Form Instructions to Parties Submitting
            Diesel Sulfur Accuracy and Precision
            Information for Approval of Test Methods
            by Facility
&EPA
United States
Environmental Protection
Agency

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   Form Instructions to Parties Submitting
     Diesel Sulfur Accuracy and Precision
   Information for Approval of Test Methods
                      by Facility
                       Compliance Division
                 Office of Transportation and Air Quality
                 U.S. Environmental Protection Agency
                        September 2014
                  (Minor Revisions September 24,2014)
                   OMB Control Number: 2060-0308
                   Expiration Date: January 31,2016
United States
Environmental Protection
Agency
EPA-420-B-14-066a
September 2014

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                                   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 guidance 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
guidance, 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 guidance and its applicability to a particular situation.  EPA may adopt  approaches
on a case-by-case basis that differ from those described in this guidance.

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 May, 2004, EPA promulgated new requirements for non-road diesel
fuel. One of the provisions of this final rule, explained in Subpart I of 40 CFR Part 80,
requires that each test facility must meet specified accuracy and precision criteria with
their chosen test method for sulfur in on-road or non-road diesel fuel additives and/or
diesel fuel.  Evidence of having met these requirements must be submitted to and
approved by the Agency before using the method to make measurements for
demonstrating compliance. There are separate accuracy and precision criteria for
diesel fuels and additives subject to the two sulfur standards -15 ppm and 500 ppm.

Depending on your test facility situation, you may be required just to meet the 15 ppm
diesel sulfur accuracy and precision criteria, you may choose to meet the 500 ppm
diesel sulfur accuracy and precision criteria, or may be required to meet both of these
accuracy and precision criteria. For diesel  fuel at the 500 ppm sulfur level, if your test
facility has chosen to use the designated test method, ASTM D 2622-03, or any of the
following alternative test methods, ASTM D 4294-03, ASTM D 5453-03a, or ASTM D
3120-03a with correlation to the designated test method, it is not necessary for your test
facility to qualify these methods for precision or accuracy.

40 CFR  80.520(a)(1) explains the 15 ppm sulfur standard for motor vehicle diesel fuel
and fuel additives.  40CFR  80.510(b)(1)(i) and  80.510(c) explains the 15 ppm  sulfur
standard for Non-road Locomotive Marine(NRLM) diesel fuel and fuel additives. 40
CFR  80.520(c) explains the 500 ppm sulfur standard for motor vehicle diesel  fuel.  40
CFR  80.510(a) explains the 500 ppm sulfur standard for NRLM diesel fuel. 40 CFR 
80.584 explains the actual accuracy and precision criteria for the applicable standards
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. This guidance deals only with the
approval of test methods at a testing facility for measuring sulfur in diesel fuel additives
or sulfur in diesel 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
qualify a method for the measurement of sulfur in diesel motor fuel or diesel motor fuel
additives, as well as, to help facilitate the timely review and approval of each test
facility's method.

Applicable Dates: These requirements for method qualification under  80.585
become effective on December 27, 2004.

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

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to the Agency in order to expedite the review and approval process. Please see Part II
for submission instructions.
Part I - Instructions for use of spreadsheet for evaluating method precision and
accuracy.

I.     Precision demonstration for motor vehicle diesel fuel and diesel fuel
      additives subject to the  15 ppm sulfur standard.

Precision Criteria,  80.584(a)(1) - a standard deviation less than 0.72 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 diesel fuel with a sulfur content in
the range of 5-15 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 "Sulfur Test Method Template", locate the worksheet
      entitled, "15 ppm S Precision".  Enter data in the light shaded green areas of the
      worksheet.  For an example of the "15 ppm S Precision" worksheet with data
      completely entered, please see the worksheet entitled, "EX -15 ppm  S
      Precision".
      Notes:
      1.     Test results must be reported in parts per million (ppm) to the number of
            significant digits specified in the method description or, if no such
            precision is indicated, to as many digits to the right of the decimal point as
            appear on the instrument readout up to three.
      2.     The date and time  of each test measurement must be  reported.
      3.     Please include the  laboratory test identification number for each test
            result.

B.    After entering the data into the light shaded green area of the "15 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 "15 ppm S
      Precision" worksheet, the standard deviation of the data set (located in cell B18),
      and an indication as to whether the 15 ppm sulfur precision criterion are met will
      be determined by the worksheet.  The indication of "PASSED" or "FAILED" is
      located in cell B17 in the worksheet, after the question, "Is 15 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
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.

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      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
II.    Accuracy demonstration for motor vehicle diesel fuel and diesel fuel
      additives subject to the 15 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 1-10 ppm sulfur
                         shall not differ from the accepted reference value of that
                         standard by more than 0.54 ppm sulfur.3
                   2.     The arithmetic average of a continuous series of at least 10
                         tests performed on a CAGSS in the range of 10-20 ppm
                         sulfur shall not differ from the accepted reference value of
                         that standard by more than 0.54 ppm sulfur.4

A.    Locate the worksheet entitled,  "15 ppm S Accuracy". Enter data in the light
      shaded green areas of the worksheet.  For an example of the "15  ppm S
      Accuracy" worksheet with data completely entered,  please see the worksheet
      entitled, "EX -15 ppm S Accuracy".
      Notes:
      1.    Test results must be reported in parts per million (ppm) to the number of
            digits specified in the method description or,  if no such precision is
            indicated, to as many digits to the right of the decimal point as appear on
            the instrument readout up to three.
      2.    It is recommended that the date and time of each test measurement be
            reported.
      3.    Please include the laboratory 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 1-10 ppm and 10-20 ppm sulfur gravimetric standards.
      5.    Since the Test Method and Laboratory Identification information for this
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.

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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            demonstration are the same as the Test Method and Laboratory
            Identification information in the "15 ppm S precision" worksheet, for your
            convenience, this information is automatically referenced from the "15
            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 "15 ppm S
      Accuracy" worksheet, this worksheet will calculate the arithmetic average for both
      the 1-10 ppm sulfur data set (located in cell B20) and the 10-20 ppm sulfur data
      set (located in cell I20).  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 B24 for the 1-10 ppm accuracy
      demonstration & located in cell I24 for the 10-20 ppm accuracy demonstration).
      This worksheet will indicate whether the 15 ppm sulfur accuracy criteria are  met
      for the candidate test method by saying "PASSED" or "FAILED" in the cell after
      the questions, "Is 1-10 ppm Sulfur Accuracy Criterion Met?" (located in cell B19)
      and "Is 10-20 ppm Sulfur Accuracy Criterion Met?" (located in cell 119).  Both of
      these accuracy criteria must be met in order for the test method to be considered
      to have met the 15 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 E23 and cell L23 (i.e., for either the 1  to 10 ppm sulfur accuracy
      demonstration or 10 to 20 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
5 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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III.    Precision demonstration for motor vehicle diesel fuel subject to the 500
ppm sulfur standard.

Precision Criterion,  80.584(a)(2) - a standard deviation less than 9.68 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 diesel fuel
(SHCADF) with a sulfur content in the range of 200-500 ppm.  The 20 results must be a
series of tests with a sequential record of analyses and no omissions.6

A.    Locate the worksheet entitled, "500 ppm S Precision".  Follow the instructions for
      Section I above, but enter the data for the SOOppm precision demonstration
      rather than that for the 15ppm demonstration. For an example of the "500 ppm S
      Precision" worksheet with data completely entered, please see the worksheet
      entitled, "EX - 500 ppm S Precision".

IV.    Accuracy demonstration for motor vehicle diesel fuel subject to the 500
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 100-200 ppm sulfur
                        shall not differ from the accepted reference value of that
                        standard by more than 7.26 ppm sulfur.7

                   2.    The arithmetic average of a continuous series of at least 10
                        tests performed on a CAGSS in the range of 400-500 ppm
                        sulfur shall not differ from the accepted  reference value of
                        that standard by more than 7.26 ppm sulfur.8

A.    Locate the worksheet entitled, "500 ppm S Accuracy".  Follow the instructions for
      section II above,  but enter the data for the SOOppm accuracy demonstration
      rather than that for the 15ppm demonstration. For an example of the "500 ppm S
      Accuracy" worksheet with data completely entered, please see the worksheet
      entitled, "EX - 500 ppm S Accuracy".
 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.

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

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

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 PART II - Instructions for submission of Accuracy and Precision data to Agency
                                 for Approval

I.     For each test facility that wishes to have a test method approved, 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 must submit the information for accuracy and
      precision criteria specified under  80.584 (Please use instructions in  Part I of
      this guidance). The approval of the test method is limited to the single test facility
      that performed the testing for accuracy and precision. The individual facility must
      submit the accuracy and  precision results for each method, including information
      on the date and time of each test measurement to demonstrate precision,
      following procedures established by the Administrator.

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.     Full test method documentation, including a description of the technology
            and/or instrumentation that makes the method functional.
      2.     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).
      3.     If requested by EPA, test results from use of the test method to analyze
            samples of commercially available fuel provided by EPA.
      4.     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

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      flash drive containing the accuracy and precision data in the spreadsheet
      described above by overnight mail or courier service to the address below.

                              Joe Sopata, Chemist
                  United States Environmental Protection Agency
                      Office of Transportation and Air Quality
                              Compliance Division
                             Fuels Compliance Center
                         1200 Pennsylvania Avenue, N.W.
                     William  Jefferson Clinton Building - North
                    6th Floor, Room 651OAA, Mail Code 6405A
                             Washington, D.C. 20004

F.    40CFR585(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 test
            method is approved.

      2.     If the Administrator denies approval of the 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 test method is not
            approved, then the 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.

      4.     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.

G.    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
9 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

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      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 1.44 ppm (for diesel fuel
             subject to the 15 ppm sulfur standard) or 19.36 ppm (for diesel fuel subject
             to the 500 ppm sulfur standard) 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 1.44 ppm  (for diesel fuel subject to the 15 ppm sulfur
             standard) or 19.36 ppm (for diesel fuel  subject to the 500 ppm sulfur
             standard), 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.

H.    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.

EPA Contact:

Joe Sopata
Ph# (202) 343-9034
Email: sopata.joe(S)epa.qov
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.arch ives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.

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                          OMB Control No. 2060-0566
                          Approval expires: 1/31/2016

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.

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