Form Instructions for Using EPA

Spreadsheet to Submit Solvent Yellow

124 Test Method Precision and

Accuracy Information 
Compliance Division

Office of Transportation and Air Quality

U.S. Environmental Protection Agency

March 2013

(Minor Revisions February 20, 2013)

OMB Control Number: 2060-0308

Expiration Date: January 31, 2016

Form Instructions for Using EPA

Spreadsheet to Submit Solvent Yellow

124 Test Method Precision and

Accuracy Information 

EPA-420-B-13-020

March 2013
i

Disclaimer

The discussion in this document is intended solely as instructions. The statutory 

provisions and EPA regulations described here 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. These instructions do not confer legal rights 

or impose legal obligations upon any member of the public.

While we have made every effort to ensure the accuracy of the discussion in these 

instructions, 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 

these instructions and its applicability to a particular situation. EPA may adopt 

approaches on a case-by-case basis that differ from those described in these 

instructions. 

Mention of trade names or commercial products does not constitute endorsement or 

recommendation for their use.

The sampling, sample preparation, and testing methods qualified for use in accordance 

with the requirements of section 40 CFR § 80.582 may involve the use of hazardous 

materials, operations and equipment. These instructions do not address the associated 

safety problems which may exist. It is the responsibility of the user of the procedures 

specified in these instructions to establish appropriate safety and health practices prior 

to their use. It is also the responsibility of the user to dispose of any byproducts which 

might result from conducting these procedures in a manner consistent with applicable

safety and health requirements.

This is a living document and may be revised periodically without public notice. EPA 

welcomes public input on this document at any time.
1

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 

its chosen test method for the fuel marker solvent yellow 124 in heating oil and non-road 

locomotive and marine diesel fuels. 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. The following instructions are for use by 

those parties that need to qualify a facility/test method for measuring the concentration 

of this marker in heating oil or non-road locomotive and marine diesel fuel pursuant to 

40 CFR 80.510.1

EPA has provided a spreadsheet template for recording and evaluating the test data 

required for establishing the test method’s precision and accuracy. Use of the template 

will, we hope, help an applicant to structure and submit the needed information. It will 

also facilitate EPA’s timely review and approval of test methods. Part I below explains 

the use of the template, while Part II covers submission of the resulting structured 

information to EPA.

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

accuracy.

I. Precision demonstration for solvent yellow 124 test method.

Precision Criterion2 - a standard deviation less than 0.10 milligrams per liter, 

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 meeting 

applicable industry consensus and federal regulatory specifications with fuel marker 

solvent yellow 124 content in the range of 0.10 to 8 milligrams per liter. The 20 results 

must be a series of tests with a sequential record of analyses and no omissions.3

A. In the workbook entitled “Fuel Marker Solvent Yellow 124 Template”, locate the 

worksheet entitled, “SY124 Precision”. Enter data in the light shaded green 

areas of the worksheet. For an example of the “SY124 Precision” worksheet with 

data completely entered, please see the worksheet entitled, “EX – SY214 

Precision”. 

Notes: 

1. Test results must be reported in milligrams per liter (mg/l) to the number of 

significant digits specified in the method description or, if no such 

 

1 In certain areas of the country, solvent yellow 124 has to be used as a fuel marker in heating oil distillate 

fuel indefinitely beginning June 1, 2007 and, from June 1, 2010 through May 31, 2012, in locomotive and 

marine distillate fuel.

2

 § 80.582(b)(1). 3

 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

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 sample identification number for each 

test result. 

B. After entering the data into the light shaded green area of the “SY 124 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 “SY 124 Precision” 

worksheet, the standard deviation of the data set (located in cell B18), and an 

indication as to whether the SY124 precision criterion is met will be displayed by 

the worksheet. The indication of “PASSED” or “FAILED” is located in cell B17 in 

the worksheet, after the question, “Is SY124 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.4 

II. Accuracy demonstration for solvent yellow 124 test method. 

Accuracy Criteria - 1. The arithmetic average of a continuous series of at least 10 

tests performed on a commercially available marker solvent 

yellow 124 standard in the range of 0.10 to 1 milligrams per 

liter solvent yellow 124 shall not differ from the accepted 

reference value of that standard by more than 0.05 

milligrams per liter.

5,6

2. The arithmetic average of a continuous series of at least 10 

tests performed on a marker solvent yellow 124 standard in 

the range of 4 to 10 milligrams per liter solvent yellow 124 

shall not differ from the accepted reference value of that 

standard by more than 0.05 milligrams per liter.

7,8

 

4

 Additional rows may be inserted to accommodate the extra data points. If these rows are added in the 

middle of the data set (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.

5

 § 80.582(b)(2)(i). 6

 As explained in § 80.582(b)(2)(iii), individual test results shall be compensated for any known chemical 

interferences.

7

 § 80.582(b)(2)(ii). 8

 As explained in § 80.582(b)(2)(iii), individual test results shall be compensated for any known chemical 

interferences.
3

A. Locate the worksheet entitled, “SY124 Accuracy”. Enter data in the light shaded 

green areas of the worksheet. For an example of the “SY124 Accuracy” 

worksheet with data completely entered, please see the worksheet entitled, “EX - 

SY124 Accuracy”. 

Notes: 

1. Test results must be reported in milligrams per liter (mg/l) 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 sample identification number for each 

test result.

4. In the appropriate rows, enter the “Name of Standard Vendor”, “Standard 

Lot Identification Number”, and “Accepted Reference Value of the 

Standard (mg/L)” in milligrams per liter for both the 0.1-1 mg/L and 4-10 

mg/L marker solvent yellow 124 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 “SY124 precision” worksheet, for your 

convenience, this information is automatically referenced from the “SY124 

Precision” worksheet.

B. After entering the data into the light shaded green area of the worksheet as 

described above: 

1. Go to the “File” menu at the top of the screen and select “Save” to save all 

of the entered data.

2. Once all data are entered into the “SY124 Accuracy” worksheet, the

worksheet will calculate the arithmetic average for both the 0.1-1 mg/L 

marker solvent yellow 124 data set (located in cell B20) and the 4-10 mg/L 

marker solvent yellow 124 (located in cell I20). It will also calculate the 

difference between the arithmetic average of the data set and the 

accepted reference value of each standard (located in cell B24 for the 0.1-

1 mg/L concentration and in cell I24 for the 4-10 mg/L concentration). 

3. The worksheet will indicate whether the marker solvent yellow 124

accuracy criteria are met for the candidate test method by saying 

“PASSED” or “FAILED” in the cell after the questions, “Is 0.1-1 mg/L 

marker solvent yellow 124 Accuracy Criterion Met?” (located in cell B19) 

and “Is 4-10 mg/L marker solvent yellow 124 Accuracy Criterion Met?” 

(located in cell I19). Both of these accuracy criteria must be met in order 

for the test method to be considered to have demonstrated sufficient 

accuracy. 

4. 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 
4

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 standards in cell E23 and cell 

L23. Note: If the applicant wishes to include more than the 10 minimum 

tests, please report the additional data by inserting rows into the 

spreadsheet.9 

 

9

 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.
5

PART II - Instructions for submission of Accuracy and Precision Information 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: 

A. For methods that are approved by a voluntary consensus-based organization 

standards body (VCSB)10, 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 § 80.582(b) (Please use instructions in Part I of this document). 

The approval of the test method is limited to the single test facility that performed 

the testing for accuracy and precision.11 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. For methods that are not approved by a VCSB12, 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 and all 

procedures that are part of the method.

13

2. Information demonstrating that the test method meets the applicable 

accuracy and precision criteria of § 80.582(b), including information on the 

date and time of each test measurement to demonstrate precision (Please 

use instructions in Part I of this guidance).14

3. If requested by EPA, test results from use of the test method to analyze 

samples of commercially available distillate fuel containing the fuel marker 

solvent yellow 124 provided by EPA.15

4. Any additional information requested by the Administrator and considered 

necessary for deciding whether to approve the test method.

C. Sample Retention16. Samples used for precision and accuracy determination 

must be retained for 90 days.

 

10 40 CFR 80.582(c)(1). 11 Where a facility has more than one functionally identical instrument implementing a single method, only one of 

the instruments must be qualified (but statistical quality control must be applied to each instrument, as indicated 

below).

12 40 CFR 80.585(c)(2). 13 40 CFR 80.585(c)(2)(i). 14 40 CFR 80.585(c)(2)(ii). 15 40 CFR 80.585(c)(2)(iv). 16 40 CFR 80.585(c)(2)(iii).
6

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.

 

Please send one paper hard copy of the information described above and a 

cover letter with your signature, along with a compact disk or 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 Air and Radiation

Compliance Division

Fuels Compliance Center

1310 L Street, N.W, (6406J), 6th Floor, Room 642

Washington, D.C. 20005

F. EPA Approval.

17 

1. Within 90 days of receipt of all materials required to be submitted under 40 

CFR 80.582(c)(1) or (2), 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 

80.582(c)(1) or (2), the Administrator will notify the applicant of the 

reasons for not approving the method. If the Administrator does not notify 

the applicant of disapproval or incomplete information during that time 

span 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 80.582(c), upon notice from the 

Administrator the approval shall be void ab initio. 

4. The qualification of any test method under the requirements of 40 CFR 

80.582 shall be valid for the duration of the period during which the fuel 

marker provisions remain applicable under the Motor Vehicle Diesel Fuel 

regulations at 40 CFR 80 Subpart I. 

 

17 40 CFR 80.582(c)(3). 
7

G. Quality Assurance procedures for solvent yellow 124 measurement 

instrumentation.

18 A test will not be considered to have been made with an 

approved test method unless the following quality control procedures are 

performed separately for each instrument used 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.19

2. Follow paragraph 7.3.1 of ASTM D 6299-02 to test 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 0.10 milligrams per liter 

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 0.10 milligrams per liter, conduct an investigation into the 

cause of 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 80.582(d)(5). 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 80.582 for five years.

 

18 40 CFR 80.582(d). 

19 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.
8

EPA Contact:

Joe Sopata 

(202) 343-9034

Fax: (202) 343-2801

Email: sopata.joe@epa.gov

OMB Control No. 2060-0308

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.