Form ECA0300 ECA Marine Fuel Sulfur Precision Demonstration

Instructions for ECA Marine Fuel
Test Method Spreadsheet

Instructions for ECA Marine Fuel

Test Method Spreadsheet

Compliance Division
Office of Transportation and Air Quality
U.S. Environmental Protection Agency

March 2016

OMB Control Number: 2060-0308
Expiration Date: March 31, 2019

EPA-420-B-16-054
March 2016

Disclaimer
The discussion in this document is intended solely as guidance. The statutory provisions and
EPA regulations described in this document contain legally binding requirements. This
document is not a regulation itself, nor does it change or substitute for those provisions and
regulations. Thus, it does not impose legally binding requirements on EPA, States, or the
regulated community. This spreadsheet template key does not confer legal rights or impose
legal obligations upon any member of the public.
While EPA has made every effort to ensure the accuracy of the discussion in this spreadsheet
example key for use with its associated spreadsheet example, the obligations of the regulated
community are determined by statutes, regulations, or other legally binding requirements. In the
event of a conflict between the discussion in this document and any statute or regulation, this
document would not be controlling.
The general description of the application process provided here may not apply to a particular
situation. Interested parties are free to raise questions about the substance of this spreadsheet
template key, its associated spreadsheet, and its applicability to a particular situation. EPA may
adopt approaches on a case-by-case basis that differ from those described in this spreadsheet
template key.
Mention of trade names or commercial products does not constitute endorsement or
recommendation for their use.
This is a living document and may be revised periodically without public notice. EPA welcomes
public input on this document at any time.

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Introduction: On April 30, 2010, EPA promulgated new requirements for ECA marine fuel.
For ECA marine fuel at the 1,000 ppm sulfur level, if your test facility has chosen to use the
designated test method, ASTM D 2622-10, or any of the following alternative test methods,
ASTM D 4294-10, ASTM D 5453-12, or ASTM D 6920-13 with correlation to the designated test
method, it is not necessary for your test facility to self-qualify these test methods for precision or
accuracy.
One of the provisions of this final rule, explained in Subpart I of 40 CFR Part 80.580(c)(ii),
provides an option for each test facility to meet specified accuracy and precision criteria with
their chosen test method for sulfur in ECA marine fuel. This option only applies to refiners and
importers of ECA marine fuel. Evidence of having met these requirements for Voluntary
Consensus Standards Body (VCSB) test methods must be demonstrated by the test facility via
self-qualification before using the method to make measurements for demonstrating compliance
(80 FR 9078, February 19, 2015). Evidence of having met these requirements for NonVoluntary Consensus Standards Body test methods must be submitted to and approved by the
Agency before using the method to make measurements for demonstrating compliance.
40 CFR § 80.510(k) explains the 1,000 ppm sulfur standard for ECA marine fuel. 40 CFR §
80.584 explains the actual accuracy and precision criteria for the applicable standard above. 40
CFR § 80.585 explains both the requirement that the criteria must be met on a facility-specific
basis and a description of the process by which methods may be approved. The following
guidance applies to any party applying to EPA for such approval of their test method at their
testing facility for ECA marine fuel. This information deals only with the approval of test methods
at a testing facility for measuring sulfur in ECA marine fuel.
The discussions of the applicable regulations in this document are not verbatim. The reader is
encouraged to read and become familiar with the applicable regulations of Subpart I of 40 CFR
Part 80. These instructions are intended to help a test facility self-qualify a VCSB test method
for the measurement of sulfur in ECA marine fuel, as well as, to help facilitate the timely review
and approval of each test facility’s Non-VCSB test method.
Applicable Dates: These requirements for method qualification under § 80.585 became
effective on June 1, 2014.
Note: Please see Part I for instructions on use of a spreadsheet template provided by the
Agency for determining compliance with the accuracy and precision criteria of § 80.584. We
encourage parties to use this spreadsheet to structure their development of the information and
data needed for a method qualification application and to submit it to the Agency for Non-VCSB
test methods in order to expedite the review and approval process. Please see Part II for
submission instructions.

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Part I - Instructions for use of spreadsheet for evaluating method precision and accuracy.
I.

Precision demonstration for ECA marine fuel subject to the 1,000 ppm sulfur
standard.

Precision Criteria, § 80.584(a)(3) - a standard deviation less than 18.07 ppm, computed from
the results of a minimum of 20 repeat tests made over 20 days on samples taken from a single
homogeneous commercially available ECA marine fuel with a sulfur content in the range of 700­
1,000 ppm. The 20 results must be a series of tests with a sequential record of analyses and no
omissions. 1
A.

In the workbook entitled “ECA Marine Fuel Sulfur Test Spreadsheet Example”, locate the
worksheet entitled, “1,000 ppm S Precision”. Enter data in the light shaded green areas
of the worksheet. For an example of the “1,000 ppm S Precision” worksheet with data
completely entered, please see the worksheet entitled, “EX – 1,000 ppm S Precision”.
Notes:
1.
Test results must be reported in parts per million (ppm) to the number of digits
specified in method description of EPA’s designated primary test method, ASTM
D2622-10.
2.
The date and time of each test measurement must be reported.
3.
Please include the laboratory sample test identification number for each test
result.

B.

After entering the data into the light shaded green area of the “1,000 ppm S Precision”
worksheet, go to the “File” menu at the top of the screen and select “Save” to save your
data. Once all the data are entered into the “1,000 ppm S Precision” worksheet, the
standard deviation of the data set (located in cell B19), and an indication as to whether
the 1,000 ppm sulfur precision criterion are met will be determined by the worksheet.
The indication of “PASSED” or “FAILED” is located in cell B18 in the worksheet, after the
question, “Is 1,000 ppm Sulfur Precision Criterion Met?”. If the worksheet is missing
required data, an indication of “REQUIRED DATA MISSING” will appear after this
question. There is a QC data entry check for each test result in column E (i.e., if data is
entered in a test result cell, an indication of “OK” will appear next to that cell, but if no
data is entered in a test result cell, an indication of “DATA REQUIRED IN CELL #” will
appear next to that cell). Note: If the applicant wishes to include more than the 20
minimum tests, please report the additional data by adding rows to the spreadsheet. 2

1

A laboratory 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

Additional rows may be inserted to accommodate the extra data points. If these rows are added in the
middle (say around row 25), the equations that analyze the data will be automatically adjusted. If
difficulties are encountered in doing this, please call for help.

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II.

Accuracy demonstration for ECA marine fuel subject to the 1,000 ppm sulfur
standard.

Accuracy Criterion -

1.

The arithmetic average of a continuous series of at least 10 tests
performed on a commercially available gravimetric sulfur standard
(CAGSS) in the range of 300-400 ppm sulfur shall not differ from
the accepted reference value of that standard by more than 13.55
ppm sulfur. 3

2.

The arithmetic average of a continuous series of at least 10 tests
performed on a CAGSS in the range of 900-1,000 ppm sulfur shall
not differ from the accepted reference value of that standard by
more than 13.55 ppm sulfur. 4

A.

Locate the worksheet entitled, “1,000 ppm S Accuracy”. Enter data in the light shaded
green areas of the worksheet. For an example of the “1,000 ppm S Accuracy”
worksheet with data completely entered, please see the worksheet entitled, “EX - 1,000
ppm S Accuracy”.
Notes:
1.
Test results must be reported in parts per million (ppm) to the number of digits
specified in method description of EPA’s designated primary test method, ASTM
D2622-10.
2.
It is recommended that the date and time of each test measurement be reported.
3.
Please include the laboratory sample test identification number for each test
result.
4.
In the appropriate rows, enter the “Vendor Name of Gravimetric Standard”, “Lot
Identification Number of Gravimetric Standard”, and “Accepted Reference Value
of the Gravimetric Standard (ppm)” in parts per million for both the 300-400 ppm
and 900-1,000 ppm sulfur gravimetric standards.
5.
Since the Test Method and Laboratory Identification information for this
demonstration are the same as the Test Method and Laboratory Identification
information in the “1,000 ppm S precision” worksheet, for your convenience, this
information is automatically referenced from the “1,000 ppm S Precision”
worksheet.

B.

After entering the data into the light shaded green area of the worksheet as described
above, go to the “File” menu at the top of the screen and select “Save” to save all of the
entered data. Once all data are entered into the “1,000 ppm S Accuracy” worksheet, this
worksheet will calculate the arithmetic average for both the 300-400 ppm sulfur data set
(located in cell B21) and the 900-1,000 ppm sulfur data set (located in cell I21). This
worksheet will also calculate the difference between the arithmetic average of the data
set and the accepted reference value of each respective gravimetric standard (located in
cell B25 for the 300-400 ppm accuracy demonstration & located in cell I25 for the 900­
1,000 ppm accuracy demonstration). This worksheet will indicate whether the 1,000

3

Individual test results shall be compensated for any known chemical interferences.

4

Individual test results shall be compensated for any known chemical interferences.

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ppm sulfur accuracy criteria are met for the candidate test method by saying “PASSED”
or “FAILED” in the cell after the questions, “Is 300-400 ppm Sulfur Accuracy Criterion
Met?” (located in cell B20) and “Is 900-1,000 ppm Sulfur Accuracy Criterion Met?”
(located in cell I20). Both of these accuracy criteria must be met in order for the test
method to be considered to have met the 1,000 ppm accuracy criteria. If the worksheet
is missing required data, an indication of “REQUIRED DATA MISSING” will appear after
the applicable question. There is a QC data entry check for each test result in column E
and column L (i.e., if data is entered in a test result cell, an indication of “OK” will appear
next to that cell, but if no data is entered in a test result cell, an indication of “DATA
REQUIRED IN CELL #” will appear next to that cell). There is also a QC data entry
check on the concentration of the gravimetric standard in cell E24 and cell L24 (i.e., for
either the 300 to 400 ppm sulfur accuracy demonstration or 900 to 1,000 ppm sulfur
accuracy demonstration, if the concentration of gravimetric standard falls within the
applicable concentration range, an indication of “OK” will appear in the respective cell, if
the concentration of the gravimetric standard falls below the applicable concentration
range, an indication of “ARV TOO LOW IN CONCENTRATION” will appear in the
respective cell, if the concentration of the gravimetric standard is above the applicable
concentration range, an indication of “ARV TOO HIGH IN CONCENTRATION” will
appear in the respective cell). Note: If the applicant wishes to include more than the 10
minimum tests, please report the additional data by inserting rows into the spreadsheet. 5

PART II - Instructions for submission of Accuracy and Precision data to Agency for NonVCSB Test Method Approval
For each test facility that wishes to have a Non-VCSB test method approved for
ECA marine fuel, the following information must be submitted to the Agency for
approval:
A.

40 CFR 80.585(a). For methods that are approved by a voluntary consensus-based
organization standards body (VCSB), such as the American Society for Testing and
Materials (ASTM) or International Standards Organization (ISO), each individual test
facility demonstrate is has met the accuracy and precision criteria specified under §
80.584 via self-qualification (Please see Part I of this spreadsheet example key). The
self-qualification of the VCSB test method is limited to the single test facility that
performed the testing for accuracy and precision.

B.

40 CFR 80.585(b). For methods that are not approved by a VCSB, for such a method to
be approved, the following information must be submitted to the Administrator by each
test facility for each test method that it wishes to have approved:
1.

5

Full test method documentation, including a description of the technology and/or
instrumentation that makes the method functional.

Additional rows may be inserted to accommodate the extra data points. If these rows are inserted in the
middle of the range (say after row 30) the equations for the average and other functions will be
automatically adjusted. Extra rows inserted for one of the two standard levels, while appearing in the
range for the other standard level, will not affect the calculations for the level where no data were added.

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2.

3.
4.

Information demonstrating that the test method meets the applicable accuracy
and precision criteria of § 80.584, including information on the date and time of
each test measurement to demonstrate precision (Please use instructions in Part
I of this guidance).
If requested by EPA, test results from use of the test method to analyze samples
of commercially available fuel provided by EPA.
Any additional information requested by the Administrator and considered
necessary for deciding whether to approve the test method.

C.

40 CFR 80.585(c). Sample Retention. Samples used for precision and accuracy
determination must be retained for 90 days.

D.

Confidential Business Information Claim. You may claim the information you submit as
confidential business information (CBI) by clearly marking your submission. Please be
sure to indicate your CBI claim where asked on the spreadsheet and clearly indicate that
your submission contains information claimed as CBI in your cover letter. If no such
written claim is made, then the information you submit may be made available to the
public by EPA without further notice. EPA’s regulations regarding CBI are at 40 CFR
Part 2.

E.

Please send one paper hard copy of your applicable information described above that
includes a cover memo with your signature, along with a compact disk or thumb drive
containing the accuracy and precision data in the spreadsheet described above by
overnight mail or courier service to the address below.
U.S. Environmental Protection Agency

William Jefferson Clinton Building - North

Mail Code 6405A, Room 6520V; (202) 343-9038

1200 Pennsylvania Ave NW

Washington, DC 20004

F.

40 CFR 585(d). EPA Approval.
1.

Within 90 days of receipt of all materials required to be submitted under 40 CFR
80.585(a) or (b), the Administrator shall determine whether the Non-VCSB test
method is approved.

2.

If the Administrator denies approval of the Non-VCSB test method, within 90
days of receipt of all materials required to be submitted under 40 CFR 80.585(a)
or (b), the Administrator will notify the applicant of the reasons for not approving
the method. If the Administrator does not notify the applicant within 90 days of
receipt of the application, that the Non-VCSB test method is not approved, then
the Non-VCSB test method shall be deemed approved.

3.

If the Administrator finds that and individual test facility has provided false or
inaccurate information under 40 CFR 80.585, upon notice from the Administrator
the approval shall be void ab initio.

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4.

G.

H.

9

Non-VCSB test method/test facility approval shall be valid for five years from the
date of approval by the Administrator and shall not be extended. If the method is
later approved by a VCSB, the approval shall remain valid so long as the
conditions of 40 CFR 80.585(a) are met.

40 CFR 80.585(e). Quality Assurance procedures for sulfur measurement
instrumentation. A test method shall not be considered a test using an approved test
method unless the following quality control procedures are performed separately for
each instrument to make measurements:
1.

Follow all mandatory provisions of ASTM D 6299-02 and construct control charts
from the mandatory quality control testing prescribed in paragraph 7.1 of the
reference method, following guidelines under A 1.5.1 for individual observation
charts and A 1.5.2 for moving range charts. 9

2.

Follow paragraph 7.3.1 of ASTM D 6299-02 to check standards using a
reference material at least monthly or following any major change to the
laboratory equipment or test procedure. Any deviation from the accepted
reference value of a check standard greater than 36.14 ppm must be
investigated.

3.

Samples of test batches must be retained for 30 days or the period equal to the
interval between quality control sample tests, whichever is longer.

4.

Upon discovery of any quality control testing violation of paragraph A 1.5.1.3 or A
1.5.2.1 of ASTM D 6299-02, or any check standard deviation greater than 36.14
ppm, conduct an investigation into the cause or such violation or deviation and,
after restoring method performance to statistical control, retest retained samples
from batches originally tested since the last satisfactory quality control material or
check standard testing occasion.

40 CFR 80.586. Record retention requirements for approved test methods. Each
individual test facility must retain records related to the establishment of accuracy and
precision values, all test method documentation, and any quality control test and
analysis under title 40 CFR sections 80.584 and 80.585 for five years.

The Director of the Federal Register approved the incorporation by reference of ASTM D 6299-02,
Standard Practice for Applying Statistical Quality Assurance Techniques to Evaluate Analytical
Measurement System Performance, as prescribed in 5 U.S.C. 552(a) and 1 CFR Part 51. Anyone may
purchase copies of this standard from the American Society for Testing and Materials, 100 Barr Harbor
Dr., West Conshohocken, PA 19428. Anyone 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,
Washington, D.C. 20460 or at the National Archives and Records Administration (NARA). For information
on the availability of this material at NARA, call 202-741-6030 or go to:
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.

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EPA Contact:
Joe Sopata
U.S. Environmental Protection Agency
OAR/OTAQ/CD/FCPC
(202) 343-9034
Email: [email protected]

OMB Control No. 2060-0308

Approval expires: 3/31/2019

The public reporting and recordkeeping burden for this collection of information is estimated to
average 180 hours per response. Send comments on the Agency’s need for this information,
the accuracy of the providing burden estimates, and any suggested methods for minimizing
respondent burden, including through the use of automated collection techniques to the
Director, Collection Strategies Division, U.S. Environmental Protection Agency (2822T), 1200
Pennsylvania Ave., NW, Washington, D.C. 20460. Include the OMB control number in any
correspondence. Do not send the completed form to this address.