• Abstract and Figures
• Public Full-text

Environmental Protection Agency Pt. 63, App. A APPENDIX A TO PART 63—TEST METHODS posed as an alternative test method to meet an applicable requirement or in the absence METHOD 301—FIELD VALIDATION OF POLLUT- of a validated method. Additionally, the val- ANT MEASUREMENT METHODS FROM VARIOUS idation procedures of Method 301 are appro- WASTE MEDIA priate for demonstration of the suitability of alternative test methods under 40 CFR parts USING METHOD 301 59, 60, and 61. If, under 40 CFR part 63 or 60, 1.0 What is the purpose of Method 301? you choose to propose a validation method other than Method 301, you must submit and 2.0 What approval must I have to use Method obtain the Administrator’s approval for the 301? candidate validation method. 3.0 What does Method 301 include? 2.0 What approval must I have to use Method 301? 4.0 How do I perform Method 301? If you want to use a candidate test method REFERENCE MATERIALS to meet requirements in a subpart of 40 CFR part 59, 60, 61, 63, or 65, you must also request 5.0 What reference materials must I use? approval to use the candidate test method according to the procedures in Section 16 of SAMPLING PROCEDURES this method and the appropriate section of 6.0 What sampling procedures must I use? the part (§ 59.104, § 59.406, § 60.8(b), § 61.13(h)(1)(ii), § 63.7(f), or § 65.158(a)(2)(iii)). 7.0 How do I ensure sample stability? You must receive the Administrator’s writ- ten approval to use the candidate test meth- DETERMINATION OF BIAS AND PRECISION od before you use the candidate test method to meet the applicable federal requirements. 8.0 What are the requirements for bias? In some cases, the Administrator may decide 9.0 What are the requirements for precision? to waive the requirement to use Method 301 for a candidate test method to be used to 10.0 What calculations must I perform for meet a requirement under 40 CFR part 59, 60, isotopic spiking? 61, 63, or 65 in absence of a validated test method. Section 17 of this method describes 11.0 What calculations must I perform for the requirements for obtaining a waiver. comparison with a validated method? 3.0 What does Method 301 include? 12.0 What calculations must I perform for analyte spiking? 3.1 Procedures. Method 301 includes min- imum procedures to determine and docu- 13.0 How do I conduct tests at similar sources? ment systematic error (bias) and random error (precision) of measured concentrations OPTIONAL REQUIREMENTS from exhaust gases, wastewater, sludge, and other media. Bias is established by com- 14.0 How do I use and conduct ruggedness paring the results of sampling and analysis testing? against a reference value. Bias may be ad- 15.0 How do I determine the Limit of Detection justed on a source-specific basis using a cor- for the candidate test method? rection factor and data obtained during the validation test. Precision may be determined OTHER REQUIREMENTS AND INFORMATION using a paired sampling system or quadru- plicate sampling system for isotopic spiking. 16.0 How do I apply for approval to use a A quadruplicate sampling system is required candidate test method? when establishing precision for analyte spik- ing or when comparing a candidate test 17.0 How do I request a waiver? method to a validated method. If such proce- 18.0 Where can I find additional information? dures have not been established and verified for the candidate test method, Method 301 19.0 Tables. contains procedures for ensuring sample sta- bility by developing sample storage proce- USING METHOD 301 dures and limitations and then testing them. Method 301 also includes procedures for rug- 1.0 What is the purpose of Method 301? gedness testing and determining detection Method 301 provides a set of procedures for limits. The procedures for ruggedness testing the owner or operator of an affected source and determining detection limits are re- to validate a candidate test method as an al- quired for candidate test methods that are to ternative to a required test method based on be applied to multiple sources and optional established precision and bias criteria. These for candidate test methods that are to be ap- validation procedures are applicable under 40 plied at a single source. CFR part 63 or 65 when a test method is pro- 3.2 Definitions. 641 VerDate Sep<11>2014 17:25 Sep 20, 2019 Jkt 247166 PO 00000 Frm 00651 Fmt 8010 Sfmt 8002 Q:\40\40V16.TXT PC31 kpayne on VMOFRWIN702 with $$_JOB Pt. 63, App. A 40 CFR Ch. I (7–1–19 Edition) Affected source means an affected source as dures in Sections 5.1 through 5.4 of this defined in the relevant part and subpart method. under Title 40 (e.g., 40 CFR parts 59, 60, 61, 63, 5.1 Exhaust Gas Test Concentration. You and 65). must obtain a known concentration of each Candidate test method means the sampling analyte from an independent source such as and analytical methodology selected for field a specialty gas manufacturer, specialty validation using the procedures described in chemical company, or chemical laboratory. Method 301. The candidate test method may You must also obtain the manufacturer’s be an alternative test method under 40 CFR certification of traceability, uncertainty, part 59, 60, 61, 63, or 65. and stability for the analyte concentration. Paired sampling system means a sampling 5.2 Tests for Other Waste Media. You must system capable of obtaining two replicate obtain the pure liquid components of each samples that are collected as closely as pos- analyte from an independent manufacturer. sible in sampling time and sampling location The manufacturer must certify the purity, (collocated). traceability, uncertainty, and shelf life of Quadruplicate sampling system means a sam- the pure liquid components. You must dilute pling system capable of obtaining four rep- the pure liquid components in the same type licate samples (e.g., two pairs of measured medium or matrix as the waste from the af- data, one pair from each method when com- fected source. paring a candidate test method against a 5.3 Surrogate Analytes. If you demonstrate validated test method, or analyte spiking to the Administrator’s satisfaction that a with two spiked and two unspiked samples) surrogate compound behaves as the analyte that are collected as close as possible in sam- does, then you may use surrogate compounds pling time and sampling location. for highly toxic or reactive compounds. A Surrogate compound means a compound surrogate may be an isotope or compound that serves as a model for the target com- that contains a unique element (e.g., chlo- pound(s) being measured (i.e., similar chem- rine) that is not present in the source or a ical structure, properties, behavior). The sur- derivation of the toxic or reactive compound rogate compound can be distinguished by the if the derivative formation is part of the candidate test method from the compounds method’s procedure. You may use laboratory being analyzed. experiments or literature data to show be- havioral acceptability. 4.0 How do I perform Method 301? 5.4 Isotopically-Labeled Materials. Isotope First, you use a known concentration of an mixtures may contain the isotope and the analyte or compare the candidate test meth- natural analyte. The concentration of the od against a validated test method to deter- isotopically-labeled analyte must be more mine the bias of the candidate test method. than five times the concentration of the nat- Then, you collect multiple, collocated simul- urally-occurring analyte. taneous samples to determine the precision SAMPLING PROCEDURES of the candidate test method. Additional pro- cedures, including validation testing over a 6.0 What sampling procedures must I use? broad range of concentrations over an ex- tended time period are used to expand the You must determine bias and precision by applicability of a candidate test method to comparison against a validated test method multiple sources. Sections 5.0 through 17.0 of using isotopic spiking or using analyte spik- this method describe the procedures in de- ing (or the equivalent). Isotopic spiking can tail. only be used with candidate test methods ca- pable of measuring multiple isotopes simul- REFERENCE MATERIALS taneously such as test methods using mass spectrometry or radiological procedures. 5.0 What reference materials must I use? You must collect samples according to the You must use reference materials (a mate- requirements specified in Table 301–1 of this rial or substance with one or more properties method. You must perform the sampling ac- that are sufficiently homogenous to the cording to the procedures in Sections 6.1 analyte) that are traceable to a national through 6.4 of this method. standards body (e.g., National Institute of 6.1 Isotopic Spiking. Spike all 12 samples Standards and Technology (NIST)) at the with isotopically-labelled analyte at an level of the applicable emission limitation or analyte mass or concentration level equiva- standard that the subpart in 40 CFR part 59, lent to the emission limitation or standard 60, 61, 63, or 65 requires. If you want to ex- specified in the applicable regulation. If pand the applicable range of the candidate there is no applicable emission limitation or test method, you must conduct additional standard, spike the analyte at the expected test runs using analyte concentrations high- level of the samples. Follow the applicable er and lower than the applicable emission spiking procedures in Section 6.3 of this limitation or the anticipated level of the tar- method.

Load more

  268

Copy Link