['Air Programs']
['Hazardous Air Pollutants']
05/06/2022
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Table 1 to Subpart PPPP of Part 63 - Operating Limits if Using the Emission Rate With Add-On Controls Option
If you are required to comply with operating limits by §63.4491(c), you must comply with the applicable operating limits in the following table:
| For the following device . . . | You must meet the following operating limit . . . | And you must demonstrate continuous compliance with the operating limit by . . . |
|---|---|---|
| 1. Thermal oxidizer | a. The average combustion temperature in any 3-hour period must not fall below the combustion temperature limit established according to §63.4567(a). | i. Collecting the combustion temperature data according to §63.4568(c); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average combustion temperature at or above the temperature limit. |
| 2. Catalytic oxidizer | a. The average temperature measured just before the catalyst bed in any 3-hour period must not fall below the limit established according to §63.4567(b); and either | i. Collecting the temperature data according to §63.4568(c); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average temperature before the catalyst bed at or above the temperature limit. |
| b. Ensure that the average temperature difference across the catalyst bed in any 3-hour period does not fall below the temperature difference limit established according to §63.4567(b)(2); or | i. Collecting the temperature data according to §63.4568(c); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average temperature difference at or above the temperature difference limit. | |
| c. Develop and implement an inspection and maintenance plan according to §63.4567(b)(4). | i. Maintaining an up-to-date inspection and maintenance plan, records of annual catalyst activity checks, records of monthly inspections of the oxidizer system, and records of the annual internal inspections of the catalyst bed. If a problem is discovered during a monthly or annual inspection required by §63.4567(b)(4), you must take corrective action as soon as practicable consistent with the manufacturer's recommendations. | |
| 3. Regenerative carbon adsorber | a. The total regeneration desorbing gas (e.g., steam or nitrogen) mass flow for each carbon bed regeneration cycle must not fall below the total regeneration desorbing gas mass flow limit established according to §63.4567(c); and | i. Measuring the total regeneration desorbing gas (e.g., steam or nitrogen) mass flow for each regeneration cycle according to §63.4568(d); and ii. Maintaining the total regeneration desorbing gas mass flow at or above the mass flow limit. |
| b. The temperature of the carbon bed, after completing each regeneration and any cooling cycle, must not exceed the carbon bed temperature limit established according to §63.4567(c). | i. Measuring the temperature of the carbon bed after completing each regeneration and any cooling cycle according to §63.4568(d); and ii. Operating the carbon beds such that each carbon bed is not returned to service until completing each regeneration and any cooling cycle until the recorded temperature of the carbon bed is at or below the temperature limit. | |
| 4. Condenser | a. The average condenser outlet (product side) gas temperature in any 3-hour period must not exceed the temperature limit established according to §63.4567(d). | i. Collecting the condenser outlet (product side) gas temperature according to §63.4568(e); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average gas temperature at the outlet at or below the temperature limit. |
| 5. Concentrators, including zeolite wheels and rotary carbon adsorbers | a. The average gas temperature of the desorption concentrate stream in any 3-hour period must not fall below the limit established according to §63.4567(e); and | i. Collecting the temperature data according to §63.4568(f); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average temperature at or above the temperature limit. |
| b. The average pressure drop of the dilute stream across the concentrator in any 3-hour period must not fall below the limit established according to §63.4567(e). | i. Collecting the pressure drop data according to §63.4568(f); ii. Reducing the pressure drop data to 3-hour block averages; and iii. Maintaining the 3-hour average pressure drop at or above the pressure drop limit. | |
| 6. Emission capture system that is a PTE according to §63.4565(a) | a. The direction of the air flow at all times must be into the enclosure; and either | i. Collecting the direction of air flow, and either the facial velocity of air through all natural draft openings according to §63.4568(g)(1) or the pressure drop across the enclosure according to §63.4568(g)(2); and ii. Maintaining the facial velocity of air flow through all natural draft openings or the pressure drop at or above the facial velocity limit or pressure drop limit, and maintaining the direction of air flow into the enclosure at all times. |
| b. The average facial velocity of air through all natural draft openings in the enclosure must be at least 200 feet per minute; or | i. See items 6.a.i and 6.a.ii. | |
| c. The pressure drop across the enclosure must be at least 0.007 inch H2O, as established in Method 204 of appendix M to 40 CFR part 51. | i. See items 6.a.i and 6.a.ii. | |
| 7. Emission capture system that is not a PTE according to §63.4565(a) | a. The average gas volumetric flow rate or duct static pressure in each duct between a capture device and add-on control device inlet in any 3-hour period must not fall below the average volumetric flow rate or duct static pressure limit established for that capture device according to §63.4567(f). | i. Collecting the gas volumetric flow rate or duct static pressure for each capture device according to §63.4568(g); ii. Reducing the data to 3-hour block averages; and iii. Maintaining the 3-hour average gas volumetric flow rate or duct static pressure for each capture device at or above the gas volumetric flow rate or duct static pressure limit. |
Table 2 to Subpart PPPP of Part 63 - Applicability of General Provisions to Subpart PPPP of Part 63
You must comply with the applicable General Provisions requirements according to the following table
| Citation | Subject | Applicable to subpart PPPP | Explanation |
|---|---|---|---|
| §63.1(a)(1)-(12) | General Applicability | Yes | |
| §63.1(b)(1)-(3) | Initial Applicability Determination | Yes | Applicability to subpart PPPP is also specified in §63.4481. |
| §63.1(c)(1) | Applicability After Standard Established | Yes | |
| §63.1(c)(2) | Applicability of Permit Program for Area Sources | No | Area sources are not subject to subpart PPPP. |
| §63.1(c)(5) | Extensions and Notifications | Yes | |
| §63.1(c)(6) | Reclassification | Yes | |
| §63.1(e) | Applicability of Permit Program Before Relevant Standard is Set | Yes | |
| §63.2 | Definitions | Yes | Additional definitions are specified in §63.4581. |
| §63.3 | Units and Abbreviations | Yes | |
| §63.4(a)(1)-(2) | Prohibited Activities | Yes | |
| §63.4(b)-(c) | Circumvention/Fragmentation | Yes | |
| §63.5(a) | Construction/Reconstruction | Yes | |
| §63.5(b)(1), (3), (4), (6) | Requirements for Existing, Newly Constructed, and Reconstructed Sources | Yes | |
| §63.5(d)(1)(i)-(ii)(F), (d)(1)(ii)(H), (d)(1)(ii)(J), (d)(1)(iii), (d)(2)-(4) | Application for Approval of Construction/Reconstruction | Yes | |
| §63.5(e) | Approval of Construction/Reconstruction | Yes | |
| §63.5(f) | Approval of Construction/Reconstruction Based on Prior State Review | Yes | |
| §63.6(a) | Compliance With Standards and Maintenance Requirements—Applicability | Yes | |
| §63.6(b)(1)-(5), (b)(7) | Compliance Dates for New and Reconstructed Sources | Yes | Section 63.4483 specifies the compliance dates. |
| §63.6(c)(1), (2), (5) | Compliance Dates for Existing Sources | Yes | Section 63.4483 specifies the compliance dates. |
| §63.6(e)(1)(i)-(ii) | Operation and Maintenance | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4500(b) for general duty requirement. |
| §63.6(e)(1)(iii) | Operation and Maintenance | Yes | |
| §63.6(e)(3)(i), (e)(3)(iii)-(ix) | SSMP | Yes before January 5, 2021. No on and after January 5, 2021 | |
| §63.6(f)(1) | Compliance Except During SSM | Yes before January 5, 2021. No on and after January 5, 2021 | |
| §63.6(f)(2)-(3) | Methods for Determining Compliance | Yes | |
| §63.6(g) | Use of an Alternative Standard | Yes | |
| §63.6(h) | Compliance With Opacity/Visible Emission Standards | No | Subpart PPPP does not establish opacity standards and does not require continuous opacity monitoring systems (COMS). |
| §63.6(i)(1)-(14), (16) | Extension of Compliance | Yes | |
| §63.6(j) | Presidential Compliance Exemption | Yes | |
| §63.7(a)(1) | Performance Test Requirements—Applicability | Yes | Applies to all affected sources. Additional requirements for performance testing are specified in §§63.4564, 63.4565, and 63.4566. |
| §63.7(a)(2), except (a)(2)(i)-(viii) | Performance Test Requirements—Dates | Yes | Applies only to performance tests for capture system and control device efficiency at sources using these to comply with the standards. Section 63.4560 specifies the schedule for performance test requirements that are earlier than those specified in §63.7(a)(2). |
| §63.7(a)(3)-(4) | Performance Tests Required By the Administrator, Force Majeure | Yes | |
| §63.7(b)-(d) | Performance Test Requirements—Notification, Quality Assurance, Facilities Necessary for Safe Testing, Conditions During Test | Yes | Applies only to performance tests for capture system and add-on control device efficiency at sources using these to comply with the standards. |
| §63.7(e)(1) | Conduct of Performance Tests | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4500 and §63.4564(a). |
| §63.7(e)(2)-(4) | Conduct of Performance Tests | Yes | |
| §63.7(f) | Performance Test Requirements—Use Alternative Test Method | Yes | Applies to all test methods except those of used to determine capture system efficiency. |
| §63.7(g)-(h) | Performance Test Requirements—Data Analysis, Recordkeeping, Reporting, Waiver of Test | Yes | Applies only to performance tests for capture system and add-on control device efficiency at sources using these to comply with the standards. |
| §63.8(a)(1)-(2) | Monitoring Requirements—Applicability | Yes | Applies only to monitoring of capture system and add-on control device efficiency at sources using these to comply with the standards. Additional requirements for monitoring are specified in §63.4568. |
| §63.8(a)(4) | Additional Monitoring Requirements | No | Subpart PPPP does not have monitoring requirements for flares. |
| §63.8(b) | Conduct of Monitoring | Yes | |
| §63.8(c)(1) | Continuous Monitoring System (CMS) Operation and Maintenance | Yes before January 5, 2021. No on and after January 5, 2021 | Section 63.4568 specifies the requirements for the operation of CMS for capture systems and add-on control devices at sources using these to comply. |
| §63.8(c)(2)-(3) | CMS Operation and Maintenance | Yes | Applies only to monitoring of capture system and add-on control device efficiency at sources using these to comply with the standard. Additional requirements for CMS operations and maintenance are specified in §63.4568. |
| §63.8(c)(4) | CMS | No | Section 63.4568 specifies the requirements for the operation of CMS for capture systems and add-on control devices at sources using these to comply. |
| §63.8(c)(5) | COMS | No | Subpart PPPP does not have opacity or visible emission standards. |
| §63.8(c)(6) | CMS Requirements | No | Section 63.4568 specifies the requirements for monitoring systems for capture systems and add-on control devices at sources using these to comply. |
| §63.8(c)(7) | CMS Out-of-Control Periods | Yes | |
| §63.8(c)(8) | CMS Out-of-Control Periods and Reporting | No | Section 63.4520 requires reporting of CMS out-of-control periods. |
| §63.8(d)-(e) | Quality Control Program and CMS Performance Evaluation | No | Subpart PPPP does not require the use of continuous emissions monitoring systems. |
| §63.8(f)(1)-(5) | Use of an Alternative Monitoring Method | Yes | |
| §63.8(f)(6) | Alternative to Relative Accuracy Test | No | Subpart PPPP does not require the use of continuous emissions monitoring systems. |
| §63.8(g) | Data Reduction | No | Sections 63.4567 and 63.4568 specify monitoring data reduction. |
| §63.9(a)-(d) | Notification Requirements | Yes | |
| §63.9(e) | Notification of Performance Test | Yes | Applies only to capture system and add-on control device performance tests at sources using these to comply with the standards. |
| §63.9(f) | Notification of Visible Emissions/Opacity Test | No | Subpart PPPP does not have opacity or visible emission standards. |
| §63.9(g) | Additional Notifications When Using CMS | No | Subpart PPPP does not require the use of continuous emissions monitoring systems. |
| §63.9(h)(1)-(3), (5)-(6) | Notification of Compliance Status | Yes | Section 63.4510 specifies the dates for submitting the notification of compliance status. |
| §63.9(i) | Adjustment of Submittal Deadlines | Yes | |
| §63.9(j) | Change in Previous Information | Yes | |
| §63.9(k) | Electronic reporting procedures | Yes | Only as specified in §63.9(j). |
| §63.10(a) | Recordkeeping/Reporting—Applicability and General Information | Yes | |
| §63.10(b)(1) | General Recordkeeping Requirements | Yes | Additional requirements are specified in §§63.4530 and 63.4531. |
| §63.10(b)(2)(i)-(ii) | Recordkeeping of Occurrence and Duration of Startups and Shutdowns and of Failures to Meet Standards | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4530(h). |
| §63.10(b)(2)(iii) | Recordkeeping Relevant to Maintenance of Air Pollution Control and Monitoring Equipment | Yes | |
| §63.10(b)(2)(iv)-(v) | Actions Taken to Minimize Emissions During SSM | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4530(h)(4) for a record of actions taken to minimize emissions during a deviation from the standard. |
| §63.10(b)(2)(vi) | Recordkeeping for CMS Malfunctions | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4530(h) for records of periods of deviation from the standard, including instances where a CMS is inoperative or out-of-control. |
| §63.10(b)(2)(vii)-(xii) | Records | Yes | |
| §63.10(b)(2)(xiii) | No | Subpart PPPP does not require the use of continuous emissions monitoring systems. | |
| §63.10(b)(2)(xiv) | Yes | ||
| §63.10(b)(3) | Recordkeeping Requirements for Applicability Determinations | Yes | |
| §63.10(c)(1), (5)-(6) | Additional Recordkeeping Requirements for Sources with CMS | Yes | |
| §63.10(c)(7)-(8) | Additional Recordkeeping Requirements for Sources with CMS | No | See §63.4530(h) for records of periods of deviation from the standard, including instances where a CMS is inoperative or out-of-control. |
| §63.10(c)(10)-(14) | Additional Recordkeeping Requirements for Sources with CMS | Yes | |
| §63.10(c)(15) | Records Regarding the SSMP | Yes before January 5, 2021. No on and after January 5, 2021 | |
| §63.10(d)(1) | General Reporting Requirements | Yes | Additional requirements are specified in §63.4520. |
| §63.10(d)(2) | Report of Performance Test Results | Yes | Additional requirements are specified in §63.4520(b). |
| §63.10(d)(3) | Reporting Opacity or Visible Emissions Observations | No | Subpart PPPP does not require opacity or visible emissions observations. |
| §63.10(d)(4) | Progress Reports for Sources With Compliance Extensions | Yes | |
| §63.10(d)(5) | SSM Reports | Yes before January 5, 2021. No on and after January 5, 2021 | See §63.4520(a)(7). |
| §63.10(e)(1)-(2) | Additional CMS Reports | No | Subpart PPPP does not require the use of continuous emissions monitoring systems. |
| §63.10(e)(3) | Excess Emissions/CMS Performance Reports | No | Section 63.4520(b) specifies the contents of periodic compliance reports. |
| §63.10(e)(4) | COMS Data Reports | No | Subpart PPPP does not specify requirements for opacity or COMS. |
| §63.10(f) | Recordkeeping/Reporting Waiver | Yes | |
| §63.11 | Control Device Requirements/Flares | No | Subpart PPPP does not specify use of flares for compliance. |
| §63.12 | State Authority and Delegations | Yes | |
| §63.13 | Addresses | Yes | |
| §63.14 | IBR | Yes | |
| §63.15 | Availability of Information/Confidentiality | Yes |
[85 FR 41156, July 8, 2020; 85 FR 73907, Nov. 19, 2020]
Table 3 to Subpart PPPP of Part 63 - Default Organic HAP Mass Fraction for Solvents and Solvent Blends
You may use the mass fraction values in the following table for solvent blends for which you do not have test data or manufacturer's formulation data and which match either the solvent blend name or the chemical abstract series (CAS) number. If a solvent blend matches both the name and CAS number for an entry, that entry's organic HAP mass fraction must be used for that solvent blend. Otherwise, use the organic HAP mass fraction for the entry matching either the solvent blend name or CAS number, or use the organic HAP mass fraction from table 4 to this subpart if neither the name or CAS number match.
| Solvent/solvent blend | CAS. No. | Average organic HAP mass fraction | Typical organic HAP, percent by mass |
|---|---|---|---|
| 1. Toluene | 108-88-3 | 1.0 | Toluene. |
| 2. Xylene(s) | 1330-20-7 | 1.0 | Xylenes, ethylbenzene. |
| 3. Hexane | 110-54-3 | 0.5 | n-hexane. |
| 4. n-Hexane | 110-54-3 | 1.0 | n-hexane. |
| 5. Ethylbenzene | 100-41-4 | 1.0 | Ethylbenzene. |
| 6. Aliphatic 140 | 0 | None. | |
| 7. Aromatic 100 | 0.02 | 1% xylene, 1% cumene. | |
| 8. Aromatic 150 | 0.09 | Naphthalene. | |
| 9. Aromatic naphtha | 64742-95-6 | 0.02 | 1% xylene, 1% cumene. |
| 10. Aromatic solvent | 64742-94-5 | 0.1 | Naphthalene. |
| 11. Exempt mineral spirits | 8032-32-4 | 0 | None. |
| 12. Ligroines (VM & P) | 8032-32-4 | 0 | None. |
| 13. Lactol spirits | 64742-89-6 | 0.15 | Toluene. |
| 14. Low aromatic white spirit | 64742-82-1 | 0 | None. |
| 15. Mineral spirits | 64742-88-7 | 0.01 | Xylenes. |
| 16. Hydrotreated naphtha | 64742-48-9 | 0 | None. |
| 17. Hydrotreated light distillate | 64742-47-8 | 0.001 | Toluene. |
| 18. Stoddard solvent | 8052-41-3 | 0.01 | Xylenes. |
| 19. Super high-flash naphtha | 64742-95-6 | 0.05 | Xylenes. |
| 20. Varsol ® solvent | 8052-49-3 | 0.01 | 0.5% xylenes, 0.5% ethylbenzene. |
| 21. VM & P naphtha | 64742-89-8 | 0.06 | 3% toluene, 3% xylene. |
| 22. Petroleum distillate mixture | 68477-31-6 | 0.08 | 4% naphthalene, 4% biphenyl. |
Table 4 to Subpart PPPP of Part 63 - Default Organic HAP Mass Fraction for Petroleum Solvent Groups a
You may use the mass fraction values in the following table for solvent blends for which you do not have test data or manufacturer's formulation data.
| Solvent type | Average organic HAP mass fraction | Typical organic HAP, percent by mass |
|---|---|---|
| a Use this table only if the solvent blend does not match any of the solvent blends in Table 3 to this subpart by either solvent blend name or CAS number and you only know whether the blend is aliphatic or aromatic. b Mineral Spirits 135, Mineral Spirits 150 EC, Naphtha, Mixed Hydrocarbon, Aliphatic Hydrocarbon, Aliphatic Naphtha, Naphthol Spirits, Petroleum Spirits, Petroleum Oil, Petroleum Naphtha, Solvent Naphtha, Solvent Blend. c Medium-flash Naphtha, High-flash Naphtha, Aromatic Naphtha, Light Aromatic Naphtha, Light Aromatic Hydrocarbons, Aromatic Hydrocarbons, Light Aromatic Solvent. | ||
| Aliphatic b | 0.03 | 1% Xylene, 1% Toluene, and 1% Ethylbenzene. |
| Aromatic c | 0.06 | 4% Xylene, 1% Toluene, and 1% Ethylbenzene. |
Table 5 to Subpart PPPP of Part 63—List of HAP That Must Be Counted Toward Total Organic HAP Content if Present at 0.1 Percent or More by Mass
| Chemical name | CAS No. |
| 1,1,2,2-Tetrachloroethane | 79-34-5 |
| 1,1,2-Trichloroethane | 79-00-5 |
| 1,1-Dimethylhydrazine | 57-14-7 |
| 1,2-Dibromo-3-chloropropane | 96-12-8 |
| 1,2-Diphenylhydrazine | 122-66-7 |
| 1,3-Butadiene | 106-99-0 |
| 1,3-Dichloropropene | 542-75-6 |
| 1,4-Dioxane | 123-91-1 |
| 2,4,6-Trichlorophenol | 88-06-2 |
| 2,4/2,6-Dinitrotoluene (mixture) | 25321-14-6 |
| 2,4-Dinitrotoluene | 121-14-2 |
| 2,4-Toluene diamine | 95-80-7 |
| 2-Nitropropane | 79-46-9 |
| 3,3?-Dichlorobenzidine | 91-94-1 |
| 3,3?-Dimethoxybenzidine | 119-90-4 |
| 3,3?-Dimethylbenzidine | 119-93-7 |
| 4,4?-Methylene bis(2-chloroaniline) | 101-14-4 |
| Acetaldehyde | 75-07-0 |
| Acrylamide | 79-06-1 |
| Acrylonitrile | 107-13-1 |
| Allyl chloride | 107-05-1 |
| alpha-Hexachlorocyclohexane (a-HCH) | 319-84-6 |
| Aniline | 62-53-3 |
| Benzene | 71-43-2 |
| Benzidine | 92-87-5 |
| Benzotrichloride | 98-07-7 |
| Benzyl chloride | 100-44-7 |
| beta-Hexachlorocyclohexane (b-HCH) | 319-85-7 |
| Bis(2-ethylhexyl)phthalate | 117-81-7 |
| Bis(chloromethyl)ether | 542-88-1 |
| Bromoform | 75-25-2 |
| Captan | 133-06-2 |
| Carbon tetrachloride | 56-23-5 |
| Chlordane | 57-74-9 |
| Chlorobenzilate | 510-15-6 |
| Chloroform | 67-66-3 |
| Chloroprene | 126-99-8 |
| Cresols (mixed) | 1319-77-3 |
| DDE | 3547-04-4 |
| Dichloroethyl ether | 111-44-4 |
| Dichlorvos | 62-73-7 |
| Epichlorohydrin | 106-89-8 |
| Ethyl acrylate | 140-88-5 |
| Ethylene dibromide | 106-93-4 |
| Ethylene dichloride | 107-06-2 |
| Ethylene oxide | 75-21-8 |
| Ethylene thiourea | 96-45-7 |
| Ethylidene dichloride (1,1-Dichloroethane) | 75-34-3 |
| Formaldehyde | 50-00-0 |
| Heptachlor | 76-44-8 |
| Hexachlorobenzene | 118-74-1 |
| Hexachlorobutadiene | 87-68-3 |
| Hexachloroethane | 67-72-1 |
| Hydrazine | 302-01-2 |
| Isophorone | 78-59-1 |
| Lindane (hexachlorocyclohexane, all isomers) | 58-89-9 |
| m-Cresol | 108-39-4 |
| Methylene chloride | 75-09-2 |
| Naphthalene | 91-20-3 |
| Nitrobenzene | 98-95-3 |
| Nitrosodimethylamine | 62-75-9 |
| o-Cresol | 95-48-7 |
| o-Toluidine | 95-53-4 |
| Parathion | 56-38-2 |
| p-Cresol | 106-44-5 |
| p-Dichlorobenzene | 106-46-7 |
| Pentachloronitrobenzene | 82-68-8 |
| Pentachlorophenol | 87-86-5 |
| Propoxur | 114-26-1 |
| Propylene dichloride | 78-87-5 |
| Propylene oxide | 75-56-9 |
| Quinoline | 91-22-5 |
| Tetrachloroethene | 127-18-4 |
| Toxaphene | 8001-35-2 |
| Trichloroethylene | 79-01-6 |
| Trifluralin | 1582-09-8 |
| Vinyl bromide | 593-60-2 |
| Vinyl chloride | 75-01-4 |
| Vinylidene chloride | 75-35-4 |
[85 FR 41160, July 8, 2020]
Appendix A to Subpart PPPP of Part 63 - Determination of Weight Volatile Matter Content and Weight Solids Content of Reactive Adhesives
1.0 Applicability and Principle
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.
2.0 Materials and Apparatus
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.
Material and Apparatus Notes
1 - The foil, film, or sheet should be thick or rigid enough so that it can be easily handled in the test procedure.
3.0 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).
Procedure A
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).
Procedure B
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).
Procedural Notes
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).
4.0 Calculations
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
Procedure A
Weight of original specimen (S) = (B)?(A)
Weight of post-bake specimen (P) = (D)?(A)
Total Weight Loss (L) = (S)?(P)
Procedure B
Weight of original specimen (S) = (F)?(G)
Weight of post-bake specimen (P) = (D)?(A)
Total Weight Loss (L) = (S)?(P)
Procedure A and Procedure B
Weight Percent Volatile Matter Content
(V) = [(Total weight loss)/(Initial specimen weight)] × 100 = [(L)/(S)] × 100
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:
V = [V1 V2 V3 V4]/4
Where:
Vi = the weight percent volatile matter content of specimen i of the material.
4.3 The weight percent solids content of the material is calculated from the weight percent volatile content of the material.
Weight Percent Solids Content (N) = 100?(V)
Calculation Notes
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).
[85 FR 41161, July 8, 2020]
Source: 69 FR 20990, Apr. 19, 2004, unless otherwise noted.
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