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10/24/14 

Tier 3 Questions 

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

identification of the test method used to measure the sulfur content of the batch, as 

determined under §80.330” is required when submitting annual reporting. Questions: Does 

EPA intend that the test method is to include the year versioning of the test method? How 

does EPA plan to have refiners and importers include this information on the reporting form 

and when will the new format be released? 

2. According to §80.1610(a)(4), the concentration of all denaturants used in DFE is limited to a 

maximum of 3.0 volume percent. However in the renewable fuel definition of §80.1401(2) 

“Ethanol covered by this definition shall be denatured as required and defined in 27 CFR 

parts 19 through 21. Any volume of denaturant added to the undenatured 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 have 3 vol% denaturant but only allow 2 

vol% to be included for purposes of determining compliance with Subpart M? 

3. The final rule is defining the Quality control material for use in the statistical control by 

ASTM D6299. Quote from 79 FR 23587: 

We proposed similar precision and accuracy SQC requirements for each instrument used to 

measure absolute and VCSB-approved and non-VCSB proprietary methods for measuring 

method-defined parameters in the laboratory. We proposed that every instrument would 

test a quality control (QC) material514 either once per 20 production tests or once per week 

and maintain both an ‘‘I’’ chart515 and an ‘‘MR’’ chart.516

 

514 See ASTM D6299–10e1, paragraph 3.2.3 for a definition 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 system. 

But probably the following paragraph might be the correct 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 measurement system, a stable and homogeneous material 

having physical or chemical properties, or both, similar to those of typical samples tested by the 

analytical measurement system. The material is properly stored to ensure sample integrity, and 

is available in sufficient quantity for repeated, long term testing. 

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

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 October 28, 2013 are exempt from the 

requirements of paragraphs (l)(1) through (3) of this section. 

6. May RFG ILCP or MO ILCP samples be used to comply 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-Defined Fuel Parameters. 

Beginning January 1, 2016, a test shall not be considered a test using an approved test 

method unless the following quality control procedures are performed separately for each 

instrument used to make measurements: 

(1) Accuracy SQC. Every facility shall conduct tests of every instrument with a 

commercially available check standard as defined in the ASTM D6299 at least three 

times a year 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 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 evaluation of alternate VCSB test methods 

against the reference method and reporting of the results 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 requirements 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 reference 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 D1319 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 commercially 
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available inter-laboratory cross-check program (ILCP) data may be used as is without 

imposing the reference installations requirements of this section, provided that the 

number of non-outlying results is greater than 16 for both the designated and alternative 

test methods. The determination of ARV of check standards 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 VCSB 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 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 

8. The language in §80.46(a)(1) was revised to say “Beginning January 1, 2016, the sulfur 

content of gasoline must be determined by a test method 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.” Further, in §80.47(b)(3) it says “The test 

method specified at §80.46(a)(1) and in use prior to 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 the word “must” was used intentionally, 

how does that reconcile with the exemption in §80.47(b)(3)? 

9. In the Tier 3 rule, there are a number of places that 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, pursuant 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 (PBMS). See 78 FR 29964. This 

initially lead us to believe this new requirement would go into effect concurrent with PBMS 

starting in 2016. However, the final Tier 3 rule makes 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 include the identification of test methods? 

If the requirement is effective immediately, when will the Unified Report Form be updated? 

10. The language in 80.1603(d) Oxygenate added downstream from the refinery or import 

facility is confusing and difficult to reconcile with 80.69(a) relative to reformulated gasoline. 

Currently, refiners certify reformulated gasoline after 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: 
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(1) For oxygenate added to reformulated gasoline, RBOB, conventional gasoline, or 

CBOB, the refiner or importer shall calculate the sulfur content of the batch by 

volume weighting the sulfur content of the conventional gasoline or CBOB and the 

sulfur content of the added oxygenate pursuant to the following requirements: ... 

The beginning of the paragraph talks about reformulated 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 only applicable to conventional gasoline 

and CBOB? Additionally, in 80.1603(d)(1)(ii) it goes on to talk about determining the sulfur 

content of the oxygenate added downstream of the refinery and says you can either test the 

sulfur on a sample of oxygenate or assume a value of 5.00 ppm if the oxygenate is denatured 

ethanol. How does this work when you are adding ethanol to RBOB at the refinery lab and 

testing the sample after the addition of the ethanol? Or, again, is this section really only for 

conventional gasoline and CBOB and we should continue 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 states)? Section 80.1654 states that the 

refiner may use testing methods approved in Title 13 of the California Code instead of testing 

methods required under 80.1630. Section 80.1630 states the following: 

(a) Sample and test each batch of gasoline and certified ethanol denaturant. 

 (1) Refiners and importers shall collect a representative sample from each batch 

of gasoline produced or imported and test each sample 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 80.47 (testing). 

Section 80.1630 is specific to sulfur in gasoline. Does this mean that for other gasoline 

properties, the California exemption outlined in Section 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 correlating to the designated EPA test methods 

and these designated methods are “grandfathered” under 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?