### Name of Method:

Organization ID No. (as in ASTM D XXXX-XX):
Laboratory Name: Laboratory Street Address:

Laboratory City: Laboratory State: Laboratory Zip code: Laboratory Contact Person:
Laboratory Contact Phone Number
Laboratory Contact Facsimile Number Laboratory Contact E-mail Address

Is 1,000 ppm Sulfur Precision Criterion Met?

standard dev iation Laboratory Test Identification Number Date Time Test Result (ppm) **REQUIRED DATA MISSING** Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made av ailable to the public by EPA without further notice. All questions of confidentiality will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by typing "Yes" or "No" in the adjacent cell.)

**1,000 ppm Sulfur Precision Criterion** - a standard dev iation less than 18.07 ppm, computed from the results of a minimum of 20 repeat tests made ov er 20 days on samples taken from a single homogenous commerically av ailable ECA Marine fuel with a sulfur range of 700 to 1,000 ppm. The 20 results must be a series of tests with a sequential record of the analyses and no omissions. A lab facility 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. **1,000 ppm ECA Marine Fuel Sulfur Precision Demonstration [ECA0300 (insert form number):OMB # 2060-0308 Expires 1/31/2016]**

**REQUIRED DATA MISSING Test Method** 

**Laboratory Identification**

### Data Entry QC Check on Test Result DATA REQUIRED IN CELL D20 DATA REQUIRED IN CELL D21 DATA REQUIRED IN CELL D22 DATA REQUIRED IN CELL D23 DATA REQUIRED IN CELL D24 DATA REQUIRED IN CELL D25 DATA REQUIRED IN CELL D26 DATA REQUIRED IN CELL D27 DATA REQUIRED IN CELL D28 DATA REQUIRED IN CELL D29 DATA REQUIRED IN CELL D30 DATA REQUIRED IN CELL D31 DATA REQUIRED IN CELL D32 - a standard dev iation less than 18.07 ppm, computed from the results of a minimum of 20 repeat tests made ov er 20 days on samples taken from a single homogenous commerically av ailable ECA Marine fuel with a sulfur range of 700 to 1,000 ppm. The 20 results must be a series of tests with a sequential record of the analyses and no omissions. A lab facility 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 **1,000 ppm ECA Marine Fuel Sulfur Precision Demonstration [ECA0300 (insert form number):OMB # 2060-0308 Expires 1/31/2016]**

### DATA REQUIRED IN CELL D33

DATA REQUIRED IN CELL D34 DATA REQUIRED IN CELL D35 DATA REQUIRED IN CELL D36 DATA REQUIRED IN CELL D37 DATA REQUIRED IN CELL D38 DATA REQUIRED IN CELL D39**1,000 ppm ECA Marine Fuel Sulfur A** **ccuracy Demonstration [ECA 0300 (insert EPA**  **External form number):OMB # 2060-0308 Expires 1/31/2016]**

Name of Method: Organization ID No. (as in ASTM D XXXX-XX):
Laboratory

Name: Laboratory

Street Address: Laboratory

City : Laboratory

State: Laboratory

Zip code: Laboratory

Contact Person: Laboratory

Contact Phone Number Laboratory

Contact Facsimile Number Laboratory

Contact E-mail Address

Is 300-400 ppm Sulfur Accuracy Criterion Met? Arithmetic Average (ppm) Vendor Name of Gravimetric Standard Lot Identification Number of Gravimetric

Standard Accepted Reference Value (ARV) of Gravimetric Standard (ppm)

Difference between Arithmetic Average and ARV of Gravimetric Standard

Laboratory

Test Identification Number Date Time Test Result (ppm) **300 to 400 ppm A ccuracy Criterion**  - the arithmetic average of a continuous series of at least 10 tests performed on a commercially

available gravim etric sulfur standard in the range of 300 to 400 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be compensated for any known chemical interferences.

**REQUIRED DA TA**  **MISSING REQUIRED DA** 

**TA MISSING**  

### REQUIRED DA

**TA MISSING**  **gravimetric sulfur standard Test Method** 

0 0 **Laboratory Identification**

0 0 0 0
Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made available to the public by EPA without further notice. All questions of confidentiality will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by typing "Yes" or "No" in the adjacent cell.) 0 0 0 0 0

**Ac curacy Criterion for 300-400 ppm** Is 900-1,000 ppm Sulfur Accuracy

Criterion Met? Arithmetic Average (ppm) Vendor Name of Gravimetric Standard Concentration QC Check on ARV Lot Identification Number of Gravimetric Standard

ARV TOO LOWIN CONCENTRATION Accepted Reference Value (ARV) of Gravimetric Standard (ppm) Difference between Arithmetic Average and ARV of Gravimetric Standard
Data Entry

QC Check on Test Result Laboratory Test Identification Number Date Time
DATA REQUIRED IN CELL D26 DATA REQUIRED IN CELL D27 - the arithmetic average of a continuous series of at least 10 tests performed on a commercially

available gravim etric sulfur standard in the range of 300 to 400 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be compensated for any known **900 to 1,000 ppm A ccuracy Criterion**  - the arithmetic average of a continuous series of at least 10 tests performed on a commercially available gravim etric sulfur standard in the range of 900 to 1000 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be compensated for any known chemical interferences.

**REQUIRED DA**

**TA MISSING** 

**REQUIRED DA**

**TA MISSING**  

### REQUIRED DA

**TA MISSING**  **gravimetric sulfur standard Ac** **curacy Criterion for 900-1,000 ppm** Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made available to the public by EPA without further notice. All questions of confidentiality will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by typing "Yes" or "No" in the adjacent cell.)DATA REQUIRED IN CELL D28

DATA REQUIRED IN CELL D29 DATA REQUIRED IN CELL D30 DATA REQUIRED IN CELL D31 DATA REQUIRED IN CELL D32 DATA REQUIRED IN CELL D33 DATA REQUIRED IN CELL D34 DATA REQUIRED IN CELL D35Concentration QC Check on ARV

ARV TOO LOWIN CONCENTRATION

Test Result (ppm) Data Entry QC Check on Test Result DATA REQUIRED IN CELL J26 DATA REQUIRED IN CELL J27 - the arithmetic average of a continuous series of at least 10 tests performed on a commercially available gravim etric sulfur standard in the range of 900 to 1000 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be compensated for any known chemical interferences.

**REQUIRED DA**

**TA MISSING** 

**REQUIRED DA**

**TA MISSING**  

### REQUIRED DA

**TA MISSING** DATA REQUIRED IN CELL J28 DATA REQUIRED IN CELL J29 DATA REQUIRED IN CELL J30 DATA REQUIRED IN CELL J31 DATA REQUIRED IN CELL J32 DATA REQUIRED IN CELL J33 DATA REQUIRED IN CELL J34 DATA REQUIRED IN CELL J35OMB Control Number: 2060-0308

Name of Method: Organization ID No. (as in ASTM D XXXX-XX): Laboratory Name: Laboratory Street Address:

Laboratory City: Laboratory State: Laboratory Zip code: Laboratory Contact Person: Laboratory Contact Phone Number Laboratory Contact Facsimile Number Laboratory Contact E-mail Address

No

Is 15 ppm Sulfur Precision Criterion Met?

standard deviation Laboratory Test Identification Number Date Time Test Result (ppm) Data Entry QC Check on Test Result ######### 1/26/2013 8:00 AM 755.000 OK ######### 1/27/2013 8:00 AM 780.000 OK ######### 1/28/2013 8:00 AM 765.000 OK ######### 1/29/2013 8:00 AM 750.000 OK ######### 1/30/2013 8:00 AM 745.000 OK ######### 2/1/2013 8:00 AM 760.000 OK ######### 2/2/2013 8:00 AM 763.000 OK ######### 2/3/2013 8:00 AM 772.000 OK ######### 2/5/2013 8:00 AM 749.000 OK ######### 2/6/2013 8:00 AM 730.000 OK ######### 2/7/2013 8:00 AM 740.000 OK ######### 2/8/2013 8:00 AM 760.000 OK ######### 2/9/2013 8:00 AM 745.000 OK ######### 2/10/2013 8:00 AM 750.000 OK ######### 2/11/2013 8:00 AM 756.000 OK ######### 2/12/2013 8:00 AM 763.000 OK ######### 2/13/2013 8:00 AM 765.000 OK ######### 2/14/2013 8:00 AM 763.000 OK ######### 2/15/2013 8:00 AM 777.000 OK ######### 2/16/2013 8:00 AM 750.000 OK

EPA External No. 5900-352 202-343-2801 sopata.joe@epa.gov

**PASSED** 12.42 Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made available to the public by EPA without further notice. All questions of confidentiality will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by typing "Yes" or "No" in the adjacent cell.)

**1,000 ppm Sulfur Precision Criterion**- 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 homogenous commerically available ECA Marine fuel with a sulfur range of 700 to 1,000 ppm. The 20 results must be a series of tests with a sequential record of the analyses and no omissions. A lab facility 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. 202-343-9034 **1,000 ppm ECA Marine Fuel Sulfur Precision Demonstration [ECA030]** Expires 1/31/2016 **Test Method** Standard Test Method for Sulfur in Petroleum Products by W avelength ASTM D2622-10 **Laboratory Identification** USEPA National and Vehicle Fuels Emissions Laboratory/OAR 2565 Plymouth Road, Mailcode AATSG Ann Arbor Michigan 48105 Joe Sopata**1,000 ppm ECA Marine Fuel Sulfur A** **ccuracy Demonstration [ECA 0300 (insert EPA**  **external form number):OMB # 2060-0308 Expires 1/31/2016]**

Name of Method: Organization ID No. (as in ASTM D XXXX-XX):
Laboratory

Name: Laboratory

Street Address: Laboratory

City : Laboratory

State: Laboratory

Zip code: Laboratory

Contact Person:
Laboratory

Contact Phone Number
Laboratory

Contact Facsimile Number
Laboratory

Contact E-mail Address

Is 300-400 ppm Sulfur Accuracy Criterion Met? Arithmetic Average (ppm) Vendor Name of Gravimetric Standard Lot Identification Number of Gravimetric

Standard Accepted Reference Value (ARV) of Gravimetric Standard (ppm)

Difference between Arithmetic Average and ARV of Gravimetric Standard

Laboratory

Test Identification Number Date Time Test Result (ppm) ######### 1/28/2013 8:00 AM 352.000 ALDS45678

350.00

2 

### PA**SSED** 352.00 NIST sopata.joe@epa.gov

**Ac curacy Criterion for 300-400 ppm**  **gravimetric sulfur standard** Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made available to the public by EPA without further notice. All questions of confidentiality

will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by typing "Yes" or "No" in the adjacent cell.)

**300 to 400 ppm A ccuracy Criterion**  - the arithmetic average of a continuous series of at least 10 tests performed on a commercially

available gravim etric sulfur standard in the range of 300 to 400 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be compensated for any

known chemical interferences. 202-343-2801 **Test Method** Standard Test Method for Sulfur in Petroleum Products by W avelength Dispersive X-ray Fluorescence ASTM D2622-10 **Laboratory Identification** USEPA National and Vehicle Fuels Em issions Laboratory /OAR 2565 Plymo uth Road, Mailcode AATSG Ann Arbor Michigan 48105 Joe Sopata

202-343-9034######### 1/28/2013 8:30 AM 354.000 ######### 1/28/2013 9:00 AM 350.000 ######### 1/28/2013 9:30 AM 348.000 ######### 1/28/2013 10:00 AM 340.000 ######### 1/28/2013 10:30 AM 360.000 ######### 1/28/2013 11:00 AM 356.000 ######### 1/28/2013 11:30 AM 357.000 ######### 1/28/2013 12:00 PM 352.000 ######### 1/28/2013 12:30 PM 351.000No

Is 900-1000 ppm Sulfur Accuracy

Criterion Met? Arithmetic Average (ppm) Vendor Name of Gravimetric Standard Concentration QC Check on ARV Lot Identification Number of Gravimetric Standard

OK Accepted Reference Value (ARV) of Gravimetric Standard (ppm) Difference between Arithmetic Average and ARV of Gravimetric Standard Data Entry

QC Check on Test Result Laboratory Test Identification Number Date Time Test Result (ppm) OK ######### 1/29/2013 8:00 AM 960.000 ALDS53478

950.00

1.7 

### PA**SSED** 951.70 NIST **Ac curacy Criterion for 900-1000 ppm**  **gravimetric sulfur standard** Confidential Business Information Claim. A company may assert a business confidentiality claim covering the information contained in this submission. If no such claim is made the information may be made available to the public by EPA without further notice. All questions of confidentiality

will be handled pursuant to 40 CFR Part 2. Is confidentiality claimed for the information in this submission? (Note: Please answer by

- the arithmetic average of a continuous series of at least 10 tests performed on a commercially

available gravim etric sulfur standard in the range of 300 to 400 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by more than 13.55 ppm. Individual test results shall be **900 to 1000 ppm A ccuracy Criterion**  - the arithmetic average of a continuous series of at least 10 tests performed on a commercially available gravim etric sulfur standard in the range of 900 to 1000 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by mo re than 13.55 ppm. Individual test results shall be compensated for any known chemical interferences. Standard Test Method for Sulfur in Petroleum Products by W avelength Dispersive X-ray Fluorescence

USEPA National and Vehicle Fuels Em issions Laboratory /OAR 2565 Plymo uth Road, Mailcode AATSGOK ######### 1/29/2013 8:30 AM 940.000 OK ######### 1/29/2013 9:00 AM 942.000 OK ######### 1/29/2013 9:30 AM 962.000 OK ######### 1/29/2013 10:00 AM 953.000 OK ######### 1/29/2013 10:30 AM 957.000 OK ######### 1/29/2013 11:00 AM 949.000 OK ######### 1/29/2013 11:30 AM 950.000 OK ######### 1/29/2013 12:00 PM 956.000 OK ######### 1/29/2013 12:30 PM 948.000Concentration QC Check on ARV

OK

Data Entry

QC Check on Test Result OK - the arithmetic average of a continuous series of at least 10 tests performed on a commercially available gravim etric sulfur standard in the range of 900 to 1000 ppm sulfur shall not differ from the accepted reference value (ARV) of that standard by mo re than 13.55 ppm. Individual test results shall be compensated for any known chemicalOK OK OK OK OK OK OK OK OK