40 CFR § 63.786 - Test methods and procedures.
(a) For the compliance procedures described in § 63.785(c) (1) through (c)(3), Method 24 of 40 CFR part 60, appendix A, is the definitive method for determining the VOC content of coatings, as supplied or as applied. When a coating or thinner contains exempt compounds that are volatile HAP or VOHAP, the owner or operator shall ensure, when determining the VOC content of a coating, that the mass of these exempt compounds is included.
(b) For the compliance procedure described in § 63.785(c)(4), the Administrator must approve the test method for determining the VOHAP content of coatings and thinners. As part of the approval, the test method must meet the specified accuracy limits indicated below for sensitivity, duplicates, repeatability, and reproducibility coefficient of variation each determined at the 95 percent confidence limit. Each percentage value below is the corresponding coefficient of variation multiplied by 2.8 as in the ASTM Method E180-93: Standard Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals (incorporation by reference - see § 63.14).
(1) Sensitivity. The overall sensitivity must be sufficient to identify and calculate at least one mass percent of the compounds of interest based on the original sample. The sensitivity is defined as ten times the noise level as specified in ASTM Method D3257-93: Standard Test Methods for Aromatics in Mineral Spirits by Gas Chromatography (incorporation by reference - see § 63.14). In determining the sensitivity, the level of sample dilution must be factored in.
(2) Repeatability. First, at the 0.1-5 percent analyte range the results would be suspect if duplicates vary by more than 6 percent relative and/or day to day variation of mean duplicates by the same analyst exceeds 10 percent relative. Second, at greater than 5 percent analyte range the results would be suspect if duplicates vary by more than 5 percent relative and/or day to day variation of duplicates by the same analyst exceeds 5 percent relative.
(3) Reproducibility. First, at the 0.1-5 percent analyte range the results would be suspect if lab to lab variation exceeds 60 percent relative. Second, at greater than 5 percent range the results would be suspect if lab to lab variation exceeds 20 percent relative.
(4) Any test method should include information on the apparatus, reagents and materials, analytical procedure, procedure for identification and confirmation of the volatile species in the mixture being analyzed, precision and bias, and other details to be reported. The reporting should also include information on quality assurance (QA) auditing.
(5) Multiple and different analytical techniques must be used for positive identification if the components in a mixture under analysis are not known. In such cases a single column gas chromatograph (GC) may not be adequate. A combination of equipment may be needed such as a GC/mass spectrometer or GC/ infrared system. (If a GC method is used, the operator must use practices in ASTM Method E260-91 or 96: Standard Practice for Gas Chromatography [incorporation by reference - see § 63.14].)
(c) A coating manufacturer or the owner or operator of an affected source may use batch formulation data as a test method in lieu of Method 24 of appendix A to 40 CFR part 60 to certify the as-supplied VOC content of a coating if the manufacturer or the owner or operator has determined that batch formulation data have a consistent and quantitatively known relationship to Method 24 results. This determination shall consider the role of cure volatiles, which may cause emissions to exceed an amount based solely upon coating formulation data. Notwithstanding such determination, in the event of conflicting results, Method 24 of appendix A of 40 CFR part 60 shall take precedence.
(d) Each owner or operator of an affected source shall use or ensure that the manufacturer uses the form and procedures mentioned in appendix A of this subpart to determine values for the thinner and coating parameters used in Equations 1 and 2 of this subpart. The owner or operator shall ensure that the coating/thinner manufacturer (or supplier) provides information on the VOC and VOHAP contents of the coatings/thinners and the procedure(s) used to determine these values.
(e) For add-on control systems approved for use in limiting emissions from coating operations pursuant to § 63.783(c), performance tests shall be conducted under such conditions as the Administrator specifies to the owner or operator based on representative performance of the affected source for the period being tested. Upon request, the owner or operator shall make available to the Administrator such records as may be necessary to demonstrate the conditions present during performance tests.
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