) 1.6
no greater than 30 s. If the sample to be tested contains any reactive
Potential Volatiles
diluent with a vapor pr
...