§ 63.365 - Test methods and procedures.

§ 63.365 Test methods and procedures.

(a) General —

(1) Performance testing

. The owner or operator of a source subject to the emissions standards

for facility where EtO use is less than 100 pounds per year. If you own or operate an affected source at a facility where EtO use is less than 100 lb/yr that is subject to an emission standard in § 63.362

shall

, you must comply with the performance testing requirements in § 63.7

of subpart A of this part

, according to the applicability in

Table 1 of § 63.360, and in

table 6 to this subpart, using the methods in paragraph (b) or (c) of this section, following the applicable procedures for initial compliance and continuous compliance in paragraphs (d), (e), and (f) of this section.

(2) Facilities subject to capture efficiency. If you are subject to capture efficiency requirements in § 63.362, you must follow the applicable procedures for initial and continuous compliance in paragraph (f) of this section.

ethylene oxide

(b) Efficiency at the sterilization chamber vent. California Air Resources Board (CARB) Method 431 or the following procedures shall be used to determine the efficiency of all types of control devices used to comply with § 63.362(c), sterilization chamber vent standard.

(1) First evacuation of the sterilization chamber. These procedures shall be performed on an empty sterilization chamber, charged with a typical amount of ethylene oxide, for the duration of the first evacuation under normal operating conditions (i.e., sterilization pressure and temperature).

(i) The amount of ethylene oxide loaded into the sterilizer (W_c) shall be determined by either:

(A) Weighing the

Test methods for facility where EtO use is less than 100 pounds per year. You must use the following test methods to determine the average mass emissions of EtO in lb/hr at the inlet of a control system (M_{APCD, i}) and/or outlet of a control system or stack (E_{APCD, o}).

(1) Select the location of the sampling ports and the number of traverse points according to Method 1 of appendix A-1 to part 60 of this chapter. Alternatively, for ducts less than 0.3 meter (12 in.) in diameter, you may choose to locate sample ports according to Method 1A of appendix A-1 to part 60 of this chapter.

(2) Determine the flow rate through the control system exhaust(s) continuously during the test period according to either Methods 2, 2A, or 2C of appendix A-1 to part 60 of this chapter, as appropriate. If using Method 2, 2A, or 2C, you must complete velocity traverses immediately before and subsequently after each test run. If your test run is greater than 1 hour, you must also complete a velocity traverse at least every hour. Average the velocity collected during a test run and calculate volumetric flow as outlined in the appropriate method.

(3) Determine the oxygen and carbon dioxide concentration of the effluent according to Method 3A or 3B of appendix A-2 to part 60 of this chapter. The manual procedures (but not instrumental procedures) of voluntary consensus standard ANSI/ASME PTC 19.10-1981 (incorporated by reference, see § 63.14) may be used as an alternative to EPA Method 3B.

(4) Determine the moisture content of the stack gas according to Method 4 of appendix A-3 to part 60 of this chapter. Alternatively, you may use an on-line technique that has been validated using Method 301 of appendix A to this part.

(5) Determine the EtO concentration according to either paragraph (b)(5)(i) or (ii) of this section.

(i) Follow Method 320 of appendix A to this part and the following paragraphs (5)(i)(A) through (D).

(A) The instrumentation used for measurement must have the measurement range to properly quantify the EtO in the gas stream. Additionally, for outlet emission streams, the instrumentation must have a method detection limit an order of magnitude below concentration equivalent of the emission limit.

(B) Instrumentation used must be continuous in nature with an averaging time of one minute or less.

(C) Calibration Spectra and all other analyte spiking required in the method must use EtO gaseous cylinder standard(s) which meet the criteria found in Performance Specification 19 of appendix B to part 60 if this chapter.

(D) Other methods and materials may be used; however, these alternative test methods are subject to Administrator approval.

(ii) Alternatively, ASTM D6348-12 (Reapproved 2020), (incorporated by reference, see § 63.14) may be used with the following conditions:

(A) The test plan preparation and implementation in the Annexes to ASTM D 6348-12 (R2020), Sections A1 through A8 are mandatory; and

(B) In ASTM D6348-12 (R2020) Annex A5 (Analyte Spiking Technique), the percent (%) R must be determined for each target analyte (equation A5.5). In order for the test data to be acceptable for a compound, %R must be 70% ≥ R ≤ 130%. If the %R value does not meet this criterion for a target compound, the test data is not acceptable for that compound and the test must be repeated for that analyte (i.e., the sampling and/or analytical procedure should be adjusted before a retest). The %R value for each compound must be reported in the test report, and all field measurements must be corrected with the calculated %R value for that compound by using equation 1 to this paragraph:

(6) Calculate the mass emission of EtO by using equations 2 and 3 to this paragraph:

Where:

M_{APCD, i} = average inlet mass rate of EtO per hour, lb/hr

C_EtO,i = inlet EtO concentration, ppmdv.

Qi = average inlet volumetric flow per hour at standard conditions, dscf/hr

44.05 = molecular weight (MW) of EtO, lb/lb-mole

MW/385.1 × 10⁶ = conversion factor, from ppmv at standard conditions to lb/cf

E_{APCD, o} = average outlet mass rate of EtO per hour, lb/hr

C_EtO,o = outlet EtO concentration, ppbdv.

Q_o = average outlet volumetric flow per hour at standard conditions, dscf/hr

MW/385.1 × 10⁹ = conversion factor, from ppbv at standard conditions to lb/cf

(c) Alternative approach for SCVs for facility where EtO use is less than 100 pounds per year. If you do not own or operate a single-item sterilizer, to demonstrate compliance with the percent emission reduction standards for emissions streams that are comprised only of SCVs, you may use the following procedures as an alternative to paragraph (b) of this section to determine the mass emissions of EtO being emitted via sterilization chamber(s) vents prior to the controls.

(1) Determine the mass (M_SCV,n) of EtO used for each charge and at each sterilization chamber used during the performance tests using the procedures in either paragraph (c)(1)(i) or (ii) of this section.

(i) Weigh the EtO gas cylinder(s) used to charge the sterilizer(s) before and after charging. Record these weights to the nearest 45 g (0.1 lb)

. Multiply the total mass of gas charged by the weight percent ethylene oxide present in the gas.

(B) Installing calibrated rotameters at the sterilizer inlet and measuring flow rate and duration of sterilizer charge. Use the following equation to convert flow rate to weight of ethylene oxide:

where:

W_c = weight of ethylene oxide charged, g (lb)

F_v

and calculate the theoretical mass (M_SCV,n) vented to the controls using equation 4 to this paragraph.

Where:

M_SCV,n = Theoretical total mass of EtO vented to controls per charge, g (lb) M_charge = total mass of sterilizer gas charge, g (lb) %E.O._w = weight percent of EtO

(ii) Install a calibrated rate meter at the sterilizer inlet(s) and continuously measure the flow rate (Q_m) and duration of each sterilizer charge. Calculate the theoretical mass (M_SCV,n) vented to the controls using equation 5 to this paragraph.

Where:

M_SCV,n = Total mass of EtO sent to controls per charge Q_m = volumetric flow rate, liters per minute (L/min) corrected to 20 °C and 101.325 kilopascals (kPa) (scf per minute (scfm) corrected to 68 °F and 1 atmosphere of pressure (atm))

; the flowrate must be constant during time (t)

t = time, min

%EO_V = volume fraction ethylene oxide

SV = standard volume, 24.05 liters per mole (L/mole) = 22.414 L/mole ideal gas law constant corrected to 20 °C and 101.325 kPa (385.32 scf per mole (scf/mole) = 359 scf/mole ideal gas law constant corrected to 68 °F and 1 atm).

T_n = time duration of each charge, min _n = number of EtO charges %E.O._v = volume fraction percent of EtO MW = molecular weight of

ethylene oxide

EtO, 44.05 grams per gram-mole (g/g-mole) (44.05 pounds per pound-mole (lb/lb-mole))

, or

(C) Calculating the mass based on the conditions of the chamber immediately after it has been charged using the following equation:

where:

P = chamber pressure, kPa (psia)

V = chamber volume, liters (L) (ft³)

R = gas constant, 8.313 L·kPa/g-mole·(10.73 psia·ft³/mole°R)

T = temperature, K (°R)

Note:

If the ethylene oxide concentration is in weight percent, use the following equation to calculate mole fraction:

where:

W_EO = weight percent of ethylene oxide

W_x = weight percent of compound in the balance of the mixture

MW_x = molecular weight of compound in the balance gas mixture

(ii) The residual mass of ethylene oxide in the sterilizer shall be determined by recording the chamber temperature, pressure, and volume after the completion of the first evacuation and using the following equation:

where:

W_r = weight of ethylene oxide remaining in chamber (after the first evacuation), in g (lb)

(iii) Calculate the total mass of ethylene oxide at the inlet to the control device (W_i) by subtracting the residual mass (W_r) calculated in paragraph (b)(1)(ii) of this section from the charged weight (W_c) calculated in paragraph (b)(1)(i) of this section.

(iv) The mass of ethylene oxide emitted from the control device outlet (W_o) shall be calculated by continuously monitoring the flow rate and concentration using the following procedure.

(A) Measure the flow rate through the control device exhaust continuously during the first evacuation using the procedure found in 40 CFR part 60, appendix A, Test Methods 2, 2A, 2C, or 2D, as appropriate. (Method 2D (using orifice plates or Rootstype meters) is recommended for measuring flow rates from sterilizer control devices.) Record the flow rate at 1-minute intervals throughout the test cycle, taking the first reading within 15 seconds after time zero. Time zero is defined as the moment when the pressure in the sterilizer is released. Correct the flow to standard conditions (20 °C and 101.325 kPa (68 °F and 1 atm)) and determine the flow rate for the run as outlined in the test methods listed

SV = standard volume, 24.05 liters per gram-mole (L/g-mole) at 20 °C and 101.325 kPa (385.1 scf per pound-mole (scf/lb-mole) at 68 °F and 1 atm).

(2) Determine the mass rate of EtO sent to controls during the performance test using equation 6 to this paragraph.

Where:

M_SCV = Total mass of EtO sent to controls per hour, g/hr (lb/hr) M_SCV,n = Total mass of EtO sent to controls per charge per chamber, g (lb) T_t = Total time of the performance test, hour n = Total number of charges during testing period f = Portion of EtO use that is assumed to be routed to the control system (0.93 if aeration is conducted in separate vessel; 0.98 otherwise)

(d) Compliance determination for facility where EtO use is less than 100 pounds per year. Each compliance demonstration shall consist of three separate runs using the applicable methods in paragraph (b) or (c) of this section. To determine compliance with the relevant standard, arithmetic mean of the three runs must be used. These procedures may be performed over a run duration of 1-hour (for a total of three 1-hour runs), except for the SCV testing from this category, where each run shall consist of the entirety of the sterilizer chamber evacuation and subsequent washes. The owner or operator may not conduct performance tests during periods of malfunction. The owner or operator must record the process information that is necessary to document operating conditions during the test and include in such record an explanation to support that such conditions represent the entire range of normal operation, including operational conditions for maximum emissions if such emissions are not expected during maximum production. The owner or operator must also account for the control system residence time when conducting the performance test. Upon request, the owner or operator shall make available to the Administrator such records as may be necessary to determine the conditions of performance tests. The following procedures shall be used to demonstrate compliance with a removal efficiency standard. In addition to these procedures, the procedures in paragraph (e) of this section must be followed to establish the operating parameter limits for each applicable emission control(s).

(1) You may determine the mass rate emissions of the stream prior to the control system and at the outlet of the control system using the test methods in paragraph (b) of this section.

(B) Test Method 18 or 25A, 40 CFR part 60, appendix A (hereafter referred to as Method 18 or 25A, respectively), shall be used to measure the concentration of ethylene oxide.

(1) Prepare a graph of volumetric flow rate versus time corresponding to the period of the run cycle. Integrate the area under the curve to determine the volume.

If the vent stream is comprised only of one or more SCVs, then you may use the procedures in paragraph (c) of this section for the mass rate emissions at the inlet.

(2) Calculate the total mass of

ethylene oxide by using the following equation:

Where:

Wo = Mass of ethylene oxide, g (lb)

C = concentration of ethylene oxide in ppmv

V = volume of gas exiting the control device corrected to standard conditions, L (ft³)

1/10⁶ = correction factor L_EO/10⁶ L_{TOTAL GAS} (ft³_EO/10⁶ ft³_{TOTAL GAS})

(3) Calculate the efficiency by the equation in paragraph (b)(1)(v) of this section.

(C) [Reserved]

(v) Determine control device efficiency (% Eff) using the following equation:

where:

% Eff = percent efficiency

W_i = mass flow rate into the control device

W_o = mass flow rate out of the control device

(vi) Repeat the procedures in paragraphs (b)(1) (i) through (v) of this section three

EtO per hour that is routed to the control system by summing the mass of EtO per hour from each vent.

(3) Determine percent emission reduction (%ER) using the equation 7 to this paragraph:

Where:

% ER = percent emission reduction M_APCD,i = total mass of EtO per hour to the control device E_APCD,o = total mass of EtO per hour from the control device

(4) Repeat these procedures two additional times. The arithmetic average percent efficiency of the three runs shall determine the overall efficiency of the control system.

(e) Determination of operating limits for control device(s).

(2) [Reserved]

(c) Concentration determination. The following procedures

If you are using performance testing to demonstrate compliance with removal efficiency standards, and if you are not demonstrating continual compliance with the applicable standard(s) using an EtO CEMS, you must also determine the operating limit(s) for each control device and then monitor the parameter(s) for each control device. The procedures in the following paragraphs shall be used to

determine the ethylene oxide concentration. (1) Parameter monitoring. For determining the ethylene oxide concentration required

establish the parameter operating limits to be continually monitored in § 63.364.

(

e), follow the procedures in PS 8 or PS 9 in 40 CFR part 60, appendix B. Sources complying with PS 8 are exempt from the relative accuracy procedures in sections 2.4 and 3 of PS-8. (2) Initial compliance

1) Acid-water scrubbers. The procedures in paragraph (e)(1) of this section shall be used to determine the operating limits for acid-water scrubbers.

(i) Ethylene glycol concentration. For determining the ethylene

oxide concentration required in § 63.363(c)(2), the procedures outlined in Method 18 or Method 25 A (40 CFR part 60, appendix A) shall be used. A Method 18 or Method 25A test consists of three 1-hour runs. If using Method 25A to determine concentration, calibrate and report Method 25A instrument results using ethylene oxide as the calibration gas. The arithmetic average of the ethylene oxide concentration of the three test runs shall determine the overall outlet ethylene oxide concentration from the control device.

(d) Efficiency determination at the aeration room vent (not manifolded). The following procedures shall be used to determine the efficiency of a control device used to comply with § 63.362(d), the aeration room vent standard.

(1) Determine the concentration of ethylene oxide at the inlet and outlet of the control device using the procedures in Method 18 or 25A in 40 CFR part 60, appendix A. A test is comprised of three 1-hour runs.

(2) Determine control device efficiency (% Eff) using the following equation:

Where:

% Eff = percent efficiency

W_i = mass flow rate into the control device

W_O = mass flow rate out of the control device

(3) Repeat the procedures in paragraphs (d)(1) and (2) of this section three times. The arithmetic average percent efficiency of the three runs shall determine the overall efficiency of the control device.

(e) Determination of baseline parameters for acid-water scrubbers.

glycol concentration operating limit, you must establish the maximum ethylene glycol concentration as the ethylene glycol concentration averaged over three test runs; use the sampling and analysis procedures in ASTM D3695-88 (incorporated by reference, see § 63.14) to determine the ethylene glycol concentration.

(ii) Scrubber liquor tank level. During the performance test, you must monitor and record the scrubber liquor tank level to the nearest 1⁄4 inch at the end of each of the three test runs. Use the data collected during the most recent performance test to calculate the average scrubber liquor tank level. This scrubber liquor tank level is the maximum operating limit for your scrubber liquor tank. Repeat this procedure for every scrubber liquor tank that is included in the performance test.

(iii) Scrubber liquor pH. During the performance test, you must monitor and record the scrubber liquor pH at least once every 15 minutes during each of the three test runs. You must use pH monitors as described in § 63.364(b)(3). Use the data collected during the most recent performance test to calculate the average scrubber pH measured. This scrubber liquor pH is the maximum operating limit for your acid-water scrubber. Repeat this procedure for every scrubber liquor tank that is included in the performance test.

(2) Thermal oxidizers. The procedures in this paragraph shall be used to determine the operating limits for thermal oxidizers.

(i) During the performance test, you must monitor and record the temperature at least once every 15 minutes during each of the three test runs. You must monitor the temperature in the firebox of the thermal oxidizer or immediately downstream of the firebox. You must use temperature monitors as described in § 63.364(c)(4).

(ii) Use the data collected during the performance test to calculate and record the average temperature for each test run maintained during the performance test. The average temperature of the test runs is the minimum operating limit for your thermal oxidizer, unless it exceeds the recommended maximum oxidation temperature provided by the oxidation unit manufacturer. If this occurs, the minimum operating limit for your thermal oxidizer consists of the recommended maximum oxidation temperature provided by the oxidation unit manufacturer.

(iii) Paragraphs (e)(2)(i) and (ii) of this section must be completed for each thermal oxidizer that is involved in the performance test.

(3) Catalytic oxidizers. The procedures in this paragraph shall be used to determine the

monitored parameters established in § 63.363(b), (d), or (e) for acid-water scrubbers and to monitor the parameters as established

operating limits for catalytic oxidizers.

(i) Prior to the start of the performance test, you must check the catalyst bed for channeling, abrasion, and settling. If problems are found during the inspection, you must replace the catalyst bed or take other correction action consistent with the manufacturer's recommendations.

(ii) During the performance test, you must monitor and record the temperature at the inlet to the catalyst bed and the temperature difference across the catalyst bed at least once every 15 minutes during each of the three test runs. You must use temperature monitors as described in § 63.364(

b

c)(4).

(

1) Ethylene glycol concentration. For determining the ethylene glycol concentration, the facility owner or operator shall establish the maximum ethylene glycol concentration as the ethylene glycol concentration averaged over three test runs; the sampling and analysis procedures in ASTM D 3695-88, Standard Test Method for Volatile Alcohols in Water By Direct Aqueous-Injection Gas Chromatography, (incorporated by reference—see § 63.14) shall be used to determine the ethylene glycol concentration.

(2) Scrubber liquor tank level. For determining the scrubber liquor tank level, the sterilization facility owner or operator shall establish the maximum liquor tank level based on a single measurement of the liquor tank level during one test run.

(f) [Reserved]

(g) An owner or operator of a sterilization facility seeking to demonstrate compliance with the standards found at § 63.362(c), (d), or (e)

iii) Use the data collected during the performance test to calculate and record the average temperature at the inlet to the catalyst bed and the average temperature difference across the catalyst bed maintained for each test run, and then calculate the arithmetic averages of the test runs. These arithmetic averages of the test runs are the minimum operating limits for your catalytic oxidizer, unless it exceeds the recommended maximum oxidation temperature provided by the oxidation unit manufacturer. If this occurs, the minimum operating limit for your catalytic oxidizer consists of the recommended maximum oxidation temperature provided by the oxidation unit manufacturer.

(iv) Paragraphs (e)(3)(i) through (iii) of this section must be completed for each catalytic oxidizer that is involved in the performance test.

(4) Gas/solid reactors. During the performance test, you must monitor and record the gas/solid reactor pressure drop at least once every 15 minutes during each of the three test runs. Use the data collected during the most recent performance test to calculate the gas/solid reactor pressure measured. This gas/solid reactor pressure is the maximum operating limit for your gas/solid. Repeat this procedure for every gas/solid reactor that is included in the performance test.

(5) Other control system for facility where EtO use is less than 100 pounds per year. If you seek to demonstrate compliance with a standard found at § 63.362 with a control device other than an acid-water scrubber

or

, catalytic

or thermal oxidation unit shall

oxidizer, thermal oxidizer, or gas/solid reactor, you must provide to the Administrator the information requested under § 63.363(

f

e).

The owner or operator shall submit

You must submit a monitoring plan that contains the following items: a description of the device; test results collected in accordance with § 63.363(

f

e) verifying the performance of the device for controlling

ethylene oxide

EtO emissions to the atmosphere to the levels required by the applicable standards; the appropriate operating parameters that will be monitored, identifying the ongoing QA procedures and performance specifications that will be conducted on the instruments; the frequency of conducting QA and performance checks; and the frequency of measuring and recording to establish continuous compliance with the standards.

The

Your monitoring plan

submitted identifying the compliance monitoring

is subject to the Administrator's approval.

The owner or operator of the sterilization facility shall

Upon approval by the Administrator you must install, calibrate, operate, and maintain the monitor(s) approved by the Administrator based on the information submitted

by the owner or operator. The owner or operator shall include in the information submitted to the Administrator

in your monitoring plan. You must include in your monitoring plan proposed performance specifications and quality assurance procedures for

their

your monitors. The Administrator may request further information and shall approve appropriate test methods and procedures.

(

h) An owner or operator of a sterilization facility seeking to demonstrate compliance with the requirements of § 63.363 or § 63.364, with a monitoring device or procedure other than a gas chromatograph or a flame ionization analyzer, shall provide to the Administrator information describing the operation of the monitoring device or procedure and the parameter(s) that would demonstrate continuous compliance with each operating limit. The Administrator may request further information and will specify appropriate test methods and procedures.

[59 FR 62589, Dec. 6, 1994, as amended at 66 FR 55584, Nov. 2, 2001; 79 FR 11283, Feb. 27, 2014]

f) Determination of compliance with PTE requirement. If you are required to operate any portion of your facility with PTE, you must demonstrate initial compliance with the requirements of this subpart by following the procedures of paragraphs (f)(1) through (3) of this section, as applicable, during the initial compliance demonstration or during the initial certification of the CEMS tests.

(1) Determine the capture efficiency by verifying the capture system meets the criteria in section 6 of Method 204 of appendix M to part 51 of this chapter and directs all the exhaust gases from the enclosure to an add-on control device.

(2) Ensure that the air passing through all NDOs flows into the enclosure continuously. If the facial velocities (FVs) are less than or equal to 9,000 meters per hour (492 feet per minute), the continuous inward flow of air shall be verified by continuous observation using smoke tubes, streamers, tracer gases, or other means approved by the Administrator over the period that the volumetric flow rate tests required to determine FVs are carried out. If the FVs are greater than 9,000 meters per hour (492 feet per minute), the direction of airflow through the NDOs shall be presumed to be inward at all times without verification.

(3) If you are demonstrating continuous compliance through monitoring the volumetric flow rate, you must monitor and record the volumetric flow rate (in cubic feet per second) from the PTE through the stack(s) at least once every 15 minutes during each of the three test runs. Use the data collected during the most recent compliance demonstration to calculate the average volumetric flow rate measured during the compliance demonstration. This volumetric flow rate is the minimum operating limit for the stack. Repeat this procedure for every stack that is included in the compliance demonstration.