Appendix A to Subpart D of Part 59 - Determination of Volatile Matter Content of Methacrylate Multicomponent Coatings Used as Traffic Marking Coatings

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.