(a) You must control emissions from each cupola as specified in Table 2 to this subpart.

(b) You must meet the following operating limits for each cupola:

(1) Begin within one hour after the alarm on a bag leak detection system sounds, and complete in a timely manner, corrective actions as specified in your operations, maintenance, and monitoring plan required by § 63.1187 of this subpart.

(2) When the alarm on a bag leak detection system sounds for more than five percent of the total operating time in a six-month reporting period, develop and implement a written quality improvement plan (QIP) consistent with the compliance assurance monitoring requirements of § 64.8(b)-(d) of 40 CFR part 64.

(3) Additionally, on or after the applicable compliance date for each new or reconstructed cupola, you must either:

(i) Maintain the operating temperature of the incinerator so that the average operating temperature for each three-hour block period never falls below the average temperature established during the performance test, or

(ii) Maintain the percent excess oxygen in the cupola at or above the level established during the performance test. You must determine the percent excess oxygen using the following equation:

(a) You must control emissions from each curing oven or combined collection/curing operations as specified in Table 2 to this subpart.

(b) You must meet the following operating limits for each curing oven or combined collection/curing operation:

(1) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder formulation at or below the specification ranges of the resin and binder used during the performance test.

(2) Maintain the operating temperature of each incinerator so that the average operating temperature for each three-hour block period never falls below the average temperature established during the performance test.

(a) Cupolas and curing ovens or combined collection/curing operations. You must comply with the emissions limits specified in Table 2 to this subpart no later than the dates specified in Table 2 to this subpart.

(b) At all times, you must operate and maintain any affected source, including associated air pollution control equipment and monitoring equipment, in a manner consistent with safety and good air pollution control practices for minimizing emissions. Determination of whether such operation and maintenance procedures are being used will be based on information available to the Administrator which may include, but is not limited to, monitoring results, review of operation and maintenance procedures, review of operation and maintenance records, and inspection of the source.

This subpart establishes national emission standards for hazardous air pollutants emitted from existing, new, and reconstructed cupolas and curing ovens at facilities that produce mineral wool.

The definitions of key words used in this subpart are in the Clean Air Act (Act), in § 63.2 of the general provisions in subpart A of this part, and in § 63.1196 of this subpart.

You are subject to this subpart if you own or operate an existing, new, or reconstructed mineral wool production facility that is located at a plant site that is a major source of hazardous air pollutant (HAP) emissions, meaning the plant emits or has the potential to emit any single HAP at a rate of 9.07 megagrams (10 tons) or more per year or any combination of HAPs at a rate of 22.68 megagrams (25 tons) or more per year.

To comply with the PM standards, you must meet all of the following:

(a) Install, adjust, maintain, and continuously operate a bag leak detection system for each fabric filter.

(b) Do a performance test as specified in § 63.1188 of this subpart and show compliance with the PM emission limits while the bag leak detection system is installed, operational, and properly adjusted.

(c) Begin corrective actions specified in your operations, maintenance, and monitoring plan required by § 63.1187 of this subpart within one hour after the alarm on a bag leak detection system sounds. Complete the corrective actions in a timely manner.

(d) Develop and implement a written QIP consistent with compliance assurance monitoring requirements of 40 CFR 64.8(b) through (d) when the alarm on a bag leak detection system sounds for more than five percent of the total operating time in a six-month reporting period.

To comply with the carbon monoxide, carbonyl sulfide, hydrogen fluoride, and hydrogen chloride standards, you must meet the following:

(a) Install, calibrate, maintain, and operate a device that continuously measures the operating temperature in the firebox of each thermal incinerator.

(b) Conduct a performance test as specified in § 63.1188 that shows compliance with the carbon monoxide, carbonyl sulfide, hydrogen fluoride, and hydrogen chloride emissions limits specified in Table 2 to this subpart, while the device for measuring incinerator operating temperature is installed, operational, and properly calibrated. Establish the average operating temperature based on the performance test as specified in § 63.1185(a).

(c) Following the performance test, measure and record the average operating temperature of the incinerator as specified in § 63.1185(b) of this subpart.

(d) Maintain the operating temperature of the incinerator so that the average operating temperature for each three-hour block period never falls below the average temperature established during the performance test.

(e) Operate and maintain the incinerator as specified in your operations, maintenance, and monitoring plan required by § 63.1187 of this subpart.

To comply with the formaldehyde, phenol, and methanol standards, you must meet all of the following:

(a) Install, calibrate, maintain, and operate a device that continuously measures the operating temperature in the firebox of each thermal incinerator.

(b) Conduct a performance test as specified in § 63.1188 while manufacturing the product that requires a binder formulation made with the resin containing the highest free-formaldehyde content specification range. Show compliance with the formaldehyde, phenol, and methanol emissions limits, specified in Table 2 to this subpart, while the device for measuring the control device operating parameter is installed, operational, and properly calibrated. Establish the average operating parameter based on the performance test as specified in § 63.1185(a).

(c) During the performance test that uses the binder formulation made with the resin containing the highest free-formaldehyde content specification range, record the free-formaldehyde content specification range of the resin used, and the formulation of the binder used, including the formaldehyde content and binder specification.

(d) Following the performance test, monitor and record the free-formaldehyde content of each resin lot and the formulation of each batch of binder used, including the formaldehyde, phenol, and methanol content.

(e) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder formulation at or below the specification ranges established during the performance test.

(f) Following the performance test, measure and record the average operating temperature of the incinerator as specified in § 63.1185(b) of this subpart.

(g) Maintain the operating temperature of the incinerator so that the average operating temperature for each three-hour block period never falls below the average temperature established during the performance test.

(h) Operate and maintain the incinerator as specified in your operations, maintenance, and monitoring plan required by § 63.1187 of this subpart.

(i) With prior approval from the Administrator, you may do short-term experimental production runs using resin where the free-formaldehyde content, or binder formulations where the formaldehyde content, is higher than the specification ranges of the resin and binder used during previous performance tests, or using experimental pollution prevention process modifications without first doing additional performance tests. Notification of intent to perform a short-term experimental production run must include the following information:

(1) The purpose of the experimental run.

(2) The affected production process.

(3) How the resin free-formaldehyde content or binder formulation will deviate from previously approved levels or what the experimental pollution prevention process modifications are.

(4) The duration of the experimental run.

(5) The date and time of the experimental run.

(6) A description of any emissions testing to be done during the experimental run.

A bag leak detection system must meet the following requirements:

(a) The bag leak detection system must be certified by the manufacturer to be capable of detecting PM emissions at concentrations of 10 milligrams per actual cubic meter (0.0044 grains per actual cubic foot) or less.

(b) The sensor on the bag leak detection system must provide output of relative PM emissions.

(c) The bag leak detection system must have an alarm that will sound automatically when it detects an increase in relative PM emissions greater than a preset level.

(d) The alarm must be located in an area where appropriate plant personnel will be able to hear it.

(e) For a positive-pressure fabric filter, each compartment or cell must have a bag leak detector. For a negative-pressure or induced-air fabric filter, the bag leak detector must be installed downstream of the fabric filter. If multiple bag leak detectors are required (for either type of fabric filter), detectors may share the system instrumentation and alarm.

(f) Each triboelectric bag leak detection system must be installed, operated, adjusted, and maintained so that it follows EPA's “Fabric Filter Bag Leak Detection Guidance” (EPA-454/R-98-015, September 1997). Other bag leak detection systems must be installed, operated, adjusted, and maintained so that they follow the manufacturer's written specifications and recommendations.

(g) At a minimum, initial adjustment of the system must consist of establishing the baseline output in both of the following ways:

(1) Adjust the range and the averaging period of the device.

(2) Establish the alarm set points and the alarm delay time.

(h) After initial adjustment, the range, averaging period, alarm set points, or alarm delay time may not be adjusted except as specified in the operations, maintenance, and monitoring plan required by § 63.1187 of this subpart. In no event may the range be increased by more than 100 percent or decreased by more than 50 percent over a 365 day period unless a responsible official as defined in § 63.2 of the general provisions in subpart A of this part certifies in writing to the Administrator that the fabric filter has been inspected and found to be in good operating condition.

(a) During the performance test, you must establish the average operating temperature of an incinerator as follows:

(1) Continuously measure the operating temperature of the incinerator.

(2) Determine and record the average temperatures in consecutive 15-minute blocks.

(3) Determine and record the arithmetic average of the recorded average temperatures measured in consecutive 15-minute blocks for each of the one-hour performance test runs.

(4) Determine and record the arithmetic average of the three one-hour average temperatures during the performance test runs. The average of the three one-hour performance test runs establishes the temperature level to use to monitor compliance.

(b) To comply with the requirements for maintaining the operating temperature of an incinerator after the performance test, you must measure and record the average operating temperature of the incinerator as required by §§ 63.1182 and 63.1183 of this subpart. This average operating temperature of the incinerator is based on the arithmetic average of the one-hour average temperatures for each consecutive three-hour period and is determined in the same manner described in paragraphs (a)(1) through (a)(4) of this section.

You may change control device and process operating parameter levels established during performance tests and used to monitor compliance if you do the following:

(a) You must notify the Administrator of your desire to expand the range of a control device or process operating parameter level.

(b) Upon approval from the Administrator, you must conduct additional performance tests at the proposed new control device or process operating parameter levels. Before operating at these levels, the performance test results must verify that, at the new levels, you comply with the emission limits in §§ 63.1178 and 63.1179 of this subpart.

(a) An operations, maintenance, and monitoring plan must be submitted to the Administrator for review and approval as part of your application for the title V permit.

(b) The operations, maintenance, and monitoring plan must include the following:

(1) Process and control device parameters you will monitor to determine compliance, along with established operating levels or ranges for each process or control device.

(2) A monitoring schedule.

(3) Procedures for properly operating and maintaining control devices used to meet the standards in §§ 63.1178 and 63.1179 of this subpart. These procedures must include an inspection of each incinerator at least once per year. At a minimum, you must do the following as part of an incinerator inspection:

(i) Inspect all burners, pilot assemblies, and pilot sensing devices for proper operation. Clean pilot sensor if necessary.

(ii) Ensure proper adjustment of combustion air, and adjust if necessary.

(iii) Inspect, when possible, all internal structures (such as baffles) to ensure structural integrity per the design specifications.

(iv) Inspect dampers, fans, and blowers for proper operation.

(v) Inspect motors for proper operation.

(vi) Inspect, when possible, combustion chamber refractory lining. Clean, and repair or replace lining if necessary.

(vii) Inspect incinerator shell for proper sealing, corrosion, and/or hot spots.

(viii) For the burn cycle that follows the inspection, document that the incinerator is operating properly and make any necessary adjustments.

(ix) Generally observe whether the equipment is maintained in good operating condition.

(x) Complete all necessary repairs as soon as practicable.

(4) Procedures for keeping records to document compliance.

(5) Corrective actions you will take if process or control device parameters vary from the levels established during performance testing. For bag leak detection system alarms, example corrective actions that may be included in the operations, maintenance, and monitoring plan include:

(i) Inspecting the fabric filter for air leaks, torn or broken bags or filter media, or any other condition that may cause an increase in emissions.

(ii) Sealing off defective bags or filter media.

(iii) Replacing defective bags or filter media, or otherwise repairing the control device.

(iv) Sealing off a defective fabric filter compartment.

(v) Cleaning the bag leak detection system probe, or otherwise repairing the bag leak detection system.

(vi) Shutting down the process producing the particulate emissions.

You must meet the following performance test requirements:

(a) All monitoring systems and equipment must be installed, operational, and properly calibrated before the performance tests.

(b) Conduct a performance test, consisting of three test runs, for each cupola and curing oven or combined collection/curing operation subject to this subpart at the maximum production rate to demonstrate compliance with each of the applicable emissions limits specified in Table 2 to this subpart.

(c) Following the initial performance or compliance test to be conducted within 180 days of the effective date of this rule, you must conduct a performance test to demonstrate compliance with each of the applicable emissions limits specified in Table 2 to this subpart, at least once every 5 years.

(d) To demonstrate compliance with the applicable emission limits specified in Table 2 to this subpart, measure emissions of PM, carbon monoxide, carbonyl sulfide, hydrogen fluoride, and hydrogen chloride from each existing, new, or reconstructed cupola.

(e) To demonstrate compliance with the applicable emission limits specified in Table 2 to this subpart, measure emissions of formaldehyde, phenol, and methanol from each existing, new, or reconstructed curing oven or combined collection/curing operation.

(f) To demonstrate compliance with the applicable emission limits specified in Table 2 to this subpart, measure emissions at the outlet of the control device for PM, carbon monoxide, carbonyl sulfide, hydrogen fluoride, hydrogen chloride, formaldehyde, phenol, and methanol.

(g) To determine the average melt rate, measure and record the amount of raw materials, excluding coke, charged into and melted in each cupola during each performance test run. Determine and record the average hourly melt rate for each performance test run. Determine and record the arithmetic average of the average hourly melt rates associated with the three performance test runs. The average hourly melt rate of the three performance test runs is used to determine compliance with the applicable emission limits.

(h) Compute and record the average emissions of the three performance test runs and use the equations in § 63.1190 of this subpart to determine compliance with the applicable emission limits.

(i) Comply with control device and process operating parameter monitoring requirements for performance testing as specified in this subpart.

You must use the following test methods to determine compliance with the applicable emission limits:

(a) Method 1 in appendix A to part 60 of this chapter for the selection of the sampling port locations and number of sampling ports.

(b) Method 2 in appendix A to part 60 of this chapter for stack gas velocity and volumetric flow rate.

(c) Method 3 or 3A in appendix A to part 60 of this chapter for oxygen and carbon dioxide for diluent measurements needed to correct the concentration measurements to a standard basis.

(d) Method 4 in appendix A to part 60 of this chapter for moisture content of the stack gas.

(e) Method 5 in appendix A to part 60 of this chapter for the concentration of PM. Each PM test run must consist of a minimum run time of three hours and a minimum sample volume of 3.75 dscm (135 dscf).

(f) Method 10 in appendix A to part 60 of this chapter for the concentration of CO, using the continuous sampling option described in section 7.1.1 of the method. Each CO test run must consist of a minimum run time of one hour.

(g) Method 318 at 40 CFR part 60, appendix A to this part for the concentration of formaldehyde, phenol, methanol, and carbonyl sulfide.

(h) Method to determine the free-formaldehyde content of each resin lot in appendix A of this subpart.

(i) Method 26A or 320 at 40 CFR part 60, appendix A to this part for the concentration of hydrogen fluoride and hydrogen chloride.

(a) Using the results of the performance tests, you must use the following equation to determine compliance with the PM emission limit:

(b) Using the results from the performance tests, you must use the following equation to determine compliance with the carbon monoxide, carbonyl sulfide, hydrogen fluoride, hydrogen chloride, formaldehyde, phenol, and methanol numerical emissions limits as specified in Table 2 to this subpart:

You must submit written or electronic notifications to the Administrator as required by § 63.9(b) through (h). Electronic notifications are encouraged when possible. These notifications include, but are not limited to, the following:

(a) Notification that the following types of sources are subject to the standard:

(1) An area source that increases its emissions so that it becomes a major source.

(2) A source that has an initial startup before the effective date of the standard.

(3) A new or reconstructed source that has an initial startup after the effective date of the standard and doesn't require an application for approval of construction or reconstruction under § 63.5(d) of the general provisions in subpart A of this part.

(b) Notification of intention to construct a new major source or reconstruct a major source where the initial startup of the new or reconstructed source occurs after the effective date of the standard and an application for approval of construction or reconstruction under § 63.5(d) of the general provisions in subpart A of this part is required.

(c) Notification of special compliance obligations for a new source that is subject to special compliance requirements in § 63.6(b)(3) and (4) of the general provisions in subpart A of this part.

(d) Notification of a performance test at least 60 calendar days before the performance test is scheduled to begin.

(e) Notification of compliance status.

You must meet the following recordkeeping requirements:

(a) Maintain files of all information required by § 63.10(b) of the general provisions in subpart A of this part, including all notifications and reports.

(b) Maintain records of the following information also:

(1) Cupola production (melt) rate (Mg/hr (tons/hr) of melt).

(2) All bag leak detection system alarms. Include the date and time of the alarm, when corrective actions were initiated, the cause of the alarm, an explanation of the corrective actions taken, and when the cause of the alarm was corrected.

(3) The free-formaldehyde content of each resin lot and the binder formulation, including formaldehyde content, of each binder batch used in the manufacture of bonded products.

(4) Incinerator operating temperature and results of incinerator inspections. For all periods when the average temperature in any three-hour block period fell below the average temperature established during the performance test, and all periods when the inspection identified incinerator components in need of repair or maintenance, include the date and time of the problem, when corrective actions were initiated, the cause of the problem, an explanation of the corrective actions taken, and when the cause of the problem was corrected.

(c) Retain each record for at least five years following the date of each occurrence, measurement, corrective action, maintenance, record, or report. The most recent two years of records must be retained at the facility. The remaining three years of records may be retained off site.

(d) Records must be maintained in a form suitable and readily available for expeditious review, according to § 63.10 of the General Provisions that are referenced in Table 1 to this subpart. Electronic recordkeeping is encouraged.

(e) Report the required information on paper or on a labeled computer disk using commonly available and compatible computer software.

You must prepare and submit reports to the Administrator as required by this subpart and § 63.10 of the general provisions in subpart A of this part. These reports include, but are not limited to, the following:

(a) Within 60 days after the date of completing each performance test (as defined in § 63.2) required by this subpart, you must submit the results of the performance tests, including any associated fuel analyses, following the procedure specified in either paragraph (a)(1) or (2) of this section.

(1) For data collected using test methods supported by the EPA's Electronic Reporting Tool (ERT) as listed on the EPA's ERT Web site (http://www.epa.gov/ttn/chief/ert/index.html), you must submit the results of the performance test to the EPA via the Compliance and Emissions Data Reporting Interface (CEDRI). CEDRI can be accessed through the EPA's Central Data Exchange (CDX) (http://cdx.epa.gov/epa_home.asp). Performance test data must be submitted in a file format generated through the use of the EPA's ERT. Alternatively, you may submit performance test data in an electronic file format consistent with the extensible markup language (XML) schema listed on the EPA's ERT Web site, once the XML schema is available. If you claim that some of the performance test information being submitted is confidential business information (CBI), you must submit a complete file generated through the use of the EPA's ERT or an alternate electronic file consistent with the XML schema listed on the EPA's ERT Web site, including information claimed to be CBI, on a compact disc, flash drive, or other commonly used electronic storage media to the EPA. The electronic media must be clearly marked as CBI and mailed to U.S. EPA/OAPQS/CORE CBI Office, Attention: Group Leader, Measurement Policy Group, MD C404-02, 4930 Old Page Rd., Durham, NC 27703. The same ERT or alternate file with the CBI omitted must be submitted to the EPA via the EPA's CDX as described earlier in this paragraph.

(2) For data collected using test methods that are not supported by the EPA's ERT as listed on the EPA's ERT Web site, you must submit the results of the performance test to the Administrator at the appropriate address listed in § 63.13.

(b) [Reserved]

(c) A report of each event as required by § 63.10(b) of the general provisions in subpart A of this part, including a report if an action taken during a startup, shutdown, or malfunction is inconsistent with the procedures in the plan as described in § 63.6(e)(3) of the general provisions in subpart A of this part.

(d) An operations, maintenance, and monitoring plan as specified in § 63.1187 of this subpart.

(e) A semiannual report as required by § 63.10(e)(3) of the general provisions in subpart A of this part if measured emissions exceed the applicable standard or a monitored parameter varies from the level established during performance testing. The report must contain the information specified in § 63.10(c) of the general provisions, as well as the relevant records required by § 63.1192(b) of this subpart.

(f) A semiannual report stating that no excess emissions or deviations of monitored parameters occurred during the reporting period as required by § 63.10(e)(3)(v) of the general provisions in subpart A of this part if no deviations have occurred.

(g) All reports required by this subpart not subject to the requirements in paragraph (a) of this section must be sent to the Administrator at the appropriate address listed in § 63.13. If acceptable to both the Administrator and the owner or operator of a source, these reports may be submitted on electronic media. The Administrator retains the right to require submittal of reports subject to paragraph (a) of this section in paper format.

The general provisions in subpart A of this part define requirements applicable to all owners and operators affected by NESHAP in part 63. See Table 1 of this subpart for general provisions that apply (or don't apply) to you as an owner or operator subject to the requirements of this subpart.

(a) This subpart can be implemented and enforced by the U.S. EPA, or a delegated authority such as the applicable State, local, or Tribal agency. If the U.S. EPA Administrator has delegated authority to a State, local, or Tribal agency, then that agency, in addition to the U.S. EPA, has the authority to implement and enforce this subpart. Contact the applicable U.S. EPA Regional Office to find out if implementation and enforcement of this subpart is delegated to a State, local, or Tribal agency.

(b) In delegating implementation and enforcement authority of this subpart to a State, local, or Tribal agency under subpart E of this part, the authorities contained in paragraph (c) of this section are retained by the Administrator of U.S. EPA and cannot be transferred to the State, local, or Tribal agency.

(c) The authorities that cannot be delegated to State, local, or Tribal agencies are as specified in paragraphs (c)(1) through (4) of this section.

(1) Approval of alternatives to the requirements in §§ 63.1177 through 63.1180.

(2) Approval of major alternatives to test methods under § 63.7(e)(2)(ii) and (f), as defined in § 63.90, and as required in this subpart.

(3) Approval of major alternatives to monitoring under § 63.8(f), as defined in § 63.90, and as required in this subpart.

(4) Approval of major alternatives to recordkeeping and reporting under § 63.10(f), as defined in § 63.90, and as required in this subpart.

Terms used in this subpart are defined in the Act, in § 63.2 of the general provisions in subpart A of this part, and in this section as follows:

Bag leak detection system means a monitoring device for a fabric filter that identifies an increase in particulate matter emissions resulting from a broken filter bag or other malfunction and sounds an alarm.

Bonded product means mineral wool to which a hazardous air pollutant-based binder (containing such hazardous air pollutants as phenol or formaldehyde) has been applied.

Closed-top cupola means a cupola that operates as a closed (process) system and has a restricted air flow rate.

CO means, for the purposes of this subpart, emissions of carbon monoxide that serve as a surrogate for emissions of carbonyl sulfide, a compound included on the list of hazardous air pollutants in section 112 of the Act.

Combined collection/curing operations means the combination of fiber collection operations and curing ovens used to make bonded products.

Cupola means a large, water-cooled metal vessel to which is charged a mixture of fuel, rock and/or slag, and additives. As the fuel is burned, the charged mixture is heated to a molten state for later processing to form mineral wool.

Curing oven means a chamber in which heat is used to thermoset a binder on the mineral wool fiber used to make bonded products.

Fabric filter means an air pollution control device used to capture particulate matter by filtering gas streams through fabric bags. It also is known as a baghouse.

Formaldehyde means, for the purposes of this subpart, emissions of formaldehyde that, in addition to being a HAP itself, serve as a surrogate for organic compounds included on the list of hazardous air pollutants in section 112 of the Act, including but not limited to phenol.

Hazardous air pollutant means any air pollutant listed in or pursuant to section 112(b) of the Act.

I means the owner or operator of a mineral wool production facility.

Incinerator means an enclosed air pollution control device that uses controlled flame combustion to convert combustible materials to noncombustible gases. For the purposes of this subpart, the term “incinerator” means “regenerative thermal oxidizer”.

Melt means raw materials, excluding coke, that are charged into the cupola, heated to a molten state, and discharged to the fiber forming and collection process.

Melt rate means the mass of molten material discharged from a single cupola over a specified time period.

Mineral wool means a fibrous glassy substance made from natural rock (such as basalt), blast furnace slag or other slag, or a mixture of rock and slag. It may be used as a thermal or acoustical insulation material or in the making of other products to provide structural strength, sound absorbency, fire resistance, or other required properties.

New Source means any affected source that commences construction or reconstruction after May 8, 1997 for purposes of determining the applicability of the emissions limits in Rows 1-4 of Table 2. For all other emission limits new source means any affected source that commences construction or reconstruction after November 25, 2011.

Open-top cupola means a cupola that is open to the outside air and operates with an air flow rate that is unrestricted and at low pressure.

PM means, for the purposes of this subpart, emissions of particulate matter that serve as a surrogate for metals (in particulate or volatile form) on the list of hazardous air pollutants in section 112 of the Act, including but not limited to: antimony, arsenic, beryllium, cadmium, chromium, lead, manganese, nickel, and selenium.

Slag means the by-product materials separated from metals during smelting and refining of raw ore.

You means the owner or operator of a mineral wool production facility.

(a) The provisions set forth in this subpart apply at all times.

(b) You must not shut down items of equipment that are utilized for compliance with this subpart during times when emissions are being, or are otherwise required to be, routed to such items of equipment.

(c) Startup begins when fuels are ignited in the cupola. Startup ends when the cupola produces molten material.

(d) Shutdown begins when the cupola has reached the end of the melting campaign and is empty. No molten material continues to flow from the cupola during shutdown.

(e) During periods of startups and shutdowns you must operate your cupola according to one of the following methods:

(1) You must keep records showing that your emissions were controlled using air pollution control devices operated at the parameters established by the most recent performance test that showed compliance with the standard; or

(2) You must keep records showing the following:

(i) You used only clean fuels during startup and shutdown; and

(ii) You operate the cupola during startup and shutdown with three percent oxygen over the fuel demand for oxygen.

The method in this appendix was specifically developed for water-soluble phenolic resins that have a relatively high free-formaldehyde (FF) content such as insulation resins. It may also be suitable for other phenolic resins, especially those with a high FF content.

2.1 a. The basis for this method is the titration of the hydrochloric acid that is liberated when hydroxylamine hydrochloride reacts with formaldehyde to form formaldoxine:

b. Free formaldehyde in phenolic resins is present as monomeric formaldehyde, hemiformals, polyoxymethylene hemiformals, and polyoxymethylene glycols. Monomeric formaldehyde and hemiformals react rapidly with hydroxylamine hydrochloride, but the polymeric forms of formaldehyde must hydrolyze to the monomeric state before they can react. The greater the concentration of free formaldehyde in a resin, the more of that formaldehyde will be in the polymeric form. The hydrolysis of these polymers is catalyzed by hydrogen ions.

2.2 The resin sample being analyzed must contain enough free formaldehyde so that the initial reaction with hydroxylamine hydrochloride will produce sufficient hydrogen ions to catalyze the depolymerization of the polymeric formaldehyde within the time limits of the test method. The sample should contain approximately 0.3 grams (g) free formaldehyde to ensure complete reaction within 5 minutes.

3.1 Balance, readable to 0.01 g or better.

3.2 pH meter, standardized to pH 4.0 with pH 4.0 buffer and pH 7 with pH 7.0 buffer.

3.3 50-mL burette for 1.0 N sodium hydroxide.

3.4 Magnetic stirrer and stir bars.

3.5 250-mL beaker.

3.6 50-mL graduated cylinder.

3.7 100-mL graduated cylinder.

3.8 Timer.

4.1 Standardized 1.0 N sodium hydroxide solution.

4.2 Hydroxylamine hydrochloride solution, 100 grams per liter, pH adjusted to 4.00.

4.3 Hydrochloric acid solution, 1.0 N and 0.1 N.

4.4 Sodium hydroxide solution, 0.1 N.

4.5 50/50 v/v mixture of distilled water and methyl alcohol.

5.1 Determine the sample size as follows:

a. If the expected FF is greater than 2 percent, go to Part A in 5.1.c to determine sample size.

b. If the expected FF is less than 2 percent, go to Part B in 5.1.d to determine sample size.

c. Part A: Expected FF ≥2 percent.

I. The following table shows example levels:

ii. It is very important to the accuracy of the results that the sample size be chosen correctly. If the milliliters of titrant are less than 15 mL or greater than 30 mL, reestimate the needed sample size and repeat the tests.

d. Part B: Expected FF <2 percent

I. The following table shows example levels:

ii. If the milliliters of titrant are less than 5 mL or greater than 30 mL, reestimate the needed sample size and repeat the tests.

5.2 Weigh the resin sample to the nearest 0.01 grams into a 250-mL beaker. Record sample weight.

5.3 Add 100 mL of the methanol/water mixture and stir on a magnetic stirrer. Confirm that the resin has dissolved.

5.4 Adjust the resin/solvent solution to pH 4.0, using the prestandardized pH meter, 1.0 N hydrochloric acid, 0.1 N hydrochloric acid, and 0.1 N sodium hydroxide.

5.5 Add 50 mL of the hydroxylamine hydrochloride solution, measured with a graduated cylinder. Start the timer.

5.6 Stir for 5 minutes. Titrate to pH 4.0 with standardized 1.0 N sodium hydroxide. Record the milliliters of titrant and the normality.

Test values should conform to the following statistical precision:

This method was prepared by K.K. Tutin and M.L. Foster, Tacoma R&D Laboratory, Georgia-Pacific Resins, Inc. (Principle written by R. R. Conner.)

9.1 GPAM 2221.2.

9.2 PR&C TM 2.035.

9.3 Project Report, Comparison of Free Formaldehyde Procedures, January 1990, K. Tutin.