Appendix A to Subpart D of Part 59 - Determination of Volatile Matter Content of Methacrylate Multicomponent Coatings Used as Traffic Marking Coatings
40:6.0.1.1.7.4.6.15.45 : Appendix A
Appendix A to Subpart D of Part 59 - Determination of Volatile
Matter Content of Methacrylate Multicomponent Coatings Used as
Traffic Marking Coatings 1.0 Principle and Applicability
1.1 Applicability. This modification to Method 24 of appendix A
of 40 CFR part 60 applies to the determination of volatile matter
content of methacrylate multicomponent coatings used as traffic
marking coatings.
1.2 Principle. A known amount of methacrylate multicomponent
coating is dispersed in a weighing dish using a stirring device
before the volatile matter is removed by heating in an oven.
2.0 Procedure
2.1 Prepare about 100 milliliters (mL) of sample by mixing the
components in a storage container, such as a glass jar with a screw
top or a metal can with a cap. The storage container should be just
large enough to hold the mixture. Combine the components (by weight
or volume) in the ratio recommended by the manufacturer. Tightly
close the container between additions and during mixing to prevent
loss of volatile materials. Most manufacturers' mixing instructions
are by volume. Because of possible error caused by expansion of the
liquid when measuring the volume, it is recommended that the
components be combined by weight. When weight is used to combine
the components and the manufacturer's recommended ratio is by
volume, the density must be determined by section 3.5 of Method 24
of appendix A of 40 CFR part 60.
2.2 Immediately after mixing, take aliquots from this 100 mL
sample for determination of the total volatile content, water
content, and density. To determine water content, follow section
3.4 of Method 24 of appendix A of 40 CFR part 60. To determine
density, follow section 3.5 of Method 24. To determine total
volatile content, use the apparatus and reagents described in
section 3.8.2 of Method 24 and the following procedures:
2.2.1 Weigh and record the weight of an aluminum foil weighing
dish and a metal paper clip. Using a syringe as specified in
section 3.8.2.1 of Method 24, weigh to 1 milligrams (mg), by
difference, a sample of coating into the weighing dish. For
methacrylate multicomponent coatings used for traffic marking use
3.0 ±0.1 g.
2.2.2 Add the specimen and use the metal paper clip to disperse
the specimen over the surface of the weighing dish. If the material
forms a lump that cannot be dispersed, discard the specimen and
prepare a new one. Similarly, prepare a duplicate. The sample shall
stand for a minimum of 1 hour, but no more than 24 hours before
being oven dried at 110 ±5 degrees Celsius for 1 hour.
2.2.3 Heat the aluminum foil dishes containing the dispersed
specimens in the forced draft oven for 60 minutes at 110 ±5 degrees
Celsius. Caution - provide adequate ventilation, consistent with
accepted laboratory practice, to prevent solvent vapors from
accumulating to a dangerous level.
2.2.4 Remove the dishes from the oven, place immediately in a
desiccator, cool to ambient temperature, and weigh to within 1 mg.
After weighing, break up the film of the coating using the metal
paper clip. Weigh dish to within 1 mg. Return to forced draft oven
for an additional 60 minutes at 110 ±5 degrees Celsius.
2.2.5 Remove the dishes from the oven, place immediately in a
desiccator, cool to ambient temperature, and weigh to within 1
mg.
2.2.6 Run analyses in pairs (duplicate sets for each coating
mixture until the criterion in section 4.3 of Method 24 of appendix
A of 40 CFR part 60 is met. Calculate the weight of volatile matter
for each heating period following Equation 24-2 of Method 24 and
record the arithmetic average. Add the arithmetic average for the
two heating periods to obtain the weight fraction of the volatile
matter.
3.0 Data Validation Procedure
3.1 Follow the procedures in Section 4 of Method 24 of appendix
A to 40 CFR part 60.
3.2 If more than 10 percent of the sample is lost when the
sample is being broken up in 2.2.4, the sample is invalid.
4.0 Calculations
Follow the calculation procedures in Section 5 of Method 24 of
appendix A of 40 CFR part 60.
