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10/24/14



### Tier 3 Questions

1. The language in §80.370(a)(7) states “The sulfur co ntent of the batch, along with

identification of the test method used to measure t he sulfur content of the batch, as determined under §80.330” is required when submitti ng annual reporting. Questions: Does EPA intend that the test method is to include the y ear versioning of the test method? How does EPA plan to have refiners and importers includ e this information on the reporting form

and when will the new format be released?

2. According to §80.1610(a)(4), the concentration of a ll denaturants used in DFE is limited to a maximum of 3.0 volume percent. However in the rene wable fuel definition of §80.1401(2) “Ethanol covered by this definition shall be denatu red as required and defined in 27 CFR parts 19 through 21. Any volume of denaturant adde d to the u nden a tured ethanol by a producer or importer in excess of 2 volume percent shall not be included in the volume of ethanol for purposes of determining compliance with the requirements under this subpart.” Question: Did EPA intend that DFE be allowed to hav e 3 vol% denaturant but only allow 2 vol% to be included for purposes of determining com pliance with Subpart M?

3. The final rule is defining the Quality control mate rial for use in the statistical control by ASTM D6299. Quote from 79 FR 23587: We proposed similar precision and accuracy SQC requ irements for each instrument used to measure absolute and VCSB-approved and non-VCSB pro prietary methods for measuring method-defined parameters in the laboratory. We pr oposed that every instrument would test a quality control (QC) material 514 either once per 20 production tests or once per we ek

and maintain both an ‘‘I’’ chart 515 and an ‘‘MR’’ chart. 516

514 See ASTM D6299–10e1, paragraph 3.2.3 for a definit ion and Section 6 for guidance, selection, construction, handling, storage and use of reference material samples.

Where 3.2.3 check standard, n—in QC testing , a material having an accepted reference value used to determine the accuracy of a measurement sys tem.

But probably the following paragraph might be the c orrect reference:

3.2.8 quality control (QC) sample, n— for use in quality assurance programs to determine and monitor the precision and stability of a measuremen t system, a stable and homogeneous material having physical or chemical properties, or both, si milar to those of typical samples tested by the analytical measurement system. The material is pro perly stored to ensure sample integrity, and is available in sufficient quantity for repeated, l ong term testing.

The check standard is a much more expensive option that the quality control sample.2

4. The reference in 80.47(l)(3) is unclear. Does the outcome of the D6708 assessment need to be incorporated into the VCSB test method by the go verning body before the alternative

method can be used?

(3) Include information reported in the test method that demonstrates the test method has been evaluated using ASTM D6708 and whether the com parison is a “null” result or whether a correlation equation needs to be applied that predicts designated test method results from the applicable method-defined alternat ive test method.

5. The reference in 80.47(l)(4) is unclear. Does “ in use” mean by the testing community at large or by a particular lab or organization?

(4) The test methods specified at §§80.2(w) and 80. 46(a)(1), (a)(2), (b)(1), (c)(1), (d)(1), (e)(1), (f)(1), and (g)(1) and in use prior to Octo ber 28, 2013 are exempt from the requirements of paragraphs (l)(1) through (3) of th is section.

6. May RFG ILCP or MO ILCP samples be used to compl y with the accuracy QC procedure referenced in 80.47(o)(1)?

(o) Accuracy and Precision Statistical Quality Control (SQC) Requirements for the Voluntary Consensus Standard Based (VCSB) Method-De fined Fuel Parameters

. Beginning January 1, 2016, a test shall not be cons idered a test using an approved test method unless the following quality control procedu res are performed separately for each

instrument used to make measurements:

(1) Accuracy SQC. Every facility shall conduct tests of every instru ment with a commercially available check standard as defined in the ASTM D6299 at least three times a year using good laboratory practices. The c heck 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 facili ty. The Accepted Reference Value of the check standard must be determined by the respective designated test method for the fuel parameter following the guidelines of ASTM D6299.

7. The language in 80.47(k)(4) requests D6708 evalu ation of alternate VCSB test methods against the reference method and reporting of the r esults of the bias evaluation. Per 80.47(k)(4) which exempts the statistics generated by ASTM inter-laboratory cross check programs from the reference installation requiremen ts and deems ILCP statistics suitable for

D6708 assessment of alternative VCSB test methods. Can any subset of recent cross-check program results of an alternative method and refere nce method be assessed using D6708 methodology to generate the information required in section (3)? For example, could the 2013 ASTM RFG ILCP aromatic results reported for D1 319 and D5769 be used in the

D6708 bias assessment?

(4) For a voluntary consensus standards body, such as ASTM, or for a commercially available industry crosscheck program, the summary statistics (mean and standard error = standard deviation/square root [number of results]) from the VCSB or commercially3

available inter-laboratory cross-check program (ILC P) data may be used as is without imposing the reference installations requirements o f this section, provided that the number of non-outlying results is greater than 16 f or both the designated and alternative

test methods. The determination of ARV of check st andards as specified in ASTM D6299, clause 6.2.2.1 and Note 7 shall be followed for the inter-laboratory crosscheck program. The use of VCSB or commercially available ILCP data as described above is

deemed suitable for an ASTM D6708 assessment of VCS B alternative test methods.

Also see 80.47(l)(3):

(3) Include information reported in the test method that demonstrates the test method has been evaluated using ASTM D6708 and whet her the comparison is a “null” result or whether a correlation equation needs to b e applied that predicts designated test method results from the applicable method-defined a lternative test method

8. The language in §80.46(a)(1) was revised to say “Be ginning January 1, 2016, the sulfur content of gasoline must be determined by a test me thod approved under §80.47.” (Emphasis added.) In other subsections in §80.46, for other fuel parameters, there is a similar phrase, except the word “may” is used instead of “must.” F urther, in §80.47(b)(3) it says “The test method specified at §80.46(a)(1) and in use prior t o October 28, 2013 is exempt from the requirements of (b)(1) and (2) of this subsection.” Questions: Did EPA intend to use the word “may” instead of “must” in §80.46(a)(1)? If t he word “must” was used intentionally, how does that reconcile with the exemption in §80.4 7(b)(3)?

9. In the Tier 3 rule, there are a number of places th at address what information is to be reported for gasoline batches. For example, see §80.75 and §80.105. One of the new data elements required in the Tier 3 rule is the test method used for the reported property. For instance, in the new §80.105(a)(5)(v) it says we are to report “ The properties, along with identification of the test method used to measure those properties, p ursuant to §80.101(i).” This new requirement was initially discussed in the preamble to the proposed Tier 3 rule in the section related to Performance Based Measurement Systems (P BMS). See 78 FR 29964. This initially lead us to believe this new requirement w ould go into effect concurrent with PBMS starting in 2016. However, the final Tier 3 rule m akes no reference to the effective date of this new requirement, so it appears it is effective immediately (i.e. June 27, 2014). Questions: When must our gasoline batch reports in clude the identification of test methods? If the requirement is effective immediately, when w ill the Unified Report Form be updated?

10. The language in 80.1603(d) Oxygenate added downstream from the refinery or imp ort facility is confusing and difficult to reconcile with 80.69( a) relative to reformulated gasoline. Currently, refiners certify reformulated gasoline a fter the addition of ethanol to the RBOB sample at the refinery lab, as required by Section 80.69(a). Section 80.1603(d) states the following:4

(1) For oxygenate added to reformulated gasoline, R BOB, conventional gasoline, or CBOB, the refiner or importer shall calculate the s ulfur content of the batch by volume weighting the sulfur content of the conventi onal gasoline or CBOB and the sulfur content of the added oxygenate pursuant to t he following requirements: ...

The beginning of the paragraph talks about reformul ated gasoline and RBOB, in addition to conventional gasoline and CBOB; however, the end of the sentence only refers to conventional gasoline and CBOB. Is this section on ly applicable to conventional gasoline and CBOB? Additionally, in 80.1603(d)(1)(ii) it go es on to talk about determining the sulfur content of the oxygenate added downstream of the re finery and says you can either test the sulfur on a sample of oxygenate or assume a value o f 5.00 ppm if the oxygenate is denatured ethanol. How does this work when you are adding et hanol to RBOB at the refinery lab and testing the sample after the addition of the ethano l? Or, again, is this section really only for conventional gasoline and CBOB and we should contin ue to follow current practice for

RBOB?

11. How do the performance based testing requirements apply to California refineries that produce non-CARB gasoline for export (to other stat es)? Section 80.1654 states that the refiner may use testing methods approved in Title 1 3 of the California Code instead of testing methods required under 80.1630. Section 80.1630 st ates the following:

(a) Sample and test each batch of gasoline and certifie d ethanol denaturant. (1) Refiners and importers shall collect a repr esentative sample from each batch of gasoline produced or imported and test each samp le to determine its sulfur content for compliance with requirements under this subpart prior to the gasoline leaving the refinery or import facility, using the sampling and testing methods provided in this section or §§80.8 (sampling) and 8 0.47 (testing).

Section 80.1630 is specific to sulfur in gasoline. Does this mean that for other gasoline properties, the California exemption outlined in Se ction 80.81 applies? Section 80.81 requires

the California refineries to correlate the results from the California Title 13 methods to the EPA

methods. If the California refineries have been co rrelating to the designated EPA test methods and these designated methods are “grandfathered” un der the Tier 3 regulations, then we assume these labs do not need to qualify any test methods. Do the QA/QC requirements in Section 80.47 apply to these California refinery labs?