# EFFECT OF GASOLINE P ROPERTIES ON EXHAUST EMISSIONS FROM TIER 2 LIGHT

- DUTY VEHICLES PHASE 3 FINAL REPORT

US EPA Contract EP

- C

- 07

- 028, Work Assignments 1

- 03, 2

- 03, and 3

- 0 1 NREL Subcontract Nos. ACI

- 8

- 88613

- 01, AFT

- 9

- 99319

- 01 and AFT

- 9

- 99155

- 01

SwRI ® 

## Project No s . 03

. 14175.03, 03.14936.03, 03.14993, and 03.15777.01 (Rev 1)

Prepared for:

D r . Rafal Sobotowski U.S. Environmental Protection Agency 2000 Traverwood Drive Ann Arbor, Michigan 48105

and

Dr. Douglas Lawson National Renewable Energy Laboratory 1617 Cole Boulevard

Golden, CO 80401

Prepared by:

Mr. Kevin Whitney Light

- Duty Vehicle Emissions Department of Emissions R&D

January 2011



# SOUTHWEST RESEARCH INSTITUTE ****

SAN ANTONIO , TX ● HOUSTON, TX ● WASHINGTON, DC

# EFFECT OF GASOLINE P ROPERTIES ON EXHAUST EMISSIONS FROM TIER 2 LIGHT

- DUTY VEHICLES PHASE 3 FINAL REPORT

US EPA Contract EP

- C

- 07

- 028, Work Assignments 1

- 03, 2

- 03, and 3

- 0 1 NREL Subcontract Nos. ACI

- 8

- 88613

- 01, AFT

- 9

- 99319

- 01 and AFT

- 9

- 99155

- 01

SwRI ® 

## Project No s . 03

. 14175.03, 03.14936.03, 03.14993, and 03.15777.01 (Rev 1)

Prepared for:

Dr

. Rafal Sobotowski U.S. Environmental Protection Agency 2000 Traverwood Drive Ann Arbor, Michigan 48105

and

Dr. Douglas Lawson National Renewable Energy Laboratory 1617 Cole Boulevard

Golden, CO 80401

January 2011

Prepared by: Approved by:

_________________________________ __________________________________ Kevin A Whitney, Manager Jeff J. White, Director

EMISSIONS RESEARCH AND DEVELOPMENT DEPARTMENT

ENGINE, EMISSIONS AND VEHICLE RESEARCH DIVISION

This report shall not be reproduced, except in full, without the written approval of Southwest Research Institute ®

. Results a nd discussion given in this report relate only to the test items described in this report.SwRI R eport 03.15 777.01 (Rev 1) 

### ii FOREW O RD

This report covers work the Southwest Research Institute (SwRI®) Office of Automotive Engineering has conduct ed for the U.S. Environmental Protection Agency (EPA)
, the National Renewable Energy Laboratory (NREL) , and the Coordinating Research Council (CRC) in support of the Energy Policy Act of 2005 (EPAct). Section 15 06 of EPAct requires EPA to produce an updated fuel effects model representing the 2007 light

- duty gasoline fleet, including determination of the emissions impacts of increased renewable fuel use

. This report covers the exhaust emissions testing of fifteen light

- duty vehicles with twenty

- seven E0 through E20 test fuels, and four light

- duty flexible fuel vehicles (FFVs) on an E85 fuel, as part of the EPAct Gasoline Light

- Duty Exhaust Fuel Effects Test Program

. This
progra m will also be referred to as the EPAct/V2/E

- 89 Program based on the designations used for it by the EPA, NREL and CRC, respectively

.

I t is expected that this report will be an attachment or a chapter in the overall EPAct/V2/E

- 89 Program report prepared b y EPA and NREL. Other EPAct/V2/E

- 89 reports are expected to cover the following:

**•** 

### Fuel formulation, analysis, and procurement

.

**•** 

### Room temperature and 50°F emissions testing of three fuels using nineteen Tier 2 vehicles (known as Phase s 1, 2, and FTP)

.

**•** 

### Room temperature, 95°F, and 20°F testing of three fuels using six Tier 2 vehicles (Phase 4)

.

**•** 

### Room temperature, 95°F, and 20°F testing of three fuels using three high

- emitting vehicles (Phase 5).

This effort was authorized by EPA Contract EP

- C

- 07

- 028, Wo rk Assignments (WA) 1

- 03
, 2

- 03, and 3

- 01 as well as NREL Subcontract Nos. ACI

- 8

- 88613

- 01, AFT

- 9

- 99319

- 01 and AFT

- 9

- 99155

- 01. The project was based on SwRI Proposal Nos. 03

- 55287 versions A through E to NREL, and SwRI Proposal Nos. 03

- 55242 , 03

- 55242A, and 03

- 56310 versions A through G to EPA. The overall program was identified within SwRI under Project Nos. 03

. 14175.03, 03.14936.03, 03.14993, and 03.15777.01

. The project technical monitors were D r

. Rafal Sobotowski of EPA, Dr. Douglas Lawson of NREL, and Messrs. J im Uihlein of Chevron and Dominic DiCicco of Ford on behalf of CRC. The SwRI Program Manager was Kevin Whitney , while Eugene Jimenez oversaw day

- to

- day operations

. Testing o ccurred between March 2009 and June 20 10

.SwRI R eport 03.15 777.01 (Rev 1) 

### iii TABLE OF CONTENTS

Page

FOREW O RD

................................ ................................ ................................ ................................ .. ii

LIST OF TABLES

................................ ................................ ................................ ........................... v

LIST OF FIGURES

................................ ................................ ................................ ......................... v

ACKNOWLEDGEMENTS

................................ ................................ ................................ ........... v i

ACRONYMS AND ABBREVIATIONS

................................ ................................ ..................... vii

1.0 INTRODUCTION

................................ ................................ ................................ ............... 1 2.0 TECHNICAL APPROACH

................................ ................................ ................................ . 2

2.1 Test Fuels

................................ ................................ ................................ ............................. 2 2.2 Test Vehicles

................................ ................................ ................................ ...................... 11 2.3 Crankcase Lubricants

................................ ................................ ................................ ......... 13

2.3.1 Ford Explorer Crankcase Lubricant Issues

................................ ................................ ....... 13

2.4 Test Procedure

................................ ................................ ................................ ................... 13

2.4.1 Test Matrix

................................ ................................ ................................ ......................... 14 2.4.2 Drift Checks

................................ ................................ ................................ ....................... 1 6 2.4.3 Vehicle Conditioning

................................ ................................ ................................ ......... 1 6 2.4.4 Chassis Dynamometer

................................ ................................ ................................ ....... 1 8

2.5 Regulated and Unregulated Emissions

................................ ................................ .............. 1 8

2.5.1 Speciation of Volatile Organic Compounds

................................ ................................ ...... 20 2.5.2 Determination of NMOG

................................ ................................ ................................ ... 21

2.6 OBD Data

................................ ................................ ................................ ........................... 22

3.0 ISSUES ENCOUNTERED WHILE TESTING

................................ ................................ 23

3.1 Ford Explorer Low Oil Level

................................ ................................ ............................ 23 3.2 Ford Explorer Evaporative System MIL

................................ ................................ ............ 23 3.3 Saturn Outlook Transmission Module Malfunction

................................ .......................... 24 3.4 Fuel Carryover

................................ ................................ ................................ ................... 24

4.0 CLOSURE

................................ ................................ ................................ ......................... 2 6SwRI R eport 03.15 777.01 (Rev 1) 

### iv TABLE OF CONTENTS (CONT’D)

APPENDICES Pages

A FUEL CHANGE PROCEDURE

................................ ................................ ............... A1

- A5

B PETROSPEC RESULTS FO R INDIVIDUAL FUEL DR UMS

................................ B1

- B3

C DETAILS OF FORD F

- 150 MISFUELING EVENT

................................ ...................... C1

D ON

- ROAD OPERATION FOR I NACTIVE TEST VEHICLE S

............................... C1

- C2

E FUEL USED IN ON

- ROAD OPERATION FOR INACTI VE TEST VEHICLES

......... E1

F OIL SAMPLE SUMMARY

................................ ................................ ............................. F1

G FORD EXPLORER OIL LE VEL INCIDENT

................................ .......................... G1

- G2

H VEHICLE CONDITIONING AND TEST EXECUTION R EQUESTS

................. H1

- H1 3

I DETAILED MEASUREMENT AND ANALYSIS METHODS

................................ I1

- I16

J EPACT NMOG CALCULATI ON PROTOCOL

................................ ......................... J1

- J5

K LOD/LOQ METHOD

................................ ................................ ................................ K1

- K9

L EPA FUEL SAMPLING PR OCEDURE FOR CARRYOVE R EXPERIMENTS

........... L1

M FUEL BLENDING EXPERI MENT TO CHARACTERIZE CARRYOVER EFFECTS

................................ ................................ ................................ ......................... M1

N ADDITIONAL FUEL CARR YOVER EXPERIMENTS

................................ ................ N1

O REFUELING LOCATION E XPERIMENTS

................................ ........................... O1

- O3SwRI R eport 03.15 777.01 (Rev 1) 

### v LIST OF TABLES

Table Page

1 T est F uel S pecification

................................ ................................ ................................ ........ 3

2 Test Fuel Properties Determined From the EPAct/V2/E

- 89 Fuels Round Robin

............... 5

3 Sw RI Fuel Codes

................................ ................................ ................................ ............... 1 0

4 Phase 3 Test Vehicles

................................ ................................ ................................ ........ 1 1

5 Mileage Accumulation Fuel Properties

................................ ................................ ............. 1 2

6 Incremental Addition o f Fuels a nd Vehicles t o t he Test Matrix

................................ ........ 1 5

7 Repeatability Criteria f or Triplicate Testing

................................ ................................ ...... 1 5

8 Fuel Change, Conditio n ing, a nd Test Execution Sequence

................................ ............... 1 7

9 Vehicle Chassi s Dynamometer Settings

................................ ................................ ............ 1 8

10 VOC Speciation Schedule

................................ ................................ ................................ .. 2 1

11 Troubleshooting o f the Ford Explorer Evaporative System M IL

................................ ...... 2 3

LIST OF FIGURES

Figure Page

1 Constant

- Temperature Storage of Unopened Fuel Drums

................................ ................... 9SwRI R eport 03.15 777.01 (Rev 1) 

### vi ACKNOWLEDGEMENTS

SwRI acknowledges the following:

**•** The Environmental Protection Agency for their financial support

**•** The Department of Energy Office of Biomass Programs and Office of Vehicle Technologies for their financial support provided through the National Renewable Energy Laboratory

**•** The Coordinating Research Council for technical support and for providing the test vehi cles following the expiration of their leases

**•** The Lubrizol Corporation for supplying all crankcase lubricants used in this
programSwRI R eport 03.15 777.01 (Rev 1) 

### vii ACRONYMS AND ABBREVIATIONS

°F

.................... degrees Fahrenheit
IBP

................. initial boiling point
API

................. American Petroleum Institute
ASTM

............ American Society for Testing and Materials
Btu

.................. British thermal unit
CARB

............. California Air Resources Board
CH 4


### ................. methane
CO

.................. carbon monoxide
CO 2


### ................. carbon dioxide
CRC

............... Coordinating Research Council
DTC

............... diagnostic trouble code
DVPE

............. dry vapor pressure equivalent
EPA

................ U

. S

. Environmental Protection Agency
EPAct

............. 200 5 Energy Policy Act
E0

................... gasoline with no ethanol
E10

................. gasoline nominally containing 10 percent volume of ethanol
E15

................. gasoline nominally containing 15 percent volume of ethanol
E20

................. gasoline nominally containing 20 percent volume of ethanol E85.............gasoline nominally containing 85 percent volume of ethanol
FBP

................ final boiling point
FTP

................. Federal Test Procedure

g

..................... gram H 2 

### O

................ water
HP

.................. horsepower
HPLC

............. high performance liquid chromatography
IBP

................. initial boiling po int
k g

................... kilogram
kPa

................. kilopascal
lb

.................... pound mass
LOD

............... limit of detection LOQ

............... limit of quantification
LTFT

.............. long

- term fuel trim

mg

.................. milligram
MIL

................ malfunction indicator lightSwRI R eport 03.15 777.01 (Rev 1) 

### viii ACRONYMS AND ABBREVIATIONS (CONT’D)

MJ

.................. megajoule

m l

................... milliliter
MON

.............. motor octane number mph

................ miles per hour
NH 3


### ................ ammonia
NMHC

........... non

- methane hydrocarbons
NMOG

........... non

- methane organic gases
NO

.................. nitric oxide
NO 2


### ................ nitrogen dioxide
NO X 

### ................ oxides of nitrogen
NREL

............. National Renewable Energy Laboratory
O 2


### ................... oxygen OBD

............... on

- board diagnostics
PM

.................. particulate matter

ppm

................ p arts per million psi

................... pounds per square inch
RON

............... research octane number
RPM

............... revolutions per minute
RUL

............... regular unleaded
RVP

................ Reid vapor pressure
S TFT

.............. short

- term fuel trim
SwRI

.............. Southwest Research Institute
THC

............... total hydrocarbons VOC............volatile organic compounds
vol...

............... volume
WA

................. w ork a ssignment
WAM

............. w ork a ssignment managerSwRI R eport 03.15 777.01 (Rev 1) 

### 1 of 26 1.0 INTRODUCTION

Since September 2007, Southwest Research Institute (SwRI) has been conducting work on a series of tasks and assignments, the results of which are now collectively known as the EPAct/V2/E

- 89 emissions test program. The work began under the direction of the U.S. Environmental Protection Agency (EPA ) to fulfill requirements for emissions m odeling outlined in the Energy Policy Act of 2005 (EPAct). Section 1506 of the EPAct requires the production of an updated fuel effects mo del representing the 2007 light

- duty gasoline fleet, including
assessment of the emissions impacts of increased renew able fuel use. By January 2009, SwRI had completed Phases 1 and 2 of the EPAct/V2/E

- 89 program. These phases, described in a separate report, involved testing of 19 light duty cars and trucks (subsequently referred to as the “EPAct fleet”) on three fuels , at two temperatures.

In March 2009
, SwRI began work on Phase 3, which was jointly supported by EPA, the U.S. Department of Energy through the National Renewable Energy Laboratory (NREL), and the Coordinating Research Council (CRC). This report covers w ork conducted for Phase 3, which involved the testing of fifteen vehicles from the EPAct fleet using twenty

- seven test fuels with ethanol content ranging from 0 to 20 percent by volume , and testing of four f lexible

- f uel v ehicles (FFVs) from the EPAct flee t on an E85 fuel

. Phase 3 testing was completed in June 2010.SwRI R eport 03.15 777.01 (Rev 1) 

### 2 of 26 2.0 TECHNICAL APPROACH

2.1 Test Fuels

Twenty

- eight test fuels were evaluated in Phase 3 of the EPAct /V2/E

- 89 Pro gram . Fuel procurement is detailed in SwRI Final Report 03.14295/03

- 51563E “ V2/EPAct/E

- 89 Fuel Blending

, ” which has been submitted separately. Target fuel specifications are given in Table 1. The actual properties of test fuel as determined from the EPAct/V 2/E

- 89 Fuels Round Robin are listed in Table 2

.

T wenty

- seven of the twenty

- eight t est fuels were procured by SwRI from Haltermann Products. EPA established a fuel development protocol for this p rogram . Using this protocol, all test fuels were formulated by Rafal Sobotowski of the EPA in conjunction with Haltermann, who provided EPA with data for all their blendstock components. The procurement of Fuels 1 through 16, Fuel 30, and Fuel 31 was funded by EPA Contract No. EP

- C

- 07

- 028, while NR EL Subcontract No. ACI

- 8

- 88612

- 01 funded the procurement of Fuels 20 through 28. The E85 Fuel 29 was provided to the program by the CRC.SwRI R eport 03.15777 .01 (Rev 1) 

### 3 of 26 TABLE 1. TEST FUEL SPECIFICAT ION

N OTE : Properties in bold were varied within the fuel matrix Test Fuel Specification

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 Density, 60 o F g/cm 3 D4052 NA Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report API Gravity, 60 o F o API D4052 NA Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report

Ethanol Content vol. % D5599 E0: < 0.1; E10: ± 0.5; E15: ± 0.5; E20: ±0.5;

E85: ±2 10 0 10 10 0 10 0 0 0 10 10 10 0 0 0 10

Total Content of Oxygenates Other than Ethanol vol. % D5599

- <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1 <0.1

T10 oF D86

- <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 <158 T50 oF D86 ± 4 150 240 220 220 240 190 190 220 190 220 190 150 220 190 190 220 T90 oF D86 ± 5 300 340 300 340 300 340 300 300 340 340 300 340 340 340 300 300 FBP oF D86

- <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 <437 DVPE psi D5191 ± 0.25 10.0 10.0 7.0 10.0 7.0 7.0 7.0 10.0 10.0 7.0 10.0 10.0 7.0 7.0 10.0 7.0 Aromatics vol. % D1319 ± 1.5 15.0 15.0 15.0 15.0 35.0 15.0 15.0 15.0 35.0 35.0 35.0 35.0 35.0 15.0 35.0 35.0 Olefins vol. % D1319 ± 1.5 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 7 Benzene vol. % D3606 ± 0.15 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 S mg/kg D5453 ± 5 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 25 (R + M)/2

- Calc.

- ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 C mass % Calc.

- Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report

H mass % D4808 Method A - Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report

O mass % D5599

- Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Gross Heat of Combustion Btu/lb D4809

- Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Water Content mg/kg E1064

- Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Report Copper Strip Corrosion, 3h at 122 o F

- D130

- <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 Solvent-Washed Gum Content mg/100 ml D381

- < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 Oxidation Stability minute D525

- >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 >240 TEST FUELS E0/E10 Fuels

PROPERTY UNIT METHOD BLENDING TOLERANCESwRI R eport 03.15777 .01 (Rev 1) 

### 4 of 26 TABLE 1 (CONT’D). TEST FUEL SPECIFICAT ION

a



### – fuel provided by CRC N OTE : Properties in bold were varied within the fuel matrix 

## Test Fuel Specification

20 21 22 23 24 25 26 27 28 29 a 30 31 Density, 60 o F g/cm 3 D4052 NA Report Report Report Report Report Report Report Report Report Report Report Report API Gravity, 60 o F o API D4052 NA Report Report Report Report Report Report Report Report Report Report Report Report

Ethanol Content vol. % D5599 E0: < 0.1; E10: ± 0.5; E15: ± 0.5; E20: ±0.5;

E85: ±2 20 20 20 20 20 20 15 15 15 81 10 20

Total Content of Oxygenates Other than Ethanol vol. % D5599

- <0.2 <0.2 <0.2 <0.2 <0.2 <0.2 <0.15 <0.15 <0.15 <2.0 <0.1 <0.2

T10 oF D86

- <158 <158 <158 <158 <158 <158 <158 <158 <158 Report <158 <158 T50 oF D86 ± 4 165 165 165 165 165 165 160 220 220 Report 150 165 T90 oF D86 ± 5 300 300 300 340 340 340 340 340 300 Report 325 325 FBP oF D86

- <437 <437 <437 <437 <437 <437 <437 <437 <437 Report <437 <437 DVPE psi D5191 ± 0.25 7.0 7.0 10.0 7.0 10.0 10.0 10.0 7.0 7.0 6.9 10.0 7.0 Aromatics vol. % D1319 ± 1.5 15.0 35.0 15.0 15.0 15.0 35.0 35.0 15.0 35.0 Report 35.0 35.0 Olefins vol. % D1319 ± 1.5 7 7 7 7 7 7 7 7 7 Report 7 7 Benzene vol. % D3606 ± 0.15 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 0.62 Report 0.62 0.62 S mg/kg D5453 ± 5 25 25 25 25 25 25 25 25 25 15 25 25 (R + M)/2

- Calc.

- ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 ≥ 87.0 Report ≥ 87.0 ≥ 87.0 C mass % Calc.

- Report Report Report Report Report Report Report Report Report Report Report Report

H mass % D4808 Method A - Report Report Report Report Report Report Report Report Report Report Report Report

O mass % D5599

- Report Report Report Report Report Report Report Report Report Report Report Report Gross Heat of Combustion Btu/lb D4809

- Report Report Report Report Report Report Report Report Report Report Report Report Water Content mg/kg E1064

- Report Report Report Report Report Report Report Report Report <10,000 Report Report Copper Strip Corrosion, 3h at 122 o F

- D130

- <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 <No. 1 na <No. 1 <No. 1 Solvent-Washed Gum Content mg/100 ml D381

- < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 < 5 Oxidation Stability minute D525

- >240 >240 >240 >240 >240 >240 >240 >240 >240 na >240 >240 

### E85 CRC Fuels

TEST FUELS 

### E15/E20 Fuels

PROPERTY UNIT METHOD BLENDING TOLERANCESwRI R eport 03.15777 .01 (Rev 1) 

### 5 of 26 TABLE 2

. TEST FUEL PROPERTIES DETERMINED FROM THE EPACT /V2/E

- 89 FUELS ROUND ROBIN

1 2 3 4 5 6 7 8 9

Density, 60 o F g/cm 3 D4052 0.7211 0.7220 0.7350 0.7346 0.7573 0.7342 0.7208 0.7191 0.7454

API Gravity, 60 o F o API D4052 64.6 64.3 60.8 60.9 55.2 61.1 64.6 65.1 58.2

Ethanol vol. % D5599 10.03 <0.10 10.36 9.94 <0.10 10.56 <0.10 <0.10 <0.10 Total Content of Oxygenates Other Than Ethanol vol. % D5599 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10

Distillation IBP ° F 92.9 83.5 106.4 89.9 94.1 106.7 100.1 83.7 85.3
5% evap ° F 112.5 105.4 136.0 115.9 128.6 130.4 127.6 108.1 105.1
10% evap ° F 117.3 121.7 141.7 126.3 145.4 135.9 137.0 123.4 115.1
20% evap ° F 123.9 154.4 148.9 140.9 172.6 142.6 149.0 151.6 130.3
30% evap ° F 131.2 190.6 155.0 151.7 199.4 148.3 161.7 185.1 147.2
40% evap ° F 139.9 218.5 175.1 161.2 222.1 153.4 176.6 204.4 167.7
50% evap ° F 148.9 236.7 217.5 221.9 237.0 188.5 193.1 221.1 192.8
60% evap ° F 172.3 252.7 230.2 245.9 247.2 228.2 210.2 233.5 224.7
70% evap ° F 224.1 271.7 243.6 270.0 258.5 267.7 228.6 246.4 260.3
80% evap ° F 254.6 305.9 257.1 303.5 273.1 310.1 251.5 264.0 292.2
90% evap ° F 300.2 340.1 295.9 337.5 300.0 340.4 298.4 303.1 341.8
95% evap ° F 334.5 353.0 334.4 352.0 323.5 352.7 329.3 330.5 363.5

FBP ° F 368.0 375.3 368.9 369.8 357.8 369.2 361.8 360.9 384.7
DVPE (EPA equation) psi D5191 10.07 10.20 6.93 10.01 6.95 7.24 7.15 10.20 10.30

Aromatics vol. % D1319 15.4 14.1 15.0 15.5 34.7 15.0 17.0 15.7 35.8

Olefins vol. % D1319 7.6 6.8 7.6 6.8 6.9 8.8 7.5 6.4 6.2

Saturates vol. % calculated a 67.0 79.1 67.0 67.8 58.4 65.6 75.5 78.0 58.0

Benzene vol. % D3606 0.62 0.51 0.61 0.54 0.51 0.68 0.55 0.50 0.54

Sulfur mg/kg D5453 30 23 22 21 24 23 23 23 23

RON

- D2699 94.8 96.0 98.0 97.1 96.7 96.3 91.2 95.5 94.5

MON

- D2700 86.3 88.6 87.6 87.6 86.3 86.6 84.2 87.8 84.8
(RON+MON)/2

- calculated 90.6 92.3 92.8 92.4 91.5 91.5 87.7 91.7 89.7

C mass % D5291 mod. 81.70 85.12 81.61 82.21 86.58 81.52 85.16 85.12 87.03

H mass % D5291 mod. 14.02 14.43 14.17 14.12 12.92 14.21 14.25 14.32 12.82

O mass % D5599 3.9 <0.1 3.9 3.7 <0.1 4.0 <0.1 <0.1 <0.1

Net Heat of Combustion MJ/kg D4809 41.950 43.960 41.536 41.952 42.948 41.785 43.735 44.037 43.209

Water mass % E-1064 0.071 0.010 0.059 0.077 0.014 0.073 0.019 0.020 0.009

Lead g/l D3237

- <0.001

- - <0.003

- <0.001 0.001 <0.001
Copper Strip Corrosion

- D130 1A 1A 1A 1A 1A 1A 1A 1A 1A

Solvent Washed Gum Content mg/100ml D381 <0.5 <0.5 <0.5 1.5 <0.5 <0.5 <0.5 <0.5 <0.5
Oxidation Stability min. D525 >240 >240 >240 >240 >240 >240 >240 >240 >240

a Saturates = 100 - D1319 Aromatics - D1319 Olefins - D5599 Ethanol
NOTE: Properties in bold were varied within the fuel matrix. FUEL

D86 ( OptiDist or equivalent for E10, E15 and

E20 fuels) PROPERTY UNIT TEST METHODSwRI R eport 03.15777 .01 (Rev 1) 

### 6 of 26 TABLE 2 (CONT'D)

. TEST FUEL PROPERTIES DETERMINED FROM THE EPACT /V2/E

- 89 FUELS ROUND ROBIN

10 11 12 13 14 15 16 20 21

Density, 60 o F g/cm 3 D4052 0.7644 0.7596 0.7517 0.7540 0.7223 0.7428 0.7636 0.7425 0.7754

API Gravity, 60 o F o API D4052 53.4 54.6 56.5 56.0 64.2 58.8 53.6 58.9 50.8

Ethanol vol. % D5599 9.82 10.30 9.83 <0.10 <0.10 <0.10 10.76 20.31 20.14 Total Content of Oxygenates Other Than Ethanol vol. % D5599 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10

Distillation IBP ° F 104.7 92.0 91.3 96.6 100.4 84.7 104.5 107.9 106.3
5% evap ° F 130.0 115.4 110.7 127.0 126.5 105.5 133.0 137.3 134.7
10% evap ° F 136.3 124.4 116.9 139.8 135.5 115.6 139.2 142.6 141.3
20% evap ° F 144.3 137.6 125.0 158.7 147.3 130.5 147.8 149.7 150.3
30% evap ° F 151.0 148.1 133.8 178.2 160.0 146.6 155.1 155.3 157.1
40% evap ° F 161.6 156.5 142.8 199.9 175.1 166.3 172.1 159.6 162.6
50% evap ° F 217.1 189.3 152.2 222.5 192.8 189.7 218.8 162.7 167.6
60% evap ° F 261.5 231.1 198.5 245.2 212.0 216.2 237.5 179.9 217.3
70% evap ° F 290.4 251.4 275.1 269.8 237.3 243.0 251.9 234.8 255.2
80% evap ° F 317.5 270.0 307.9 303.5 280.1 265.9 268.6 253.1 275.3
90% evap ° F 340.2 298.6 339.8 337.9 338.5 299.4 300.6 298.7 305.0
95% evap ° F 354.3 325.0 357.7 354.4 354.5 329.3 330.8 336.6 331.3

FBP ° F 372.4 360.8 375.9 377.5 377.5 363.7 365.6 371.9 360.5
DVPE (EPA equation) psi D5191 7.11 9.93 10.13 6.92 7.14 10.23 7.12 6.70 7.06

Aromatics vol. % D1319 34.0 35.0 34.8 34.1 16.9 35.3 35.6 15.2 35.5

Olefins vol. % D1319 6.1 6.9 6.9 6.3 8.5 7.2 6.8 7.4 7.1

Saturates vol. % calculated a 50.1 47.8 48.5 59.6 74.6 57.4 46.9 57.1 37.3

Benzene vol. % D3606 0.52 0.54 0.57 0.51 0.52 0.54 0.62 0.61 0.61

Sulfur mg/kg D5453 25 24 19 23 24 24 23 22 22

RON

- D2699 98.5 97.8 100.4 95.8 91.5 95.0 101.0 101.9 101.4

MON

- D2700 87.2 85.6 88.0 85.8 84.6 84.9 88.3 89.3 87.5
(RON+MON)/2

- calculated 92.9 91.7 94.2 90.8 88.1 90.0 94.7 95.6 94.5

C mass % D5291 mod. 83.47 83.68 83.32 86.76 85.28 86.88 83.40 78.06 79.90

H mass % D5291 mod. 12.83 12.61 12.68 13.15 14.29 12.79 12.66 14.01 12.43

O mass % D5599 3.6 3.7 3.6 <0.1 <0.1 <0.1 3.9 7.6 7.1

Net Heat of Combustion MJ/kg D4809 41.210 41.175 41.373 43.171 43.519 43.108 41.013 40.057 39.285

Water mass % E-1064 0.067 0.066 0.066 0.014 0.015 0.012 0.066 0.138 0.128

Lead g/l D3237 <0.003

- <0.003 <0.001 <0.001 <0.001

- <0.003 0.009
Copper Strip Corrosion

- D130 1A 1A 1A 1A 1A 1A 1A 1A 1A

Solvent Washed Gum Content mg/100ml D381 <0.5 0.5 <0.5 1.5 <0.5 0.5 1 <0.5 0.5
Oxidation Stability min. D525 >240 >240 >240 >240 >240 >240 >240 >240 >240

a Saturates = 100 - D1319 Aromatics - D1319 Olefins - D5599 Ethanol
NOTE: Properties in bold were varied within the fuel matrix. PROPERTY UNIT TEST METHOD FUEL

D86 ( OptiDist or equivalent for E10, E15 and

E20 fuels)SwRI R eport 03.15777 .01 (Rev 1) 

### 7 of 26 TABLE 2 (CONT'D)

. TEST FUEL PROPERTIES DETERMINED FROM THE EPACT /V2/E

- 89 FUELS ROUND ROBIN

22 23 24 25 26 27 28 30 31

Density, 60 o F g/cm 3 D4052 0.7371 0.7476 0.7422 0.7702 0.7593 0.7434 0.7699 0.7508 0.7742

API Gravity, 60 o F o API D4052 60.3 57.6 58.9 52.0 54.6 58.6 52.1 56.8 51.1

Ethanol vol. % D5599 20.51 20.32 20.51 20.03 15.24 14.91 14.98 9.81 20.11 Total Content of Oxygenates Other Than Ethanol vol. % D5599 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10 <0.10

Distillation IBP ° F 89.8 109.0 89.7 89.0 88.7 104.8 103.9 90.9 105.8
5% evap ° F 118.8 133.3 115.9 113.7 109.6 135.3 136.3 110.3 132.5
10% evap ° F 129.6 138.9 126.9 125.5 117.1 142.3 144.2 116.7 139.1
20% evap ° F 144.3 146.2 142.8 142.1 127.8 152.0 154.0 125.4 147.7
30% evap ° F 153.7 152.3 153.2 153.3 138.6 158.0 160.2 133.9 155.1
40% evap ° F 159.5 157.8 160.4 160.9 149.8 163.8 165.8 143.1 161.3
50% evap ° F 163.2 162.5 165.1 166.9 160.3 221.5 216.6 152.9 167.3
60% evap ° F 167.2 171.6 172.9 191.3 174.7 265.1 240.2 197.2 214.0
70% evap ° F 233.9 270.9 266.1 281.6 277.0 274.9 251.6 267.3 271.6
80% evap ° F 253.6 311.4 305.5 310.3 306.5 311.3 268.4 294.6 297.0
90% evap ° F 297.3 338.2 338.1 337.9 338.7 340.3 298.8 323.8 325.2
95% evap ° F 334.5 350.0 350.3 352.7 356.7 351.9 327.3 341.8 342.1

FBP ° F 369.9 364.6 368.2 371.8 377.3 372.2 363.2 366.1 365.6
DVPE (EPA equation) psi D5191 10.21 6.84 10.12 10.16 10.21 6.97 6.87 10.23 6.98

Aromatics vol. % D1319 15.0 15.9 15.3 35.2 35.6 14.9 34.5 35.5 35.5

Olefins vol. % D1319 6.9 7.5 7.3 6.6 6.5 7.4 7.0 6.5 6.8

Saturates vol. % calculated a 57.6 56.4 56.9 38.1 42.7 62.9 43.5 48.2 37.6

Benzene vol. % D3606 0.59 0.63 0.62 0.65 0.62 0.56 0.59 0.58 0.60

Sulfur mg/kg D5453 21 21 21 26 23 26 24 23 25

RON

- D2699 101.8 97.4 100.8 102.2 101.7 100.8 102.7 100.5 101.7

MON

- D2700 89.3 86.8 88.6 88.3 88.5 89.2 89.4 88.1 88.2
(RON+MON)/2

- calculated 95.6 92.1 94.7 95.3 95.1 95.0 96.1 94.3 95.0

C mass % D5291 mod. 78.24 78.34 78.47 80.62 81.48 80.27 81.78 83.17 79.90

H mass % D5291 mod. 13.85 13.86 13.86 12.38 12.45 14.01 12.62 13.00 12.49

O mass % D5599 7.7 7.5 7.6 7.2 5.6 5.5 5.4 3.6 7.2

Net Heat of Combustion MJ/kg D4809 40.031 39.915 40.114 38.855 40.384 41.062 40.383 41.304 39.391

Water mass % E-1064 0.113 0.112 0.108 0.117 0.088 0.090 0.091 0.086 0.143

Lead g/l D3237 0.004 <0.003 0.005 0.001 <0.003 <0.003 <0.003

- <0.003
Copper Strip Corrosion

- D130 1A 1A 1A 1A 1A 1A 1A 1A 1A

Solvent Washed Gum Content mg/100ml D381 <0.5 0.5 0.5 <0.5 <0.5 0.5 <0.5 <0.5 0.5
Oxidation Stability min. D525 >240 >240 >240 >240 >240 >240 >240 >240 >240

a Saturates = 100 - D1319 Aromatics - D1319 Olefins - D5599 Ethanol
NOTE: Properties in bold were varied within the fuel matrix. PROPERTY UNIT TEST METHOD FUEL

D86 ( OptiDist or equivalent for E10, E15 and

E20 fuels)SwRI R eport 03.15777 .01 (Rev 1) 

### 8 of 26 TABLE 2 (CONT'D)

. TEST FUEL PROPERTIES DETERMINED FROM THE EPACT /V2/E

- 89 FUELS ROUND ROBIN

PROPERTY UNIT TEST METHOD FUEL 29
Density, 60 o F g/cm 3 D4052 0.7797

API Gravity, 60 o F o API D4052 49.8

Uncorrected Ethanol mass % D5501 mod. 79.59

Uncorrected Methanol mass % D5501 mod. 0.01

Ethanol vol. % D5501 mod. 77.15

Methanol vol. % D5501 mod. <0.01 Estimated Hydrocarbon
Content vol. % calculated a 22.14

Distillation IBP ° F 99.0
5% evap ° F 132.9
10% evap ° F 154.3
20% evap ° F 167.6
30% evap ° F 170.3
40% evap ° F 171.2
50% evap ° F 171.8
60% evap ° F 172.1
70% evap ° F 172.5
80% evap ° F 172.9
90% evap ° F 173.9
95% evap ° F 176.2

FBP ° F 265.8
DVPE (EPA equation) psi D5191 8.92

Benzene vol. % D5580 0.12

S mg/kg D5453 16

C mass % D5291 mod. 57.74

H mass % D5291 mod. 12.80

O mass % D5501 mod. 27.19

mass % E203 0.93

vol. % E203 0.72

Net Heat of Combustion MJ/kg D4809 30.058

Solvent Washed Gum mg/100 ml D381 1.9

Unwashed Gum mg/100 ml D381 1.8
Acidity (as acetic acid) mass % D1613 0.0021
pHe

- D6423 8.08
Inorganic Chloride mg/kg D7319 nd

Copper mg/l D1688 b 0.02

a Estimated hydrocabon contenet = 100 - D5501 Ethanol - E203 Water

b D1688 modified as outlined in D4806 NOTE: Fuel provided by CRC D86

WaterSwRI R eport 03.15777 .01 (Rev 1) 

### 9 of 26 All fuels were maintained in sealed epoxy

- lined 5B drums. All unopened drums were kept in a temperature

- controlled facility (SwRI Building 205, Figure 1). The storage temperature for unopened drums was 70°F ± 5°F. Once a week, necessary unopened fuel dr ums were transported from Building 205 to a dedicated cold

- storage facility located behind the emissions laboratory. Prior to opening a drum, it was conditioned to a temperature of less than 50°F. Once a drum of fuel was opened, it continued to be stored at 45°F ± 5°F. The temperature of both fuel storage facilities was continuously recorded, and was verified at least once a day.

FIGURE 1 . CONSTANT

- TEM P E RAT U RE STORAGE OF UNOPENED FUEL DRUMS

All fuels received independent identifiers which included the EPAct fuel number, a n SwRI fuel code, and a project

- specific supplementary three

- letter code (Table 3 ). All fuel drums and corresponding work requests included all three designators in an effort to assure the correct fuel was being used at any point in the test program. Additionally, each individual drum was labeled numerically.SwRI R eport 03.15777 .01 (Rev 1) 

### 10 of 26 TABLE 3 . SWRI FUEL CODES

When a vehicle received a fuel change, the appropriate fuel drum was removed from the cold box. The SwRI fuel code and supplemental three

- letter fuel name were verified by two individuals prior to a refueling event (see fuel change procedure in Appendix A ), and the individual fuel drum number was recorded. In an effort to ensure correct drum labeling, when each new drum of fuel was opened
, a sample was collected in order to verify select fuel properties with a PetroSpec portable gasoline analyzer. The re sults of these analyses are given in Appendix B . Based on these results, SwRI did not observe any fuel drum mislabeling during this
program. Test Fuel SwRI Fuel Code SwRI Fuel Name
Fuel 1 EM-6995-F SAT
Fuel 2 EM-6953-F ELP
Fuel 3 EM-7053-F FLG
Fuel 4 EM-6996-F HOU
Fuel 5R a EM-7061-F MCI
Fuel 6 EM-7092-F IND
Fuel 7 EM-6954-F JNU
Fuel 8 GB-6936-F BWI
Fuel 9 EM-6955-F KAW
Fuel 10 EM-7093-F LNK
Fuel 11 EM-7055-F MIA
Fuel 12 EM-6997-F MLS
Fuel 13 EM-6965-F CLF
Fuel 14 EM-6956-F BNA
Fuel 15 EM-6957-F OAK
Fuel 16 EM-7056-F OSH
Fuel 20 EM-7057-F PHX
Fuel 21 EM-7058-F RNO
Fuel 22 EM-7001-F SLC
Fuel 23 EM-7059-F SFO
Fuel 24 EM-6998-F TEX
Fuel 25 EM-7073-F TUL
Fuel 26 EM-7094-F YAK
Fuel 27 EM-7095-F BOS
Fuel 28 EM-7096-F NBA
Fuel 29 EM-9675-F E85
Fuel 30 EM-7060-F BUF
Fuel 31 EM-7074-F GPZ

a Fuel 5 was reblended prior to being used in the test program. 5R refers to the reblended version of the fuel.SwRI R eport 03.15777 .01 (Rev 1) 

### 11 of 26 There was one confirmed case of vehicle misfueling, which occurred with the Ford F

- 150. In the 45 th 

### week of tes ting, the F

- 150 was apparently refueled from an improperly

labeled drum of slop fuel, which contained a mixture of both gasoline and diesel fuel

. Immediately following the misfueling, the vehicle had a rough idle. After the improper fuel was discovered, the fuel tank of the vehicle was cleaned, the fuel filter was replaced, and the fuel system was flushed. Additional exhaust emission tests were conducted with the fuel that was in the tank prior to the misfueling event, which showed emissions results simi lar to previous tests. EPA and NREL approved these results, and testing of this vehicle resumed. A more detailed description of this incident is given in Appendix C

.

2.2 Test Vehicles

As specified by EPA and NREL, sixteen vehicles were utilized in the Phase 3 test program (Table 4 ). Fifteen of these vehicles were used to test the twenty

- seven E0, E10, E15 and E20 fuels. Three of these fifteen vehicles (Chevrolet Impala FFV, Chevrolet Silverado FFV, Ford F

- 150 FFV) and one additional flexible fuel vehicle (Dodge Caravan FFV ) were used to test the E85 F uel 29. All vehicles were leased by SwRI for two years at the initiation of Phase 1 of the V2/EPAct/E

- 89 program. Due to changes and additions to the overall program, the term of the two

- year leases expired prior to the completion of all Phase 3 testing. The Coordinating Research Council then purchased the test vehicles and made them available to the test program for the remainder of i ts duration.

TABLE 4 . PHASE 3 TEST VEHICLES

GM 2008 Chevrolet Cobalt CCOB 2.4L I4 8GMXV02.4025 5 NA 4,841

GM 2008 Chevrolet Impala FFV CIMP 3.5L V6 8GMXV03.9052 5 L2 5,048 a

GM 2008 Saturn Outlook SOUT 3.6L V6 8GMXT03.6151 5 L2 5,212 a

GM 2008 Chevrolet Silverado FFV CSIL 5.3L V8 8GMXT05.3373 5 NA 5,347 b

Toyota 2008 Toyota Corolla TCOR 1.8L I4 8TYXV01.8BEA 5 U2 5,019 a
Toyota 2008 Toyota Camry TCAM 2.4L I4 8TYXV02.4BEA 5 U2 4,974 b

Toyota 2008 Toyota Sienna TSIE 3.5L V6 8TYXT03.5BEM 5 U2 4,997

Ford 2008 Ford Focus FFOC 2.0L I4 8FMXV02.0VD4 4 U2 5,150 a,b

Ford 2008 Ford Explorer FEXP 4.0L V6 8FMXT04.03DB 4 NA 6,799 c

Ford 2008 Ford F-150 FFV F150 5.4L V8 8FMXT05.44HF 8 NA 5,523 a
Chrysler 2008 Dodge Caliber DCAL 2.4L I4 8CRXB02.4MEO 5 NA 4,959
Chrysler 2008 Dodge Caravan FFV d DCAR 3.3L V6 8CRXT03.3NEP 8 NA 5,282
Chrysler 2008 Jeep Liberty JLIB 3.7L V6 8CRXT03.7NE0 5 NA 4,785

Honda 2008 Honda Civic HCIV 1.8L I4 8HNXV01.8LKR 5 U2 4,765

Honda 2008 Honda Odyssey HODY 3.5L V6 8HNXT03.54KR 5 U2 4,850

Nissan 2008 Nissan Altima NALT 2.5L I4 8NSXV02.5G5A 5 L2 5,211 b

a – These vehicles were added to the Phase 3 test matrix at a later date. Prior to their inclusion in the matrix, they received on-road miles every other week.

b – These vehicles were included in an FTP interim test program (EPA WA 1-09) conducted between Phases 1 and 2.

c – During Phase 1, the initial 4,000 miles of vehicle break-in was conducted with the wrong crankcase lubricant viscosity grade. An additional 2,000-mile break-in was conducted with the correct lubricant viscosity grade.

d – Dodge Caravan FFV was only tested with E85

MAKE MO DEL YEAR BRAND MO DEL VEHICLE NAME ENGINE ENGINE FAMILY EPA T2 BIN CA CERT PHASE 3 STARTING O DO METERSwRI R eport 03.15777 .01 (Rev 1) 

### 12 of 26 Prior to the initiation of Phase 1 of the program, each vehicle was brought up to 4,000 odometer miles to eliminate any engine break

- in issues. This was accomplished by operating the vehicles on mileage ac cumulation dynamometers over the Standard Road Cycle using a non

oxygenated, commercial, 87 octane gasoline (Table 5 ) . The engine crankcase lubricant was drained and replaced with the appropriate manufacturer

- recommended viscosity grade at the start of mi leage accumulation, and at 2,000 miles. The 2,000

- mile fill of oil remained in the test vehicles throughout the conduct of Phases 1, 2, and 3 of the EPAct program. The vehicle odometer readings at the start of Phase 3 are included in Table 4

.

TABLE 5

. MILEAGE ACCUMULATION FUEL PROPERTIES

Due to the nature of the randomized test matrix, as well as the incremental addition of test vehicles to the program, there were periods of time when vehicles were not involved in active testing. In an attempt to minimize vehicle maintenance issues due to extended inactivity, those vehicles were operated by an experienced driver once every two weeks over an on

- road course around the perimeter of the SwRI campus (Appendix D ). Prior to each drive, each vehicle received a brief visual inspection to ensure proper tire inflation and fluid levels. One “lap” was completed, which was approximately 8 miles in length and about 20 minutes in duration. Speed limits ranged from 35 to 45 mph, and the drive included six traffic signals and two stop signs. This task was conducted using an early discarded version of E0 Fuel 5, which was procured prior to use of the EPA

- specified fuel development protocol. Properties of this fuel are inc luded in Appendix E

. Density, 60 o 

### F g/cm 3 

### D4052 0.7329 API Gravity, 60 o 

### F o 

### API D4052 61.5
Ethanol Content vol. % D5599 <0.1
IBP oF D86 82
T10 oF D86 109
T50 oF D86 194
T90 oF D86 342
FBP oF D86 416
DVPE psi D5191 11.1
Aromatics vol. % D1319 26.2
Olefins vol. % D1319 7.7
Benzene vol. % D3606 0.95
S mg/kg D5453 15.9 (R + M)/2

- Calc. 87.5
Net Heat of Combustion Btu/lb D4809 18,734 UNIT METHOD Valero RUL PROPERTYSwRI R eport 03.15777 .01 (Rev 1) 

### 13 of 26 2.3 Crankcase Lubricant s

GF

- 4 category crankcase lubricants of two viscosity grades (5W20 and 5W30) were provided by the Lubrizol Corporation. As mentioned in Section 2.2, lubricants were broken in for 2,000 miles prior to the init iation of Phase 1 of the program. The lubricants remained unchanged throughout the conduct of program Phases 1, 2, and 3. Four

- ounce engine oil samples were taken from each vehicle at the start and end of the 2,000

- mile lubricant break

- in (at the 2,000

- and 4,000

- mile vehicle break

- in intervals), and following emissions testing of the 3 rd



### , 15 th 

### , and 27 th 

### fuels in the Phase 3 test sequence. The oil samples were shipped in batches to Dr. Ewa Bardasz of Lubrizol for analysis. To accommodate for the oil sam ples taken over the course of the program, each vehicle’s sump was overfilled by 12 ounces during the oil change at the mid

- point of the 4,000

- mile vehicle break

- in. A summary of the oil samples collected and shipped to Lubrizol is given in Appendix F

.

2 .3.1 Ford Explorer Crankcase Lubricant Issues

An incorrect oil viscosity was used in the Ford Explorer during break

- in. Ford specifies 5W

- 30 grade for the 4.0L V

- 6 engine and 5W

- 20 for the 4.6L V

- 8. The test vehicle was equipped with the 4.0L V

- 6, and was incorrectly filled with the 5W

- 20 oil at both the start of mileage accumulation and at the 2,000

- mile oil change. The vehicle had accumulated 4,000 miles when this error was discovered. After discussing this situation with all involved parties, the vehicle received a single flush with 5W

- 30 oil (2 drains and 2 fills with oil filter changes) and an additional 2,000 miles were accumulated on the Ford Explorer to break

- in th e correct oil.

There also appeared to be an oil level issue with the Explorer. When the oil sample was collected following testing of the 15 th 

### fuel, the technician noticed that the oil level was below the minimum oil level on the dip stick. Following e xtensive discussions with all sponsors, an additional 20 ounces of fresh crankcase lubricant were added to the Ford Explorer before resuming testing. Details of this incident are given in Appendix G

. As a result of this situation, starting in the 22 nd 

### w eek of Phase 3, the oil level on all vehicle s was checked monthly. These checks were taken on a level floor inside the emissions lab following a minimum 12

- hour soak at room temperature (72 ° F ± 2 ° F). Initial results showed the Toyota Camry oil level was between 1/4 and 1/8 of the distance from the fill level to the full level on the dipstick. The oil level of this vehicle was monitored weekly, but did not change during the rest of the program . No other vehicles had oil level issues.

2.4 Test Procedure
All vehicle/fuel combinations were tested using the California Unified Cycle, also known as the LA92. For this program, the LA92 was conducted as a three

- phase, cold

- start test in a manner similar to the FTP, and FTP weighting factors were used to calcul ate composite emission
rates. In order to supplement data being collected during Phase 4 of this test program, t he four FFVs were also tested over the FTP cycle , only when operating on E85.

Testing was conducted during the day shift while vehicle prepar ation , fuel changes, sulfur purges, and conditioning were conducte d during a second shift. All vehicle soaks and tests wereSwRI R eport 03.15777 .01 (Rev 1) 

### 14 of 26 conducted at a nominal temperature of 72°F. The representative bulk oil temperature of a vehicle’s sump was stabilized to 72°F ± 3 °F prior to conducting any emission test.

SwRI made a good faith effort to maintain intake air humidity during testing at 75 ± 5 grains H 2 

### O/lb dry air. However, despite substantial time and effort in upgrading and refining our test cell facilities to me et the requested humidity requirements, the system was incapable of maintaining these conditions 100 percent of the time. SwRI was typically able to maintain absolute humidity during testing within the desired range 95 percent of the time. It should be

n oted that in cases where outdoor ambient conditions were rapidly changing, the system was not able to meet the 95

- percent target. SwRI flagged these tests in the test log and provided a humidity quality check metric within each individual test file. Test s where humidity was outside the desired range for more than five percent of the time were reviewed with EPA and NREL, who provided guidance to SwRI regarding whether or not an individual test should be repeated. Under Phase 1 of the program, SwRI determi ned and verified PM sample flow rates that provide d proportionality. Those same flow rates were used for Phase 3 . The CVS blower was kept on for approximately 20 minutes before each emission test in an effort to ensure tunnel stability.

2.4.1 Test Matri x
The test matrix was designed to be randomized for each vehicle/fuel combination. Duplicate tests were conducted “back

- to

- back”, with the option for a third test based on repeatability criteria as detailed below. During the first nine weeks of testing , EPA specified vehicle/fuel assignments in an effort to determine the necessary amount of conditioning to allow a vehicle’s fuel control system to adapt to a new ethanol concentration. This involved switching vehicles back and forth between E0 and higher ethanol concentration blends. Development of the vehicle conditioning procedure is discussed in further detail in Section 2.4.3. Once this issue was resolved, vehicle/fuel assignments were made randomly using an EPA

- provided algorithm.

Testing started with five E0 fuels as shown in Table 6 . Additional fuels were added to the test matrix based on both the requirements of the vehicle conditioning study and on fuel availability. All fuels were available and included in the random matrix s tarting in the 12 th 

### week of testing. Due to funding constraints, only ten vehicles were included in the original test matrix. Two additional vehicles were added to the matrix in the 25 th 

### week of testing, and three additional vehicles were added in the 37 th 

### week of testing.SwRI R eport 03.15777 .01 (Rev 1) 

### 15 of 26 TABLE 6 . INCREMENTAL ADDITION OF FUELS AND VEHICLES TO THE TEST MATRIX

PHASE 3

WEEK FUELS ADDED VEHICLES a ADDED VEHICLE/FUEL ASSIGNMENTS

Week 1 2, 7, 8, 9 and 15 CCOB, TCAM, FEXP, DCAL, HODY

EPA Week 2 None CSIL, TSIE, DLIB, HCIV, NALT Week 3 None None Week 4 1, 12, 13 None Week 5 None None Week 6 22, 24 None Week 7 None None Week 8 3, 4, 5, 11, 14, 16, 20, 21, 23, 30 None Week 9 None None Week 10 None None Random for rest of
program , except for E85 Week 12 6, 10, 25, 26, 27, 28, 31 None Week 25 None FFOC, SOUT Week 37 None CIMP, F150, TCOR Week 55 29 (E85) DCAR Last fuel tested Week 60 End of Phase 3 testing

a

- Vehicle designations are explained in Table 3



### Each vehicle/fuel combination was tested at least twice. After two tests were completed and the acquired data passed all quality control verifications, the need for a third test was determined by following the variability criteria shown in Table 7 . If th e ratio of any of the criteria pollutants (THC, NO X 

### , or CO 2 

### ) on a pair of tests for a given vehicle/fuel combination exceeded the levels shown in Table 7 , a third test was conducted. The need for a third test was flagged in the daily test log.

TABLE 7

. REPEATABILITY CRITER IA FOR TRIPLICATE TE STING

DILUTE GASEOUS EMISSION CRITERIA FOR REQUIRI NG A THIRD TEST (COMPOS ITE CYCLE EMISSIONS)
CO 2 

### Ratio of higher / lower > 1.03
NO X 

### Ratio of higher / lower > 2.7
THC Ratio of higher / lower > 2.0

In addition to emissions repeatability criteria, the following criterion was used to trigger a review of the information related to the cranking events to determine if an additional replicate test was necessary for a given vehicle/fuel combination:

abs( cr anking time in test 1

- cranking time in test 2) > 1 sec

These flagged tests were reviewed with EPA and NREL, who provided guidance on the need for additional tests.SwRI R eport 03.15777 .01 (Rev 1) 

### 16 of 26 2.4.2 Drift Checks

The test program included drift checks that were conducted at the beginning, midpoint, and end of the Phase 3 test matrix. Due to concerns at the beginning of Phase 3 about vehicles properly adapting to different ethanol contents, the drift check procedure was modified. In a best attempt to ensure that the test vehicle s were similarly adapted during start

- , mid

- , and end

- point testing, the test matrix was manipulated so the immediate history prior to mid

- and end

- point testing was substantially similar to that at the beginning of Phase 3.

Specifically, all vehicles were operated on two successive E0 fuels for the first three weeks of testing, which had been immediately preceded by operation on an E20 fuel at the end of Phase 2 of the program. The second E0 fuel for each vehicle was designated as the drift check fuel. With the assistance of EPA, SwRI scheduled mid

- and end

- point testing to be immediately preceded by an E20 or E15 fuel and then an E0 fuel with properties substantially similar to the first Phase 3 fuel on which each vehicle was tested.

Due to the scheduling of end

- point drift checks, five of the original ten vehicles completed testing during Week 34, while the remainder of the original ten vehicles completed testing during Week 37. (Note that the Ford Explorer did not complete end

- point tes ting until much later in the program due to a MIL issue described in Section 3.2.)

2.4.3 Vehicle C onditioning

The vehicle fuel change and conditioning procedure used at the beginning of the program had been developed during the conduct of Phases 1 and 2. However, as EPA analyzed the data from Phases 1 and 2, they determined that the conditioning sequence was not sufficient for one of the vehicles to fully adapt to a new ethanol concentration following a switch from an E20 fuel to an E0 fuel . Therefore , the beginning of Phase 3 included a study to reassess the vehicle conditioning procedure. Long

- term fuel trim (LTFT) and short

- term fuel trim (STFT) were monitored during the conduct of successive two

- phase LA

- 92 test cycles and were analyzed by EPA for stabilization. Based on the results of this study, all vehicles were conditioned with three successive two

- phase LA92s except for the CCOB, NALT, HCIV, HODY, and TCAM , which were all conditioned with five successive two

- phase LA92s starting in the third week of testing. Prior to the third week, all vehicles were conditioned with three LA92s. The final vehicle fuel change and conditioning sequence is given in Table 8 . OBD data, including LTFT and STFT, were collected during all conditioning runs and were loaded onto the program file transfer site on a daily basis so that they could be accessed and reviewed by EPA and NREL . Example test requests for vehicle conditioning and testing are given in Appendix H

.SwRI R eport 03.15777 .01 (Rev 1) 

### 17 of 26 TABLE 8 . FUEL CHANGE, CONDITIO N ING, AND TEST EXECUTION SEQUENCE

STEP DESCRIPTION 1 Drain vehicle fuel completely via fuel rail whenever possible. When switching to E85 only, drive vehicle to fully warm up engine. 2 Turn vehicle ignition to RUN position for 30 seconds (60 seconds when switching to E85) to allow controls to allow fuel level reading to stabilize. Confirm the return of fuel gauge reading to

zero. 3 Turn ignition off. Fill fuel tank to 40% with next test fuel in sequence. Fill

- up fuel temperature
must be less than 50°F. 4 Start vehicle and execute catalyst sulfur removal procedure described in Appendix C of CRC E

60 Program report. Apply side fan cooling to the fuel tank to alleviate the heating effect of the exhaust system. Engine oil temperature in the sump will be measured and recorded during the sulfur removal cycle. 5 a 

### Perform four vehicle coast downs from 70 to 30 mph, with the last two measured. If the individual run fails to meet the repeatability criteria established in Phases 1 and 2 of th e program, the vehicle will be checked for any obvious and gross source of change in the vehicle’s mechanical friction. 6 Drain fuel and refill to 40% with test fuel. Fill

- up fuel must be less than 50°F. 7 b 

### Drain fuel again and refill to 40% with test fuel. Fill

- up fuel must be less than 50°F. 8 Soak vehicle for at least 12 hours to allow fuel temperature to stabilize to the test temperature. 9 c 

### Move vehicle to test area without starting engine. Start vehicle and perform three 2

- phase (bags 1 and 2 ) LA92 cycles. During these prep cycles, apply side fan cooling to the fuel tank to alleviate the heating effect of the exhaust system. Following the first two prep cycles, allow vehicle to idle in park for two minutes, then shut

- down the engine for 2

- 5 minutes. Following the last prep cycle, allow the vehicle to idle for two minutes, then shut down the engine in preparation for the soak. 10 Move vehicle to soak area without starting the engine. 11 Park vehicle in soak area at proper temperature (75 °F) for 12

- 36 hours. During the soak period, maintain the nominal charge of the vehicle’s battery using an appropriate charging device. 12 Move vehicle to test area without starting engine. 13 Perform LA92 cycle emissions test. 14 Move vehicle to soak area without starting the engine. 15 Park vehicle in soak area of proper temperature for 12

- 36 hours. During the soak period, maintain the nominal charge of the vehicle’s battery using an appropriate charging device. 16 Move vehicle to test area without starting the engine. 17 Perform LA92 emissions test. 18 Determine whether third replicate is necessary, based on data variability criteria (see Table 6 ). 19 If a third replicate is required, repeat steps 14, 15, 16 and 17. 20 If third replicate is not required, return to step 1 and proceed with next vehicle in test sequence.

a

– Vehicle coastdown repeatability criteria referred to in Step 5 were provided by EPA as follows:



### • maximum difference of 0.5 seconds between back

- to

- back coastdown runs from 70 to 30 mph



### • maximum ±7 percent difference in average 70 to 30 mph coastdown time from the running average for a given vehicle b

– Some vehicles received only two fuel drains and fi lls, i.e. Step 7 was skipped. See section 3.4 for details.

c

– Conduct five 2

- phase LA92 test cycles for the following vehicles: CCOB, NALT, HCIV, HODY, and TCAM.SwRI R eport 03.15777 .01 (Rev 1) 

### 18 of 26 2.4.4 Chassis Dynamometer

All tests were conducted using a Horiba 48

- inch single

- roll electric chassis dynamometer. A single test site and a single test driver were used for this entire program. Different drivers were used for sulfur purges and vehicle conditioning. The dynamome ter electrically simulates inertia weights up to 12,000 lb over the FTP test cycle , and provides programmable road load simulation of up to 150 hp continuous at 65 mph.

Chassis dynamometer settings were derived from target road load coefficients as repor ted in EPA’s on

- line Test Car List Data Files. Target road load coefficients and subsequently

derived chassis dynamometer settings were approved by EPA prior to the initiation of testing (Table 9 ).

TABLE 9 . VEHICLE CHASSI S DYNAMOMETER SETTINGS

2.5 Regulated and Unregulated E missions

The emissions measured and reported were THC, NMHC (by FID), NMOG, NO X 

### , NO 2 

### , CO, CO 2 

### , PM, alcohols, carbonyl compounds, and speciated hydrocarbons. Details on measurement accuracy and precision, sampling and analytical methods, sample handling and custody, equipment, calibrations, and quality control are provided in Appendix I

.

Gaseous emissions were determined in a manner consistent with EPA prot ocols for light

duty emission testing as given in the CFR
, Title 40, Part 86. A constant volume sampler was used to collect proportional dilute exhaust in Kynar bags for analysis of carbon monoxide (CO), carbon dioxide (CO 2 

### ), total hydrocarbons (THC), met hane (CH 4 

### ), and oxides of nitrogen (NO X 

### )

. For the determination of particulate matter (PM) mass emissions, a proportional sample of dilute exhaust was drawn through Whatman Teflon membrane filters . The PM sampling method was compliant to CFR
, Title 40, P art 1065. A, lbs B, lbs/mph C lbs/mph 2 A, lbs B, lbs/mph C lbs/mph 2
2008 GM Chevrolet Cobalt CCOB 3,125 21.51 0.5409 0.01521 4.22 0.20100 0.017055 11.5 2008 GM Chevrolet Impala FFV CIMP 3,875 19.87 0.4397 0.01752 8.320 0.11210 0.018601 11.4 2008 GM Saturn Outlook SOUT 5,000 38.61 0.3921 0.02818 19.860 0.07430 0.030294 17.2 2008 GM Chevrolet C1500 Silverado FFV CSIL 5,500 28.80 0.8005 0.03219 18.130 0.31630 0.035662 19.9 2008 Toyota Toyota Corolla TCOR 2,875 22.10 0.1500 0.01886 8.080 -0.02580 0.020902 10.2 2008 Toyota Toyota Camry TCAM 3,625 29.16 0.1659 0.01844 10.110 -0.15630 0.019592 11.1 2008 Toyota Toyota Sienna TSIE 4,500 38.41 0.0249 0.02946 16.270 -0.12110 0.029718 15.1 2008 Ford Ford Focus FFOC 3,000 27.66 0.2892 0.01697 15.240 0.07660 0.018743 11.3 2008 Ford Ford Explorer FEXP 4,750 32.35 0.6076 0.02716 14.350 0.43360 0.028153 17.4 2008 Ford Ford F150 FFV F150 5,250 27.26 0.9495 0.02932 4.300 0.83540 0.029383 19.7 2008 Chrysler Dodge Caliber DCAL 3,500 52.75 -0.3153 0.02826 15.990 -0.20400 0.025692 14.4 2008 Chrysler Dodge Caravan FFV DCAR 4,750 35.94 0.6505 0.02155 18.470 0.30710 0.023981 16.3 2008 Chrysler Jeep Liberty JLIB 4,250 29.53 0.4040 0.02955 9.410 0.13330 0.031781 16.5 2008 Honda Honda Civic HCIV 3,000 23.18 0.1904 0.01699 8.120 0.05150 0.017724 10.0 2008 Honda Honda Odyssey HODY 4,750 28.70 0.6915 0.02167 11.170 0.24850 0.024710 15.7 2008 Nissan Nissan Altima NALT 3,500 47.47 -0.4531 0.02414 19.710 -0.30660 0.021358 11.4 ROAD LOAD HP @ 50 mph ETW,

lbs SET COEFFICIENTS TARGET COEFFICIENTS
NAME MODEL YEAR MAKE BRAND MODELSwRI R eport 03.15777 .01 (Rev 1) 

### 19 of 26 In addition to the dilute, bagged exhaust samples, continuous raw exhaust mass emissions rates were measured on a second

- by

- second basis for THC, CH 4 

### , CO, NO X 

### , CO 2 

### and O 2 

### at the tailpipe. These measurements were performed during the first test of each vehicle/fuel combination at a sampling frequency of 1 Hz. Dilution air flow was measured with a smooth approach orifice, and a critical flow ventur i measured bulkstream dil ute exhaust flow. Measured dilution air flow was subtracted from the bulkstream flow to calculate raw exhaust flow to determine continuous raw mass emission rates.

Additionally, select alcohols and carbonyls were measured during emission tests. The

mea surement of alcohols in exhaust was accomplished by bubbling the exhaust through glass impingers containing deionized water after which samples were analyzed by gas chromatography. An HPLC procedure was utilized for the analysis of carbonyls. Samples wer e collected using DNPH cartridges and were extracted with acetonitrile. S peciated hydrocarbons were determined by gas chromatography.

Exhaust emissions were measured as shown below.

CONSTITUENT ANALYSIS METHOD Total Hydrocarbon Heated Flame Ionization Detector (bag, modal) Methane Gas Chromatography (bag , modal ) Carbon Monoxide Non

- Dispersive Infrared Analysis (bag, modal) Carbon Dioxide Non

- Dispersive Infrared Analysis (bag, modal) Oxides of Nitrogen Chemiluminescence Analysis (bag, modal) Nitric Oxide Chemiluminescence Analysis (bag only) Oxygen Magnetopneumatic Detector (modal only) Particulate Matter Part 1065 Gravimetric Measurement (bag only) N on

- methane Hydrocarbons Calculated from THC and CH 4 

### (bag, modal) N on

- methane O rganic G ases Calculated as specified in Section 2.5.2 (bag only ) N itrogen D ioxide Calculated from difference of NO X 

### and NO (bag only) C 1 

### – C 12 

### HC Speciation Gas Chromatography (bag only) Alcohols Gas Chromatography (bag only) Carbonyls Liquid Chromatography (bag only)

During Phases 1 and 2 of the test program, continuous raw NH 3 

### measurements were made. Results showed NH 3 

### spikes of several hundred ppm during testing of many vehicles. These concentrations were sufficient to cause poising of the NO 2 

### - to

- NO converter in the continuous raw NO X 

### analyzer. In an attempt to minimize this problem, prior to the start of Phase 3 SwRI installed two NH 3 

### adsorbers in series upstream of the continuous raw emission measurement sample train. These adsorbers were changed daily. Additionally, the NO 2 

### - to

- NO converter was purged with 5,000

- ppm (nominal) NO X 

### for five minutes following every test in an effort to reverse any NH 3 

### poising of the converter that may have occurred during testing. The NO X 

### analyzer was then purged fo r another three minutes with zero nitrogen prior to initiating the normal pre

- test zero

- span sequence.SwRI R eport 03.15777 .01 (Rev 1) 

### 20 of 26 2

. 5

. 1 S peciation of Volatile Organic Compounds

Phase

- level (bag

- by

- bag) speciated volatile organic compounds ( VOCs ) included C 1 

### - C 12 

### hydrocarbons
, light alcohols, aldehydes, and ketones. S ampling and analysis of C 2 

### - C 12 

### hydrocarbons was conducted in a manner similar to CARB method 1002/1003, “Procedure for the Determination of C 2 

### - C 12 

### Hydrocarbons in Automotive Exhaust Samples by Gas Chromatography”. Sampling and analysis of alcohols was done in a manner similar to CARB method 1001, “Determination of Alcohols in Automotive Source Samples by Gas Chromatography”. Sampling and analysis of carbonyl compounds was conducted in a manner similar to CARB meth od 1004, “Determination of Aldehyde and Ketone compounds in Automotive Source Samples by High Performance Liquid Chromatography”. A nalysis of C 2 

### - C 4 

### HC samples was conducted within one hour of completion of an emissions test. Subsequent analysis of the additional compounds of interest was done within 4 hour s of emission test completion.

During the analysis of C 2 

### - C 4 

### hydrocarbons, special consideration was given to 1,3

- butadiene. Because of the instability of 1,3

- butadiene, the analysis of C 2 

### - C 4 

### hydr ocarbon samples collected during Bag 1 of a test cycle was initiated within one hour of collection. The speciation of C 5 

### - C 12 

### hydrocarbon samples collected in Bag 1 of the test cycle was completed within 4 hours of collection.

Sampling and analysis of light alcohols was accomplished b y bubbling exhaust through glass impinge rs containing deionized water, and samples were analyzed with a gas chromatograph. Analysis included the following compounds: methanol, ethanol, isopropanol, and n

- propanol. Alcohol samples were sealed and stored at a temperature below 40 o 

### F immediately following collection. Most of these samples were analyzed on the day they were collected, but no later than within six calendar days.

Samples of carbonyl compounds were collected in cartridge type samplers. These samples were extracted immediately following collection (within 15 minutes) and the extracts sealed and stored immediately at a temperature below 40 o 

### F. Most of these extracts were analyzed on the day they were collected, bu t no later than within three calendar days. An effort was made to detect the presence of a tautomer of acrolein
, acrolein

- x, which can be a measurement artifact. No acrol ei n

- x was found in any exhaust sample.

Storage of alcohol and carbonyl samples was segregated to prevent any cross

contamination of samples.

The speciation schedule was conducted as shown in Table 10 . Alcohols and carbonyls were determined during Bag 1 for all tests. In addition, Bag 1 C 1 

### - C 12 

### speciation was performed on the first test of all vehicles while operating on Fuels 3, 4, 6, 7, 10, 13, 14, 21, 23, 27, 28, and 31 . For the Honda Civic, Toyota Corolla, Chevrolet Impala, Ford F150 , and Chevrolet Silverado
, three

- bag speciation was conducted with these fuels on th e first test

. Three

- bag speciation was also conducted on all E85 tests.SwRI R eport 03.15777 .01 (Rev 1) 

### 21 of 26 TABLE 10 . V OC SPECIATION SCHEDULE

Test Phase (Bag) Test Repeat Test 1 Test 2 Test 3 (If Needed) Fuel Set A a Fuel Set B b E85 Fuel c Fuel Set A a Fuel Set B b E85 Fuel c Fuel Set A a Fuel Set B b E85 Fuel c

1 Alcohols Carbonyls C 1 - C 12 Speciation Alcohols Carbonyls C 1 - C 12 Speciation Alcohols Carbonyls Alcohols Carbonyls C 1 - C 12 Speciation Alcohols Carbonyls C 1 - C 12 Speciation Alcohols Carbonyls Alcohols Carbonyls C 1 - C 12 Speciation d Alcohols Carbonyls C 1 - C 12 Speciation Alcohols Carbonyls

2 none C 1 - C 12 Speciation e e

Alcohols e Carbonyls e C 1 - C 12 Speciation Alcohols Carbonyls none C 1 - C 12 Speciation d ,e Alcohols d ,e Carbonyls d ,e C 1 - C 12 Speciation Alcohols Carbonyls none C 1 - C 12 Speciation d ,e Alcohols d ,e Carbonyls d ,e C 1 - C 12 Speciation Alcohols Carbonyls

3 none C 1 - C 12 Speciation e e

Alcohols e Carbonyls e C 1 - C 12 Speciation Alcohols Carbonyls none C 1 - C 12 Speciation d ,e Alcohols d ,e Carbonyls d ,e C 1 - C 12 Speciation Alcohols Carbonyls none C 1 - C 12 Speciation d ,e Alcohols d ,e Carbonyls d ,e C 1 - C 12 Speciation Alcohols Carbonyls

a

– Fuel Set A: Fuels 1, 2, 5, 8, 9, 11, 12, 15, 16, 20, 22, 24, 25, 26, & 30 b

– Fuel Set B: Fuels 3, 4, 6, 7, 10, 13, 14, 21, 23, 27, 28, & 31

c

– Three

- bag speciation conducted on all E85 tests d

– C 1 - C 12 speciation conducted only if results from Test 1 were void

e

– Only the Honda Civic, Toyota Corolla, Chevrolet Impala, Ford F150, and Chevrolet Silverado received three

- bag speciation



### The following daily sequence was used for the analysis of VOC samples:

**•** VOC samples collected during Bag 1 of the test cycle were analyzed first, in the sequence of vehicle tests.

**•** If a vehicle requiring VOC sampling during all three bags of the test cycle was t ested, the Bag 1 was analyzed first, followed immediately by the Bag 3 sample and finally by the Bag 2 sample.

**•** Background samples were analyzed last, in the sequence of vehicle tests.

2

. 5

. 2 Determination of NMOG

An EPA

- provided protocol for calculating NMHC and NMOG (Appendix J ) was followed. Bag

- level NMHC and NMOG were calculated for all bags where the required measurements were available. In cases where one or more components of the bag

- level NMHC and NMOG calculation were n ot measured (for example, when alcohols and carbonyls were not measured in Bags 2 and 3), bag

- level NMHC and NMOG mass emissions were calculated assuming the missing measurements were below method detection limits. These bag

- level NMHC and NMOG calculatio ns were then used to calculate composite weighted NMHC and NMOG mass emissions.

During the early conduct of Phase 3, SwRI observed media interferences that impacted our limits of detection (LOD) and limits of quantification (LOQ) for alcohols and carbony ls. In conjunction with EPA and NREL, SwRI developed an LOD/LOQ determination method which accounted for these media interferences (Appendix K ).SwRI R eport 03.15777 .01 (Rev 1) 

### 22 of 26 2.6 OBD Data

Additional available data were acquired at 1 Hz from each vehicle’s onboard diagnostic (OBD) system during all emissions tests using a DBK70 data acquisition system. The data, when available, included:

**•** RPM

**•** Vehicle speed

**•** Engine load

**•** Short term fuel trim

- bank 1

**•** Long term fuel trim

- bank 1

**•** MIL status

**•** Absolute throttle position

**•** Engine coolant temperat ure

**•** Short term fuel trim

- bank 2

**•** Long term fuel trim

- bank 2

**•** Fuel/air commanded equivalence ratio

**•** Alcohol fuel percent (if available)

**•** Manifold absolute pressure

**•** Spark advance

**•** PID $42 Control Module Voltage

**•** Air flow rate from mass air flow sensorSwRI R eport 03.15777 .01 (Rev 1) 

### 23 of 26 3.0 ISSUES ENCOUNTERED W HILE TESTING

3.1 Ford Explorer Low Oil Level

At one point during the course of the program, 20 ounces of crankcase lubricant had to be added to the sump. This issue is detailed in Section 2.3.1.

3.2 Ford Explorer E vaporative System MIL

During the 27 th 

### week of testing, the Ford Explorer illuminated a malfunction indicator light (MIL

– a.k.a. “check engine light”) for diagnostic trouble code (DTC) P 0 455

- Evaporative Emission System Leak Detected (Gross L eak/ No flow) . This star ted a series of troubleshooting events that are summarized in Table 11 . On

- road test ing seemed to indicate that code was not due to the fuel change procedure or operation of the vehicle on the chassis dynamometer. Following extensive discussions that inc luded Dominic DiCicco of Ford, the team decided that the MIL would not have an adverse affect on emissions testing, and the vehicle was placed back into the test matrix.

TABLE 11 . TROUBLESHOOTING OF THE F ORD EXPLORER EVA P OR AT IVE SYSTEM MIL

DATE ACTION

9/16/2009 Fuel change to E20 Fuel 31; key off

9/17/2009 MIL light during vehicle conditioning, E20 Fuel 31; PO455

- Evaporative Emission System Leak Detected (Gross Leak/ No F low)
9/23/2009 Vehicle sent to dealer; performed a smoke test; Canister vent solenoid replaced

9/26/2009 Fuel change to E20 Fuel 21; key off

9/27/2009 MIL light during vehicle conditioning, E20 Fuel 21; PO455

- Evaporative Emission System Leak Detected (Gross Leak/ No F low)
10/5/2009 Vehicle sent to dealer; performed a smoke test ; capless fuel filler door was cleaned as it had dirt and grime

10/12/2009 Fuel change to E20 Fuel 21; key off

10/13/2009 MIL light during vehicle conditioning, E10 Fuel 12; PO455

- Evaporative Emission System Leak Detected (Gross Leak/ No F low)
10/16/2009 SwRI performed an IDS test and a smoke test and a leak test by pressurizing the evap system and found no leaks.

10/26/2009 FEXP was taken to the test track where we ran 9 WOT up to 70 mph. The MIL did not light. The next day we ran through the three LA 9 2 (2

- bag) prep sequence on the dyno. The MIL did light approximately 500 seconds (~24 miles) into the third LA 92. This means the fuel change procedure is probably not the cause for the MIL.

10/28/2009 Vehicle was driven on road approximately 50 miles. Pending code P0422, but no MIL light

11/20/2009 Vehicle sent to the dealer; The EVAP system was smoke tested and the capless fuel assembly was replaced. I was told that the technician drove the vehicle for more than 10 miles to confirm that the code did not reappear.
11/21/2009 Fuel change to E15 Fuel 28; key off

11/22/2009 MIL light during vehicle conditioning, E15 Fuel 28; PO455

- Evaporative Emission System Leak Detected (Gross Leak/ No F low)

12/1/2009 Dealership performed IDS Diagnosis, PO455 code. EVAP test found capless retainer broken. Replaced retainer and retested ok.

12/8/2009 MIL light during vehicle conditioning, E15 Fuel 28; PO455

- Evaporative Emission System Leak Detected (Gross Leak/ No F low)SwRI R eport 03.15777 .01 (Rev 1) 

### 24 of 26 Following Phase 3 testing, SwRI performed additional evaporative system l eak check s with an IDS scan tool per instructions given by Ford, and the data files were forwarded to Ford for review. Subsequent coordination among SwRI, Ford, and our local Ford dealership allowed
us to determine that the FTP sensor had an internal fault causing the sign al to become erratic during vehicle operation , after which the vehicle was repaired.

3.3 Saturn Outlook Transmission M odule M alfunction

A MIL illuminated during the second test of Fuel 16 with the Saturn Outlook. The diagnostic trouble codes (DTCs) were Tran Control Sys Malfunction and U0073

- Control Module Comm. Bus Off. The same codes illuminated while operating the vehicle on the mileage accumulation dynamom eter during the initial vehicle break

- in. At that time, the vehicle was taken to the dealership where the codes were cleared. The vehicle was driven 10 miles but the codes did not reappear. The Saturn Outlook then completed mileage accumulation and was t ested on six fuels in Phases 1 and 2.

Review of the emissions results from the two test s on Fuel 16 did not show a significant difference. With EPA’s and NREL’s approval, the codes were cleared and the vehicle was placed back into the test program. Fou r days later, the MIL came on again during testing, with the same DTCs. This time the driver noticed that the vehicle’s engine was revving higher than usual at cruising speeds and shifting hard during the first two bags. Bag 3 did not have the same issue s. With EPA’s and NREL’s approval, the vehicle was taken to the dealer for diagnosis, but they were not able to find any problems. There was concern that the DBK system used to collect OBD data may have somehow been interfering with proper vehicle operat ion. The next set of tests was conducted without OBD data acquisition, and the MIL did not illuminate. All subsequent tests were conducted without OBD data acquisition, and the MIL did not illuminate.

3.4 Fuel C arryover
On May 27, 2009, SwRI noticed a n issue with results for the Nissan Altima tested on Fuel 13. Fuel 13 was an E0 fuel, yet w e found low level s of ethanol in exhaust samples from both tests

. We checked the original fuel sample from the drum used to fuel the vehicle, and also pulled a sam ple from the vehicle . Both samples were tested with the Petro S pec portable gasoline analyzer . The drum sample showed no ethanol and the vehicle's fuel tank showed 1.5 wt % ethanol. This suggested fuel carryover in the Altima . This sample was sent to EPA for analysis by ASTM D5599 method and was found to contain 1.44 vol % of ethanol , equivalent to a fuel carryover rate of 7.2% following two drains and 40 % fills. This ethanol concentration indicate d that approximately 3 gallo ns of the previous fuel remain ed in Altima’ s tank after it has been drained via the fuel rail. From this point forward, except for mid

- and end

- point tests, the Altima received three fuel flushes during the fuel change sequence.

SwRI checked the rest of the P hase 3 results for the Altima, Camry, Odyssey, and Civic. All vehicles showed measurable levels of ethanol when testing with an E0 fuel that was immediately preceded by an E20 fuel.SwRI R eport 03.15777 .01 (Rev 1) 

### 25 of 26 To better understand this situation, SwRI collected fuel samples during tests leading up to mid

- point testing, when all vehicles changed from an E15/E20 fuel to an E0 fuel. S w RI’s and EPA’s analyses of ethanol content in the samples by D5599 indicated tha t the following percentages of the previous fuel were retained in the tanks of the test vehicles following fuel change s which included two drains and 40 % fills :

**•** Honda Odyssey: 8.8 vol %

**•** Toyota Sienna: 5.0 vol %

**•** Honda Civic: 4.2 vol %

**•** Nissan Altima: 6.1 vol %

**•** Toyota Camry: 5.3 vol%

**•** All r emaining vehicles: 2.1 vol % to 3.2 vol %

Based on these results, EPA and NREL directed SwRI to p repare several 95%/5% and 5%/95% blends of the test fuels with the most extreme combinations of distillation properties and ethanol content to determine the effect of 5% fuel carryover on T50, T90 and RVP. The fuel sampling procedure used during these experiments is given in Appendix L , while the test matrix is given in Appendix M

.

Because the two results from the Altima ha d such a wide spread (3.7% vs. 7.2%), SwRI performed additional refueling experiments with the Altima, Odyssey, Camry, Civic, and Sienna to determine the variability of fuel carryover measurements. These experiments showed that a third fuel flush was effe ctive in reducing fuel carryover to less than one percent. The procedure and results are given in Appendix N . Based on these results, starting on August 1, 2010, SwRI incorporated a third fuel drain and fill into the vehicle change procedure for the Alti ma, Odyssey, Sienna, Civic, and Camry

. Fuel carryover was characterized for the Focus, Outlook, Impala, F

- 150, and Corolla before they were added to the test matrix. Based on results, these five vehicles received triple drains and fills during fuel chan ges.
As part of the investigation into fuel carryover, EPA was interested in the impact of different refueling locations on in

- tank fuel carryover. Starting in August 2009, all vehicles were refueled in an assigned location. However, e arly in the condu ct of Phase 3, refueling of a test vehicle may have occurred in one of two locations. Each location was sloped in a different direction, which may have affected the amount of fuel remaining in a vehicle’s tan k after being drained. These additional refueling experiments were conducted with the Silverado
, Camry
, Sienna
, Caliber
, Civic
, Odyssey , and Altima . They involved collecting fuel samples at the two different refueling locations while changing between and E0 and an E20 fuel. The test procedure is given in Appendix O . The results of these experiments were provided to EPA for further analysis.SwRI R eport 03.15777 .01 (Rev 1) 

### 26 of 26 4.0 CLOSURE

SwRI conducted exhaust emission testing of fifteen light

- duty vehicles operating on twenty

- seven test fuels with ethanol contents ranging from 0 to 20 percent by volume and four light

- duty flexible fuel vehicles (FFVs) operating on an E85 fuel , as part of Phase 3 of the EPAct/V2/E

- 89 test program. Vehicle testing for this phase of the program was car ried out between March 2009 and June 2010. This work was conducted for the Environmental Protection Agency (EPA), the National Renewable Energy Laboratory (NREL) and the Coordinating Research Council (CRC) and was authorized by EPA Contract EP

- C

- 07

- 028
, Work Assignments 1

- 03
, 2

- 03 and 3

- 01 , and NREL Subcontract No s

. ACI

- 8

- 88613

- 01, AFT

- 9

- 99319

- 01 and AFT

9

- 99155

- 01

. All test results have been posted on SwRI’s secure file transfer site to which both EPA and NREL have access.

## APPENDIX A

FUEL CHANGE PROCEDURE

### 2 of 3 

### Fuel Change Procedure / Coastdown Sequence

Date: Vehicle: Chevrolet Impala FFV : EPA-CIMP



### Test #: EPA-CIMP-P3-27-3FC Fuel #: 27

First Fuel Change



### □ With key off, drain fuel from vehicle



### □

□ drain until fuel flow drops off. Stop drain immediately

. DO NOT OVERDRAIN.



### □

□ Turn ignition key off.



### □ Locate fuel drum:

EPA Fuel No. 27 SwRI Fuel Name BOS SwRI Fuel Code EM-7095-F 

### Drum No 

### EPAct Test Fleet 03.14936.03.202

Tuesday, January 19, 2010

After first 1 minute of drain, fill a 4 oz. sample bottle from the plastic drain tube and label bottle as instructed by supervisor or project leader.

Turn ignition to run position for 30 seconds allowing fuel gauge level to stabilize. Confirm fuel level reads zero. If gage does not read zero, use the Bosch scan tool to verify fuel level.

Page 1 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace 

### Drum No



### . (Record Drum Number) Verify fuel fill drum matches using “2-person rule”

Initials: _________, _________

Verify fuel temperature: __________ should be 45 ± 2 °F



### □ Fill tank with 6.8 gallons of fuel. Record time ___________.



### □ Record fuel information from box above on vehicle windshield.



### □ Place fuel drum back into cold box.



### □ PUSH vehicle into lab within 10 minutes of refueling. Record time __________.



### □ Install vehicle on Dyno. Record drive wheel tire pressures. RT_____ LF_____.



### □

□ Place cooling fans to cool the exhaust. Connect the correct transfer pipe to the vehicle and run out the roof with flex pipe.

Page 1 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace

### 2 of 3 

### Fuel Change Procedure / Coastdown Sequence

Date: Vehicle: Chevrolet Impala FFV : EPA-CIMP



### Test #: EPA-CIMP-P3-27-3FC Fuel #: 27



### □ Dyno computer setup procedure



### □ Horiba trace setup procedure



### □

□

□ Run the sulfur purge procedure described on the last page.



### □ Record sulfur purge completion time. _______________



### □ EPAct Test Fleet 03.14936.03.202

Tuesday, January 19, 2010

Connect thermocouple #1 to record oil temperature.

Start the vehicle. Idle in neutral. Using the OBD scan tool, read and record the long term fuel trim

Place vehicle in neutral with engine idling. Using the OBD scan tool, read and record the long term fuel trim

Page 2 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace 

### □

□ Coast down 1.



### □ Coast down 2.



### □ Coast down 3, print.



### □ Coast down 4, print.



### □

□ Remove vehicle from dyno and move to the fuel drain area. g



### Within 5 minutes of completing the sulfur purge procedure begin coast downs. Use the speed range from 70 - 10 mph and record in 5 mph increments.

Type the coastdown data from runs 3 and 4 into the coastdown analysis Excel program. If the program notes a repeatability failure, check for incorrect inputs. If repeatability cannot be accomplished, remove vehicle and begin fuel change procedure on backup vehicle and notify supervisor. If test repeatability is indicated OK, continue with this procedure.

Page 2 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace

### 2 of 3 

### Fuel Change Procedure / Coastdown Sequence

Date: Vehicle#: Chevrolet Impala FFV : EPA-CIMP



### Test #: EPA-CIMP-P3-27-3FC Fuel #: 27

Second Fuel Change



### □ Drain fuel from vehicle until flow drops off. Stop drain immediately. DO NOT OVERDRAIN.



### □

□ Locate fuel drum:

EPA Fuel No. 27 SwRI Fuel Name BOS SwRI Fuel Code EM-7095-F 

### Drum No. (Record Drum Number) Verify fuel fill drum matches using “2-person rule”

Initials: _________, _________ 

### EPAct Test Fleet 03.14936.03.202

Tuesday, January 19, 2010

Turn ignition to run position for 30 seconds allowing fuel gauge level to stabilize. Confirm fuel level reads zero. If gage does not read zero, use the Bosch scan tool to verify fuel level.

Page 3 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace 

### Verify fuel temperature: __________ should be 45 ± 2 °F



### □ Fill 

### tan k 

### w i 

### t h 

### 6.8 ga ll 

### ons o f f 

### ue l



### . R 

### ecor d 

### t i 

### me ___________.



### Note: For vehicles HODY, NALT, TSIE, HCIV, TCAM

#N/ A #N/ A #N/ A 

### These vehicles (only) require a third fuel change. If you are not working on one of these five vehicles, skip the third fuel change and return fuel drum to the cold box.

Page 3 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace

### 2 of 3 

### Fuel Change Procedure / Coastdown Sequence

Date: Vehicle#: Chevrolet Impala FFV : EPA-CIMP



### Test #: EPA-CIMP-P3-27-3FC Fuel #: 27

Third Fuel Change For Odyssey, Altima, Sienna, Civic, and Camry only.



### □ Drain fuel from vehicle until flow drops off. Stop drain immediately. DO NOT OVERDRAIN.



### □

□ Locate fuel drum: EPA Fuel No. 27 SwRI Fuel Name BOS SwRI Fuel Code EM-7095-F 

### Drum No. (Record Drum Number) Verify fuel fill drum matches using “2-person rule”

Initials: _________, _________ 

### EPAct Test Fleet 03.14936.03.202

Tuesday, January 19, 2010

Turn i g 

### nition to run p 

### osition for 30 seconds allowin g 

### fuel g 

### au g 

### e level to stabilize.

Page 4 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace 

### Verify fuel temperature: __________ should be 45 ± 2 °F



### □ Fill tank with 6.8 g 

### allons of fuel. Record time

___________ 

### .



### □ Place fuel drum back into cold box.



### □ PUSH vehicle into lab and park in 75° F soak area for at least 12 hours..

Lead Technician’s Signature:___________________________

Page 4 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace

### 2 of 3 

### Fuel Change Procedure / Coastdown Sequence

Date: Vehicle#: Chevrolet Impala FFV : 

### EPA-CIMP

Test #: EPA-CIMP-P3-27-3FC Fuel #: 27

SULFUR PURGE PROCEDURE



### □ idle 30 seconds

□ 55 mph 5 minutes

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 m p 

### h 

### 03.14936.03.202
Tuesday, January 19, 2010 

### EPAct Test Fleet

Page 5 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace 

### p



### □ hold speed 15 seconds

□ 30 mph 1 minute

□ idle 30 seconds

□ 55 mph 5 minutes

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration > 5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ WOT acceleration >5 seconds >70 mph

□ hold speed 15 seconds

□ 30 mph 1 minute

□ idle 30 seconds

Page 5 of 5 R:\03Projects\DEER\03-13363_EPA\Forms (Lab Check Lists)\2010 01-29\Fuel Change 2.xls Revised 12/01/2009. Julia DeGrace

## APPENDIX B

PETROSPEC RESULTS FO R INDIVIDUAL FUEL DR UMSTop/Bottom Drum No. Ethanol content (% vol) Aromatic content (% vol) T90 (°F) Fuel 1 Top 2 11.7 15.3 307 Top 3 11.6 15.6 308 Bottom 6 11.7 15.9 319

Top 7 11.7 15.8 321 Fuel 2 Top 3 0.0 15.4 294 Bottom 4 0.0 14.9 322

Top 5 0.0 15.1 325 Top 6 0.0 15.9 332 Top 7 0.0 15.3 327 Top 2 0.0 14.8 333 Top 8 0.0 16.7 332 Fuel 3 Top 4 12.0 15.6 314 Top 5 12.0 15.7 319 Bottom 6 12.0 15.8 324 Bottom 7 12.1 11.1 323

Top 2 12.0 15.6 315 Top 3 11.9 18.5 314 Fuel 4 Top 2 11.4 16.8 323 Top 3 11.3 16.7 326 Top 7 11.4 16.8 336 Top 5 11.4 17.1 332 Top 8 11.4 17.3 335 Fuel 5B Top 1 0.0 37.2 323 Fuel 5 Top 3 0.0 37.3 323 Bottom 5 0.0 42.0 307 Bottom 5 0.0 37.5 329

Top 4 0.0 41.8 304 Top 8 0.0 37.3 340 Bottom 7 0.0 37.6 332 Fuel 6 Top 4 12.3 16.7 323 Bottom 5 12.2 16.8 320

Top 3 12.3 16.3 315 Top 6 12.4 16.7 317 Fuel 7 Top 2 0.0 18.0 321 Top 3 0.0 18.2 321 Top 4 0.0 18.0 319 Top 1 0.0 16.7 321 Top 9 0.0 18.5 328 Top 7 0.0 18.2 328 Bottom 8 0.0 18.7 341

Top 5 0.0 18.8 323 Fuel 8 Top 2 0.0 17.0 320 Top 3 0.0 16.8 321 Top 4 0.0 16.7 326 Top 1 0.0 16.7 321 Top 7 0.0 17.0 331 Fuel 9 Top 2 0.0 35.8 327 Top 4 0.0 36.3 329 Top 3 0.0 36.0 333 Top 5 0.0 36.2 328 Top 1 0.0 34.9 331 Top 7 0.0 36.5 340 Top 8 0.0 36.5 344 Bottom 7 0.0 36.8 338 Updated 6/22/10 Petrospec Analysis on EPAct FuelsTop/Bottom Drum No. Ethanol content (% vol) Aromatic content (% vol) T90 (°F) Updated 6/22/10 Petrospec Analysis on EPAct Fuels

Fuel 10 Bottom 1 11.3 36.9 304 Top 1 11.2 34.9 331 Top 2 11.2 35.1 330 Bottom 3 11.2 35.0 331 Bottom 6 11.2 34.9 343 Bottom 7 11.2 35.1 337

Top 4 11.2 35.1 334 Fuel 11 Top 3 11.4 37.1 312 Top 1 11.3 36.9 304 Top 2 11.2 35.4 331 Top 6 11.4 37.4 315 Top 7 11.5 37.5 316 Fuel 12 Top 1 11.3 36.4 363 Top 7 11.3 35.6 348 Bottom 6 11.2 35.7 342

Top 4 11.3 36.1 331 Fuel 13 Top 2 0.0 36.5 354 Top 1 0.0 36.4 363 Top 3 0.0 37.0 354 Top 7 0.0 36.9 366 Top 4 0.0 37.0 351 Top 6 0.0 36.8 367 Fuel 14 Top 1 0.0 38.0 321 Top 2 0.0 18.2 324 Bottom 6 0.6 19.1 331 Bottom 7 0.0 17.7 332

Top 8 0.0 17.6 329 Bottom 4 0.0 18.2 336

Top 3 0.0 17.8 327 Top 7 0.0 18.5 331 Fuel 15 Top 2 0.0 38.0 334 Top 3 0.0 38.5 319 Bottom 4 0.0 37.9 324

Top 1 0.0 36.6 299 Top 8 0.0 36.4 336 Bottom 7 0.0 38.4 343

Top 9 0.0 38.6 337 Fuel 16 Top 2 11.8 36.8 295 Top 3 11.8 36.8 303 Top 1 11.8 36.6 299 Top 3 11.8 36.7 301 Top 5 11.8 36.8 307 Fuel 20 Top 2 19.4 17.0 320 Top 1 19.3 17.0 316 Top 4 19.5 17.4 324 Top 5 19.4 7.5 325 Fuel 21 Top 2 19.0 38.0 289 Top 1 19.0 37.8 289 Top 3 18.9 38.0 290 Top 5 19.0 38.3 303 Top 6 19.1 38.1 296 Top 8 19.0 38.1 305 Top 4 19.0 38.4 296 Top 9 18.9 38.2 300Top/Bottom Drum No. Ethanol content (% vol) Aromatic content (% vol) T90 (°F) Updated 6/22/10 Petrospec Analysis on EPAct Fuels

Fuel 22 Bottom 1 19.3 17.4 329 Top 1 19.3 17.0 329 Top 2 19.5 17.0 322 Top 3 19.4 16.9 321 Top 4 19.4 17.0 325 Bottom 7 19.2 17.7 322

Top 6 19.4 17.1 322 Top 8 19.4 17.4 333 Fuel 23 Top 2 19.5 17.5 325 Top 1 19.5 16.1 320 Bottom 6 19.3 18.7 341

Top 3 19.6 18.6 329 Top 2 19.5 18.5 329 Top 7 19.5 18.7 330 Fuel 24 Top 1 19.3 17.4 329 Top 2 19.5 17.5 325 Top 3 19.4 17.7 327 Bottom 4 19.5 17.7 324

Top 5 19.4 17.7 327 Top 8 19.3 18.1 337 Top 8 19.5 18.0 333 Fuel 25 Top 2 19.0 37.1 320 Bottom 3 19.2 37.0 321 Bottom 4 19.1 37.4 321

Top 5 19.0 37.4 323 Bottom 8 19.1 37.6 339 Bottom 9 19.1 37.4 325

Top 10 19.2 37.6 336 Fuel 26 Top 2 15.8 35.6 326 Top 3 15.8 35.4 323 Top 4 15.8 35.7 323 Top 7 15.8 36.0 339 Top 9 16.0 36.6 328 Fuel 27 Top 2 15.8 34.8 323 Top 3 15.8 16.1 319 Top 4 15.9 16.3 318 Bottom 6 16.0 16.6 320

Top 7 15.9 16.3 326 Fuel 28 Top 2 15.6 36.5 289 Top 3 15.8 36.2 293 Bottom 4 15.7 36.6 296

Top 6 15.7 36.5 307 Bottom 7 15.7 36.5 298 Bottom 8 15.7 36.5 309

Top 8 15.9 36.1 330 Top 9 15.6 36.4 300 Fuel 30 Top 1 11.2 37.2 329 Top 2 11.0 37.3 329 Top 3 11.2 37.2 330 Top 4 11.2 37.3 332 Top 5 11.2 37.7 332 Top 7 11.3 37.7 336 Fuel 31 Top 2 19.1 38.2 321 Top 3 19.2 38.6 324 Top 5 19.0 38.4 320 Bottom 6 19.1 38.5 322

Top 8 19.2 38.4 332

## APPENDIX C

DETAILS OF FORD F

- 150 MISFUELING EVENTSwRI R eport 03.15777 .01 

### C

- 1 Tuesday, March 9, 2010 The day

- shift ran the F150 on test F150

- P3

- 5

- T2. The night

- shift crew then performed a fuel change on the F150 during which the tank was drained and 10.6 gallons of Fuel 26 (Drum #5) were added. The vehicle was pushed onto the dynamometer where it was started and it idled very rough for 2 minutes before it was turned off and pushed off the dynamometer

. Wednesday, March 10, 2010 Five gallons of Fuel 26 (Drum #6) were put into the F150. To verify the fuel pump was working, the fuel line was removed from the fuel rail and a small amount of fuel was drained by energizing the fuel pump manually. The fuel pump worked correctly.

Friday, March 12, 2010 A fuel sample was pulled from the F150 and had the smell of gasoline and diesel. A PetroSpec analysis conf irmed the fuel contained some diesel. The fuel tank was drained and “extra Fuel 5” was added. The vehicle started after a few cranks and ran normally.

Wednesday, March 17, 2010 The fuel tank was removed from the F150 and it was wiped clean by removing the fuel sending unit. The external fuel filter was also replaced.

Thursday, March 18, 2010 Everything was put back together and it was filled with three gallons of “extra Fuel 5”. The vehicle appeared to operate normally.

Saturday, March 20, 2010 The fuel used prior to the misfueling event, Fuel 5, was installed in the vehicle and a sulfur purge was conducted.

Sunday, March 21, 2010 The vehicle was conditioned without incident.

Tuesday, March 23, 2010 Results from additional test conducted on Fuel 5 on Monday and Tuesday were submitted to EPA and NREL for review. Results looked very similar to Fuel 5 tests conducted prior to the misfueling event. The vehicle was approved to continue testing with the n ext fuel.

## APPENDIX D

ON

- ROAD OPERATION FOR I NACTIVE TEST VEHICLE SSwRI R eport 03.15777 .01 

### D

- 1 1. ______ Verify that the fuel gage level before driving. Gage reads more than 1⁄2 a tank. Continue to step 4. Gage reads less than 1⁄2 a tank

 Top off fuel tank

 Added ______ gallons of Fuel 5.

2. _____ Locate fuel drum:

EPA Fuel No. 5 SwRI Fuel Code GA

- 6759

- F 

### Drum No.

Verify fuel fill drum matches using “2

- person rule”

Initials: _________, _________

3.

_____ Place fuel drum back into cold box.

4. _____ Verify all four tires are at proper pressures.

5. _____ Verify proper engine oil and coolant levels.

6.

_____ Record the odometer reading __________.

7.

_____ Drive the vehicle using attached driving instructions.

8.

_____ Record the odometer reading __________.

9.

_____ Record the time of completion __________.

Lead Technician’s Signature:___________________________SwRI R eport 03.15777 .01 

### D

- 2

## APPENDIX E

FUEL USED IN ON

- ROAD OPERATION FOR INACTIVE TEST VEHICLESPRODUCT: EPA Matrix Fuel 5 Batch No.: WC1121GP02
TMO No.: MTS PRODUCT CODE: HF0678-5 Tank No.: Gage Analysis Date: 5/23/2008 Shipment Date:
TEST METHOD UNITS SPECIFICATIONS RESULTS
MIN TARGET MAX Distillation - IBP ASTM D86 °F 95
5% °F 125
10% °F 158 144
20% °F 172
30% °F 200
40% °F 227
50% °F 236 244 244
60% °F 254
70% °F 266
80% °F 278
90% °F 295 305 298
95% °F 316
Distillation - EP °F 373 Recovery vol % Report 99
Residue vol % Report 0.8
Loss vol % Report 0.2 Gravity ASTM D4052 °API Report 53.4 Specific Gravity ASTM D4052 - Report 0.7672 Reid Vapor Pressure ASTM D5191 psi 6.50 6.80 6.79
Carbon ASTM D5291 wt fraction Report 86.9 Hydrogen ASTM D4808-A wt fraction Report TBD Hydrogen ASTM D5291 wt fraction Report 12.7 Oxygen ASTM D5599 wt fraction Report <0.1 Oxygen, other then ETOH ASTM D5599 wt fraction 0.10 0.01
Ethanol content ASTM D5599 wt % 0.05 <0.01
Water content ASTM E1064 mg/kg Report 52 Sulfur ASTM D5453 ppm wt 20 30 23
Lead ASTM D3237 g/l 0.01 <0.01 Composition, aromatics ASTM D1319 vol % 38.5 41.5 38.6 Composition, olefins ASTM D1319 vol % 5.5 8.5 5.7 Composition, saturates ASTM D1319 vol % Report 56.0
Benzene ASTM D3606 vol % 0.47 0.77 0.54 Existent gum, washed ASTM D381 mg/100mls 5.0 <0.5
Research Octane Number ASTM D2699 91.0 95.0 94.0
Motor Octane Number ASTM D2700 83.0 87.0 84.7
R+M D2699/2700 87.0 91.0 89.4 Corrosion, Copper ASTM D130 1 1a Oxidation stability ASTM D525 minutes 240 >240
Net Heat of Combustion ASTM D4809-A BTU/lb Report 18417

APPROVED BY: ANALYST DSL

## APPENDIX F

OIL SAMPLE SUMMARYVehicles Sample Interval Date of Sample Date Shipped to Lubrizol Vehicle Odometer start of oil break-in 3/21/2008 4/2/2008 2,139 end of oil break-in 3/27/2008 4/2/2008 4,142 after 3rd Phase 3 fuel 4/3/2009 4/5/2009 5,098 after 15th Phase 3 fuel 7/17/2009 8/4/2009 6,574 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,636

start of oil break-in 4/4/2008 4/18/2008 2,315 end of oil break-in 4/7/2008 4/18/2008 4,318 after 3rd Phase 3 fuel 12/17/2009 2/2/2010 5,280 after 15th Phase 3 fuel 3/25/2010 4/7/2010 7,139 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,712

start of oil break-in 4/4/2008 4/18/2008 2,240 end of oil break-in 4/8/2008 4/18/2008 4,241 after 3rd Phase 3 fuel 10/1/2009 2/2/2010 5,552 after 15th Phase 3 fuel 12/15/2009 2/2/2010 6,649 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,779

start of oil break-in 3/31/2008 4/2/2008 2,151 end of oil break-in 4/4/2008 4/18/2008 4,152 after 3rd Phase 3 fuel 4/7/2009 4/5/2009 5,586 after 15th Phase 3 fuel 7/24/2009 8/4/2009 6,795 after 27th Phase 3 fuel 4/28/2010 7/19/2010 8,778

start of oil break-in 3/10/2008 3/20/2008 2,064 end of oil break-in 3/18/2008 3/20/2008 4,064 after 3rd Phase 3 fuel 12/17/2009 2/2/2010 5,222 after 15th Phase 3 fuel 3/25/2010 4/7/2010 7,055 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,860

start of oil break-in 3/6/2008 3/20/2008 2,068 end of oil break-in 3/12/2008 3/20/2008 4,072 after 3rd Phase 3 fuel 4/3/2009 4/5/2009 5,149 after 15th Phase 3 fuel 7/17/2009 8/4/2009 6,366 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,901

start of oil break-in 3/11/2008 3/20/2008 2,251 end of oil break-in 3/18/2008 3/20/2008 4,253 after 3rd Phase 3 fuel 4/8/2009 4/5/2009 5,209 after 15th Phase 3 fuel 7/24/2009 8/4/2009 6,327 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,901

start of oil break-in 3/21/2008 4/2/2008 2,094 end of oil break-in 3/27/2008 4/2/2008 4,095 after 3rd Phase 3 fuel 9/17/2009 2/2/2010 5,449 after 15th Phase 3 fuel 11/13/2009 2/2/2010 6,493 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,901

start of oil break-in 4/9/2008 4/18/2008 39,556 end of oil break-in 4/14/2008 4/18/2008 39,556 after 3rd Phase 3 fuel 4/3/2009 4/5/2009 6,989 after 15th Phase 3 fuel 7/17/2009 8/4/2009 8,300 after 27th Phase 3 fuel 4/28/2010 7/19/2010 10,091

start of oil break-in 3/20/2008 4/2/2008 2,162 end of oil break-in 3/28/2008 4/2/2008 4,167 after 3rd Phase 3 fuel 12/17/2009 2/2/2010 5,708 after 15th Phase 3 fuel 3/25/2010 4/7/2010 7,189 after 27th Phase 3 fuel 4/28/2010 7/19/2010 8,002

start of oil break-in 3/25/2008 4/2/2008 2,119 end of oil break-in 4/3/2008 4/18/2008 4,121 after 3rd Phase 3 fuel 4/3/2009 4/5/2009 5,143 after 15th Phase 3 fuel 7/17/2009 8/4/2009 6,484 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,804

start of oil break-in 3/25/2008 4/2/2008 2,041 end of oil break-in 4/3/2008 4/18/2008 4,044 after 3rd Phase 3 fuel 4/9/2009 4/5/2009 4,972 after 15th Phase 3 fuel 7/17/2009 8/4/2009 6,165 after 27th Phase 3 fuel 4/28/2010 7/19/2010 7,236

start of oil break-in 3/10/2008 3/20/2008 2,080 end of oil break-in 3/14/2008 3/20/2008 4,081 after 3rd Phase 3 fuel 4/9/2009 4/5/2009 4,983 after 15th Phase 3 fuel 7/24/2009 8/4/2009 6,304 after 27th Phase 3 fuel 4/28/2010 7/19/2010 8,214

start of oil break-in 3/14/2008 3/20/2008 2,050 end of oil break-in 3/18/2008 3/20/2008 4,055 after 3rd Phase 3 fuel 3/31/2009 4/5/2009 5,074 after 15th Phase 3 fuel 7/10/2009 8/4/2009 6,515 after 27th Phase 3 fuel 4/28/2010 7/19/2010 8,070

start of oil break-in 3/28/2008 4/2/2008 2,151 end of oil break-in 4/2/2008 4/2/2008 4,152 after 3rd Phase 3 fuel 4/3/2009 4/5/2009 5,431 after 15th Phase 3 fuel 7/10/2009 8/4/2009 6,786 after 27th Phase 3 fuel 4/28/2010 7/19/2010 8,405 EPA-HCIV - 2008 Honda Civic

EPA-HODY - 2008 Honda Odyssey

EPA-NALT - 2008 Nissan Altima EPA-TCAM - 2008 Toyota Camry

EPA-TSIE - 2008 Toyota Sienna

EPA-FFOC - 2008 Ford Focus

EPA-FEXP - 2008 Ford Explorer

EPA-F150 - 2008 Ford F150 FFV

EPA-DCAL - 2008 Dodge Caliber EPA-CCOB - 2008 Chevrolet Cobalt

EPA-CIMP - 2008 Chevrolet Impala FFV

EPA-SOUT - 2008 Saturn Outlook

EPA-CSIL - 2008 Chevrolet Silverado FFV

EPA-TCOR - 2008 Toyota Corolla

EPA-JLIB - 2008 Jeep Liberty

## APPENDIX G

FORD EXPLORER OIL LE VEL INCIDENTSwRI R eport 03.15777 .01 

### G

- 1 Oil Level Check Procedure

1. Drive vehicle for 10 minutes. 2. Allow vehicle to sit for 10 minutes in a designated level space. 3. Take dipstick reading. 4. Confirm dipstick reading. 5. Immediately after dipstick reading add 8 oz. of specified 5W

- 30 engine oil. 6. Idle vehicle 2 minutes. 7. Allow vehicle to sit for 10 minutes in a designated level space. 8. Take dipstick reading. 9. Confirm dipstick reading. 10. Email oil level information to team along with a recommendation for possible additional fill. 11. If necessary, add oil based on team feedback.

a. Drive vehicle for 10 minutes. b. Allow vehicle to sit for 10 minutes in a designated level space.

c. Take dipstick reading. d. Confirm dipstick reading.

e. Email oil leve l information to team. 12. Release vehicle back into test program.
13. 

### Record oil level on dipstick for all tests vehicles monthly

.


### Reading taken on 08/10/2009

Added 8 oz. on 08/12/2009

Added 8 oz. on 08/12/2009; 16 oz. total added

Added 4 oz. on 08/17/2009; 20 oz. total added MIN MAX MIN MAX

MIN MAX

MIN MAXSwRI R eport 03.15777 .01 

### G

- 2 To minimize logistics and effort in monthly oil level readings, SwRI changed the measurement procedure so that all readings for all vehicles were taken inside the shop following an overnight soak. To correlate the two conditions, SwRI checked all oil leve ls following engine operation, then following an overnight soak: 1. Drive vehicle for 10 minutes. 2. Allow vehicle to sit for 10 minutes in a designated level space. 3. Take dipstick reading. 4. Confirm dipstick reading. 5. Allow vehicle to soak overnight in designated s oak area. 6. Confirm that engine oil sump temperature is 72 +/

- 2F. 7. Take dipstick reading. 8. Confirm dipstick reading.
9. 

### Repeat steps 5 through 8 monthly

## APPENDIX H

VEHICLE CONDITIONING AND

TEST EXECUTION REQUE STS

## APPENDIX I

DETAILED MEASUREMENT

AND ANALYSIS METHODSSwRI R eport 03.15777 .01 

### I

- 1 A. QA OBJECTIVES FOR TESTI NG OF LIGHT

- DUTY VEHICLES

The QA objectives for precision, accuracy, and completeness are presented in Table 1. All measurements will be representative of the fuels, vehicle engine exhaust, and conditions being measured. Completeness equals number of tests performed divided by number of tests proposed times 100.

TABLE 1. PRECISION, ACCURACY, AND COMPLETE NESS OBJECTIVES FOR LIGHT

DUTY ENGINES

Measurement Experimental Precision Parameter (Method) Reference Conditions Std. Dev. Accuracy,% Completeness,%

HC SwRI and Dilute 0.04 a ±15 b >95 (FID) SAE a,b Exhaust

CO SwRI and Dilute 0.06 b ±20 b >95 (NDIR) SAE a,b Exhaust

CO 2 SwRI and Dilute 4 b ±5 b >95
(NDIR) SAE a,b Exhaust

NO x SwRI and Dilute 0.08 a ±10 b >95 (CL) SAE a,b Exhaust

Particulate, 47 mm SwRI and Dilute 0.05 a ±10 b >95 (Gravimetric) SAE a,b Exhaust

Fuel Economy SwRI and Dilute 1 a ±5 b >95 (Carbon Balance) SAE a,b Exhaust

Aldehydes EPA (1,2) Dilute See Appendix K >95 (DNPH/HPLC) CRC (3) Exhaust

Alcohols EPA (1,2) Dilute See Appendix K >9 5 (water impinger/GC

- FID) CRC (3) Ex haust

________________________ a Precision experienced at SwRI, but precision is vehicle dependent. b Accuracy goals were based on SwRI experience and SAE Technical Paper 790232, "Identification, Quantification

and Reduction of Sources of Variability in Vehicle Emissions and Fuel Economy Measurements," N.J. Sheth and T.I. Rice, 1979.

c ±100% of defined detection limit; precision generally improves with increased sample concentration.SwRI R eport 03.15777 .01 

### I

- 2 B. SAMPLING METHODS

The sampling system is comprised primarily of the exhaust sampling system to which continuous measurement devices, a dilute ex haust bag sampler, impinger and cartridge samplers, and particle filters are attached. The sampling procedures employed for the determination of regulated and unregulated emissions for light

- duty engines are identified below. In the event of errors, mish aps, or deviations from procedure, the project leader, Kevin Whitney is to be notified.

All procedures will be designed to maximize test

- to

- test repeatability. For example, the following steps will be taken:

**•** The position and angle of the vehicle cooling fan shall be consistent for each vehicle and each test.

**•** The airflow around the vehicle during tests shall be kept consistent.

**•** To the extent possible, the CARB laboratory correlation program will be used in support of this program’s QA procedures.

**•** Sample side verification of exhaust analyzers will be performed monthly by sampling span gases from a sample bag.

**•** Sample flow proportionality will be verified after each emissions test. For PM samples, a proportionality statistic will be calculated. For other parameters, the constancy of tunnel flows will be verified.

**•** Duplicate vehicle coastdown checks from 70 to 30 mph will be performed following each sulfur purge procedure

.
**•** A check will be performed before, during, and at the en d of each test to assure than manually controlled parameters are set and adhered to during each test.

**•** Battery chargers will be utilized to maintain the state of battery charge of test vehicles between vehicle prep pro cedures and emissions tests.

**•** The LA92 driving cycle will be used for the vehicle prep procedures to match the driving cycle used in emissions tests.

**•** NOx analyzers will be equipped with NH3 traps to prevent contamination of NOx
converters.

B.1. Exhaust Gas Sampling System Description

A Horiba selectable flow CVS syste m will be used to sample exhaust emissions. Test technicians first connect the vehicle exhaust pipe to the CVS inlet. While the vehicle operates on the dynamometer, an adjustable

- speed turbine blower dilutes the exhaust with ambient air. This dilution p revents the exhaust moisture from condensing and provides controllable sampling conditions. A sample pump and a control system transfers diluted exhaust aliquots to several different Kynar bags during specific phases of each test run. Regulating needle v alves maintain constant sample flow rates for the alcohol impingers and DNPH cartridges, and mass flow controllers maintain proper flow into the bags. Exhaust backpressure will be recorded continuously at the tailpipe during emissions testing. Table 2 su mmarizes the CVS system specifications.SwRI R eport 03.15777 .01 

### I

- 3 TABLE 2. CVS SPECIF ICATIONS

Measurement Variable Operating Range Expected in Field Instrument Description Range Accuracy How Verified / Determined

Pressure 950 to 1050 millibar Horiba Variable

Flow Constant Volume Sampler 0 to 1500 millibar **±** 2 % reading Sensors calibrated and verified during installation. Temperature 20 to 45 °C 0 to 100 °C **±** 2 % reading Volumetric Flow Rate 200 to 500 ft 3 /min 150 to 1100 ft 3 /min **±** 0.5 % reading



### B.2. Dilute Exhaust Bag Sampling

The Kynar bags (sample and background) specified for HC speciation analysis will be removed from the Horiba sampling system, marked with a sample ID/custody label, and transported to the GC laboratory. Analysis of sample Bag 1 will begin immediately (within one hour) for the C 1 

### - C 4 

### analysis and within four hours for the benzene

- toluene and C 5 

### - C 12 

### analysis. Times that analyses are started will be reported. For tests in which multiple test phases will be analyzed for HC speciation, ana lysis order shall be: Bag 1, Bag 3, Bag 2, Background Bags.

B.3. Carbonyl Compound Sampling

Heated (235 ±15  ̊ F ) sample lines from the dilution tunnel carry sample gas to a cart which holds the DNPH sampling cartridges. The cart includes controls for the flow rate and measures the volume sampled. Thermocouples with electronic readouts allow recording of the gas temperature sampled, so coupled with the recorded barometric pressure, the volume sampled can be corrected to standard temperature and pressure.

Immediately following the end of the sampled test phase (within 15 minutes), the DNPH cartridge will be extracted with 5.0 ml acetonitrile in accordance with the manufacturer’s instructions. The extract will be promptly sealed and analyzed (within one h our), or stored at <40 ° 

### F for no longer than three calendar days until analysis. Every effort will be made to analyze the sample the same day. Samples and sampling media will be stored separately from calibration standards.

B.4. Alcohol Sampling

Heated (235 ±15  ̊ F ) sample lines from the dilution tunnel carry sample gas to a cart which holds glass impingers filled with ultra

- pure water. The cart includes controls for the flow rate and measures the volume sampled. Thermocouples with electronic readouts a llow recording of gas temperature sampled, so coupled with the recorded barometric pressure, the volume sampled can be corrected to standard temperature and pressure. The impingers are maintained in an ice bath during sampling.

Immediately following the end of the sampled test phase, the impinger contents will be carefully transferred to sealed containers and stored at <40 ° 

### F for no longer than six calendar days until analysis. Every effort will be made to analyze the samples on the same day as collectio n. Samples and sampling media will be stored separately from calibration standards.SwRI R eport 03.15777 .01 

### I

- 4 Ethanol recovery will be checked during every blank test conducted in this program. Recovery shall be ≥92 percent.

B.5. Filter Sampling and Weighing

Whatman Teflo filters with polypropylene support rings will be used for particulate matter (PM) measurements. Particle filters are stored, conditioned, and weighed in a room at SwRI that strictly conforms to 40 CFR 86.1312 and Part 1065. A PM filter field blank will be tested daily. This field blank shall be a tared filter that is installed in a sample holder, then returned to the filter room for weighing by the same procedures as actual samples.

C. SAMPLE HANDLING AND CUSTODY

Only PM filters, bag, impinger, and c artridge samples involve manual handling, because gaseous emission measurements are made and recorded by the computer

- controlled data system associated with the continuous sampling system.

C.1. Particle Filters

Particle filters are managed by a bar code tracking system. Test I.D., date, time, and technician name are tracked with this system. This procedure is compliant with 40 CFR 86.1312 and Part 1065.

C.2. Bag Samples

Because bag samples may be handled by multiple analysts, a bag sample tag is aff ixed to each sample or background bag. With this tag, progress and times of analysis can be recorded. A bag sample tag is shown in Figure 1.SwRI R eport 03.15777 .01 

### I

- 5 BAG ANALYSIS

S A M P L E

Project No. 13363.01.101 EPA Work Assignment 0

- 1

Test No.: Date: / /

Dyno 8 Operator:

Bag Description

LA

- 92 Unified Cycle

□ Bag 1 End of Test :____ :_____
□ Bag 2 End of Test :____ :_____
□ Bag 3 End of Test :____ :_____

Analysis Required Analysis Start (Time) Analyzed by:

□ C 1 

### - C 4 

### speciation :

□ Benz

- Tol speciation :

□ C 5 

### - C 12 

### speciation :

FIGURE 1. BAG SAMPL E TAGSwRI R eport 03.15777 .01 

### I

- 6 C.3. Cartridge and Impinger Samples

Sampling of carbonyl compounds is to be performed with DNPH cartridges, and alcohols, with liquid impingers, as described above. Tracking of sample times and extraction times will be made by recording times on the cartridge tag (Figure 2) and impinger dat a sheet (Figure 3).

ALDEHYDE DNPH CARTRIDGE

Project No. 13363.01.101 EPA Work Assignment 0

- 1

Test No.: Date: / /

Dyno 8 Analyst:

Bag Description

LA

- 92 Unified Cycle □ Bag 1 End of Test :____ :_____ □ Bag 2 End of Test :____ :_____ □ Bag 3 End of Test :____ :_____

Cartridge Extraction Required within 15 min Extraction (Time) Analyst Initials:

□ Bag 1 :

□ Bag 2 :

□ Bag 3 :

□ Background :

FIGURE 2. DNPH CARTRIDGE TAGSwRI R eport 03.15777 .01 

### I

- 7 Project 13363.01.101 Date: / / Dyno 8 Initials:
Test Number: 

### DNPH Cartridge Alcohol Impinger Sample Background Sample Background Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°

Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°

Test Cycle: Temp: Temp: Temp: Temp:

Barameter, “Hg: Counts: Counts: Counts: Counts:

End Time: Sx 1° Sx 2° Sx 1° Sx 2°



### FIGURE 3. IMPINGER AND CARTRIDGE SAMPLI NG DATA SHEET

D. ANALYTICAL METHODS

The analytical procedures employed for the determination of regulated and unregulated emissions for light

- duty engines are given below. 

### In the event of errors, mishaps, or deviations from procedure, the project leader, Kevin Whitney is to be notified.

D.1. Filter Weighing

The chamber in which the PM filters are conditioned and weighed conforms to 40 CFR 86. 1339 and Part 1065 without deviation.

D.2. Gaseous Analyzers

Horiba analytical benches equipped with either MEXA 7000

- Series analyzers are used t o determine NMHC, CO, NO X 

### , and CO 2 

### concentrations in dilute exhaust. Sample pumps transfer the dilute exhaust from Kynar bags to each analyzer as commanded by the control system. Each analyzer used for these measurements is accurate to **±** 2 percent. Table 3 provides a summary of the emissions analyzers to be used.SwRI R eport 03.15777 .01 

### I

- 8 TABLE 3 . EMISSION ANALYZER SPECIFICATIONS

Measurement Variable Expected Operating

Range Instrument Mfg., Model / Type Instrument Range(s) Accuracy a How Verified / Determined

THC 0

- 100 ppmC Horiba FIA

- 220

or FIA

- 726LE

/ FID 0

- 10 ppmC

0

- 50 ppmC

0

- 1000 ppmC

**±** 1.0 % FS

or **±** 2.0 % of the calibration point a Gas divider with protocol calibration gases at 11 points (minimum) spaced throughout span (including zero) NO X 0

- 100 ppm Horiba CLA

- 220 or CLA

- 750LE

/ CL 0

- 30 ppm

0

- 100 ppm

0

- 300 ppm

Low CO 0

- 50 ppm Horiba AIA

- 210 or AIA

- 721LE

/ NDIR 0

- 10 ppm

0

- 50 ppm

CO 0

- 1000 ppm Horiba AIA

- 220

or AIA

- 721A

/ NDIR 0

- 1000 ppm

CO 2 0

- 1.5 % Horiba AIA

- 220

or AIA

- 722

/ NDIR 0

- 4 %

a The most stringent accuracy specification applies for each calibration point.



### E. QUALITY CONTROL

SwRI verifies performance of each analyzer through a series of zero and calibration gas challenges. Each zero and calibration gas must conform to certain specifications and/or be NIST

- traceable. Table 4 summarizes the applicable QA/QC checks. If all cal ibration gases and QA/QC checks meet their specifications, then SwRI will infer that the emissions analyzers meet Table 1 accuracy specifications.

SwRI verifies all new Standard Reference Material (SRM) or other NIST

- traceable reference gas concentrations with an emissions analyzer that has been calibrated within the last 30 days. The operator will first zero the analyzer with a certified zero grade gas and then span it with a NIST SRM (or equivalent) three times to ensure stability and minimal analyzer d rift.

The operator will then introduce the new reference gas into the analyzer and record the concentration, followed by reintroduction of the NIST SRM to ensure that the analyzer span point does not drift more than ±0.1 percent of span point. The operat or will repeat these last two steps until three consistent values are obtained. The mean of these three determinations must be within one percent of its NIST SRM concentration. SwRI will then consider the reference gas as suitable for emissions analyzer calibrations.SwRI R eport 03.15777 .01 

### I

- 9 For chemical evaluations, QC measures are generally specified in the analytical method. A summary of actions taken to ensure data quality for analytical procedures is presented in Table 5

.

TABLE 4 . EMISSION ANALYZER QA/QC CHECKS

QA/QC Check When Performed / Frequency Expected or Allowable Result Response to Check Failure or Out of Control Condition

NIST

- traceable calibration gas verifications Prior to being put into service Average of three readings must be within **±** 1 % of verified NIST SRM concentration Identify cause of any problem and correct; discard bottle and replace if necessary

Zero

- gas verification against NIST certified zero gases Prior to being put into service HC < 1 ppmC CO < 1 ppm CO 2 < 400 ppm NO x < 0.1 ppm O 2 between 18 and 21% Discard bottle and replace

Gas divider linearity verification Monthly All points within **±** 2 % of linear fit FS within **±** 0.5 % of known value Identify cause of any problem and correct; replace gas divider if
necessary

Analyzer calibrations Monthly All values within **±** 2% of point

or **±** 1% of FS; Zero point within **±** 0.2% of FS

Identify cause of any problem and correct; recalibrate analyzer Wet CO 2 interference check Monthly CO 0 to 300 ppm, interference ≤ 3 ppm

CO > 300 ppm, interference ≤ 1% FS

NO X analyzer interference check Monthly CO 2 interference ≤ 3%

NO X analyzer water quench check Once, before each phase of program Proper opreration

NO X analyzer converter efficiency check Monthly NO x converter efficiency > 95%



### TABLE 5

. SUMMARY OF QA/QC CHECKS FOR ANALYTICAL PROCEDURES

Procedure Type Blank Field Blank Duplicate Analysis Continuing Calibration Check Holding Time Preservation During Storage Light Alcohols GC

- FID 1 per batch 1 per day 1 per 10 samples 1 per 10 samples 6 days Keep at <4 ◦ 

### F Aldehydes and Ketones HPLC

- UV 1 per batch 1 per day 1 per 10 samples 1 per 10 samples 15 minutes to extraction; 3 days Keep at <4 ◦ 

### F

HC Speciation GC

- FID 1 per day n/a no end of day 1 hour for C2

- C4 Analysis protect from UV light Particulate

Matter Mass Gravimetric Reference filter every

2 hours n/a At least three
measurements on each filter Monthly reference

check Filters may be out of chamber

only ≤ 1 hr Temperature and humidity controlSwRI R eport 03.15777 .01 

### I

- 10 F. INSTRUMENT/EQUIPMENT TESTING, INSPECTION, AND MAIN TENANCE

Gaseous analyzers conform to 40 CFR 86.1311 without deviation. Internal QC checks and corrective actions are summarized in Table 6

.

TABLE 6 . INTERNAL QUALITY CONTROL CHECKS AND CORRECTIVE ACTION

EQUIPMENT AND/OR MEASUREMENT OPERATIONAL CHECK CONTROL LIMIT(S) ( reference no.) CORRECTIVE ACTION

Driver's aid Speed agreement a EPA (29) Repair and/or recalibrate

CVS Propane recovery b ±2% (25,29 ) Check for leaks and by procedural
assessment Speed, RPM a ±5% (25,29) Check speed sensor and recalibrate rpm Engine Dynamometer Load and Speed, RPM a Federal Register (25) Check and/or repair load cell and rpm indicator; recalibrate

CO bag analyzer CaSO 4 and ascarite conditioning column Blue indicator of CaSO 4 (25,29) Change CaSO 4 and ascarite column soon after CaSO 4 indicator turns color. Leak

check before continuing bag analysis.

NO x bag analyzer Percent efficiency of NO 2 to NO converter b Percent efficiency greater than 90% (25,29) Repair analyzer

Sampling bags Leak

- check bags before and after each test Bag holds gauge vacuum pressure of 27.6 in. Hg Discard bag and note finding in test results. Repeat test as applicable.

HFID analyzer Leak

- check sampling system a Flowmeter float is at zero position Correct leak before sample analysis

Sample gas temperature immediately before heated filter and before the HFID a 375±10 **°** F (25,29) Locate sampling line heating problem and correct before conducting sample analysis Zero and span before each
range c Zero at 0.0 of full

- scale and span to set value (25,29) Determine problem and adjust zero and span accordingly Pre

- analysis and post

analysis zero and span of each range c Zero and span drift

- limit of 2% of full

- scale chart deflection (25,29) Repeat test

Pre

- analysis and post

analysis tunnel HC back

grounds c Continuous tunnel and bag HC backgrounds agree to within l% of full

- scale chart deflection (2 5,29) Determine cause for discrepancy and
correctSwRI R eport 03.15777 .01 

### I

- 11 TABLE 6 . INTERNAL QUALITY CONTROL CHECKS AND CORRECTIVE ACTION

EQUIPMENT AND/OR MEASUREMENT OPERATIONAL CHECK CONTROL LIMIT(S) ( reference no.) CORRECTIVE ACTION

47 mm filter sampling system Leak

- check sampling system a Flowmeter float is at zero position Correct leak before particulate sampling

Sampling rate c Flowrate constant ±5% throughout test Check for leaks or restrictions on sampling line and filter 47 mm reference filters Weight tolerance c ±1% of the nominal filter loading (27) Reweigh all filters being conditioned Particle Dilution Tunnel Particle sampling zone temperature c 125 **°** F or less Increase level of sample dilution

Aldehydes and ketones Leak

- check sampling system c Flowmeter float is at zero position Correct leak before sample collection

Sampling rate c Flowrate constant ±5% throughout test Check for leaks or restrictions on sampling line and filter Dry gas meter volume d Compare to flowmeter estimate Recalibrate or replace dry gas meter

Aldehydes and ketones Sample identification c Date, project, cycle, and test no. if designated Correct labeling

Sample preparation c Within 15 minutes of end of sampled phase Void sample

Sample analysis c Within 3 days of end of sampled date Void sample

HC, CO, NO x , and CO bag analyzers Leak

- check analyzer sampling system a Flowmeter float at zero position Correct leak before bag analysis

Zero and span before each
range c Zero at 0.0 of full

- scale and span to set value (25,29) If not adjustable using analyzer zero and gain control within specified limits, repair analyzer Pre

- analysis and post

analysis zero and span of each range c Zero and span drift limit of 2% of full

- scale meter reading (25,29) Repeat bag analysis



### In the event of out of specification conditions, equipment should be repaired and recalibrated. If a significant delay will result, the project leader, Kevin Whitney is to be notified.

G. I NSTRUMENT/EQUIPMENT CALIBRATION AND FREQ UENCY

Sampling and analytical methodologies and test procedures adhere to Title 40 CFR Parts 86 and 600 requirements. All equipment calibrations are conducted according to the schedules in 40 CFR § 86.116. Table 7 summarizes the relevant calibrations, Title 40 CFR citations, and their frequencies. Calibrations and QA/QC checks are discussed in more detail below.SwRI R eport 03.15777 .01 

### I

- 12 TABLE 7 . EQUIPMENT CALIBRA TIONS SUMMARY

Equipment Description Title 40 CFR Procedure Calibration Frequency
CO analyzer § 86.121 Monthly
CO 2 

### analyzer § 86.122 Monthly HC analyzer § 86.124 Monthly
NO X 

### analyzer § 86.123 Monthly Chassis dynamometer § 86.118 Daily CVS system § 86.119 Weekly Speciated Hydrocarbons EPA (41) 

### Each Sample Set
Alcohols EPA (39) 

### Each Sample Set Aldehydes and Ketones EPA (1, 2, 3) 

### Each Sample Set

Analytical equipment in the chemistry laboratories is calibrated at least once daily, with a calibration verification performed at the end of the batch.

G.1. Gas Meter Calibrations



## A ll gas meters, selected from the list of routinely used instruments given in the recall database, are calibrated to conform to 40 CFR 86.1320. Any necessary correction is made by mechanically adjusting the meter and recalibrating.

G.2. Gaseous Analyzers

The gaseous analyzers to be utilized in this program are discussed in the following sections.

G.2.1

. Hydrocarbon Analyzers

The HC analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1321.

G.2.2

. Carbon Monoxide Analyzers

The CO analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1322 and 40 CFR 89.320.

G.2.3

. Oxides of Nitrogen Analyzers

The NO x 

### analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1323 and 40 CFR 89.321.SwRI R eport 03.15777 .01 

### I

- 13 G.2.4

. Ca rbon Dioxide Analyzers

The carbon dioxide (CO 2 

### ) analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1324 and 40 CFR 89.322.

G.2.5

. Methane Analyzers

The methane analyzers used in this testing program are calibrated in conformance with 40 CFR 86.1325, without deviation.

G.3. Analyzer Gases

The gases used for instrument calibration conform to 40 CFR 86.114 and 40 CFR 89.312 without deviation.

SwRI verifies each new working zero air (or N 2 

### ) cylinder’s impurities to ensure that it is suitable for emissions analyzer zero checks. Comparisons between a certified Vehicle Emission Zero (VEZ) Gas (or equivalent) and the candidate zero gas will serve this purpose. SwRI will employ an emissions ca rt (or suite of instruments) that has been calibrated within the last 30 days for this procedure. The operator will zero the analyzers with certified VEZ gas and span them with NIST

- traceable reference gases to ensure stability and minimal analyzer drift. The operator will then introduce the candidate cylinder’s zero gas to the sample train and record the HC, CO, CO 2 

### , and NO x 

### values. The results must fall within specified ranges for the zero gas to be deemed suitable for instrumental analyzer calibrations.

Prior to the monthly exhaust emission analyzer calibrations, SwRI verifies the calibration gas divider linearity with an HC analyzer known to have a linear response and a HC span gas. The operator will first zero and then span the instrument such that the span occupies 100 meter or chart divisions. The operator will operate the divider in each of its settings in descendin g order and compare the observed results with a linear scale. The difference between the commanded and observed concentrations must be within ±2.0 percent of the commanded concentration. Also, this difference must be less than **±** 0.5 percent of the span va lue.

NIST

- traceable calibration gases, in conjunction with a verified gas divider and zero gas, will create individual gas concentrations with which to challenge each instrumental analyzer. The gas divider will generate 11 concentrations in 10 percent in crements from 0 to 100 percent of each analyzer’s span. Analyzer response at each point must be within **±** 2.0 percent of the concentration or **±** 1.0 percent of span, whichever is more stringent. Zero gas response must be within **±** 0.2 percent of span (the CFR requires **±** 0.3 percent). If any point is outside these limits, operators will generate a new calibration curve.SwRI R eport 03.15777 .01 

### I

- 14 REFERENCES

1. Smith, L.R., Parness, M.A., Fanick, E.R., and Dietzmann, H.E., "Analytical Procedures for Characterizing Unregulated Emissions from Vehicles Using Middle

- Distillate Fuels," Interim Report to the Environmental Protection Agency under Contract 68

- 02

- 2497, Report No. EPA 600/2

- 80

- 068, April 1980.

2. Die tzmann, H.E., Smith, L.R., et al, "Analytical Procedures for Characterizing Unregulated Pollutant Emissions from Motor Vehicles," EPA Report 600/2/79

- 17, February 1979.

3. Smith, L.R., "Characterization of Exhaust Emissions from Alcohol

- Fueled Vehicles," Final Report, Project CAPE

- 30

- 81, Coordinating Research Council, Inc., May 1985.

4. Ames, B., McCann, J., and Yamasaki, E., "Methods for Detecting Carcinogens and Mutagens with the Salmonella/Mammalian

- Microsome Mutagenicity Test," Mutation Research, 31, pp. 347

- 364, 1975.

5. Hames, R.J., Slone, R.J., Perez, J.M., and Johnson, J.H., "Cooperative Evaluation of Techniques for Measuring Diesel Exhaust Odor Using The Diesel Odor Analysis System (DOAS)," SAE Paper 800422, present ed at Congress Exposition, Detroit, Michigan, February 1980.

6. Based on data provided by EPA/RTP (Peter A. Gabele, May 5, 1982).

7. Personal communication with Gail Hutchins, Gailbraith Laboratories, May 17, 1982.

8. Swarin, S.J., and Williams, R.L., " Liquid Chromatographic Determination of Benzo(a)pyrene in Diesel Exhaust Particulate: Verification of the Collection and Analytical Methods," Research Publication GMR

3127, General Motors Research Laboratories, Warren, Michigan, October 1979.

9. Measurem ent and Characterization of Diesel Exhaust Emission" (CRC

- APRAC Project No. CAPI

- l

- 64), Chemical Characterization Panel, CRC

- Program Group on Composition of Diesel Exhaust, Coordinating Research Council, Inc., December 1980.

10. Federal Register, "Heavy

- Duty Engines for 1979 and Later Model Years," Vol. 45, No. 174, September 8, 1977.

11. Federal Register, Vol. 42, No. 124, Tuesday, June 28, 1977.

12. Federal Register, Vol. 45, Wednesday, March 5, 1980.

13. Bykowski, B. B., "Characterization of Diesel Emissions from Operation of a Light

- Duty Diesel Vehicle on Alternate Source Diesel Fuels," Final Report, Contract No. 68

- 03

- 2884, Task Specification Number 3, U.S. Environmental Protection Agency, November 1981.

14. Bykowski, B. B., "Characterization of Diesel Emissions as a Function of Fuel Variables," Final Report, Contract 68

- 03

- 2707, U.S. Environmental Protection Agency, April 1981.

15. Hare, C. T., "Characterization of Gaseous and Particulate Emissions from Ligh t

- Duty Diesels Operated on Various Fuels," Final Report, Contract 68

- 03

- 2440, U.S. Environmental Protection Agency, July 1979.SwRI R eport 03.15777 .01 

### I

- 15 16. Federal Register, Volume 42, No. 124, Part III, June 28, 1977.

17. Bykowski, B. B., "Gasohol, TBA, MTBE Effects on Light

- Duty Emissions," Final Report, Contract No. 68

- 03

- 2377, Task 6, U.S. Environmental Protection Agency, October 1979.

18. Instruction Manual/Bulletin No. 21

- 78

- 220IM "Sierra 220 In

- Stack Cascade Impactors and Cyclone Preseparator," Sierra Instrumen ts, Inc., Carmel Valley, CA 93924.

19. Smith, L.R., "Nitrosamines in Vehicle Interiors," Final Report, Contract 68

- 02

- 2884, Task 2, U.S. Environmental Protection Agency, September 1981.

20. Nie, N. H., Hull, C. Hadlai, Jenkins, J. G., Steinbrenner, K., and Bent, D. H., 'SPSS', McGraw

- Hill, New York, New York 1975.

21. Health Sciences Computing Facility, "BMDP Biomedical Computer Programs, P

- Series 1979," University of California Press, Los Angeles, California, 1979.

22. Martin, S.F., "Diesel Particulat e by 1986 HD Transient Federal Test Procedure," Final Report to the Engine Manufacturers Association, October 1981.

23. Ullman, T.L., Mason, R.L., Montalvo, D.A., "Study of Fuel Cetane and Aromatic Content Effects on Regulated Emissions from Heavy

- Duty Di esel Engine," Final Report to the Coordinating Research Council, Inc., September 1990.

24. Federal Register, "Heavy

- Duty Engines for 1979 and Later Model Years," Vol .45, No. 174, September 8, 1977.

25. Federal Register, "Gaseous Emission Regulations for 1984 and Later Model Year Heavy

- Duty Engines," Vol. 45, No. 14, January 21, 1980.

26. Dietzmann, H.E., and Parness, M.A., "Study of Emissions from Trucks Over Transient Driving Cycles," Final Report to the Environmental Protection Agency under Contract 6 8

- 02

- 2993, 1980.

27. Federal Register, "Control of Air Pollution from New Motor Vehicles and New Motor Vehicle Engines; Particulate Regulation for Heavy

- Duty Diesel Engines," Wednesday, January 7, 1981.

28. Ullman, T.L., and Hare, C.T., "Emission Charact erization of an Alcohol/Diesel

- Pilot Fueled Compression

- Ignition Engine and Its Heavy

- Duty Diesel Counterpart," Final Report EPA 460/3

- 81

- 023, prepared under Contract No. 68

- 03

- 2884, Task Specification 6 for the Environmental Protection Agency, August 1981

.

29. EPA Technical Report SDSB79

- 08, "Recommended Practice for Determining Exhaust Emissions from Heavy

- Duty Vehicles under Transient Conditions," February 1979.

30. Maron, D.L., and Ames, B.N., "Revised Methods for the Salmonella Mutagenicity Test." M utation Research, Elsevier Biomedical Press, pages 173

- 215, 1983.

31. "SwRI Radiographic Inspection of Non

- nuclear Components" OP

- 17

- 40

- 001. Southwest Research Institute, San Antonio, Texas, July 1982.SwRI R eport 03.15777 .01 

### I

- 16 32. "EXAM Methods," EDAX Internat ional, Prairie View, Illinois, 1972.

33. Model 1610 Scanning Electron Microscope Operators Manual, " AMRAY, Inc. Bedford, Mass.

34. "TN

- 5500 X

- ray Analyzer Operation Manual," Tracor Northern, Middleton, Wisconsin, December 1984.

35. Personal communication with Bob Rau, X

- ray Diffraction Service, June 9, 1986.

36. "Instruction Manual for Flowsorb II 2300," Micromeritics Instrument Corp., Norcross, Georgia.

37. Element Analysis Corp. Quality Assurance, Tallahassee, Florida.

38. "Calculation o f Precision, Bias, and Method Detection Limit for Chemical and Physical Measurements," Chapter 5, issued by Quality Assurance Management and Special Studies Staff, Office of Monitoring Systems and Quality Assurance, Office of Research and Development, Unit ed State Environmental Protection Agency, Washington, DC 20460, March 30, 1984.

39. Smith, L.R. and Urban, C.M., "Characterization of Exhaust Emissions from Methanol

- and Gasoline

Fueled Automobiles," Final Report to the Environmental Protection Agency un der Contract No. 68

- 03

- 2884 Task Specifications 11 and 12 and Contract No. 68

- 03

- 3073 Work Assignments 1 and 3, EPA Publication 460/3

- 82

- 004, August 1982.

40. SAS, SAS Institute Inc., Version 5.08, 1985, Box 8000, Cary, N.C. 27511

- 8000.

41. Smith, L.R., "Butadiene Measurement Methodology," Final Report EPA 460/3

- 88

- 005 prepared for the N \ Environmental Protection Agency, under Contract No. 68

- 03

- 4044, Work Assignment B

- 1, Approved for Publication August 1988.

42. Smith, L.R., "Vapor Generation of Fuels," Final Report EPA 460/3

- 87

- 001 prepared for the Environmental Protection Agency under Contract No. 68

- 03

- 3353, Work Assignment B

- 7, August 1987.

43. "Test Procedure for the Measurement of Exhaust Emissions from Marine Engines

- ICOMIA Standard No. 34

- 88," International Council of Marine Industry Associations, 1989.

44. 40 CFR, Part 86, Subpart N.

45. Swarin, S.J., Loo, J.F., Chladek, Drouillard, M.S., and Tejada , S., "Advanced Emission Speciation Methodologies for the Auto/Oil Air Quality Improvement Research Program

- II. Aldehydes, Ketones, and Alcohols," SAE Technical Paper No. 920321, Detroit, Michigan, February 1992.

46. Schuetzle, D., Jensen, T.E., Nagy, D., Prostak, A., and Hochhauser, A., "An Overview of the Advanced Emissions Speciation Methodologies Developed for Phase I of the Auto/Oil Program," Anal. Chem. 63
, 1A

- 8A, 1991.

## APPENDIX J

EPACT NMOG CALCULATI ON PROTOCOLSwRI R eport 03.15777 .01 

### J

- 1 EPAct NMOG Calculation Protocol

19

- Feb

- 2009

The series of calculations shown here (Equations (1) through (6)) must be performed separately for each test phase (bag). The NMOG mass results can then be weighed in the usual way to form a test cycle composite emission rate.

First we calculate corrected NMHC concentration for dilute exhaust (subscript e) and dilution air (subscript d) as follows:

e AcetHO e OH Pr e EtOH e MeOH e 4 CH e e 

### AcetHO r OH Pr r EtOH r MeOH r 4 CH r FIDHC NMHC

**⋅ −**  **⋅ −**  **⋅ −**  **⋅ −**  **⋅ −**  **=** 

### (1)

d AcetHO d OH Pr d EtOH d MeOH d 4 CH d d 

### AcetHO r OH Pr r EtOH r MeOH r 4 CH r FIDHC NMHC

**⋅ −**  **⋅ −**  **⋅ −**  **⋅ −**  **⋅ −**  **=** 

### (2)

Note that these values are a ll as ppmC (so speciation results for EtOH, PrOH, and AcetHO reported in ppm of the particular chemical compound will need to be multiplied by 2 or 3 depending on the number of C atoms in the compound).

The following constant values shall be used for FI D response factors:

r CH4 = 1.15 ppmC/ppmC (this program)

r MeOH = 0.63 ppmC/ppmC (this program)

r EtOH = 0.74 ppmC/ppmC (this program)

r PrOH = 0.85 ppmC/ppmC (CARB)

r FormHO = 0.00 ppmC/ppmC (various sources)

r AcetHO = 0.51 ppmC/ppmC (this program)


### Next, we must calculate the dilution factor to be used in generating the net NMHC concentration:



## ( **) (**  **)** 4

e e e e e e e e e 

### 10 CO AcetHO FormHO EtOH OH Pr MeOH 4 CH NMHC 2 CO z 5

. 0 y 25

. 0 x 76

. 3 y 5

. 0 x x 100
DF

**−**



### ⋅ **+ +**  **+ +**  **+ +**  **+ +**  ** **  ** **  ** ** 

**− +**  **⋅ +**  **+ ⋅** 

**=** 

### (3)

The parameters x, y and z in Eq. (3) are coefficients taken from the chemical formula C x 

### H y 

### O z 

### of a test fuel. The procedure to c alculate their values is provided in Appendix 2.

Once the DF is determined, we calculate the net NMHC concentration as follows:

** **  ** **  ** ** 

**− ⋅**  **− =**  DF 1 1 NMHC NMHC NMHC d e conc 

### (4)
Then we compute NMHC mass 

### :

6

conc NMHC mix mass 

### 10 NMHC Density V NMHC

**−**



### ⋅ **⋅ ⋅**  **=** 

### (5)SwRI R eport 03.15777 .01 

### J

- 2 Equations (4) and (5) must be repeated for each emission being considered. V mix 

### is the volume of dilute exhaust collected during a given phase of the test cycle, measured in standard cubic feet. Density is the calculated gas phase density of a particular species treated as a C 1 

### H y 

### O z 

### ideal gas.

The following values of gas phase density shall be used:

Density NMHC = 16.334 g/ft 3 Density MeOH = 37.718 g/ft 3 Density EtOH = 27.115 g/ft 3 Density PrOH = 23.581 g/ft 3 Density FormHO = 35.345 g/ft 3 Density AcetHO = 25.929 g/ft 3



### To generate the NMOG figure, we need methanol, ethanol, 2

- p ropanol, formaldehyde and acetaldehyde mass emissions as computed using Eq. (4) and (5) based on measured concentration values form the speciation results (as in Eq. (1) and (2)).

Finally, then, NMOG mass emissions can be computed as follows:

mass mass mass mass mass mass mass 

### AcetHO FormHO OH Pr EtOH MeOH NMHC NMOG **+ +**  **+ +**  **+ =**  

### (6)

Once NMOG mass 

### calculations have been completed for all three phases (cold transient (ct), stabilized (s) and hot transient (ht)) of the LA92 test cycle they, calculate the total weighted NMOG emissions using the following formula:

** **  ** **  ** **  ** **  ** **  ** **  ** **  ** ** 

**+ +** 

**⋅ +**  **+ +** 

**⋅ =** 
s D ht D mass.s NMOG mass.ht NMOG 0.57

s D ct D mass.s NMOG mass.ct NMOG 0.43 wm NMOG 

### (7)

For tests where there is no bag 2 or 3 speciation data, NMOG shall be computed assuming emission levels for oxygenated species in bags 2 and 3 are zero.SwRI R eport 03.15777 .01 

### J

- 3 Attachment 1

Definitions

NMHC e 

### – Concentration of NMHC in dilute exhaust sample, ppm C equivalent FIDHC e 

### - Uncorrected concentration of HC in dilute exhaust sample as measured by the FID, ppm C equivalent CH4 e 

### – Concentration of methane in dilute exhaust sample as measured, ppm C equiv alent MeOH e 

### - Concentration of methanol in dilute exhaust sample as measured, ppm C equivalent EtOH e 

### - Concentration of ethanol in dilute exhaust sample as measured, ppm C equivalent PrOH e 

### - Concentration of 2

- propanol in dilute exhaust sample as measured, ppm C equivalent FormHO e 

### - Concentration of formaldehyde in dilute exhaust sample as measured, ppm C equivalent AcetHO e 

### - Concentration of acetaldehyde in dilute exhaust sample as measured, ppm C equivalent CO2 e 

### - Concentration of carbon dioxide in dilute exhaust sample as measured, percent CO e 

### - Concentration of carbon monoxide in dilute exhaust sample as measured, ppm

r CH4 

### - FID response to methane, ppmC/ppmC

r MeOH 

### - FID response to methanol, ppmC/ppmC

r EtOH 

### - FID response to ethanol, ppmC/ppmC

r PrOH 

### - F ID response to 2

- propanol, ppmC/ppmC

r FormHO 

### - FID response to formaldehyde, ppmC/ppmC

r AcetHO 

### - FID response to acetaldehyde, ppmC/ppmC NMHC d 

### - NMHC concentration in dilution air, ppm C equivalent FIDHC d 

### - Uncorrected HC concentration in dilution air sample as measured by the FID, ppm C equivalent CH4 d 

### - Concentration of methane in dilution air sample as measured, ppm C equivalent MeOH d 

### - Concentration of methanol in dilution air sample as measured, ppm C equivalent EtOH d 

### - Concentration of ethanol in dilution air sample as measured, ppm C equivalent PrOH d 

### - Concentration of 2

- propanol in dilution air sample as measured, ppm C equivalent FormHO d 

### - Concentration of formaldehyde in dilution air sample as mea sured, ppm C equivalent AcetHO d 

### - Concentration of acetaldehyde in dilution air sample as measured, ppm C equivalent

DF 

### - Dilution factor

x 

### - Carbon

- to

- carbon ratio in formula C x 

### H y 

### O z 

### determined as in Appendix 2 for the fuel used (by definition x=1)

y 

### - Hydrogen

- to

- carbon ratio in formula C x 

### H y 

### O z 

### determined as in Appendix 2 for the fuel used

z 

### - Oxygen

- to

- carbon ratio in formula C x 

### H y 

### O z 

### determined as in Appendix 2 for the fuel used X

– Carbon mass fraction of the fuel Y

– Hydrogen mass fraction of the fuel Z

– Oxygen mass fraction of the fuel NMHC conc 

### – Concentration of NMHC in dilute exhaust sample corrected for background, ppm C equivalent MeOH conc 

### - Concentration of methanol in dilute exhaust sample corrected for background, ppm C equivalentSwRI R eport 03.15777 .01 

### J

- 4 EtOH conc 

### - Concentration of ethanol in dilute exhaust sample corrected for background, ppm C equivalent PrOH conc 

### - Concentration of 2

- propanol in dilute exhaust sample corrected for background, ppm C equivalent FormHO conc 

### - Concentration of for maldehyde in dilute exhaust sample corrected for background, ppm C equivalent AcetHO conc 

### - Concentration of acetaldehyde in dilute exhaust sample corrected for background, ppm C equivalent V mix 

### - Volume of dilute exhaust collected during a given phase of t he test cycle, scf Density NMHC 

### – Density of NMHC treated as a C 1 

### H y 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg, g/ft 3 

### Density MeOH 

### - Density of methanol treated as a C 1 

### H y 

### O z 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg, g/ft 3 

### Density EtOH 

### - Density of ethanol treated as a C 1 

### H y 

### O z 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg, g/ft 3 

### Density PrOH 

### - Density of 2

- propanol treated as a C 1 

### H y 

### O z 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg, g/ft 3 

### Density FormHO 

### - Density of formaldehyde treated as a C 1 

### H y 

### O z 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg,ft 3 

### Density AcetHO 

### - Density of acetaldehyde treated as a C 1 

### H y 

### O z 

### ideal gas at standard conditions of 293.16 o 

### K and 760 mm Hg, g/ft 3


### M NMHC 

### - Molecular mass of NMHC treated as a C 1 

### H y 

### , g/mole, calculated according to the formula provided in Appendix 3 NMOG mass 

### - NMOG mass, g/test phase NMHC mass 

### - NMHC mass, g/test phase MeOH mass 

### - Methanol mass, g/test phase EtOH mass 

### - Ethanol mass, g/test phase PrOH mass 

### - 2

- p ropanol mass, g/test phase FormHO mass 

### - Formaldehyde mass, g/test phase AcetHO mass 

### - Acetaldehyde mass, g/test phase NMOG wm 

### – Weighted NMOG emissions, g/mile NMOG mass.ct 

### - NMOG mass emitted during the cold transient phase of the test cycle, g/test phase NMOG mass.s 

### - NMOG mass emitted during the stabilized phase of the test cycle, g/test phase NMOG mass.ht 

### - NMOG mass emitted during the hot transient phase of the test cycle, g/test phase D ct 

### - Distance driven by the test vehicle on a chassis dynamometer dur ing the cold transient phase of the LA92 test cycle, miles D s 

### - Distance driven by the test vehicle on a chassis dynamometer during the stabilized phase of the LA92 test cycle, miles D ht 

### - Distance driven by the test vehicle on a chassis dynamometer during the hot transient phase of the LA92 test cycle, milesSwRI R eport 03.15777 .01 

### J

- 5 Attachment 2

Calculation of x, y and z Coefficients in Formula C x 

### H y 

### O z 

### Using Fuel C, H and O Content Data

The carbon

- to

- carbon ratio x in formula C x 

### H y 

### O z 

### by definition equals 1. The hydrogen

- to

- carbon and oxygen

- to

- carbon ratios y and z, respectively, can be calculated using the following equations:

12.011 X 1.008

Y

y **=** 

### (A2.1) and

12.011 X 15.999 Z

z **=** 

### (A2.2) where:

X

– Carbon mass fraction of the fuel Y

– Hydrogen mass fraction of the fuel Z

– Oxygen mass fraction of the fuel


### The values of X, Y and Z will be provided by the EPA for all fuels tested in the EPAct Program.

## APPENDIX K

LOD/LOQ METHODSwRI R eport 03.15777 .01 

### K

- 1 LOD/LOQ Method for EPAct/V2/E

- 89 Program at SwRI ®



### This document is a description of the method that will be used for handling chemistry data in the EPAct/V2/E

- 89 P rogram , with respect to Limit of Detection (LOD) and Limit of Quantification (LOQ). In addition to describing the final method for processing the data, the methods used to determine and track LOD and LOQ are described, as well as the reasoning behind the method and the background and exp eriments which led to its development.

Most of this discussion is related specifically to the carbonyl and alcohol data, where potential interference from the sampling media is significant issue.

Root Issue

The primary problem for which this method wa s developed is how to properly address media interference in the measurement process when the exhaust samples themselves are at levels similar to that interference. This problem arises because we are using methods and media which were developed for use at much higher measurement levels (and which are perfectly adequate for those higher levels).

For example, based on our experiments, most of the media interference for carbonyls is on the order of 0.5 mg/mile or less, which is similar to the levels were are trying to quantify in the exhaust samples. It is important to recognize that the traditional process has been developed to determine compliance with formaldehyde standards on the order of 4 to 18 mg/mile, and to quantify even higher values on pre

- Tier 2 vehicles, where this level of blank interference represents at most 10% of the standard. We are trying to use the same process to quantify values an order of magnitude lower than that, and this has required some refinement of the process.

Proposed QA Bla nk Tracking and Data Analysis Process

It should be noted that all of this tracking is done on a compound

- by

- compound basis, so that (for instance) an issue might be observed only on acrolein while all other compounds could still be within limits.

1. The la boratory and field blanks are analyzed in a daily basis to determine a daily average blank value ( i 

### blank 

### ).
2. Data from these blanks are tracked over time, and are used to generate a 5

- day moving average ( 

### blank ), and an associated standard deviation (σ blank 

### )

. 3. The daily blanks for a given test day ( i 

### blank 

### ) are first evaluated in comparison to the previous 5

- day average as follows:

Is blank i 

# blank blank **σ** 3 **≤**

**−** ?

a. If the above answer is Yes, update the 5

- day 

### blank and σ blank 

### , and proceed with data analysis. This indicates that the current blank falls within acceptable variation from the running average, and is described in Step 4 below.SwRI R eport 03.15777 .01 

### K

- 2 b. If the above answer is No , then the cu rrent blank is outside the normal range of variation and is flagged for review. This process is described further below in Step 5.

4. Data analysis for “normal” blanks (Case 3a, answer to 3 is Yes) . Each analyzed sample (which is either a dilution air back ground or a dilute exhaust sample) is compared individually to the 5

- day 

### blank and σ blank


### .

a. Is blank d uncorrecte 

# blank sample **σ** 3 **≤**

**−** ?

b. If the answer to 4a is No , then calculate the blank corrected sample as follows:



# blank sample sample d uncorrecte corrected 

# − **=**

c. If the answer to 4a is Yes , then report 

# 0 **=** corrected 

# sample for that given sample. The means that the difference between the sample and the blank does not rise above the level of noise in the blanks (i.e., we cannot tell the difference between the sample and a media blank).

d. Analysis then proceeds normally with b ackground correction (using the dilution factor) and mass calculations. The final analyzed mass is always reported. Negative masses are reported as zero and set to zero on a bag

- by

- bag basis prior to composite calculations.

e. Analysis Complete, Proceed to Reporting.

5. Review of and processing “outlier” blanks (Case 3b, answer to 3 is No ).

a. Manual review of blank data chromatograms to determine if an analytical problem is at fault, and correct if possible. b. Manual review of blank data and association with sample/background samples to determine if the blank itself is an outlier or if there is a shift observed for all samples and blanks on that day.

c. If blank itself is an outlier, discard and process test data (as described in Step 4) using the previous 5

- day average. Do not update 

### blank and σ blank


### . d. If the shift is consistent for all samples, backgrounds, and blanks on that day, process test data (as described in Step 4) BUT use the daily average blank value

i 

### blank 

### in place of 

### blank for that day only. Do not update 

### blank and σ blank


### .

6. Media Shift.

a. If outlier behavior is consistent for three days running, blanks may have shifted. In other words, if a blank value shifts from low to high, but then stays high forSwRI R eport 03.15777 .01 

### K

- 3 three days, this may indicate a shift in the media, rather just an outlier. If this is the case, data will be reviewed.
b. If it is determined to be appropriate, 

### blank and σ blank 

### will be reset (initially with values from the three days of question). Note this will be done on a compound

by

- compound basis.

It should be noted that there are multiple review steps throughout this process in the event of outliers. It is hoped that over the course of these review steps, any proces s issues which may have contributed to either an increase in the frequency of outliers or a shift in blank values can be identified and corrected.

Background on Process Development

To establish an appropriate method for determination of the LOQ for a giv en measurement, it is necessary to understand the key factors driving measurement variability. These factors will vary depending in the measurement in question.

In the case of gaseous HC speciation measurements, the primary driver is analytical variabili ty. Experiments have indicated that the bag media do not contribute in a significant manner to the measurement, which is not unexpected given the requirements on the media with respect to HC off

- gassing, as well as the multiple purge

- evacuation processes designed to eliminate carryover. Therefore, the repeatability of the GC instrument was quantified and an LOQ was established in terms of raw area counts at 200 counts. This analytical LOQ was determined by examining repeat measurements of low

- level stand ards. LOD and LOQ are then determined by examining the ratio between the standard peak height and the noise response. The LOD is the lowest concentration where the standard

- to

- noise ratio is 3 to 1, while the LOQ is defined as the lowest concentration wh ere the standard

- to

- noise ratio is 10 to 1. These ratios follow standard good laboratory practice for GC analysis. Any analyzer response below this LOQ in terms of area counts is reported as a zero, because we cannot reliably quantify a number below this threshold. Note that this process is done on every individual measurement, including samples and backgrounds, before the numbers are fed into calculations to determine mass.

For the carbonyls, and to a lesser extent alcohols, the sample media have a muc h higher potential for interference. Table 1 shows a comparison of analytical instrument LOD versus the average blank levels, with the data given as raw area counts. The values in the table compare 3σ for the instrument (as quantified by multiple analyse s of a standard of 0.0003 ug/ml) against 3σ for the blanks (as quantified by examining multiple blanks). This comparison demonstrates that the variation in blank area counts is at a much higher level than the instrument LOD, which indicates that blank var iation is the dominant source of variability in the measurement.SwRI R eport 03.15777 .01 

### K

- 4 TABLE 1. COMPARISON OF INSTRUMENT AND BLANK VARIABILITY FOR CARBONYLS (AREA COUNTS)

To determine an appropriate method to deal with this variation, it was also necessary to determine if this variation is present on a day

- to

- day basis, a batch

- to

- batch basis (i.e., different batches or lots of cartridges), or on the basis of individual bla nks. Two data sets were used for this analysis. One data set is similar to the set shown above which includes area count values for blanks determined over a period of three months’ time, including about 60 days of data and covering more than one batch. The second data set was generated but taking 10 blanks from a single batch and analyzing all of them in a single analytical run on the same day. The results are summarized below in Table 2, with the data given as raw area counts.

TABLE 2. COMPARISON OF LONG

- TERM AND SHORT

- TERM CARBONYL COMPOUND BLANK VARIABILITY Compound Instrument LOD Blank Average FORMALDEHYDE 984 2823 ACETALDEHYDE 1285 9217 ACROLEIN 757 1115 ACETONE 661 39183 PROPIONALDEHYDE 850 1070 CROTONALDEHYDE 392 1605 N-BUTYRALDEHYDE + MEK 785 6002 BENZALDEHYDE 437 1707 HEXANALDEHYDE 326 1154 ISOVALERALDEHYDE 371 4155 VALERALDEHYDE 716 976 O-TOLUALDEHYDE 389 1659 M/P-TOLUALDEHYDE 383 1762 DIMETHYLBENZALDEHYDE 496 1291

90-day Single batch 90-day Single batch Formaldehyde 3460 3647 941 1070 Acetaldehyde 7858 6791 3072 2677 Acrolein 253 354 372 389 Acetone 21482 20767 13061 5020 Propionaldehyde 256 389 357 409 Crotonaldehyde 432 430 535 465 N-butyraldehyde & MEK 2172 1722 2001 2303 Benzaldehyde 783 593 569 316 Isovaleraldehyde 262 381 385 486 Valeraldehyde 1787 1733 1385 1283 o-Tolualdehyde 128 43 325 108 m/p-Tolualdehyde 437 255 553 149 Hexanaldehyde 1512 1898 587 746 Dimethylbenzaldehyde 267 8 430 25 Standard Deviation Average CompoundSwRI R eport 03.15777 .01 

### K

- 5 In most cases the average and standard deviations for both data sets were very similar. This indicates that the variation exists on a cartridge

- to

- cartridge basis, even within a single bat ch, and that this short

- term media variation cannot be distinguished from any longer term factors. There are a few compounds that do not follow this trend such as acetone, wherein the variations are likely also driven by daily variations in the laboratory environment.

As a result of this determination, the practice of using a daily blank for correction of samples for that given day is problematic, because the cartridge

- to

- cartridge variability means that a daily blank set may not necessarily represent the sample cartridges. Therefore, it is necessary to average a number of blanks over time to represent the media correctly. However, any method must also track sudden shifts in media which do occur from time to time, as well as dealing with individual outli ers.
Blank data for both formaldehyde and acetaldehyde are given in Figure 1 and Figure 2, respectively, showing different kinds of behavior that need to be addressed. In the case of formaldehyde, the blanks are generally well behaved, with some slow mo vement over time indicated. However, there are also individual outliers that need to be dealt with. On the other hand, the acetaldehyde blanks show periodic and significant shifts, such as a shift which occurs at about Blank 59 from a low level to a high er level. On review this shift is also present in actual test samples and backgrounds from that day, indicating a real shift in the media or process.

Similar data were examined for the heavier carbonyls, and a similar analysis was also performed for the alcohols (although in the case of alcohols only the methanol data showed evidence of variability). Based on all of these data, it was determined that a 5

- day moving window for would be appropriate to properly characterize media blank variation, while als o being short enough to detect movement of the blanks. In addition, the inclusion of a 3

- sigma outlier test to trigger manual data review accounts for detection of outlier days, which might result from either an individual blank issue or a shift which aff ects an entire test day. Finally, a provision is included to reset the daily average, in the event that a real long

- term shift is observed over several days, such as observed from time to time in the acetaldehyde data.

Figure 3 shows acetone blanks over the same time window. In this case there are several outlier days, which upon analysis were reflected in the data for that day, but then the blank levels returned to normal. Thus far, we believe that acetone is uniquely affected by laboratory environmen t given the presence of acetone in many places. In these cases, the blanks for that day should be used to process that data for that day, but the running average should not be disturbed for an outlier day.SwRI R eport 03.15777 .01 

### K

- 6 FIGURE 1. FORMALDEHYDE BLANK TRACKING

FI GURE 2. ACETALDEHYDE BLANK TRACKING Formaldehyde Blank Tracking (March 2009 - June 2009)

0 1000 2000 3000 4000 5000 6000 7000

0 20 40 60 80 100 120 140 Blank Number (2 per day)Area Counts Formaldehyde Blank Area Counts 5-Day Moving Average

Acetaldehyde Blank Tracking (March 2009 - June 2009)

0 2000 4000 6000 8000 10000 12000 14000 16000

0 20 40 60 80 100 120 140 Blank Number (2 per day)Area Counts Acetaldehyde Blank Area Counts 5-Day Moving AverageSwRI R eport 03.15777 .01 

### K

- 7 FIGURE 3. ACETONE BLANK TRACKING

Figure 4 illustrates a running example of the final blank process that was developed using formaldehyde as an example. The figure shows the five

- day running average blank value (note that there are two blanks analyzed per day, as well as the five

- day running 3σ upper and lower control limits. As noted there are occasional single blanks which rise above those limits, which would trigger review. I n these cases, the review indicates that these were outliers that were not represented in the data, and therefore, these measurements were not used to modify the running average or control limits. In one case, near Run 45 the control limits are very tight due to a period of time when the variation was small. In this case, although the blanks shown are slightly above the 3σ limit, the movement is small and still well within the historical norm, and in that case the judgment is made to utilize the data. Th is example also underscores the fact that a set of process rules are not a complete replacement for good engineering judgment. Acetone Blank Tracking (March 2009 - June 2009)

0 10000 20000 30000 40000 50000 60000 70000 80000

0 20 40 60 80 100 120 140 Blank Number (2 per day)Area Counts Acetone Blank Area Counts Series2 5-Day Moving Average

Outlier days - reflected in data for that day but not stable for more than 2-days - blanks used to process that day but NOT in running averageSwRI R eport 03.15777 .01 

### K

- 8 FIGURE 4. FINAL BLANK PROCESS EXAMPLE WITH FORMALDEHYDE

Figure 5 illustrates a similar example for methanol tracking. Met hanol appears to be affected by periodic issues which generate a low level noise in both blanks and samples, which could result in erroneous reporting of methanol and therefore affect NMOG calculation. This is confirmed by the fact that when the blanks ar e clean there is also no methanol detected in exhaust samples. The developed QA process is able to detect this noise and account for its effect on the data, so that only a significant quantity of real methanol emission would be reported, and the data are not disturbed by this process noise. In areas of media/process variability, the 3

- sigma screening value (yellow triangles) rises, as shown in Figure 5. Therefore, the LOQ screening process outlined earlier of checking the different between sample and bla nks against the five

- day 3

- sigma would be an effective screening for this issue. Formaldehyde Blank Tracking (March 2009 - June 2009)

0 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000

0 10 20 30 40 50 60 70 Day NumberArea Counts 5-DayAverage 5-Day 3Sigma + 5-Day 3Sigma - Individual Blanks

Outlier blanks not used in 5-day average

Small shift outside current 3sigma but still acceptableSwRI R eport 03.15777 .01 

### K

- 9 FIGURE 5. FINAL BLANK PROCESS EXAMPLE WITH METHANOL 

### Methanol Blank Tracking (March 2009 - June 2009)

10 210 410 610 810 1010 1210

0 10 20 30 40 50 60 70 80 Test DayArea Counts Individual Blanks 5-Day Average 5-Day 3Sigma +

Outlier day, significant effect on samples Region of blank noise, similar behavior of samples, 3sigma data screening cleans up this process issue in data

Clean blanks, no methanol in samples either

## APPENDIX L

EPA FUEL SAMPLING PR OCEDURE FOR CARRYOVER EXPERIMENTSSwRI R eport 03.15777 .01 

### L

- 1 November 12, 2008

Procedure for Sampling and Handling of Gasoline Samples

1. Make sure that the fuel in drum, sampling equipment and sample container are at 50 o 

### F

max

• It is strongly advisable that the sample contai ner be cooled in an ice chest

• Use a hand transfer pump

• The glass sampling container must meet the following requirements:

i. At least 1 qt. capacity ii. Amber colored. iii. Its cap must be equipped with a neoprene seal

2. Position the sampling tube to take the fuel sample from the mid level of whatever fuel quantity is left in the drum

• It is recommended that a separate rigid tube of required length be used to sample fuel from a full drum and from a nearly empty (~ 15% full ) drum

3. Using the hand transfer pump, activate the flow of fuel from the drum into a slop container and slop at least 1 qt. of fuel

4. Fill the sample container to 75

- 80% of capacity and seal tightly to prevent sample losses

• Make sure that during sampling the fuel flows gently (w/o splashing) into the sampling container. Use a filling tube that reaches to the bottom of the container

5. Store the sample at 0 to 1 o 

### C in a cooling bath or a refrigerator prior to opening the sample container for RVP measurement

6. Have the sample analyzed as quickly as possible

## APPENDIX M

FUEL BLENDING EXPERI MENT TO CHARACTERIZE CARRYOVER EFFECTSSwRI R eport 03.15777 .01 

### M

- 1 Investigation of Fuel Carryover Effects on Distillation Parameters July 27, 2009

Fuel 1 Fuel 2 Fuel 1 Fuel 27 Fuel 1 Fuel 6 Fuel 2 Fuel 21 Fuel 27 Fuel 21

Ethanol Content vol. % 10 0 10 15 10 10 0 20 15 20 T50 oF 150 240 150 220 150 190 240 160 220 160 T90 oF 300 340 300 340 300 340 340 300 340 300 DVPE psi 10.0 10.0 10.0 6.65 10.0 6.65 10.0 6.65 6.65 6.65 Aromatics vol. % 15 15 15 15 15 15 15 40 15 40

EtOH Target Meas. Target Meas. Target Meas. Fuel 1 Fuel 2 10 100 0 10 9.93 150 149.8 300 297.2 0 0 100 10 10.22 240 237.9 340 339 5 95 10.64 236 338.8 95 5 10.05 150.6 301.7

Fuel 1 Fuel 27 10 100 0 10 9.93 150 149.8 300 297.2 15 0 100 6.65 6.87 220 221.7 340 339.3 5 95 7.01 216.1 339.2 95 5 9.81 150.9 301.9

Fuel 1 Fuel 6 10 100 0 10 9.93 150 149.8 300 297.2 10 0 100 6.65 7.21 190 189.4 340 340.3 5 95 7.23 186 339.2 95 5 9.72 150.4 301.7

Fuel 2 Fuel 21 0 100 0 10 10.22 240 237.9 340 339 20 0 100 6.65 6.98 160 168.8 300 304.8 5 95 7.27 169.2 305.9 95 5 10.75 235.8 336.4

Fuel 27 Fuel 21 15 100 0 6.65 6.87 220 221.7 340 339.3 20 0 100 6.65 6.98 160 168.8 300 304.8 5 95 6.95 168.6 305.2 95 5 6.83 217.8 338.9

►F ollow EPAct Fuel Sampling Procedure ►Blend fuels A3, A4, B3, B4, C3, C4, D3, D4, E3 and E4 ►Perform D86 test on the fuels of each set in the course of a single day ▬ Use exclusively OptiDist equipment ▬ Use the same distillation still for all tests Fuel 27: 1/2 gal Fuel Pair E Fuel Pair D Fuel Pair C

21 2 Components Fuel Set C

Test Fuel

Fuel Set D

27

Scope of Work: PROPERTY UNIT

Test Fuel Sets Fuel Pair A Fuel Pair B

Fuel 2: 1/2 gal Fuel 6: 1 qt Fuel 21: 1/2 gal E4 E3 21 Test Fuel

B4 B3 27 1

D3

are being tested on that day Components

Fuel Set E Components Test Fuel

► Obtain samples of fuels 1,2,6,21 and 27 Sample sizes (~2X needed volume): Test Fuel

Fuel 1: 1 gal D4 2

► Note: The same fuel need not be tested twice on a given day, if it belongs to two different fuel sets which 6 1

C4 C3 Fuel Set B A3 A4

Components RVP T50 T90
Fuel Set A

Test Fuel

1 Components

## APPENDIX N

ADDITIONAL FUEL CARR YOVER EXPERIMENTSSwRI R eport 03 .15777 .01 

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- 1 Procedure

1. collect fuel sample 2. drain and flush to E20 3. run sulfur purge 4. collect fuel sample 5. drain and refill with E20 6. run single LA92 prep 7. collect fuel sample 8. drain and flush to E0 9. run sulfur purge 10. collect fuel sample 11. drain and refill with E0 12. run single LA92 prep 13. collect fuel sample 14. drain and refill with E0 15. run single LA92 prep 16. collect fuel sampleSwRI R eport 03 .15777 .01 

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- 2 Results

Vehicle Sample Description SwRI D5599 SwRI Petrospec

Vol% Wt% EPA-HODY original fuel in tank 10.4 11.9 EPA-HODY first flush to E20 18.0 17.5 EPA-HODY 2nd flush to E20 20.1 18.8 EPA-HODY first flush to E0 7.4 7.8 EPA-HODY 2nd flush to E0 1.6 1.5 EPA-HODY 3rd flush to E0 0.2 0.2

EPA-NALT original fuel in tank 10.9 11.3 EPA-NALT first flush to E20 19.3 18.0 EPA-NALT 2nd flush to E20 20.7 18.6 EPA-NALT first flush to E0 4.9 5.0 EPA-NALT 2nd flush to E0 1.4 1.3 EPA-NALT 3rd flush to E0 0.2 0.2

EPA-TSIE original fuel in tank 19.4 19.1 EPA-TSIE first flush to E20 21.5 19.6 EPA-TSIE 2nd flush to E20 21.0 19.2 EPA-TSIE first flush to E0 5.0 5.0 EPA-TSIE 2nd flush to E0 1.1 1.1 EPA-TSIE 3rd flush to E0 0.2 0.0

EPA-HCIV original fuel in tank 13.9 14.9 EPA-HCIV first flush to E20 20.4 18.8 EPA-HCIV 2nd flush to E20 21.1 19.4 EPA-HCIV first flush to E0 5.2 5.2 EPA-HCIV 2nd flush to E0 0.9 0.7 EPA-HCIV 3rd flush to E0 0.1 0.0

EPA-TCAM original fuel in tank 10.2 11.2 EPA-TCAM first flush to E20 19.1 18.2 EPA-TCAM 2nd flush to E20 20.7 18.9 EPA-TCAM first flush to E0 3.2 3.2 EPA-TCAM 2nd flush to E0 0.5 0.4 EPA-TCAM 3rd flush to E0 <0.1 0.0

NOTE: 2nd flush to E0 should be roughly equivalent to samples listed below

previous results EPA D5599 SwRI Petrospec

Vol% Wt% EPA-HODY MP-1 fuel sample 2.0 1.9 EPA-NALT MP-1 fuel sample 0.6 0.2 EPA-NALT 05/29 fuel sample 1.4 1.5 EPA-TSIE MP-1 fuel sample 0.7 0.4 EPA-HCIV MP-1 fuel sample 0.6 0.3 EPA-TCAM MP-1 fuel sample 1.6 1.5 Ethanol

Note: 2 nd flush to E0 (color

- shaded above), should be roughly equivalent to color

shaded samples listed below. The entries with the same color

- shaded areas from above and below c an be compared.

## APPENDIX O

REFUELING LOCATION E XPERIMENTSSwRI R eport 03.15777 .01 

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- 1 For each chosen vehicle SwRI conducted the fuel change sequence given in Table O

- 1. This sequence was based on what was used during the conduct of Phase 3 testing, and should be representative of the actual Phase 3 test procedure. For each vehicle, the sequence was conducted at each of two refueling locations using the same pair of E20 and E0 fuels. The refueling locations used for each chosen vehicle are given in Table O

- 2. A schematic of the refueling locations is given in Figure O

- 1. All fuel samples were collected approximately half way through each drainSwRI R eport 03.15777 .01 

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- 2 TABLE O

- 1. FUEL CHANGE SEQU ENCE

STEP DESCRIPTION REQUIRED SAMPLE ANALYSES 1 Collect fuel sample from vehicle while draining fuel via fuel rail. Density @ 60°F by D4052 Ethanol concentration by D5599 Ethanol concentration by Petrospec 2 Fill fuel tank to 40% with designated E20 Group 1 fuel. Fill

- up fuel temperature must be less than 50°F. 3 Start vehicle and execute catalyst sulfur removal procedure described in Appendix C of CRC E

- 60 Program report. Apply side fan cooling to the fuel tank to alleviate the heating effect of the exhaust system. 4 Collect fuel sample from vehicle while draining fuel via fuel rail. Density @ 60°F by D4052 Ethanol concentration by D5599 Ethanol concentration by Petrospec 5 Fill fuel tank to 40% with designated E20 Group 1 fuel. Fill

- up fuel temperature must be less than 50°F. 6 Perform three 2

- phase (bags 1 and 2) LA92 cycle s. During these prep cycles, apply side fan cooling to the fuel tank to alleviate the heating effect of the exhaust system. 7 Collect fuel sample from vehicle while draining fuel via fuel rail. Density @ 60°F by D4052 Ethanol concentration by D5599 Ethanol concentration by Petrospec 8 Fill fuel tank to 40% with designated E0 Group 2 fuel. Fill

- up fuel temperature must be less than 50°F. 9 Start vehicle and execute catalyst sulfur removal procedure described in Appendix C of CRC E

- 60 Program repor t. Apply side fan cooling to the fuel tank to alleviate the heating effect of the exhaust system. 10 Collect fuel sample from vehicle while draining fuel via fuel rail. Density @ 60°F by D4052 Ethanol concentration by D5599 Ethanol concentration by Petrospec 11 Fill fuel tank to 40% with designated E20 Group 2 fuel. Fill

- up fuel temperature must be less than 50°F. 12 Perform three 2

- phase (bags 1 and 2) LA92 cycles. During these prep cycles, apply side fan cooling to the fuel tank to alleviate t he heating effect of the exhaust system. 13 Collect fuel sample from vehicle while draining fuel via fuel rail. Density @ 60°F by D4052 Ethanol concentration by D5599 Ethanol concentration by PetrospecSwRI R eport 03.15777 .01 

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- 3 TABLE O

- 2. REFUELING LOCATI ONS

BRAND MODEL LOCATION A LOCATION B Chevrolet C1500 Silverado Containment Pad South Toyota Camry Containment Pad South Toyota Sienna Containment Pad South Dodge Caliber Containment Pad South Honda Civic Containment Pad South Honda Odyssey Containment Pad South Nissan Altima Containment Pad South

FIGURE O

- 1. SCHEMATIC OF VEHICLE REFUELING LOCATIONS CONTAINMENT PAD LARGE BOX

SMALL BOX

SOUTH LOCATION NORT H LOCATION