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Subpart DDD—National Emission Standards for Hazardo us Air Pollutants for Mineral Wool Production
Contents Subpart DDD—National Emission Standards for Hazardo us Air Pollutants for Mineral Wool Production § 63.1175 What is the purpose of this subpart? § 63.1176 Where can I find definitions of key words used in this subpart? § 63.1177 Am I subject to this subpart? Standards § 63.1178 For cupolas, what standards must I meet? § 63.1179 For curing ovens, what standards must I m eet? § 63.1180 When must I meet these standards? Compliance With Standards § 63.1181 How do I comply with the particulate matt er standards for existing, new, and reconstructed cupolas? § 63.1182 How do I comply with the carbon monoxide standards for new and reconstructed cupolas? § 63.1183 How do I comply with the formaldehyde sta ndards for existing, new, and reconstructed curing ovens? Additional Monitoring Information § 63.1184 What do I need to know about the design specifications, installation, and operation of a ba g leak detection system? § 63.1185 How do I establish the average operating temperature of an incinerator? § 63.1186 How may I change the compliance levels of monitored parameters? § 63.1187 What do I need to know about operations, maintenance, and monitoring plans? Performance Tests and Methods § 63.1188 What performance test requirements must I meet? § 63.1189 What test methods do I use? § 63.1190 How do I determine compliance? Notification, Recordkeeping, and Reporting § 63.1191 What notifications must I submit?Page 2 of 53

§ 63.1192 What recordkeeping requirements must I me et? § 63.1193 What reports must I submit? Other Requirements and Information § 63.1194 Which general provisions apply? § 63.1195 Who implements and enforces this subpart? § 63.1196 What definitions should I be aware of? §§ 63.1197-63.1199 [Reserved] Appendix A to Subpart DDD of Part 63—Free Formaldeh yde Analysis of Insulation Resins by the Hydroxylamine Hydrochlo ride Method § 63.1175 What is the purpose of this subpart? This subpart establishes national emission standard s for hazardous air pollutants emitted from existing, new , and reconstructed cupolas and curing ovens at facilitie s that produce mineral wool. § 63.1176 Where can I find definitions of key words used in this subpart? The definitions of key words used in this subpart a re in the Clean Air Act (Act), in § 63.2 of the general p rovisions in subpart A of this part, and in § 63.1196 of this su bpart. § 63.1177 Am I subject to this subpart? You are subject to this subpart if you own or opera te an existing, new, or reconstructed mineral wool produc tion facility that is located at a plant site that is a major sou rce of hazardous air pollutant (HAP) emissions, meaning th e plant emits or has the potential to emit any single HAP at a ra te of 9.07Page 3 of 53

megagrams (10 tons) or more per year or any combina tion of HAPs at a rate of 22.68 megagrams (25 tons) or more per year. Standards § 63.1178 For cupolas, what standards must I meet? (a) You must control emissions from each cupola as follows: (1) Limit emissions of particulate matter (PM) from each existing, new, or reconstructed cupola to 0.05 kilo grams (kg) of PM per megagram (MG) (0.10 pound [lb] of PM per ton ) of melt or less. (2) Limit emissions of carbonyl sulfide from each e xisting, new, or reconstructed closed-top cupola to the foll owing: (i) 3.4 lb of carbonyl sulfide per ton melt or less for existing closed-top cupolas. (ii) 0.062 lb of carbonyl sulfide per ton melt or l ess for new or reconstructed closed-top cupolas. (3) Limit emissions of carbonyl sulfide from each e xisting, new, or reconstructed open-top cupola to the follow ing: (i) 6.8 lb of carbonyl sulfide per ton melt or less for existing open-top cupolas. (ii) 3.2 lb of carbonyl sulfide per ton melt or les s for new or reconstructed open-top cupolas. (4) Limit emissions of hydrogen fluoride from each existing, new, or reconstructed cupola to the follo wing:Page 4 of 53

(i) 0.16 lb of hydrogen fluoride per ton of melt or less for existing cupolas using slag as a raw material. (ii) 0.015 lb of hydrogen fluoride per ton of melt or less for new or reconstructed cupolas using slag as a ra w material. (iii) 0.13 lb of hydrogen fluoride per ton of melt or less for existing cupolas that do not use slag as a raw material. (iv) 0.018 lb of hydrogen fluoride per ton of melt or less for new or reconstructed cupolas that do not use sl ag as a raw material. (5) Limit emissions of hydrogen chloride from each existing, new, or reconstructed cupola to the follo wing: (i) 0.44 lb of hydrogen chloride per ton of melt or less for existing cupolas using slag as a raw material. (ii) 0.012 lb of hydrogen chloride per ton of melt or less for new or reconstructed cupolas using slag as a ra w material. (iii) 0.43 lb of hydrogen chloride per ton of melt or less for existing cupolas that do not use slag as a raw material. (iv) 0.015 lb of hydrogen chloride per ton of melt or less for new or reconstructed cupolas that do not use sl ag as a raw material.(2) Limit emissions of carbon monoxide (CO ) from each new or reconstructed cupola to either of the follow ing: (i) 0.05 kg of CO per MG (0.10 lb of CO per ton) of melt or less.Page 5 of 53

(ii) A reduction of uncontrolled CO emissions by at least 99 percent. (b) You must meet the following operating limits fo r each cupola: (1) Begin within one hour after the alarm on a bag leak detection system sounds, and complete in a timely m anner, corrective actions as specified in your operations, maintenance, and monitoring plan required by §63.1187 of this su bpart. (2) When the alarm on a bag leak detection system s ounds for more than five percent of the total operating t ime in a sixmonth reporting period, develop and implement a wri tten quality improvement plan (QIP) consistent with the complian ce assurance monitoring requirements of §64.8(b)-(d) of 40 CFR p art 64. (3) Additionally, for each new or reconstructed cup ola, you must either: (i) Mm aintain the operating temperature of the incinerato r so that the average operating temperature for each three-hour block period never falls below the average temperat ure established during the performance test ., or (ii) Maintain the percent excess oxygen in the cupo la at or above the level established during the performance test. You must determine the percent excess oxygen using the following equation:Page 6 of 53

Percent	excess	oxygen =  Oxygen	available Fuel	demand	for	oxygen  − 1  ∗ 100

where:
Percent excess oxygen = Percentage of excess oxygen present above the stoichiometric balance of 1.00, (%).

1.00 = Ratio of oxygen in a cupola combustion chamber divided by the stoichiometric quantity of oxygen required to obtain complete combustion of fuel. Oxygen available = Quantity of oxygen introduced into the cupola combustion zone. Fuel demand for oxygen = Required quantity of oxygen for stoichiometric combustion of the quantity of fuel present.

§ 63.1179 For combined collection/curing operationscuring ovens , what standards must I meet? (a) You must control emissions from each existing, new, and reconstructed combined collection/curing operations by limiting emissions of formaldehyde, phenol, and methanol to the following: (1) For combined drum collection/ curing operations : (i) 0.17 lb of formaldehyde per ton melt or less, (ii) 0.85 lb of phenol per ton melt or less, and (iii) 0.28 lb of methanol per ton melt or less. (2) For combined horizontal collection/curing opera tions: (i) 0.63 lb of formaldehyde per ton melt or less, (ii) 0.12 lb of phenol per ton melt or less, and (iii) 0.049 lb of methanol per ton melt or less.Page 7 of 53

(3) For combined vertical collection/ curing operat ions: (i) 2.4 lb of formaldehyde per ton melt or less, (ii) 0.71 lb of phenol per ton melt or less, and (iii) 0.92 lb of methanol per ton melt or less. (b) You must meet the following operating limits fo r each combined collection/curing operations subcategory: (a) You must control emissions from each existing, new, or recon structed curing oven by limiting emissions of formaldehyde t o either of the following: (1) 0.03 kg of formaldehyde per MG (0.06 lb of form aldehyde per ton) of melt or less. (2) A reduction of uncontrolled formaldehyde emissi ons by at least 80 percent. (b) You must meet the following operating limits fo r each curing oven: (1) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder for mulation at or below the specification ranges of the resin and binder used during the performance test. (2) Maintain the operating temperature of each inci nerator so that the average operating temperature for each three-hour block period never falls below the average temperat ure established during the performance test. § 63.1180 When must I meet these standards?Page 8 of 53

(a) Existing cupolas and combined collection/ curing operationsovens. (1) You must install any control devices and monitoring equipment necessary to meet the standards in § 63.1178(a)(1) and (b)this subpart , complete performance testing, and demonstrate compliance with all requirements of this subpart no later than the following: ( 1i ) June 2, 2002; or ( 2ii ) June 3, 2003 if you apply for and receive a one-y ear extension under section 112(i)(3)(B) of the Act. (2) You must install any control devices and monito ring equipment necessary to meet the standards in § 63.1 178(a)(2) and through (a)(5) and § 63.1179, complete performance testing, and demonstrate compliance with all requirements of thi s subpart no later than [ insert date 3 years after date of publication in th e Federal Register ] (3) You must comply with the provisions related to the electronic reporting provisions of §§ 63.1192(d) an d 63.1193(b)(1) and (g) no later than [i nsert date of publication in the Federal Register ]. (b) New and reconstructed cupolas and combined collection /curing ovensoperations
. You must install any control devices or monitoring equipment necessary to meet t he standards in this subpart, complete performance testing, and demonstratePage 9 of 53

compliance with all requirements of this subpart by the dates in §63.7 of the general provisions in subpart A of thi s part. (c) You must comply with the standards in §§ 63.117 8 and 63.1179 of this subpart on and after the dates in p aragraphs (a) and (b) of this section. (d) At all times, you must operate and maintain any affected source, including associated air pollution control equipment and monitoring equipment, in a manner con sistent 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 ma y include, but is not limited to, monitoring results, review o f operation and maintenance procedures, review of operation and maintenance records, and inspection of the source. (d) You must comply with these standards at all tim es except during periods of startup, shutdown, or malf unction. § 63.1181 How do I comply with the particulate matt er standards for existing, new, and reconstructed cupolas? To comply with the PM standards, you must meet all of the following: (a) Install, adjust, maintain, and continuously ope rate a bag leak detection system for each fabric filter.Page 10 of 53

(b) Do a performance test as specified in § 63.1188 of this subpart and show compliance with the PM emission li mits while the bag leak detection system is installed, operati onal, and properly adjusted. (c) Begin corrective actions specified in your oper ations, maintenance, and monitoring plan required by § 63.1 187 of this subpart within one hour after the alarm on a bag le ak 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 t ime in a sixmonth reporting period. § 63.1182 How do I comply with the carbonyl sulfide, hydrogen fluoride, and hydrogen chloride standards for exist ing, new,carbon monoxide standards for new and reconstructed cupolas? To comply with the carbonyl sulfide, hydrogen fluor ide, and hydrogen chloride standards, you must meet the foll owing: (a) Install, calibrate, maintain, and operate a dev ice that continuously measures the operating temperature in the firebox of each thermal incinerator. To comply with the CO standards, you must meet all of the following:Page 11 of 53

(a) Install, calibrate, maintain, and operate a dev ice that continuously measures the operating temperature in the firebox of each thermal incinerator. (b) Conduct a performance test as specified in § 63 .1188 of this subpart that shows compliance with the carbony l sulfide, hydrogen fluoride, and hydrogen chloride emissions limits while the device for measuring incinerator operating temp erature is installed, operational, and properly calibrated. Es tablish the average operating temperature based on the performa nce test as specified in § 63.1185(a) of this subpart.(b) Do a performance test as specified in § 63.1188 of this subpart and show compliance with the CO emission limits while the de vice for measuring incinerator operating temperature is inst alled, operational, and properly calibrated. Establish the average operating temperature as specified in § 63.1185(a) of this subpart. (c) Following the performance test, measure and rec ord the average operating temperature of the incinerator as specified in § 63.1185(b) of this subpart. (d) Maintain the operating temperature of the incin erator so that the average operating temperature for each three-hour block period never falls below the average temperat ure established during the performance test.Page 12 of 53

(e) Operate and maintain the incinerator as specifi ed in your operations, maintenance, and monitoring plan r equired by § 63.1187 of this subpart. § 63.1183 How do I comply with the formaldehyde , phenol, and methanol standards for existing, new, and reconstru cted combined collection/curing operationsstandards for existing, new, and reconstructed curing ovens ? To comply with the formaldehyde , phenol, and methanol standards, you must meet all of the following: (a) Install, calibrate, maintain, and operate a dev ice that continuously measures the operating temperature in the firebox of each thermal incinerator. (b) Conduct a performance test as specified in § 63 .1188 of this subpart while manufacturing the product that r equires a binder formulation made with the resin containing t he highest free-formaldehyde content specification range. Show compliance with the formaldehyde, phenol, and methanol emissio ns limits while the device for measuring the control device o perating parameter is installed, operational, and properly c alibrated. Establish the average operating parameter based on the performance test as specified in § 63.1185(a).(b) D o a performance test as specified in § 63.1188 of this subpart while manufacturing the product that requires a binder fo rmulation made with the resin containing the highest free-for maldehydePage 13 of 53

content specification range. Show compliance with t he formaldehyde emission limits while the device for m easuring incinerator operating temperature is installed, ope rational, and properly calibrated. Establish the average operatin g temperature as specified in § 63.1185(a) of this subpart. (c) During the performance test that uses the binde r formulation made with the resin containing the high est freeformaldehyde content specification range, record th e freeformaldehyde content specification range of the res in used, and the formulation of the binder used, including the f ormaldehyde content and binder specification. (d) Following the performance test, monitor and rec ord the free-formaldehyde content of each resin lot and the formulation of each batch of binder used, including the formald ehyde, phenol, and methanol content. (d) Following the performance test, monitor and re cord the free-formaldehyde content of each resin lot and the formulation of each batch of binder used, including the formald ehyde

content. (e) Maintain the free-formaldehyde content of each resin lot and the formaldehyde content of each binder for mulation at or below the specification ranges established durin g the performance test.Page 14 of 53

(f) Following the performance test, measure and rec ord the average operating temperature of the incinerator as specified in § 63.1185(b) of this subpart. (g) Maintain the operating temperature of the incin erator so that the average operating temperature for each three-hour block period never falls below the average temperat ure established during the performance test. (h) Operate and maintain the incinerator as specifi ed in your operations, maintenance, and monitoring plan r equired 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 w here the formaldehyde content, is higher than the specificat ion ranges of the resin and binder used during previous performan ce tests, or using experimental pollution prevention process mod ifications without first doing additional performance tests. N otification of intent to perform a short-term experimental prod uction 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 bind er formulation will deviate from previously approved l evels or what the experimental pollution prevention process modif ications are.Page 15 of 53

(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 do ne during the experimental run. Additional Monitoring Information § 63.1184 What do I need to know about the design specifications, installation, and operation of a ba g leak detection system? 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 emission s at concentrations of 10 milligrams per actual cubic me ter (0.0044 grains per actual cubic foot) or less. (b) The sensor on the bag leak detection system mus t provide output of relative PM emissions. (c) The bag leak detection system must have an alar m that will sound automatically when it detects an increas e in relative PM emissions greater than a preset level. (d) The alarm must be located in an area where appr opriate plant personnel will be able to hear it. (e) For a positive-pressure fabric filter, each com partment or cell must have a bag leak detector. For a negati ve-pressure or induced-air fabric filter, the bag leak detector must bePage 16 of 53

installed downstream of the fabric filter. If multi ple bag leak detectors are required (for either type of fabric f ilter), detectors may share the system instrumentation and alarm. (f) Each triboelectric bag leak detection system mu st be installed, operated, adjusted, and maintained so th at it follows EPA's “Fabric Filter Bag Leak Detection Guidance” ( EPA-454/R-98- 015, September 1997). Other bag leak detection syst ems must be installed, operated, adjusted, and maintained so th at they follow the manufacturer's written specifications an d 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 th e device. (2) Establish the alarm set points and the alarm de lay time. (h) After initial adjustment, the range, averaging period, alarm set points, or alarm delay time may not be ad justed except as specified in the operations, maintenance, and mo nitoring 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 responsib le official as defined in § 63.2 of the general provisions in s ubpart A ofPage 17 of 53

this part certifies in writing to the Administrator that the fabric filter has been inspected and found to be in good operating condition. § 63.1185 How do I establish the average operating temperature of an incinerator? (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 i n consecutive 15-minute blocks. (3) Determine and record the arithmetic average of the recorded average temperatures measured in consecuti ve 15-minute blocks for each of the one-hour performance test ru ns. (4) Determine and record the arithmetic average of the three one-hour average temperatures during the perf ormance 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 p erformance test, you must measure and record the average opera ting temperature of the incinerator as required by §§ 63 .1182 and 63.1183 of this subpart. This average operating tem perature of the incinerator is based on the arithmetic average of the one-Page 18 of 53

hour average temperatures for each consecutive thre e-hour period and is determined in the same manner described in p aragraphs (a)(1) through (a)(4) of this section. § 63.1186 How may I change the compliance levels of monitored parameters? You may change control device and process operating parameter levels established during performance tes ts and used to monitor compliance if you do the following: (a) You must notify the Administrator of your desir e to expand the range of a control device or process ope rating parameter level. (b) Upon approval from the Administrator, you must conduct additional performance tests at the proposed new co ntrol device or process operating parameter levels. Before opera ting at these levels, the performance test results must verify th at, at the new levels, you comply with the emission limits in §§ 63.1178 and 63.1179 of this subpart. § 63.1187 What do I need to know about operations, maintenance, and monitoring plans? (a) An operations, maintenance, and monitoring plan must be submitted to the Administrator for review and appro val as part of your application for the title V permit. (b) The operations, maintenance, and monitoring pla n must include the following:Page 19 of 53

(1) Process and control device parameters you will monitor to determine compliance, along with established ope rating levels or ranges for each process or control device. (2) A monitoring schedule. (3) Procedures for properly operating and maintaini ng control devices used to meet the standards in §§ 63 .1178 and 63.1179 of this subpart. These procedures must incl ude an inspection of each incinerator at least once per ye ar. At a minimum, you must do the following as part of an in cinerator inspection: (i) Inspect all burners, pilot assemblies, and pilo t sensing devices for proper operation. Clean pilot s ensor if

necessary. (ii) Ensure proper adjustment of combustion air, an d adjust if necessary. (iii) Inspect, when possible, all internal structur es (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 ref ractory lining. Clean, and repair or replace lining if nece ssary.Page 20 of 53

(vii) Inspect incinerator shell for proper sealing, corrosion, and/or hot spots. (viii) For the burn cycle that follows the inspecti on, document that the incinerator is operating properly and make any necessary adjustments. (ix) Generally observe whether the equipment is mai ntained in good operating condition. (x) Complete all necessary repairs as soon as pract icable. (4) Procedures for keeping records to document comp liance. (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 includ e: (i) Inspecting the fabric filter for air leaks, tor n 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 compartm ent. (v) Cleaning the bag leak detection system probe, o r otherwise repairing the bag leak detection system.Page 21 of 53

(vi) Shutting down the process producing the partic ulate emissions. Performance Tests and Methods § 63.1188 What performance test requirements must I meet? You must meet the following performance test requir ements: (a) All monitoring systems and equipment must be in stalled, operational, and properly calibrated before the per formance
tests. (b) Conduct a performance test, consisting of three test runs, for each cupola and/or combined collection/cu ring operation subject to this subpart at the maximum pr oduction rate to demonstrate compliance with each of the applicab le emissions limits in §§ 63.1178 and 63.1179. (b) Do a performance test, consisting of three tes t runs, for each cupola and curing oven subject to this sub part at the maximum production rate to demonstrate compliance w ith each of the applicable emission limits in §§ 63.1178 and 63 .1179 of 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 in §§ 63.1178 and 63.1179 of this subpart at least once every 5 years . (c) Measure emissions of PM from each existing cupola.Page 22 of 53

(d) Measure emissions of PM, carbonyl sulfide, hydr ogen fluoride, and hydrogen chloride from each existing, new, or reconstructed cupola. (d) Measure emissions of PM a nd CO from each new or reconstructed cupola. (e) Measure emissions of formaldehyde, phenol, and methanol from each existing, new, or reconstructed combined collection/ curing operation. (e) Measure emissions of formaldehyde from each ex isting, new or reconstructed curing oven. (f) Measure emissions at the outlet of the control device for PM, carbonyl sulfide, hydrogen fluoride, hydrog en chloride, formaldehyde, phenol, and methanol. (f) Measure emi ssions at the outlet of the control device if complying with a nu merical emission limit for PM, CO, or formaldehyde, or at t he inlet and outlet of the control device if complying with a pe rcent reduction emission limit for CO or formaldehyde. (g) To determine the average melt rate, measure and record the amount of raw materials, excluding coke, charge d into and melted in each cupola during each performance test run. Determine and record the average hourly melt rate f or each performance test run. Determine and record the arit hmetic average of the average hourly melt rates associated with the three performance test runs. The average hourly mel t rate of thePage 23 of 53

three performance test runs is used to determine co mpliance 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 operatin g parameter monitoring requirements for performance t esting as specified in this subpart. § 63.1189 What test methods do I use? You must use the following test methods to determin e compliance with the applicable emission limits: (a) Method 1 in appendix A to part 60 of this chapt er for the selection of the sampling port locations and nu mber of sampling ports. (b) Method 2 in appendix A to part 60 of this chapt er 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 measureme nts needed to correct the concentration measurements to a standar d basis. (d) Method 4 in appendix A to part 60 of this chapt er for moisture content of the stack gas. (e) Method 5 in appendix A to part 60 of this chapt er for the concentration of PM. Each PM test run must cons ist of aPage 24 of 53

minimum run time of three hours and a minimum sampl e volume of 3.75 dscm (135 dscf). (f) Method 10 in appendix A to part 60 of this chap ter for the concentration of CO, using the continuous sampl ing option described in section 7.1.1 of the method. Each CO t est run must consist of a minimum run time of one hour. (g) Method 318 at 40 CFR part 60, appendix A to thi s part for the concentration of formaldehyde, phenol, meth anol, and carbonyl sulfide. (g) Method 318 in appendix A to this part for the concentration of formaldehyde or CO. (h) Method to determine the free-formaldehyde conte nt 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. § 63.1190 How do I determine compliance? (a) Using the results of the performance tests, you must use the following equation to determine compliance with the PM emission limit:

where: E = Emission rate of PM, kg/Mg (lb/ton) of melt.Page 25 of 53

C = Concentration of PM, g/dscm (gr/dscf). Q = Volumetric flow rate of exhaust gases, dscm/hr

(dscf/hr). K 5 1 = Conversion factor, 1 kg/1,000 g (1 lb/7,000 gr). P = Average melt rate, Mg/hr (ton/hr). (b) Using the results of the performance tests, you must use the following equation to determine compliance with the carbonyl sulfide, hydrogen fluoride, hydrogen chlor ide, formaldehyde, phenol, and methanol CO and formaldeh yde numerical emission limits:

where: E = Emission rate of measured pollutant, kg/Mg

(lb/ton) of melt. C = Measured volume fraction of pollutant, ppm. MW = Molecular weight of measured pollutant, g/g-mo le:

carbonyly sulfide = 60.07, hydrogen fluoride = 20.01, hydrogen chloride = 36.46, Formaldehyde = 30.03, Phenol = 94.11, Methanol = 32.04. CO = 28.01, Formaldehyde = 30.03. Q = Volumetric flow rate of exhaust gases, dscm/hr

(dscf/hr). K 1 = Conversion factor, 1 kg/1,000 g (1 lb/453.6 g). K 2 = Conversion factor, 1,000 L/m 3 (28.3 L/ft 3 ). K 3 = Conversion factor, 24.45 L/g-mole. P = Average melt rate, Mg/hr (ton/hr).Page 26 of 53

(c) Using the results of the performance tests, you must use the following equation to determine compliance with the CO and formaldehyde percent reduction performance stan dards:

where: %R = Percent reduction, or collection efficiency of

the control device. L i = Inlet loading of pollutant, kg/Mg (lb/ton). L o = Outlet loading of pollutant, kg/Mg (lb/ton). Notification, Recordkeeping, and Reporting § 63.1191 What notifications must I submit? You must submit written or electronic notifications to the Administrator as required by § 63.9(b) through (h) of subpart A of this part. Electronic notifications are encourag ed when possible. You must submit written notifications to the Administrator as required by § 63.9(b)-(h) of the g eneral provisions in subpart A of this part. These notifications include, but are not limited to, the following: (a) Notification that the following types of source s 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.Page 27 of 53

(3) A new or reconstructed source that has an initi al startup after the effective date of the standard an d doesn't require an application for approval of construction or reconstruction under § 63.5(d) of the general provi sions in subpart A of this part. (b) Notification of intention to construct a new ma jor source or reconstruct a major source where the init ial startup of the new or reconstructed source occurs after the effective date of the standard and an application for approva l of construction or reconstruction under § 63.5(d) of t he 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 re quirements in § 63.6(b)(3) and (4) of the general provisions in s ubpart A of this part. (d) Notification of a performance test at least 60 calendar days before the performance test is scheduled to be gin. (e) Notification of compliance status. § 63.1192 What recordkeeping requirements must I me et? You must meet the following recordkeeping requireme nts: (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 a lso:Page 28 of 53

(1) Cupola production (melt) rate (Mg/hr (tons/hr) of melt). (2) All bag leak detection system alarms. Include t he date and time of the alarm, when corrective actions were initiated, the cause of the alarm, an explanation of the corre ctive actions taken, and when the cause of the alarm was correcte d. (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 prod ucts. (4) Incinerator operating temperature and results o f incinerator inspections. For all periods when the a verage temperature in any three-hour block period fell bel ow the average temperature established during the performa nce test, and all periods when the inspection identified incinera tor components in need of repair or maintenance, includ e the date and time of the problem, when corrective actions we re initiated, the cause of the problem, an explanation of the cor rective actions taken, and when the cause of the problem wa s corrected. (c) Retain each record for at least five years foll owing the date of each occurrence, measurement, correctiv e action, maintenance, record, or report. The most recent two years of records must be retained at the facility. The remai ning three years of records may be retained off site.Page 29 of 53

(d) Records must be maintained in a form suitable a nd readily available for expeditious review, according to § 63.10 of the General Provisions that are referenced in Ta ble 3 to this subpart. Electronic recordkeeping is encouraged. (d) Retain records on microfilm, on a computer, on computer disks, on magnetic tape disks, or on micro fiche. (e) Report the required information on paper or on a labeled computer disk using commonly available and compatible computer software. § 63.1193 What reports must I submit? You must prepare and submit reports to the Administ rator as required by this subpart and § 63.10 of the general provisions in subpart A of this part. These reports include, b ut are not limited to, the following: (a) Within 60 days after the date of completing eac h performance test (as defined in § 63.2) required by this subpart, you must submit the results of the perform ance tests, including any associated fuel analyses, following t he 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 website (http://www.epa.gov/ttn/chief/ert/index.htm l), you must submit the results of the performance test to the E PA via the Compliance and Emissions Data Reporting Interface ( CEDRI). CEDRIPage 30 of 53

can be accessed through the EPA’s Central Data Exch ange (CDX) (http://cdx.epa.gov/epa_home.asp). Performance test data must be submitted in a file format generated through the us e of the EPA’s ERT. Alternatively, you may submit performanc e test data in an electronic file format consistent with the ex tensible markup language (XML) schema listed on the EPA’s ER T website, once the XML schema is available. If you claim that some of the performance test information being submitted is con fidential business information (CBI), you must submit a compl ete file generated through the use of the EPA’s ERT or an al ternate electronic file consistent with the XML schema list ed on the EPA’s ERT website, including information claimed to be CBI, on a compact disc, flash drive, or other commonly used e lectronic 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 o r 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 E RT website, you must submit the results of the performance test to the Administrator at the appropriate address listed in § 63.13.Page 31 of 53

(a) A performance test report, as required by § 63.10(d)(2) of the general provisions in subpart A of this part, that documents the process and control equipment op erating parameters during the test period, the test methods and procedures, the analytical procedures, all calculat ions, and the results of the performance tests. (b) Reserved. A startup, shutdown, and malfunction plan , as described in § 63.6(e)(3) of the general provisions in subpart A of this part, that contains specific procedures for operating and maintaining the source during periods of startu p, shutdown, and malfunction and a program of corrective action for malfunctioning process and control systems used to comply with the emission standards. In addition to the informat ion required by § 63.6(e)(3), your plan must include the followi ng: (1) Procedures to determine and record what caused the malfunction and when it began and ended. (2) Corrective actions you will take if a process o r control device malfunctions, including procedures f or recording the actions taken to correct the malfunction or min imize emissions. (3) An inspection and maintenance schedule for each process and control device that is consistent with the manu facturer's instructions and recommendations for routine and lo ng-term maintenance.Page 32 of 53

(c) A report of each event as required by § 63.10(b ) of the general provisions in subpart A of this part, inclu ding a report if an action taken during a startup, shutdown, or m alfunction is inconsistent with the procedures in the plan as des cribed in § 63.6(e)(3) of the general provisions in subpart A o f 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 mea sured emissions exceed the applicable standard or a monit ored parameter varies from the level established during performance testing. The report must contain the information sp ecified 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 emis sions or deviations of monitored parameters occurred during the reporting period as required by § 63.10(e)(3)(v) of the gener al provisions in subpart A of this part if no deviations have occ urred. (g) All reports required by this subpart not subjec t 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 own er or operator of a source, these reports may be submitte d on electronic media. The Administrator retains the rig ht to requirePage 33 of 53

submittal of reports subject to paragraph (a) of th is section in paper format. Other Requirements and Information § 63.1194 Which general provisions apply? The general provisions in subpart A of this part de fine 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 subpar t. § 63.1195 Who implements and enforces this subpart? (a) This subpart can be implemented and enforced by the U.S. EPA, or a delegated authority such as the appl icable State, local, or Tribal agency. If the U.S. EPA Administra tor has delegated authority to a State, local, or Tribal ag ency, then that agency, in addition to the U.S. EPA, has the a uthority to implement and enforce this subpart. Contact the app licable U.S. EPA Regional Office to find out if implementation a nd enforcement of this subpart is delegated to a State , local, or Tribal agency. (b) In delegating implementation and enforcement au thority of this subpart to a State, local, or Tribal agency under subpart E of this part, the authorities contained i n paragraph (c) of this section are retained by the Administrat or of U.S.Page 34 of 53

EPA and cannot be transferred to the State, local, or Tribal

agency. (c) The authorities that cannot be delegated to Sta te, local, or Tribal agencies are as specified in parag raphs (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 un der § 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. § 63.1196 What definitions should I be aware of? 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 partic ulate matter emissions resulting from a broken filter bag or oth er malfunction and sounds an alarm.Page 35 of 53

Bonded product means mineral wool to which a hazard ous air pollutant-based binder (containing such hazardous a ir 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, emissio ns of carbon monoxide that serve as a surrogate for emiss ions of carbonyl sulfide, a compound included on the list o f hazardous air pollutants in section 112 of the Act. Combined collection/curing operations means the com bination of fiber collection operations and curing ovens use d 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 ad ditives. As the fuel is burned, the charged mixture is heated t o a molten state for later processing to form mineral wool. Curing oven means a chamber in which heat is used t o thermoset a binder on the mineral wool fiber used t o 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 subpar t, emissions of formaldehyde that, in addition to bein g a HAPPage 36 of 53

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 lis ted in or pursuant to section 112(b) of the Act. I means the owner or operator of a mineral wool pro duction facility. Incinerator means an enclosed air pollution control device that uses controlled flame combustion to convert co mbustible 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 disc harged to the fiber forming and collection process. Melt rate means the mass of molten material dischar ged 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 o r 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 abso rbency, fire resistance, or other required properties.Page 37 of 53

New source means any affected source the constructi on or reconstruction of which is commenced after May 8, 1 997. Open-top cupola means a cupola that is open to the outside air and operates with an air flow rate that is unre stricted and at low pressure. PM means, for the purposes of this subpart, emissio ns of particulate matter that serve as a surrogate for me tals (in particulate or volatile form) on the list of hazard ous 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. § 63.1197 Startups and shutdowns. (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 ti mes when emissions are being, or are otherwise required to b e, routed to such items of equipment. (c) Startup begins when fuels are ignited in the cu pola. Startup ends when the cupola produces molten materi al.Page 38 of 53

(d) Shutdown begins when the cupola has reached the end of the melting campaign and is empty. No molten materi al continues to flow from the cupola during shutdown. (e) During periods of startups and shutdowns you mu st operate your cupola according to one of the followi ng methods: (1) You must keep records showing that your emissio ns were controlled using air pollution control devices oper ated at the parameters established by the most recent performan ce 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 sh utdown; and (ii) You operate the cupola during startup and shut down with three percent oxygen over the fuel demand for oxygen. §§ 63.119 78 -63.1199 [Reserved] Table 1 to Subpart DDD of Part 63—Applicability of General Provisions (40 CFR Part 63, Subpart A) to Subpart D DD of Part 63
General provisions citation Requirement Applies to subpart DDD? Explanation
§ 63.1(a)(1)- (a) ( 46 ) General Applicability Yes

63.1(a)(5) No [Reserved].

63.1(a)(6)- (a)(8) YesPage 39 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation
§ 63.1(a) (7)- (9) No [Reserved].

§ 63.1(a)(10)- (a) ( 1412 ) Yes

§ 63.1(b) (1) Initial Applicability Determination Yes

§ 63.1(b)(2) No [Reserved].

§ 63.1(b)(3) Yes

§ 63.1(c)(1) -(2) Applicability After Standard Established Yes

63.1(c)(2) Yes Some plants may be area sources. § 63.1(c)(3) -(4) No [Reserved]. § 63.1 (c)(4)- (c)(5) -(e) Yes 63.1(d) No [Reserved].

63.1(e) Applicability of Permit Program Yes

§ 63.2 Definitions Yes Additional definitions in §63.1196. § 63.3 Units and Abbreviations Yes
§ 63.4(a)(1)- (a) ( 32 ) Prohibited Activities Yes

§ 63.4(a) (4)(3)- (5) No [Reserved]. 63.4(a)(5) YesPage 40 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation
§ 63.4(b)-(c) Circumvention/Sev erability Yes
§ 63.5(a) (1)- (b)(2) Construction/Reco nstruction Applicability Yes

§ 63.5(b)( 31 )

- (4) Existing, New, Reconstructed Sources Requirements Yes

63.5(b)(2) No [Reserved]. 63.5(b)(5) No [Reserved].

§ 63.5 (b)(3)- (b)(6) Yes

§ 63.5(c) No [Reserved].

§ 63.5(d) -(f) Application for Approval of Construction/Reco nstruction Yes

63.5(e) Approval of Construction/Reco nstruction Yes

63.5(f) Approval of Construction/Reco nstruction Based on State Review Yes

§ 63.6(a) -(d) Compliance with Standards and Maintenance Applicability Yes

63.6(b)(1)- (b)(5) New and Reconstructed Sources Dates Yes

63.6(b)(6) No [Reserved]. 63.6(b)(7) YesPage 41 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation 63.6(c)(1) Existing Sources Dates Yes §63.1180 specifies compliance dates. 63.6(c)(2) Yes 63.6(c)(3)- (c)(4) No [Reserved]. 63.6(c)(5) Yes

63.6(d) No [Reserved]. 63.6(e)(1)- (e)(2) Operation & Maintenance Requirements Yes §63.1187 specifies additional requirements. § 63.6(e)(1)(i) General Duty to Mminimize Eemissions No See § 63.1180(d) for general duty requirement. § 63.6(e)(1)(ii) Requirement to Ccorrect Mmalfunctions Aas Ssoon Aas Ppossible No § 63.1187(b) specifies additional requirements.
§ 63.6(e)(1)(iii) Yes

§ 63.6(e)(2) No [Reserved]

§ 63.6(e)(3) Startup, Shutdown, and Malfunction (SSM) Plan YesNo Startups and shutdowns addressed in § 63.1197. § 63.6(f) (1) Compliance with Emission StandardsSSM E e xemption YesNoPage 42 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation § 63.6(f)(2)-(g) Yes 63.6(g) Alternative Standard Yes 63.6(h) Compliance with Opacity/VE Standards No Subpart DDD does not include VE/opacity standards. § 63.6(h)(1) SSM exemption No § 63.6(h)(2)

- (j) Yes 63.6(i)(1)- (i)(14) Extension of Compliance Yes §63.1180 specifies date. 63.6(i)(15) No [Reserved]. 63.6(i)(16) Yes 63.6(j) Exemption from Compliance Yes
§ 63.7(a) -(d) Performance TTt est ing RRr equirements Applicability Yes

63.7(b) Notification Yes 63.7(c) Quality Assurance/Test Plan Yes

63.7(d) Testing Facilities Yes
§ 63.7(e) (1) Conduct of performance Tt ests YesNo See § 63.118 08 specifies additional requirements
. § 63.7(e)(2)-(f) Yes 63.7(f) Alternative Test Method Yes
§ 63.7(g) (1) Data Analysis , Recordkeeping, and Reporting Yes

§ 63.7(g)(2) No [Reserved].Page 43 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation § 63.7(g)(3)-(h) Yes 63.7(h) Waiver of Tests Yes § 63.8(a) (1)-(b) Monitoring RRr equirements Applicability Yes

63.8(a)(2) No Subpart DDD does not require CMS performance specification s. 63.8(a)(3) No [Reserved]. 63.8(a)(4) Yes 63.8(b) Conduct of Monitoring Yes
§ 63.8(c)(1) (i)- (c)(3) General Dduty to Mminimize Eemissions and CMS OOo peration /Maint enance YesNo See § 63.1180(e) for general duty requirement. § 63.8(c)(1)(ii) Yes § 63.8(c)(1)(iii) Requirement to Ddevelop SSM Plan for CMS No

63.8(c)(4)- (c)(8) No Subpart DDD does not require COMS or CMS performance specification s. § 63.8(c)(2)- (d)(2) Yes § 63.8(d)(3) Written Pprocedures for CMS Yes, except for last sentence, which refers to SSM plan.Page 44 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation SSM plans are not required. 63.8(d) Quality Control No Subpart DDD does not require a CMS quality control program. § 63.8(e)

- (g) Yes 63.8(e) CMS Performance Evaluation No Subpart DDD does not require CMS performance evaluations. 63.8(f)(1)- (f)(5) Alternative Monitoring Method Yes 63.8(f)(6) Alternative to RATA Test No Subpart DDD does not require CEMS. 63.8(g)(1) Data Reduction Yes 63.8(g)(2) No Subpart DDD does not require COMS or CEMS. 63.8(g)(3)- (g)(5) Yes
§ 63.9(a) Notification Requirements Applicability and Ggeneral Iinformation Yes

§ 63.9(b) (1)-(2) Initial Notifications Yes § 63.9(b)(3) No [Reserved]. § 63.9(b)(4)-(5) Yes § 63.9(c) -(j) Request for Compliance Extension Yes

63.9(d) New Source Notification for YesPage 45 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation Special Compliance Requirements 63.9(e) Notification of Performance Test Yes 63.9(f) Notification of VE/Opacity Test No Subpart DDD does not include VE/opacity standards. 63.9(g) Additional CMS Notifications No Subpart DDD does not require CMS performance evaluation, COMS, or CEMS. 63.9(h)(1)- (h)(3) Notification of Compliance Status Yes 63.9(h)(4) No [Reserved]. 63.9(h)(5)- (h)(6) Yes 63.9(i) Adjustment of Deadlines Yes 63.9(j) Change in Previous Information Yes

§ 63.10(a) Recordkeeping / and RRr eporting

Applicability Rrequirements Yes

§ 63.10(b) (1) General RRr ecordkeeping RRr equirements Yes §63.1192 includes additional requirements. § 63.10(b)(2)(i) Recordkeeping of Ooccurrence and Dduration of Sstartups and Sshutdowns NoPage 46 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation
§ 63.10(b)(2)(ii) Recordkeeping of Mmalfunctions No See § 63.1193(c) for recordkeeping of (ii) occurrence and duration and (iii) actions taken during malfunction. § 63.10(b)(2)(iii) Maintenance Rrecords Yes
§ 63.10(b)(2)(iv)- (v) Actions taken to minimize emissions during SSM No

§ 63.10(b)(2)(vi) Recordkeeping for CMS malfunctions Yes
§ 63.10(b)(2)(vii) -(xiv) Other CMS requirements Yes

§ 63.10(b)(3) Recordkeeping Rrequirement for Aapplicability Ddeterminations Yes

§ 63.10(c)(1)

- (6) Additional CMS RRr ecordkeeping Rrequirements for Ssources with CMS Yes

§63.10(c)(2)- (c)(4) No [Reserved]. §63.10(c)(5) Yes §63.10(c)(6) No Subpart DDD does not require CMS performance specification s. § 63.10(c)(7)- (c) (8) Additional Rrecordkeeping Yes Formatted TablePage 47 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation Rrequirements for CMS – Iidentifying Eexceedances and Eexcess Eemissions § 63.10(c)(9) No [Reserved]. § 63.10(c)(10)- (c)( 1311 ) YesNo See § 63.1192 for recordkeeping of malfunctions. § 63.10(c) (12)- (14) NoYes Subpart DDD does not require a CMS quality control program. § 63.10(c)(15) Use of SSM Plan YesNo § 63.10(d)(1)

- (4) General Reporting Requirements Yes Additional requirements in §63.1193. §63.10(d)(2) Performance Test Results Yes §63.10(d)(3) Opacity or VE Observations No Subpart DDD does not include VE/opacity standards. § 63.10(d) (4)- (d) (5) Progress Reports/ S tartup, S hutdown, and M alfunction Reports YesNo See § 63.1193(f) for reporting of malfunctions. § 63.10(e) (1)

- (e)(2)(f) Additional CMS Reports Excess Emission/CMS Performance Reports COMS Data Reports NoYes Subpart DDD does not require CEMS or CMS performance evaluations.Page 48 of 53

General provisions citation Requirement Applies to subpart DDD? Explanation Recordkeeping/Rep orting Waiver §63.10(e)(3) Excess Emissions/CMS Performance Reports Yes

§63.10(e)(4) COMS Data Reports No Subpart DDD does not require COMS. §63.10(f) Recordkeeping/Rep orting Waiver Yes
§ 63.11(a) -(b) Control Device Requirements Applicability Flares YesNo Flares will not be used to comply with the emissions limits. §63.11(b) Flares No Flares not applicable. § 63.11(c) Alternative Work Practice for Monitoring Equipment for Leaks Yes

§ 63.11(d) Alternative Work Practice Standard Yes § 63.11(e) Yes § 63.12 State Authority and Delegations Yes
§ 63.13 Addresses Yes § 63.14 Incorporation by Reference Yes
§ 63.15 Information Availability/Conf identiality Yes

§ 63.16 Performance Track Provisions YesPage 49 of 53

Appendix A to Subpart DDD of Part 63—Free Formaldeh yde Analysis of Insulation Resins by the Hydroxylamine Hydrochlo ride Method 1. Scope The method in this appendix was specifically develo ped for water-soluble phenolic resins that have a relativel y high freeformaldehyde (FF) content such as insulation resins . It may also be suitable for other phenolic resins, especially t hose with a high FF content. 2. Principle 2.1 a. The basis for this method is the titration o f the hydrochloric acid that is liberated when hydroxylam ine hydrochloride reacts with formaldehyde to form form aldoxine:

HCHO + NH2OH:HCl → CH2:NOH + H2O + HCl b. Free formaldehyde in phenolic resins is present as monomeric formaldehyde, hemiformals, polyoxymethyle ne hemiformals, and polyoxymethylene glycols. Monomeri c formaldehyde and hemiformals react rapidly with hyd roxylamine hydrochloride, but the polymeric forms of formaldeh yde must hydrolyze to the monomeric state before they can re act. 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 hydrog en ions. 2.2 The resin sample being analyzed must contain en ough free formaldehyde so that the initial reaction withPage 50 of 53

hydroxylamine hydrochloride will produce sufficient hydrogen ions to catalyze the depolymerization of the polyme ric formaldehyde within the time limits of the test met hod. The sample should contain approximately 0.3 grams (g) f ree formaldehyde to ensure complete reaction within 5 m inutes. 3. Apparatus 3.1 Balance, readable to 0.01 g or better. 3.2 pH meter, standardized to pH 4.0 with pH 4.0 bu ffer 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. Reagents 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. ProcedurePage 51 of 53

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. Grams resin = 60/expected percent FF I. The following table shows example levels: Expected percent free formaldehyde Sample size, gra ms 2 30.0 5 12.0 8 7.5 10 6.0 12 5.0 15 4.0 ii. It is very important to the accuracy of the res ults that the sample size be chosen correctly. If the mi lliliters 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 Grams resin = 30/expected percent FF I. The following table shows example levels:Page 52 of 53

Expected percent free formaldehyde Sample size, gra ms 2 15 1 30 0.5 60 ii. If the milliliters of titrant are less than 5 m L or greater than 30 mL, reestimate the needed sample si ze and repeat the tests. 5.2 Weigh the resin sample to the nearest 0.01 gram s into a 250-mL beaker. Record sample weight. 5.3 Add 100 mL of the methanol/water mixture and st ir on a magnetic stirrer. Confirm that the resin has dissol ved. 5.4 Adjust the resin/solvent solution to pH 4.0, us ing 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 so lution, measured with a graduated cylinder. Start the timer
. 5.6 Stir for 5 minutes. Titrate to pH 4.0 with stan dardized 1.0 N sodium hydroxide. Record the milliliters of t itrant and the normality. 6. Calculations

7. Method Precision and Accuracy Test values should conform to the following statist ical precision:Page 53 of 53

Variance = 0.005 Standard deviation = 0.07 95% Confidence Interval, for a single determination = 0.2 8. Author This method was prepared by K.K. Tutin and M.L. Fos ter, Tacoma R&D Laboratory, Georgia-Pacific Resins, Inc. (Principle written by R. R. Conner.) 9. References 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.