40 CFR Appendix A to Subpart PPPP of Part 63 - Appendix A to Subpart PPPP of Part 63—Determination of Weight Volatile Matter Content and Weight Solids Content of Reactive Adhesives
1.1 Applicability: This method applies to the determination of weight volatile matter content and weight solids content for most one-part or multiple-part reactive adhesives. Reactive adhesives are composed, in large part, of monomers that react during the adhesive curing reaction, and, as a result, do not volatilize. The monomers become integral parts of the cured adhesive through chemical reaction. At least 70 weight percent of the system, excluding water and non-volatile solids such as fillers, react during the process. This method is not appropriate for cyanoacrylates. For cyanoacrylates, South Coast Air Quality Management District Test Method 316B should be used. This method is not appropriate for one-part moisture cure urethane adhesives or for silicone adhesives. For one-part moisture cure urethane adhesives and for silicone adhesives, EPA Method 24 should be used.
1.2 Principle: One-part and multiple-part reactive adhesives undergo a reactive conversion from liquid to solid during the application and assembly process. Reactive adhesives are applied to a single surface, but then are usually quickly covered with another mating surface to achieve a bonded assembly. The monomers employed in such systems typically react and are converted to non-volatile solids. If left uncovered, as in a EPA Method 24 (or ASTM D2369–10 (Reapproved 2015) e) test, the reaction is inhibited by the presence of oxygen and volatile loss of the reactive components competes more heavily with the cure reaction. If this were to happen under normal use conditions, the adhesives would not provide adequate performance. This method minimizes this undesirable deterioration of the adhesive performance.
2.1 Aluminum foil, aluminum sheet, non-leaching plastic film or non-leaching plastic sheet, approximately 3 inches by 3 inches. Precondition the foil, film, or sheet for 30 minutes in an oven at 110 ±5 degrees Celsius and store in a desiccator prior to use. Use tongs or rubber gloves or both to handle the foil, film, or sheet.
2.2 Flat, rigid support panels slightly larger than the foil, film, or sheet. Polypropylene with a minimum thickness of 1/8 inch is recommended for the support panels. Precondition the support panels for 30 minutes in an oven at 110 ±5 degrees Celsius and store in a desiccator prior to use. Use tongs or rubber gloves or both to handle the support panels.
2.3 Aluminum spacers, 1/8 inch thick. Precondition the spacers for 30 minutes in an oven at 110 ±5 degrees Celsius and store in a desiccator prior to use. Use tongs or rubber gloves or both to handle the spacers.
2.4 Forced draft oven, type IIA or IIB as specified in ASTM E145–94 (Reapproved 2001), “Standard Specification for Gravity-Convection and Forced-Ventilation Ovens” (incorporated by reference, see § 63.14).
2.5 Electronic balance capable of weighing to ±0.0001 grams (0.1 mg).
2.6 Flat bottom weight (approximately 3 lbs) or clamps.
1—The foil, film, or sheet should be thick or rigid enough so that it can be easily handled in the test procedure.
3.1 Two procedures are provided. In Procedure A the initial specimen weight is determined by weighing the foil, film, or sheet before and after the specimen is dispensed onto the foil, film, or sheet. In Procedure B the initial specimen weight is determined by weighing the adhesive cartridge (kit) before and after the specimen is dispensed.
3.2 At least four test specimens should be run for each test material. Run the test at room temperature, 74 degrees Fahrenheit (23 degrees Celsius).
1. Zero electronic balance.
2. Place 2 pieces of aluminum foil (or aluminum sheet, plastic film, or plastic sheet) on scale.
3. Record weight of aluminum foils. (A).
4. Tare balance.
5. Remove top piece of aluminum foil.
6. Dispense a 10 to 15 gram specimen of premixed adhesive onto bottom piece of aluminum foil. Place second piece of aluminum foil on top of the adhesive specimen to make a sandwich.
7. Record weight of sandwich (specimen and aluminum foils). (B).
8. Remove sandwich from scale, place sandwich between two support panels with aluminum spacers at the edges of the support panels to make a supported sandwich. The spacers provide a standard gap. Take care to mate the edges.
9. Place the supported sandwich on a flat surface.
10. Place the weight on top of the supported sandwich to spread the adhesive specimen to a uniform thickness within the sandwich. Check that no adhesive squeezes out from between the pieces of aluminum foil or through tears in the aluminum foil.
11. Allow to cure 24 hours.
12. Remove the sandwich from between the support panels. Record the weight of the sandwich. This is referred to as the 24 hr weight. (C).
13. Bake sandwich at 110 degrees Celsius for 1 hour.
14. Remove sandwich from the oven, place immediately in a desiccator, and cool to room temperature. Record post bake sandwich weight. (D).
1. Zero electronic balance.
2. Place two pieces of aluminum foil (or aluminum sheet, plastic film, or plastic sheet) on scale.
3. Record weight of aluminum foils. (A).
4. Tare balance.
5. Place one support panel on flat surface. Place first piece of aluminum foil on top of this support panel.
6. Record the weight of a pre-mixed sample of adhesive in its container. If dispensing the adhesive from a cartridge (kit), record the weight of the cartridge (kit) plus any dispensing tips. (F).
7. Dispense a 10 to 15 gram specimen of mixed adhesive onto the first piece of aluminum foil. Place second piece of aluminum foil on top of the adhesive specimen to make a sandwich.
8. Record weight of the adhesive container. If dispensing the adhesive from a cartridge (kit), record the weight of the cartridge (kit) plus any dispensing tips. (G).
9. Place the aluminum spacers at the edges of the bottom support panel polypropylene sheet. The spacers provide a standard gap.
10. Place the second support panel on top of the assembly to make a supported sandwich. Take care to mate the edges.
11. Place the supported sandwich on a flat surface.
12. Place the weight on top of the supported sandwich to spread the adhesive specimen to a uniform thickness within the sandwich. Check that no adhesive squeezes out from between the pieces of aluminum foil or through tears in the aluminum foil.
13. Allow to cure 24 hours.
14. Remove the sandwich from between the support panels. Record the weight of the sandwich. This is referred to as the 24 hr weight. (C).
15. Bake sandwich at 110 degrees Celsius for 1 hour.
16. Remove sandwich from the oven, place immediately in a desiccator, and cool to room temperature.
17. Record post-bake sandwich weight. (D).
1—The support panels may be omitted if the aluminum foil (or aluminum sheet, plastic film, or plastic sheet) will not tear and the adhesive specimen will spread to a uniform thickness within the sandwich when the flat weight is placed directly on top of the sandwich.
2—Clamps may be used instead of a flat bottom weight to spread the adhesive specimen to a uniform thickness within the sandwich.
3—When dispensing from a static mixer, purging is necessary to ensure uniform, homogeneous specimens. The weighing in Procedure B, Step 6 must be performed after any purging.
4—Follow the adhesive manufacturer's directions for mixing and for dispensing from a cartridge (kit).
4.1 The total weight loss from curing and baking of each specimen is used to determine the weight percent volatile matter content of that specimen
4.2 The weight volatile matter content of a material is the average of the weight volatile matter content of each specimen of that material. For example, if four specimens of a material were tested, then the weight percent volatile matter content for that material is:
4.3 The weight percent solids content of the material is calculated from the weight percent volatile content of the material.
1—The weight loss during curing and the weight loss during baking may be calculated separately. These values may be useful for identifying sources of variation in the results obtained for different specimens of the same material.
2—For both Procedure A and Procedure B, the weight loss during curing is (S)−[(C)−(A)] and the weight loss during baking is (C)−(D).