Section 98.414 - Monitoring and QA/QC requirements(a) The mass of fluorinated GHGs, fluorinated HTFs, or nitrous oxide coming out of the production process shall be measured using flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better. If the measured mass includes more than one fluorinated GHG or fluorinated HTF, the concentrations of each of the fluorinated GHGs or fluorinated HTFs, other than low-concentration constituents, shall be measured as set forth in paragraph (n) of this section. For each fluorinated GHG or fluorinated HTF, the mean of the concentrations of that fluorinated GHG (mass fraction) measured under paragraph (n) shall be multiplied by the mass measurement to obtain the mass of that fluorinated GHG or fluorinated HTF coming out of the production process.(b) The mass of any used fluorinated GHGs, fluorinated HTFs, or used nitrous oxide added back into the production process upstream of the output measurement in paragraph (a) of this section shall be measured using flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better. If the mass in paragraph (a) is measured by weighing containers that include returned heels as well as newly produced fluorinated GHGs or fluorinated HTFs, the returned heels shall be considered used fluorinated GHGs or fluorinated HTFs for purposes of this paragraph (b) and § 98.413(b) .(c) The mass of fluorinated GHGs, fluorinated HTFs, or nitrous oxide fed into the transformation process shall be measured using flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better.(d) The fraction of the fluorinated GHGs, fluorinated HTFs, or nitrous oxide fed into the transformation process that is actually transformed shall be estimated considering yield calculations or quantities of unreacted fluorinated GHGs, fluorinated HTFs, or nitrous oxide permanently removed from the process and recovered, destroyed, or emitted.(e) The mass of fluorinated GHGs, fluorinated HTFs, or nitrous oxide sent to another facility for transformation shall be measured using flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better.(f) The mass of fluorinated GHGs or fluorinated HTFs sent to another facility for destruction shall be measured using flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better. If the measured mass includes more than trace concentrations of materials other than the fluorinated GHG or fluorinated HTF, the concentration of the fluorinated GHG or fluorinated HTF shall be estimated considering current or previous representative concentration measurements and other relevant process information. This concentration (mass fraction) shall be multiplied by the mass measurement to obtain the mass of the fluorinated GHG or fluorinated HTF sent to another facility for destruction.(g) You must estimate the share of the mass of fluorinated GHGs or fluorinated HTFs in paragraph (f) of this section that is comprised of fluorinated GHGs or fluorinated HTFs that are not included in the mass produced in § 98.413(a) because they are removed from the production process as by-products or other wastes.(h) You must measure the mass of each fluorinated GHG or fluorinated HTF that is fed into the destruction device and that was previously produced as defined at § 98.410(b) . Such fluorinated GHGs or fluorinated HTFs include but are not limited to quantities that are shipped to the facility by another facility for destruction and quantities that are returned to the facility for reclamation but are found to be irretrievably contaminated and are therefore destroyed. You must use flowmeters, weigh scales, or a combination of volumetric and density measurements with an accuracy and precision of one percent of full scale or better. If the measured mass includes more than trace concentrations of materials other than the fluorinated GHG or fluorinated HTF being destroyed, you must estimate the concentrations of the fluorinated GHG or fluorinated HTF being destroyed considering current or previous representative concentration measurements and other relevant process information. You must multiply this concentration (mass fraction) by the mass measurement to obtain the mass of the fluorinated GHG or fluorinated HTF fed into the destruction device.(i) Very small quantities of fluorinated GHGs or fluorinated HTFs that are difficult to measure because they are entrained in other media such as destroyed filters and destroyed sample containers are exempt from paragraphs (f) and (h) of this section.(k) For purposes of Equation OO-4 of this subpart, the destruction efficiency can be equated to the destruction efficiency determined during a previous performance test of the destruction device or, if no performance test has been done, the destruction efficiency provided by the manufacturer of the destruction device.(l) In their estimates of the mass of fluorinated GHGs or fluorinated HTFs destroyed, facilities that destroy fluorinated GHGs or fluorinated HTFs shall account for any temporary reductions in the destruction efficiency that result from any startups, shutdowns, or malfunctions of the destruction device, including departures from the operating conditions defined in state or local permitting requirements and/or oxidizer manufacturer specifications.(m) Calibrate all flow meters, weigh scales, and combinations of volumetric and density measures that are used to measure or calculate quantities that are to be reported under this subpart prior to the first year for which GHG emissions are reported under this part. Calibrations performed prior to the effective date of this rule satisfy this requirement. Recalibrate all flow meters, weigh scales, and combinations of volumetric and density measures at the minimum frequency specified by the manufacturer. Use NIST-traceable standards and suitable methods published by a consensus standards organization (e.g., ASTM, ASME, ISO, or others).(n) If the mass coming out of the production process includes more than one fluorinated GHG or fluorinated HTF, you shall measure the concentrations of all of the fluorinated GHGs or fluorinated HTFs, other than low-concentration constituents, as follows:(1)Analytical Methods. Use a quality-assured analytical measurement technology capable of detecting the analyte of interest at the concentration of interest and use a procedure validated with the analyte of interest at the concentration of interest. Where standards for the analyte are not available, a chemically similar surrogate may be used. Acceptable analytical measurement technologies include but are not limited to gas chromatography (GC) with an appropriate detector, infrared (IR), fourier transform infrared (FTIR), and nuclear magnetic resonance (NMR). Acceptable methods include EPA Method 18 in appendix A-1 of 40 CFR part 60 ; EPA Method 320 in appendix A of 40 CFR part 63 ; the Protocol for Measuring Destruction or Removal Efficiency (DRE) of Fluorinated Greenhouse Gas Abatement Equipment in Electronics Manufacturing, Version 1, EPA-430-R-10-003, (March 2010) (incorporated by reference, see § 98.7 ); ASTM D6348-03 Standard Test Method for Determination of Gaseous Compounds by Extractive Direct Interface Fourier Transform Infrared (FTIR) Spectroscopy (incorporated by reference, see § 98.7 ); or other analytical methods validated using EPA Method 301 in appendix A of 40 CFR part 63 or some other scientifically sound validation protocol. The validation protocol may include analytical technology manufacturer specifications or recommendations.(2)Documentation in GHG Monitoring Plan. Describe the analytical method(s) used under paragraph (n)(1) of this section in the site GHG Monitoring Plan as required under § 98.3(g)(5) . At a minimum, include in the description of the method a description of the analytical measurement equipment and procedures, quantitative estimates of the method's accuracy and precision for the analytes of interest at the concentrations of interest, as well as a description of how these accuracies and precisions were estimated, including the validation protocol used.(3)Frequency of measurement. Perform the measurements at least once by February 15, 2011 if the fluorinated GHG product is being produced on December 17, 2010. Perform the measurements within 60 days of commencing production of any fluorinated GHG product that was not being produced on December 17, 2010. For fluorinated HTF products that are not also fluorinated GHG products, perform the measurements at least once by February 28, 2018, if the fluorinated HTF product is being produced on January 1, 2018. Perform the measurements within 60 days of commencing production of any fluorinated HTF product that was not being produced on January 1, 2018. Repeat the measurements if an operational or process change occurs that could change the identities or significantly change the concentrations of the fluorinated GHG or fluorinated HTF constituents of the fluorinated GHG or fluorinated HTF product. Complete the repeat measurements within 60 days of the operational or process change.(4)Measure all product grades. Where a fluorinated GHG or fluorinated HTF is produced at more than one purity level (e.g., pharmaceutical grade and refrigerant grade), perform the measurements for each purity level.(5)Number of samples. Analyze a minimum of three samples of the fluorinated GHGs or fluorinated HTF product that have been drawn under conditions that are representative of the process producing the fluorinated GHGs or fluorinated HTF product. If the relative standard deviation of the measured concentrations of any of the fluorinated GHGs or fluorinated HTF constituents (other than low-concentration constituents) is greater than or equal to 15 percent, draw and analyze enough additional samples to achieve a total of at least six samples of the fluorinated GHG or fluorinated HTF product.(o) All analytical equipment used to determine the concentration of fluorinated GHGs or fluorinated HTFs, including but not limited to gas chromatographs and associated detectors, IR, FTIR and NMR devices, shall be calibrated at a frequency needed to support the type of analysis specified in the site GHG Monitoring Plan as required under paragraph (n) of this section and § 98.3(g)(5) . Quality assurance samples at the concentrations of concern shall be used for the calibration. Such quality assurance samples shall consist of or be prepared from certified standards of the analytes of concern where available; if not available, calibration shall be performed by a method specified in the GHG Monitoring Plan.(p) Isolated intermediates that are produced and transformed at the same facility are exempt from the monitoring requirements of this section.(q) Low-concentration constituents are exempt from the monitoring and QA/QC requirements of this section. 74 FR 56374 , Oct. 30, 2009, as amended at 75 FR 79167 , Dec. 17, 2010; 81 FR 89270 , Dec. 9, 2016