1

From: Joe Sopata, Chemist, USEPA/OAR/OTAQ/CD/FCC To: Docket Number EPA

- HQ

- OAR

- 2011

- 0135 Subject: Supplemental Proposed Regulations: Performance Based Measurement S ystem Date: 12/21/2011

The following are proposed regulations as discussed in section i. ii , Option 2, Agency Approval of All Test Methods, in the preamble of this proposed rule.

5. Section 80.47 is revised to read as follows:

**§ 80.47 Performance Based Analytical Test Method Approach.** 

All sample handling, testing procedures and tests must be conducted using good laboratory practices.

(a) Definitions. As used in this subpart: ( 1 ) Performance

- based Analy tical Test Method Approach means a measurement sy stem based upon established performance criteria for accuracy and precision with use of

anal yt ical test methods. As used in this subpart, a measurement s ys tem used by laboratories to demonstrate that a particular anal yt ical test method is acceptable for demonstrating compliance. ( 2 ) Accuracy means the closeness of agreement between an observe d value from a single test measurement and an accepted reference value. ( 3 ) Precision means the degree of agreement in a set of measurements performed on the same propert y of identical test material. (4) Absolute fuel parameter means a fuel parameter for which a gravimetric standard is practical to construct and use. Sulfur content of gasoline, butane, or diesel fuel are examples of an absolute fuel parameter. (5) Gravimetric standard means a test material made by adding a carefull y weighed quantity of th e anal yt e to a measured quantity of another substance known not to contain any of the anal yt e, resulting in a solution with an accurately known concentrate of the anal yt e. (6) Consensus named fuels are homogeneous quantities of fuel that have been anal yz ed by a number of different laboratories (b y sending around small samples). The average concentration of some parameter of interest across all of the different laboratories is then used as the “consensus name” for that material. (7) Locally

- named reference materials are gasoline or diesel fuels that are usually from the regular production of the facility where they

are used in laboratory

quality control efforts and have been anal yz ed using the designated method (either by the facility’s lab or by

a referee lab) to obtain an estimate of their concentratio n. (8) Method

- defined fuel parameter means a fuel parameter for which an EPA

- prescribed primary test method or “designated method” defines the regulatory standard. Examples of method

- defined fuel parameters include olefin content in gasoline, Reid vapor p ressure (RVP) of gasoline, distillation parameters of gasoline, benzene content of gasoline, aromatic content of gasoline and diesel fuel, and oxy gen/ox ygenates content of gasoline.2

(9) Reference Installations are designated test method installations that are used to qualify the accuracy

of other method

- defined parameter instruments. Reference installations of the designated test method will be used to evaluate the accuracy of other method

- defined alternative test methods and to establish correlation equ ations if necessary

. (10) Correlation equation is a correction equation as determined by the use of ASTM International standard practice D6708 (incorporated by reference, see paragraph (r) of this section). This standard practice determines whether the co mparison between the alternative test method and the designated test method is a “null” result. If the comparison is not “null’, then the standard practice provides for a correlation equation that predicts designated test method results from the applicabl e method

- defined alternative test method. (11) Statistical quality

control (SQC) means a planned sy stem of activities whose purpose is to provide a level of quality that meets the needs of compliance with the standards of Part 80. This subpart prescribes specific SQC requirements for both absolute and method driven fuel parameters for both VCSB and non

- VCSB regulated parties. (12) Voluntary

consensus

- based standards body (VCSB) means a domestic or international organization that plans, develops, establ ishes, or coordinates voluntary consensus standards using agreed

- upon procedures and which possesses the attributes of openness, balance of interest, due process, and consensus, as explained in OMB Circular A

- 119 and the National Technology

Transfer and Advancement Act of 1995, P.L . 104

- 113, sec. 12(d). (13) Non

- Voluntary

consensus

- based standards bod y (non

- VCSB) means a domestic or international regulated party whose anal yt ical test method is not adopted by a VCSB organization.

(b) Precision and accuracy criteri a for approval for the absolute fuel parameter of gasoline sulfur. (1) Precision. Beginning November 30, 2013, for motor vehicle gasoline and gasoline fuel additives subject to the gasoline sulfur standard at §80. 195 and §80.1603, the maximum allo wable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory

practices taken from a single homogeneous commerciall y available gasolin e must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability of ASTM D7039

- 07 (Example: A 10ppm sulfur gasoline sample: maximum allowable standard deviation of 20
tests ≤1.5*(1.75ppm/2.77)=0.95 ppm ). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility may exclude a given sample or test result only if the exclusion is for a valid reason under good laboratory practices and it maintain s records regarding the sample and test results and the reason for excluding them. (2) Accuracy

. Beginning November 30, 2013, for motor vehicle gasoline and gasoline fuel additives subject to the gasoline sulfur standard at §80. 195 and §80.1603: (i) The arithmetic average of a continuous series of at least 10 tests performed using good laboratory

practices on a commerciall y available gravimetric sulfur standard in the range of 1

- 10 ppm shall not differ from the accepted reference value (ARV) of the stand ard b y more than 0.71 ppm sulfur;3

(ii) The arithmetic average of a continuous series of at least 10 tests performed using good laboratory

practices on a commerciall y available gravimetric sulfur standard in the range of 10

- 20 ppm shall not differ from the accepted reference value (ARV) of the standard by more than 1.00 ppm sulfur; and (iii) In apply ing the tests of paragraphs (b)(2)(i) and (b)(2)(ii) of this section, individual test results shall be compensated for an y known chemical interferences using goo d laboratory practices. (3) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (4) Samples used for precision and accuracy determination must be retained for 90 day s. (5) EPA appr oval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (b) (1) through ( 4 ) of this section, the Administrator shall determine whether the test method is approved under this section. (6) If the Administrator denies approv al of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (b) (1) through ( 4 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (7) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon noti ce from the Administrator the approval shall be void ab initio

. (c) Precision and accuracy criteri a for approval of the absolute fuel parameter of sulfur in butane. (1) Precision. Beginning November 30, 2013 , for butane subject to the butane sulfur stand ard at §80.82 and §80.1603 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single homogeneous commerciall y available butane must be less than or equal to 1.5 times the repeatabilit y “r” divided by 2.77, where “r” equals the ASTM repeatability of ASTM D6667

- 10 (Example: A 10ppm sulfur butane sample: maximum allowable standard deviation of 20 tests ≤1.5*(1.15ppm/2.77)=0.62 ppm). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility
may exclude a given sample or test result only if the exclusion is for a va lid reason under good laboratory

practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Accuracy

. Beginning November 30, 2013 , for butane subject to the butane sulfur standard at §80.82 and §0.160 3 : (i) The arithmetic average of a continuous series of at least 10 tests performed using good laboratory

practices on a commerciall y available gravimetric sulfur standard in the range of 1

- 10 ppm shall not differ from the accepted reference value (ARV) of the standard b y more than 0.47 ppm sulfur; (ii) The arithmetic average of a continuous series of at least 10 tests performed using good laboratory

practices on a commerciall y available gravimetric sulfur standard in the range of 10

- 20 ppm shall not differ from the accepted reference value (ARV) of the standard b y more than 0.94ppm sulfur; and4

(iii) In apply ing the tests of paragraphs (c)(2)(i) and (c)(2)(ii) of this section, individual test results shall be compensated for an y known chemical interferences using good laboratory practices

. (3) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (4) Samples used for precision and accuracy determination must be retained for 90 day s. (5) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (c) (1) through ( 4 ) of this section, the Administrator shall determine whether the test method is approved under this section. (6) If the Administrator deni es approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (c) (1) through ( 4 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administr ator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (7) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (d) Precision criteria for approval of the method defined fuel parameter of olefins in gasoline? (1) Precision. Beginning November 30, 2013 , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standard s of Part 80 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability

of ASTM D1319

- 10 (Example: A gasoline containing 9Vol% ole fins: maximum allowable standard deviation of 20
tests ≤1.5*(0.972Vol%/2.77)=0.53Vol%). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility may exclude a given sample or test result only if the exclusion is for a valid reason under good laboratory practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary to render a d ecision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained for 90 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (d) (1) through ( 3 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (d) (1) through ( 3 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed appr oved.5

(6) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (e) Precision criteria for approval of the metho d defined fuel parameter of aromatics in gasoline

. (1) Precision. Beginning November 30, 2013 , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standard s at Part 80 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability

of ASTM D1319

- 10 (Example: A gasoline containing 32Vol% aromatics: maximum allowable standard deviation of 20
tests ≤1.5*(1.3Vol%/2.77)=0.70Vol%). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility may exclude a given sample or test result only if the exclusion is for a valid reason under good laboratory practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained f or 90 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (e) (1) through ( 4 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Adm inistrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (e) (1) through ( 4 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. I f the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (6) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (f) Precision criteria for approval of the method defined fuel parameter of ox ygen and

ox y genate content in gasoline

. (1) Precision. Beginning November 30, 2013 , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standard s at Part 80 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests p er day) on samples using good laboratory practices taken from a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability

of ASTM 5599

- 00(2010) (Example: A gasoline containing 3Mass% total oxy gen: maximum allowable standard deviation of 20
tests ≤1.5*(0.083Mass%/2.77)=0.045Mass%). The 20 results must be a series of tests with a sequential record of anal ys is and no emissions. A laboratory facility may

exclude6

a given sample or test result only if the exclusion is for a valid reason under good laboratory

practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requeste d by the Administrator and necessary to render a decision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained for 90 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to b e submitted under paragraphs (f) (1) through ( 3 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Administrator denies approval of the test method, within 90 day s of receipt of all materia ls required to be submitted in paragraphs (f) (1) through ( 3 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the appl ication, then the test method shall be deemed approved. (6) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (g) Precision criteria for approval of the method defined fuel parameter of Reid Vapor Pressure (RVP) in gasoline. (1) Precision. Beginning November 30, 2013 , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standards of Part 80, and the volatility standards at § 80.27 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided b y 2.77, where “r” equals the ASTM repeatability of ASTM 5191

- 10b (Example: A gasoline hav ing a RVP of 6.8psi: maximum allowable standard deviation of 20 tests ≤1.5*(0.21psi/2.77)=0.11psi). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility may exclude a given sample or test re sult only if the exclusion is for a valid reason under good laboratory practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary t o render a decision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained for 90 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (g) (1) through ( 3 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (g) (1) through ( 3 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method s hall be deemed approved.7

(6) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (h) Precision criteria for ap proval of the method defined fuel parameter of gasoline distillation. (1) Precision. Beginning November 30, , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standards of Part 80 , the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability

of ASTM D86

- 11a for the initial boiling point, E10, E50, E90 and final boiling point. (Example: A gasoline having an initial boiling point of 20 0 C and a final boil ing point of 110 0 C: maximum allowable standard deviation of 20 tests for initial boiling point≤1.5*(2.84 0 C/2.77)=1.54 0 C, maximum allowable standard deviation of 20 tests for E10 ≤1.5*(1.33 0 C/2.77)=0.72 0 C, maximum allowable standard deviation of 20 tests for E50 ≤1.5*(0.74 0 C/2.77)=0.40 0 C, maximum allowable standard deviation of 20 tests for E90t≤1.5*(1.79 0 C/2.77)=0.97 0 C, and maximum allowable standard deviation of 20 tests for final boiling point≤1.5*(3.33 0 C/2.77)=1.80 0 C ). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility
may exclude a given sample or test result only if the exclusion is for a valid reason under good laboratory

practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained for 9 0 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (h) (1) through ( 3 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Adminis trator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (h) (1) through ( 3 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If th e Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (6) If the Administrator finds that an individual test facility has provide false or inaccurate information under thi s section, upon notice from the Administrator the approval shall be void ab initio

. (i) Precision criteria for approval of the method defined fuel parameter of benzene in gasoline. (1) Precision. Beginning November 30, 2013 , for motor vehicle gasoline and gasoline fuel additives subject to the gasoline standards of Part 80 and theMSAT2 standards at § § 80. 41, 80. 101, 80. 1230, the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory practices taken from a single8

homogeneous commercially available gasoline must be less than or equal to 1.5 times the repeatability

“r” divided by

2.77, where “r” equals the ASTM repeatability of ASTM D3606

- 10 (Example: A gasoline having a 1Vol% benzene: maximum allowable standard deviation of 20 tests ≤1.5*(0.04Vol%/2.77)=0.02Vol%). The 20 results must be a series of tests with a sequential record of anal ys is and no emissions. A laboratory facility may exclude a given sample or test result only if the exclusion is for a valid reason under good laboratory

practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (3) Samples used for precision and accuracy determination must be retained for 90 day s. (4) EPA approval. Within 90 day s o f the receipt of materials required to be submitted under paragraphs (i) (1) through ( 3 ) of this section, the Administrator shall determine whether the test method is approved under this section. (5) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (i) (1) through ( 3 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (6) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrat or the approval shall be void ab initio

. (j) Precision criteria for approval of the method defined fuel parameter of aromatics in diesel. (1) Precision. Beginning November 30, 2013 , for motor vehicle diesel and diesel fuel additives subject to the motor vehicle diesel standards at §80. 520, the maximum allowable standard deviation computed from the results of a minimum of 20 tests made over 20 day s (7 or fewer tests per week and 2 or fewer tests per day) on samples using good laboratory

practices taken fro m a single homogeneous commerciall y available gasoline must be less than or equal to 1.5 times the repeatability “r” divided by

2.77, where “r” equals the ASTM repeatability of ASTM D1319

- 10 (Example: A diesel fuel containing 35Vol% aromatics: maximum allo wable standard deviation of 20
tests ≤1.5*(1.3Vol%/2.77)=0.70Vol%). The 20 results must be a series of tests with a sequential record of analy sis and no emissions. A laboratory facility may exclude a given sample or test result only if the exclusion is fo r a valid reason under good laboratory practices and it maintains records regarding the sample and test results and the reason for excluding them. (2) Any

additional information requested b y the Administrator and necessary to render a decision as to approv al of the test method. (3) Samples used for precision and accuracy determination must be retained for 90 day s. (4) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (j) (1) through ( 3 ) of this section, the A dministrator shall determine whether the test method is approved under this section. (5) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (j) (1) through ( 3 ) of this s ection, the9

Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved. (6) If the Adm inistrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (k) Criteri on for designated test method reference installations use d to qualify the accuracy of other method

- defined parameter instruments. (1) Beginning November 30, 2013 , the reference installation of the method

- defined fuel parameter for the applicable designated test method must have precision equal to 1.5 times the repeatabilit y “r” of the method

- defined fuel parameter’s designated test method, where “r” is the repeatability of the designated test method. (i) Olefins in gasoline see §80.47(d)(1). (ii) Aromatics in gasoline see §80.47(e)(1). (iii) Ox ygen and Ox ygenate content of gasoline see §80.47(f)(1). (iv) Reid Vapor Pressure (RVP) of gasoline see §80.47(g)(1). (v) Gasoline Distillation see §80.47(h)(1). (vi) Benzene in Gasoline see §80.47(i)(1) (vii) Aromatics in Diesel see §80.47(j)(1). (2) The reference installation of the method

- defined fuel parameter for the applicable designated test method must be shown to be near the middle distribution of an industry monthly inter

- laboratory

crosscheck program for at least a period of five months. Specificall y, compute the difference between the instrument’s average measurement of the fuel closest to the applicable fuel standard (or to the average value for the fuel parameter in the complex model) and the robust mean for that fuel obtained by all of the

non

- outlier labs in the monthly inter

- laboratory

crosscheck program. Standardize this difference b y expressing it in robust standard deviation units. These standardized inter

laboratory

crosscheck differences should be placed in a moving average with a minimum span of five months. The instrument’s moving average in robust standard deviation units cannot be outside the central 50% of the distribution of all laboratories that participated in the inter

- laboratory

crosscheck program. (3) The reference installation of the method

- defined fuel parameter for the applicable designated test method must be shown to be in statistical quality control as specified in ASTM International D6299 (incorporated by reference, see paragraph (r) of this section) for a minimum period of five months

. (4) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (5) Samples used for precision and accuracy determination must be retained for 90 day s. (6) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (k) (1) through ( 5 ) of this section, the Administrator shall determine whether the test method is approved under this section. (7) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (k ) (1) through ( 5 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If10

the Administrator does not notify the applic ant within 90 day s of receipt of the application, then the test method shall be deemed approved. (8) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (l) Qualification criteri a for Voluntary Consensus Standard Based (VCSB) Method

- Defined Parameter Test Methods. (1) Beginning November 30, 2013
, include full test method documentation by the Voluntary Consensus St andard Based (VCSB) organization, including a description of the technology

and/or instrumentation that makes the method functional. (2) In clude i nformation reported in the test method that demonstrates the test method meets the applicable precision inform ation for the method

- defined fuel parameter as described in this section. (3) In clude i nformation reported in the test method that demonstrates the test method has been evaluated using ASTM International D6708 (incorporated by reference, see paragraph (r) of this section) and whether the comparison is a null result or whether a correlation equation needs to be applied that predicts designated test method results from the applicable method

- defined alternative test method. (4) Any

additional information reque sted b y the Administrator and necessary to render a decision as to approval of the test method. (5) Samples used for precision and accuracy determination must be retained for 90 day s. (6) EPA approval. Within 90 day s of the receipt of materials required t o be submitted under paragraphs (l) (1) through ( 5 ) of this section, the Administrator shall determine whether the test method is approved under this section. (7) If the Administrator denies approval of the test method, within 90 day s of receipt of all
mate rials required to be submitted in paragraphs (l) (1) through ( 5 ) of this section, the Administrator will notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the

a pplication, then the test method shall be deemed approved. (8) If the Administrator finds that an individual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab init io

. (m) Qualification C riteri on for Non

- Voluntary Consensus Standard Based (non

- VCSB) Method

- Defined Parameter Test Methods

. For such a method to be approved, the following information must be submitted to the Administrator by each test facility

for each method that it wishes to have approved. (1) Beginning November 30, 2013 , full and thorough test method documentation, including a description of the technology and/or instrumentation that makes the method functional so a person lacking experience with the test instrument would be able to replicate its results. (2) In formation reported in the test method that demonstrates the test method meets the applicable precision information for the method

- defined fuel parameter as described in this section. (3) Both the candidate method

- defined Non

- VCSB test method and its respective designated test method must be tested on a range of consensus named fuels or locally

- named11

reference materials that are ty pical of those anal yz ed by the facility

in practice and must
meet the data requirements for variability as required in ASTM International D6708 (incorporated b y reference, see paragraph (r) of this section). (4) The facility

using the candidate method

- defined non

- VCSB test method must statistically establish through app lication of ASTM D6708 (incorporated by reference, see paragraph (r) of this section) that the candidate method measures the same aspect of samples as applicable to its respective designated test method. (5) If the use of ASTM D6708 (incorporated b y refere nce, see paragraph (r) of this section) reveals that the candidate method

- defined non

- VCSB test method has sample

- specific biases due to matrix effects that cannot be determined as random the method is disqualified. If however, it is determined that the c andidate method

- defined non

- VCSB test method can be qualified on a narrow circumscribed range of fuels while still meeting the data requirements for variability as required in ASTM International D6708 (incorporated b y reference, see paragraph (r) of this s ection) (see (m)(3)), then the ty pes of fuels on which the qualification was achieved and for which the method is to be approved must be specified in the candidate method

- defined non

- VCSB test method description. If there is any restriction on the scope o f fuels for which the candidate method

- defined non

- VCSB test method is to be qualified, the applicant must include a discussion of how the facility plans to screen sample for conformity to the scope. If the candidate method

- defined test method is found to have minimal matrix effects, a statement to this effect must be included by the applicant in its application. (6) The candidate method

- defined non

- VCSB test method precision qualification must be conducted in the form of “cross

- method reproducibility ” (Rc m) of the candidate method and applicable designated test method as required in ASTM International D6708 (incorporated b y reference, see paragraph (r) of this section), where the Rcm must be equal to or less than 70 percent of the published reproducibility of the applicable designated test method. (7) The applicant of the candidate method

- defined non

- VCSB test method must demonstrate through the use of ASTM D6708 (incorporated by reference, see paragraph (r) of this section) whether a correlation to applica ble designated test method is necessary . If it is determined through the use of this practice that the candidate method

- defined non

- VCSB test method requires a correlation equation in order to predict designated test method results, then this correlation equation must be applied to the candidate instruments output to obtain measurement results for regulatory purposes. (8) Any

additional information requested b y the Administrator and necessary to render a decision as to approval of the test method. (9) Samp les used for precision and accuracy determination must be retained for 90 day s. (10) EPA approval. Within 90 day s of the receipt of materials required to be submitted under paragraphs (m) (1) through ( 9 ) of this section, the Administrator shall determine whether the test method is approved under this section. (11) If the Administrator denies approval of the test method, within 90 day s of receipt of all materials required to be submitted in paragraphs (m) (1) through ( 9 ) of this section, the Administrator wil l notify the applicant of the reasons for not approving the method. If the Administrator does not notify the applicant within 90 day s of receipt of the application, then the test method shall be deemed approved.12

(12) The Administrator may revoke approval of a test method under this section for cause, including, but not limited to, a determination b y the Administrator that the approved test method has proved to be inadequate in practice. (13) An independent third

- party scientific review and written report and verification of the information provided pursuant to paragraphs (m)(1) through (m)(9) of this section. The report and verification shall be based upon a site visit and review of relevant documents and shall separatel y identify each item required b y par agraphs (m)(1) through (m)(9) of this section, describe how the independent third

- party evaluated the accuracy

of the information provided, state whether the independent third

- party agrees with the information provided, and identify an y exceptions between the independent third

- part y’s findings and the information provided. (i) The information required under this section to be provided by an independent third party must be conducted by both a professional chemist and professional statistician as specified in paragraphs (m)(13)(i)(A) of this section. The verify ing chemist and statistician must be: (A) For a refiner, importer, ox ygenate producer, and ox ygen ate blender, a chemist and statistician who has received at least a bachelor’s degree in science fro m an accredited college in the United States, with professional work experience in the petroleum or ox ygenate field. (B) [Reserved] (ii) To be considered an independent third

- party under this paragraph (m)(13): (A) The third

- part y shall not be empl oy ed by the refiner, importer, oxy genate producer, or ox ygenate blender, or an y subsidiary or employee of the refiner, import facility , oxy genate producing facility , or oxy genate blender. (B) The third part y shall be free from an y interest in the refine r’s, importer’s,
oxy genate producer’s, or oxy genate blender’s business. (C) The refiner, importer, ox ygenate producer, or ox ygen ate blender shall be free from an y interest in the third

- part y’s business. (D) Use of a third

- part y that is debarred, susp ended, or proposed for debarment pursuant to the Government

- wide Debarment and Suspension regulations, 40 CFR part 32, or the Debarment, Suspension and Ineligibility provisions of the Federal Acquisition Regulations, 48 CFR, part 9, subpart 9.4 shall be de emed in noncompliance with the requirements of this section. (iii) The independent third

- part y shall retain all records pertaining to the verification required under this section for a period of five ye ars from the date of creation and shall deliver such records to the Administrator upon request. (iv) The third

- part y must provide to EPA documentation of his or her qualifications as part of the scientific review, including proof of appropriate college degree. ( 14 ) If the Administrator finds that an indiv idual test facility has provide false or inaccurate information under this section, upon notice from the Administrator the approval shall be void ab initio

. (n) Accuracy

and Precision Statistical Quality Control (SQC) Requirements for the Absolute Fuel Parameters. Beginning November 30, 2013 , a test shall not be considered a test using an approved test method unless the following qualit y control procedures are performed separatel y for each instrument used to make measurements:13

(1) Accuracy

SQC. Every fac ility shall conduct tests of every instrument with a commerciall y available gravimetric reference material, or check standard as defined in the ASTM International standard practice D6299 (incorporated by reference, see paragraph (r) of this section) on at least a quarterl y basis using good laboratory practices

. The facility

must pre

- treat and assess results from the check standard testing after at least 15 testing occasions as described in section 8.2 of this standard practice. The facilit y must construct “MR” and “I” charts with control lines as described in section 8.4 and appropriate Annex sections of this standard practice. In circumstances where the absolute difference between the mean of multiple back

- to

- back tests of the standard reference material and the accepted reference value of the standard reference material is greater than 0.75 times the published reproducibility of the test method must be investigated b y the facility. Records of the standard reference materials measurements as well as an y investigations into any exceedance of these criteria must be kept for a period of 5 y ears. (2) (i) Precision SQC. Each facility on every instrument tests a quality control material as defined in paragraph 3.2.3 in ASTM International D6299 (incorporated by reference, see paragraph (r) of this section) either once per week or once per every 20 productions tests, which ever is more frequent. The facilit y must construct and maintain an “I” chart as described in section 7 and section A1.5.1 and a “MR” chart as described in section A1.5.2. Any

violations of control limit(s) should be investigated by personnel of the facil ity and records kept for a period of 5 y ears. (ii) Validation of New QC Material. When a test facility is making a transition from one batch of QC material to the next batch of QC material, the facility will follow the “Q

Procedure” in Annex 1.9 of ASTM International standard practice D6299 (incorporated by reference, see paragraph (r) of this section). In following the Q

- Procedure if the plot of results from the old and new QC materials on its respective chart shows not special

cause signals, then the re sult of the new QC material will be considered valid. These records must be kept by

the facilit y for a period of 5 years.

(o) Accuracy

and Precision Statistical Quality Control (SQC) Requirements for the Voluntary

Consensus Standard Based (VCSB) Method

- D efined Fuel Parameters. Beginning November 30, 2013 a test shall not be considered a test using an approved test method unless the following qualit y control procedures are performed separatel y for each instrument used to make measurements: (1) Accuracy SQC. Every facility shall conduct tests of every instrument with a commerciall y available check standard as defined in the ASTM International standard practice D6299 (incorporated b y reference, see paragraph (r) of this section) on at least a quarterl y ba sis using good laboratory practices . The check standard must be an ordinary fuel with levels of the fuel parameter of interest close to either the applicable regulatory standard or the average level of use for the facility. The Accepted Reference Value o f the check standard must be determined b y the respective designated test method for the fuel parameter following the guidelines of ASTM International standard practice D6299. The facility must pre

- treat and assess results from the check standard testing after at least 15 testing occasions as described in section 8.2 of this standard practice. The facility must construct “MR” and “I” charts with control lines as described in section 8.4 and appropriate Annex sections of this standard practice. In circums tances where the14

absolute difference between the mean of multiple back

- to

- back tests of the standard reference material and the accepted reference value of the standard reference material is greater than 0.75 times the published reproducibility of the test method must be investigated b y the facility. Records of the standard reference materials measurements as well as an y investigations into any exceedance of these criteria must be kept for a period of 5 y ears. (2) (i) Precision SQC. Every facility shall conduct tests of every instrument with a quality control material as defined in paragraph 3.2.3 in ASTM International D6299 (incorporated b y reference, see paragraph (r) of this section) either once per week or once
per every 20 productions tests, whicheve r is more frequent using good laboratory practices . The facility

must construct and maintain an “I” chart as described in section 7 and section A1.5.1 and a “MR” chart as described in section A1.5.2. Any violations of control limit(s) should be investigated b y personnel of the facilit y and records kept for a period of 5 ye ars. (ii) Validation of New QC Material. When a test facility is making a transition from one batch of QC material to the next batch of QC material, the facility will follow the “Q

Proc edure” in Annex 1.9 of ASTM International standard practice D6299 (incorporated by reference, see paragraph (r) of this section). In following the Q

- Procedure if the plot of results from the old and new” QC materials on its respective chart shows no speci al

cause signals, then the result of the new QC material will be considered valid. These records must be kept by

the facilit y for a period of 5 years.

(p) Accuracy

and Precision Statistical Quality Control (SQC) Requirements for the Non

Voluntary

Consens us Standard Based (Non

- VCSB) Method

- Defined Fuel Parameters. Beginning November 30, 2013 , a test shall not be considered a test using an approved test method unless the following qualit y control procedures are performed separatel y for each instrument used to make measurements: (1) Accuracy

SQC for Non

- VCSB Method

- Defined test methods with minimal matrix effects. Every facility shall conduct test of every instrument with a commercially available check standard as defined in the ASTM International standard practice D6299 (incorporated b y reference, see paragraph (r) of this section) on at least a quarterl y basis using good laboratory

practices . The check standard must be an ordinary fuel with levels of the fuel parameter of interest close to either the appl icable regulatory standard or the average level of use for the facilit y. The Accepted Reference Value of the check standard must be determined b y the respective designated test method for the fuel parameter following the guidelines of ASTM International s tandard practice D6299. The facility must pre

- treat and assess results from the check standard testing after at least 15 testing occasions as described in section 8.2 of this standard practice. The facility must construct “MR” and “I” charts with control lines as described in section 8.4 and appropriate Annex sections of this standard practice. In circumstances where the absolute difference between the mean of multiple back

- to

- back tests of the standard reference material and the accepted reference value of the standard reference material is greater than 0.75 times the published reproducibility of the test method must be investigated b y the facility

. Records of the standard reference materials measurements as well as an y investigations into any exceedanc e of these criteria must be kept for a period of 5 y ears.15

(2) (i) Accuracy

SQC for Non

- VCSB Method

- Defined test methods with high sensitivity to matrix effects. Every facility shall conduct tests of every instrument with a production fuel on at least a quarterly basis using good laboratory practices . The production fuel must be representative of the production fuels that are routinel y anal yz ed by the facility

. The Accepted Reference Value of the production fuel must be determined by the respective refe rence installation of the designated test method for the fuel parameter following the guidelines of ASTM International standard practice D6299 (incorporated by reference, see paragraph (r) of this section). The facilit y must pre

- treat and assess results f rom the check standard testing after at least 15 testing occasions as described in section 8.2 of this standard practice. The facility must construct “MR” and “I” charts with control lines as described in section 8.4 and appropriate Annex sections of this standard practice. In circumstances where the absolute difference between the mean of multiple back

- to

- back tests of the standard reference material and the accepted reference value of the standard reference material is greater than 0.75 times the publis hed reproducibility

of the test method must be investigated by the facility . Documentation on the identity

of the reference installation and its control status must be maintained on the premises of the “method

- defined” alternative test method. Records of the standard reference materials measurements as well as an y i nvestigations into an y exceedance of these criteria must be kept for a period of 5 y ears. (ii) Each facility

is required to send every 20 th production batch of gasoline or diesel fuel to EPA’s laboratory , along with the facility ’s measurement result used to certify the batch using the respective method

- defined non

- VCSB test method. The EPA retains the right to return such sample on a blind basis for a required reanal ys is on the respective metho d

defined non

- VCSB test method within 180 day s upon receipt of such sample. (3) Precision SQC. Every facility shall conduct tests of every instrument with a quality control material as defined in paragraph 3.2.3 in ASTM International D6299 (incorporated by

reference, see paragraph (r) of this section) either once per week or once
per every 20 productions tests, whichever is more frequent using good laboratory practices . The facility

must construct and maintain an “I” chart as described in section 7 and section A1.5.1 and a “MR” chart as described in section A1.5.2. Any violations of control limit(s) should be investigated b y personnel of the facilit y and records kept for a period of 5 ye ars. (ii) Validation of New QC Material. When a test facility is m aking a transition from one batch of QC material to the next batch of QC material, the facility will follow the “Q

Procedure” in Annex 1.9 of ASTM International standard practice D6299 (incorporated by reference, see paragraph (r) of this section). In fol lowing the Q

- Procedure if the plot of results from the old and new QC materials on its respective chart shows no special

cause signals, then the result of the new QC material will be considered valid. These records must be kept by

the facilit y for a perio d of 5 y ears.
(q) Record retention requirements for the test methods approved under this subpart. (1) Each individual test facility must retain records related to the establishment of accuracy and precision values, all test method documentation, and an y s tatistical quality control testing and anal ys is under this section using good laboratory practices for a period for five y ears. (2) [Reserved]16

(r) Materials incorporated by reference. The Director of the Federal Register approved the incorporation b y ref

erence of the documents listed in this section as prescribed in 5 U.S.C. 552(a) and 1 CFR 51. Any one may inspect copies at the U.S. EPA, Air and Radiation Docket and Information Center, 1301 Constitution Ave., N.W., Room B102, EPA West Building, Washingto n, DC, 20460, under EPA docket ID Number **EPA**

**- HQ** 

**** **OAR**

**- 2011** 

**- 0135**  , or at the National Archives and Records Administration (NARA). The telephone number for the Air Docket Public Reading Room is (202) 566

- 1742. For information on the availability of this mater ial at NARA, call 202

- 741

- 6030 or go to: http://www.archives.gov//federal_register/code_of_federal_regulations/ibr_locations.htm l . For further informati on on these test methods, please contact the Environmental Protection Agency

at 734

- 214

- 4582. (1) ASTM International material. An yone may purchase copies of these materials from the ASTM International (ASTM), 100 Barr Harbor Dr., West Conshohocken, PA 194 28

- 2959, or by

contacting ASTM International customer service at 10

- 832

- 9585, or by contacting the email address of service@astm.org from the ASTM International Web site of http://www. astm.org

. (i) ASTM International standard practice D6708

- 08 (“ASTM International D6708”), “Standard Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport to Measure the Same Property of a Material”, approved December 15, 2008. (ii) ASTM International standard practice D6299

- 10 ε1 (“ASTM International D6708”), “Standard Practice for Apply ing Statistical Quality Assurance and Control Charting Techniques to Evaluate Analy tical Measurement Sy stem Performance”, approved March 1, 2010.