February 2004 • NREL/SR-540-35334 

Fuel and Fuel Additive 

Registration Testing of EthanolDiesel Blend for O2Diesel, Inc. 

E. Robert Fanick 

Southwest Research Institute 

San Antonio, TX 

O2Diesel, Inc. 

Newark, Delaware 

National Renewable Energy Laboratory 

1617 Cole Boulevard 

Golden, Colorado 80401-3393 

NREL is a U.S. Department of Energy Laboratory

Operated by Midwest Research Institute • Battelle 

Contract No. DE-AC36-99-GO10337 
February 2004 • NREL/SR-540-35334 

Fuel and Fuel Additive 

Registration Testing of EthanolDiesel Blend for O2Diesel, Inc. 

E. Robert Fanick 

Southwest Research Institute 

San Antonio, TX 

O2Diesel, Inc. 

Newark, Delaware 

NREL Technical Monitor: R. McCormick 

Prepared under Subcontract No. ZCL-3-32068-01 

National Renewable Energy Laboratory 

1617 Cole Boulevard 

Golden, Colorado 80401-3393 

NREL is a U.S. Department of Energy Laboratory

Operated by Midwest Research Institute • Battelle 

Contract No. DE-AC36-99-GO10337 
This publication was reproduced from the best available copy

submitted by the subcontractor and received no editorial review at NREL 

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Foreword 

O2Diesel, Inc. (formerly AAE Technologies, Inc.) conducted this project under subcontract number 

ZCL-3-32068-01 with the National Renewable Energy Laboratory of the United States Department of 

Energy. The Office of Energy Efficiency and Renewable Energy, Biomass Program sponsored this effort. 

Southwest Research Institute performed this project for O2Diesel, Inc. as a lower tier subcontractor. 

Messrs. Jim Peeples and Paul Vind were the technical representatives for O2Diesel, Inc. Work was 

performed under SwRI Project 08-06553, and the Principal Investigator and Project Leader for SwRI was 

Mr. E. Robert Fanick, Group Leader in the Department of Engines and Emissions Research. Dr. Joe Pan 

in the Petroleum Products Department was responsible for the PAH and NPAH analysis. The SwRI 

Project Manager for this work was Dr. Lawrence R. Smith, Manager of the Light-Duty and Unregulated 

Emissions Section. 

i 
Executive Summary 

Testing was performed on a heavy-duty diesel engine in support of the Environmental Protection Agency 

(EPA) requirements for registration of designated fuels and fuel additives (F/FA) as stipulated by 

sections 211(b) and 211(e) of the Clean Air Act (CAA). Emission generation, collection, and analysis of 

the regulated emissions and speciation of vapor-phase and semi-volatile hydrocarbon compounds were 

performed on a Detroit Diesel Series 60 engine manufactured in 2002 and meeting the 1998 federal 

heavy-duty emission standards that applied in 2002. The engine was first tested with O2DieselTM (diesel 

fuel with 7.7% ethanol and additives) after 125 hours of engine operation with the fuel. Testing involved 

one cold-start test and six hot-start tests on each of three different days. Samples were collected and 

analyzed for regulated emissions including total hydrocarbons (THC), carbon monoxide (CO), oxides of 

nitrogen (NOx), and total particulate; for hydrocarbon speciation; and for semi-volatile (vapor- and 

particulate-phases) polycyclic aromatic hydrocarbons (PAH) and nitrated polycyclic aromatic 

hydrocarbons (NPAH). The fuel was then changed to the 211b baseline fuel. After approximately five 

hours of engine operation with the baseline fuel, the above test sequence was repeated. 

In general after 125 hours of operation, both fuels gave regulated emissions that were lower than or equal 

to the corresponding 2002 emission standards when used in the Detroit Diesel engine with the exception 

of particulate. Particulate, oxides of nitrogen, and carbon monoxide emissions were found to be lower 

with O2DieselTM when compared to the 211b baseline fuel, and the hydrocarbons were higher (See 

Summary Table). Speciation of C1 to C12 hydrocarbons, C1 to C6 alcohols and ethers, aldehydes, ketones, 

and vapor- and particulate-phase PAH and NPAH compounds revealed that no additional compounds 

were present in the exhaust when the emissions were compared to the exhaust from 211b baseline fuel. 

Ethanol and five aldehydes or ketones (formaldehyde, acetaldehyde, acrolein, acetone, and 

benzaldehyde) were detected at concentrations greater than the 211b baseline fuel, but these results are 

considered typical of engines operating on fuels containing ethanol. No additional compounds which 

could be attributed to O2DieselTM were found in the exhaust above the detection limits for the analytical 

procedures, except for an unidentified C8 compound which was detected in only two of the hot-start tests 

with the O2DieselTM. 

Summary Table of Composite Regulated Emissions 

Test 

Emissions Results, g/bhp-hr 

THC CO NOx Particulate 

2002 Standard 1.3 16 4.0 0.10 

O2DieselTM 

Composite C1-H11 0.27 1.5 3.4 0.13 

Composite C2-H21 0.27 1.5 3.6 0.13 

Composite C3-H31 0.31 1.6 3.6 0.13 

Average of Three Composites 0.28 1.5 3.6 0.13 

211b Baseline Fuel 

Composite C1-H11 0.16 1.6 3.8 0.13 

Composite C2-H21 0.24 1.6 3.8 0.14 

Composite C3-H31 0.21 1.7 3.7 0.15 

Average of Three Composites 0.20 1.6 3.8 0.14 

ii 
Table of Contents 

Page 

Executive Summary ......................................................... ii

List of Figures ............................................................ iv

List of Tables ............................................................. iv

I. Introduction .......................................................... 1

II. Heavy-Duty Engine Testing .............................................. 2

A. Objective ...................................................... 2

B. Scope of Work .................................................. 2

III. Description of Analytical Methods ........................................ 12

A. Regulated Emissions ............................................ 12

B. Speciation of Volatile Hydrocarbon Compounds ....................... 14

C. Alcohols and Ethers ............................................. 16

D. PAH and NPAH ................................................ 18

IV. Quality Control and Quality Assurance .................................... 21

V. Test Results ........................................................ 23

A. Regulated Emissions ............................................ 23

B. Speciation of Volatile Hydrocarbon Compounds ....................... 23

C. Alcohols and Ethers ............................................. 25

D. PAH and NPAH ................................................ 25

VI. Summary ........................................................... 31

References ............................................................... 33

APPENDICES 

A. Heavy-Duty Emission Test Results 

B. Hydrocarbon Speciation Data C. Test Substance Information

C. Test Substance Information 

iii 
Figures 

Figure Page 

1 Graphic Representation of Torque and Speed Commands for the 

Transient Cycle for Heavy-Duty Engines .............................. 4

2 Detroit Diesel Series 60® Mounted on Test Stand ............................ 5

3 Engine Speed and Torque Map with O2DieselTM .............................. 7

4 Engine Speed and Torque Map with 211b Baseline Fuel ....................... 7

Tables 

Table Page 

1 Test Plan for Heavy-Duty Engine Testing ................................... 3

2 Engine Specifications and Features ....................................... 5

3 Cummins Durability Cycle for Aging and Engine Deterioration

Factor Determination ............................................. 6

4 Initial Blending Components for Preparing O2DieselTM ......................... 8

5 Ethanol Analysis by Protocol D-4806 ....................................... 8

6 Ethanol and Water Content from Main Fuel Tank After Phase Separation .......... 9

7 Fuel Analysis ........................................................ 10

8 Lubricity Measurements ................................................ 10

9 Sample Collection .................................................... 13

10 Selected C1 to C6 Alcohols and Ethers that Have Some Solubility in Water ......... 17

11 Summary of Regulated Emissions ........................................ 24

12 Vapor-Phase Alcohol Results ........................................... 26

13 Vapor-Phase Semi-Volatile PAH and NPAH Results .......................... 27

14 Particulate-Phase Semi-Volatile PAH and NPAH Results ...................... 28

15 Combined Vapor- and Particulate-Phase PAH and NPAH Results ............... 30

16 Summary of Composite Regulated Emissions ............................... 32

iv
I. Introduction 

This work was performed for O2Diesel, Inc. in support of the Environmental Protection Agency (EPA) 

requirements for registration of designated fuels and fuel additives (F/FA) as stipulated by sections 

211(b) and 211(e) of the Clean Air Act (CAA). In general, standard mandatory requirements for F/FA 

registrations are contained in a three tiered structure. The first two tiers generally apply to most F/FA 

manufacturers, but there are special provisions for certain types of additives and small businesses. Each 

manufacturer is required to submit basic registration data for each product being registered. Small 

businesses with less than $50 million of annual sales are excused from the first two tiers of requirements 

for F/FA which are considered baseline or non-baseline, and small businesses with less than $10 million 

annual sales are excused from Tier 2 requirements for “atypical” F/FA. Definitions of baseline, nonbaseline, and “atypical” F/FA are discussed in detail below. The other special provisions include 

experimental F/FA, relabeled products, and those exclusively for off-road use. 

Each F/FA is sorted into one of two broad "fuel families:" conventional or alternative. The conventional 

fuel families are gasoline and diesel, and the alternative fuel families include methanol, ethanol, methane, 

and propane. Each fuel family is then subdivided into three "F/FA categories:" baseline, non-baseline, 

and “atypical.” The baseline category consists of fuels and associated fuel additives which resemble the 

respective base fuel for a particular fuel family in terms of elemental composition (no elements other 

than carbon, hydrogen, oxygen, nitrogen, and sulfur), and which conform with certain quantitative limits 

for particular constituents. "Atypical" is defined as those which contain metals; or elements other than 

carbon, hydrogen, nitrogen, sulfur, and oxygen. The non-baseline category is an intermediate category 

between baseline and atypical. In the diesel fuel family, the distinction between baseline and nonbaseline is based primarily on the presence of significant concentrations of oxygen-containing 

compounds (greater than 1.0% oxygen by weight). O2DieselTM does not contain any elements other than 

carbon, hydrogen, oxygen, nitrogen, and sulfur; and falls into the non-baseline fuel family for diesel 

because it exceeds the 1.0% wt. oxygen limit. This report includes the emission measurements as part of 

the requirements for the registration of an additive or fuel as stipulated by sections 211(b) and 211(e) of 

the CAA. 

1
II. Heavy-Duty Engine Testing 

A. Objective 

The objective of this program was to provide O2Diesel, Inc. with the generation, collection, and analysis 

of combustion emission samples. Emissions generation, collection, and analysis were performed 

according to the Tier 1 requirements as identified in 40 CFR 79.57. Protocols outlined in 40 CFR 86 

Subpart D and in applicable SwRI Standard Operating Procedures (References 1 through 20) were 

followed. 

B. Scope of Work 

1. Heavy-Duty Test Protocol 

Fuel and fuel additive registration testing for Tier 1 utilizes the EPA transient test protocol. The test plan 

used for the generation and collection of combustion emission samples is shown in Table 1. Under the 

transient Federal Test Procedure (FTP), the EPA transient cycle is described by means of percent of 

maximum torque and percent of rated speed for each one-second interval over a test cycle of 1199 

seconds duration. To generate a transient cycle, an engine's full load torque curve is obtained from an 

engine speed below curb idle speed to maximum no-load engine speed. Data from this "torque curve," or 

torque map, are used with the specified speed and load percentages to form a transient cycle. A graphic 

presentation of the speed and torque commands which constitute a transient cycle is given in Figure 1 for 

illustration purposes. The first five minutes of the cycle is designated as the New York Non-Freeway 

(NYNF) portion of the test and represents city operation with extensive idle time. The second five 

minutes is called the Los Angeles Non-Freeway (LANF) portion. This part of the test also represents 

city operation, but without the excessive idle time. The third five minute section of the test is called the 

Los Angeles Freeway (LAF) portion. This part is more representative of higher speed conditions 

indicative of freeway operation. The final five minutes of the EPA transient cycle is a repeat of the 

NYNF portion. These four parts are combined to give the EPA transient cycle. 

In general, a transient test consists of both cold- and hot-start EPA transient cycle operation. The same 

engine command cycle is used in both cases. For the cold-start, the diesel engine is operated over a 

"prep" cycle, then allowed to stand overnight in an ambient soak at a temperature between 68 and 86°F. 

The cold-start transient cycle begins when the engine is cranked for cold start-up. Upon completion of 

the cold-start transient cycle, the engine is stopped and allowed to stand for 20 minutes. After this hotsoak period, a hot-start EPA transient cycle begins with engine cranking. In order to determine how well 

the engine followed the transient command cycle, engine performance is compared to engine command, 

and several statistics are computed. These computed statistics must be within tolerances specified in the 

Code of Federal Regulations (CFR). In addition to statistical parameters, the cycle work actually 

produced should be between 5 percent above and 15 percent below the work requested by the command 

cycle. 

2
Table 1. Test Plan for Heavy-Duty Engine Testing 

Step Description 

1 Perform emission instrument calibrations as required. Calibrate torque meter and check signal 

conditioning systems. Validate Constant Volume Sampler (CVS) gaseous and particulate 

sampling systems using propane recovery techniques. 

2 Install engine in transient-capable test cell and check engine condition. Engine must be new with 

less than 12 hours of previous operation. Bring engine oil level to "full" using oil specified by 

the manufacturer. 

3 Perform fuel change procedure to O2DieselTM. Change fuel filters, purge fuel supply, etc. 

Perform 125 hours of engine operation with the Cummins durability cycle. 

4 Repeat Step 1 as necessary. Operate engine at rated speed and full load for approximately 10 

minutes, then power validate engine. 

5 Conduct transient “full-throttle” torque map from low- to high-idle, and save resulting transient 

command cycle. 

6 Run at least two 20-minute practice EPA transient cycles without engine-off soak between 

cycles, and adjust dynamometer controls to meet statistical requirements for transient cycle 

operation. 

7 Soak engine overnight. Run a cold-start transient cycle. Soak engine for 20 minutes. Run six 

hot-start transient cycles with a 20 minute engine soak between each one. During the cold- and 

the first hot-start cycle, collect samples continuously for regulated emissions, total particulate, 

speciation of volatile hydrocarbon compounds, aldehydes, ketones, alcohols, ethers, and 

particulate-phase polycyclic aromatic hydrocarbons (PAH) and nitrated polycyclic aromatic 

hydrocarbons (NPAH) emissions. During all seven tests, collect samples for vapor-phase PAH 

and NPAH emissions. Combine samples to get a single weighted sample for each test day (one 

seventh cold- and six/sevenths hot-start). 

8 Repeat Step 7 two additional times on different days. 

9 Perform fuel change procedure using 211b baseline fuel. Change fuel filters, purge fuel supply, 

etc. 

10 Repeat Steps 4 through 8. 

11 Summarize data and prepare final report. 

3
FIGURE 1. GRAPHIC REPRESENTATION OF TORQUE AND SPEED COMMANDS 

FOR THE TRANSIENT CYCLE FOR HEAVY-DUTY ENGINES 

2. Heavy-Duty Engine Selection and Description

For the purpose of testing O2DieselTM, a 2002 Detroit Diesel (Serial No. 06R0697970) was selected and

provided to SwRI by O2Diesel, Inc. The engine was selected to meet the following criteria:

• Less than 12 hours on the engine chronometer

• Same type, class, and subclass which consumed the most gallons of fuel in the fuel family over 

the past three years 

• Represent the most common fuel metering system and the most common of the most important 

emission control system devices or characteristics with respect to the emission reduction 

performance for the model year in which testing began 

• One of the five highest selling models from the current model year 

• Unaltered from the specification of the original equipment manufacturer and to remain under the 

control of SwRI throughout the testing. 

Table 2 lists the engine specifications and features, and Figure 2 shows the engine mounted on the test 

stand. 

4
Table 2. Engine Specifications and Features 

Engine Parameter Comment 

Engine Type Diesel, 4-Cycle 

Model 6067-MK60 Series 60® - Truck 

Serial No. 06R0697970 

Configuration L-6 

Displacement 12.7 L (778 CID) 

Bore and Stroke 5.12 in. X 6.30 in. 

Aspiration Turbocharged 

Rated Power at rpm 400 hp at 2100 rpm 

Peak Torque at rpm 1550 lb-ft at 1200 rpm 

Idle Speed 600 rpm 

Governed Idle Speed 2225 rpm 

Combustion System DI, TC, ECM, CAC (Air to Air) 

Engine Family 2DDXH12.7EGL 

Certification 2002 Line Haul 

Date of Manufacture 7/2002 

FIGURE 2. DETROIT DIESEL SERIES 60® MOUNTED ON 

TEST STAND 

5
3. Engine Mapping and Aging Cycle

After the engine was received from O2Diesel, Inc., it was operated for 125 hours with the O2DieselTM

using the Cummins durability cycle. Table 3 presents the durability cycle. The cycle requires about 15

minutes to complete and includes extended operation at peak torque and rated power. At the start of each

cycle, the engine idles for 144 seconds before starting high power operation. The durability cycle was

conducted on a continuous basis to obtain the designated hours of engine operation.

Table 3. Cummins Durability Cycle for Aging and Engine Deterioration Factor 

Determination 

Cycle Description Time, sec 

Idle 144 

Peak Torque 36 

Rated Power 360 

High Idle 36 

Rated Power 144 

Transition to Peak Torque 36 

Peak Torque 108 

High Idle 36 

Total 900 

Emission testing was performed on the engine at the 125-hour point with the O2DieselTM. Figure 3 

illustrates the engine map used for the O2DieselTM tests at 125 hours. Testing consisted of three cold- and 

eighteen hot-start EPA transient sequences with one cold- and six hot-starts performed on each day. At 

the completion of the testing, the fuel was changed to the 211b baseline fuel. About five hours of engine 

operation were then performed. The full emissions characterization sequence with three cold- and 

eighteen hot-start transient tests was then repeated. Figure 4 illustrates the engine map used for the 

emissions characterization tests with the 211b baseline fuel. 

4. Fuel Blending and Analyses

The 211b baseline fuel (EM-4870-F) was obtained as a single batch from Halterman Products. Sufficient

fuel was obtained to perform the initial 125 hours of durability operation and emissions characterization

testing with both fuels. This base fuel was used to blend the O2DieselTM which initially contained 0.6

percent OCTIMAXTM 4931, but the concentration was later raised to 1.0 percent because of phase

separation of the fuel. This situation will be discussed in detail below.

6
FIGURE 3. SPEED AND TORQUE MAP WITH O2DIESELTM 

FIGURE 4. ENGINE SPEED AND TORQUE MAP WITH 211b 

BASELINE FUEL 

7
To obtain the ethanol-based diesel fuel formulation, about 2800 gallons of the 211b baseline fuel were 

blended according to the amounts listed in Table 4. The fuel formulation was blended by starting with 

anhydrous ethanol provided by O2Diesel, Inc. OCTIMAXTM 4931, a proprietary additive technology 

from O2Diesel, Inc., was then blended with the ethanol in drums before adding to the main tank. A 

sample of the ethanol was analyzed by ASTM prior to blending (See Table 5). This mixture was then 

blended with the 211b baseline fuel by circulating the tank for about two hours. (Note: This procedure 

was utilized for the purposes of blending the fuel for durability only.) Durability operation was begun 

with the 0.6 percent concentration of OCTIMAXTM 4931; however, durability was stopped at 

approximately 30 hours when a problem with the engine developed. This problem lead to an examination 

of the fuel. 

Table 4. Initial Blending Components for Preparing O2Diesel 

Blending Component Volume Percent Volume, gallons 

Denatured ethanol 7.7 233.4 

Base Fuel 91.3 2780 

OCTIMAXTM 4931 0.6 18.2 

Table 5. Ethanol Analysis by Protocol D-4806 

Method Property Result 

D1613 Acidity 0.0066 Mg KOH/g 

D4052s 

API@60F 47.2 

Specific Gravity@60F 0.7912 

Density@15C 0.8 

D4176 

Clear &Bright Clear & Bright 

Particulate No 

Free Water No 

Haze 1 

D5453 Sulfur Conc. 1.8 ppm 

D5501 

Ethanol 

95.81 wt. % 

96.54 vol. % 

Methanol <1 wt.% 

D5827 Chloride Content 0 ppm 

D6304 Water Content 0.852 % 

D6423 pHe 7.45 

D381 

Unwashed Gum 3 mg/100 mL 

Washed Gum <0.5 mg/100 mL 

Copper Content <0.05 ppm 

Phase separation of the fuel was noted in the main fuel tank. Samples were taken at various depths within 

the tank (bottom, one foot from the bottom, two feet from the bottom, and at the top of the fuel in the 

8 
tank which was about 3 feet from the bottom). These samples were sent for analysis by ASTM D5501 for 

ethanol content and ASTM D6304 for water content. A distinct phase separation was noted in the sample 

container that was taken from the bottom of the tank. The very bottom layer in the sample container was 

clear with the layer just above being quite cloudy. When the samples were analyzed, an interesting 

distribution of water and ethanol were noted (See Table 6). Messrs. Jim Peeples and Paul Vind, both of 

O2Diesel, Inc., indicated that this situation may occur when water, in excess of 1000 ppm, enters the fuel. 

To prevent phase separation, about 250 gallons from the bottom of the tank were removed and discarded. 

The concentration of OCTIMAXTM 4931 was then increased to 1.0 percent, and the concentration of 

ethanol remaining in the fuel was again measured. Additional anhydrous ethanol was added to the tank to 

bring the concentration back to about 7.7 percent in order to complete the durability testing. A sample of 

the fuel was taken and analyzed for ethanol and water. For emission measurements, a portion of the 

original 211b baseline fuel was blended with 1.0 percent OCTIMAXTM 4931 and 7.7 percent ethanol in a 

drum (EM-4904-F). Table 7 presents the measured fuel properties for the base fuel and the fuel used for 

emission measurements. 

Table 6. Ethanol and Water Content from Main Fuel Tank After Phase Separation 

Sample Position Ethanol, wt. % Water, ppm 

Top 5.3 846 

2 ft from Bottom 5.3 867 

1 ft from Bottom 5.1 1119 

Top Phase (Bottom) 0.7 619 

Bottom Phase (Bottom) 49.97 499670 

5. Unscheduled Maintenance

During initial engine operation (4.7 hours), an error code was noted and a loss in engine power was

observed. The engine error code indicated that the engine was not receiving a signal from the vehicle

speed sensor. Apparently, this engine was originally set up as a truck engine, and the electronic control

module (ECM) required a signal for vehicle speed. This signal was disabled to resolve the problem, and

durability operation was continued. 

At about 29.1 hours of operation, a drop in power was once again observed. When the error codes were 

examined, the power loss was determined to originate in Cylinder 4. The error code indicated that the 

injector pulse response time was very short, and the injector was not functioning properly. Durability was 

continued to 29.8 hours while engine diagnostics were being performed. When the engine was stopped, 

the power had decreased by about 15 percent. At this point, the error codes indicated that Cylinders 4, 5, 

and 6 were not functioning properly due to short pulse response time, with Cylinder 4 having a total loss 

in power. No problems were noted for Cylinders 1 through 3. The injectors were removed and sent to M 

& D Distributors to be examined for a pop test and disassembled. According to Mr. Paul Vind, O2Diesel, 

Inc., the injectors showed a good pop test. M & D Distributors was unable to flow test the injectors 

because they did not have the correct apparatus. The injectors were disassembled and no wear was 

observed, nor was any physical fault with the injectors observed. In addition, samples of the base fuel 

and O2DieselTM were analyzed for lubricity using ASTM D6078 and ASTM D6079. Table 8 presents the 

results of these measurements. These results indicated that the fuel lubricity of O2DieselTM was even 

better than the base fuel with a higher seize weight for the Ball On Cylinder Lubricity Evaluation 

(BOCLE) and a smaller scar with the High Frequency Reciprocating Rig (HFRR). 

9
--

-- --

-- --

-- --

Table 7. Fuel Analysis 

Fuel Property 

211(b) 

Specification 

for Base Fuel 

Analysis 

Base Fuel 

(EM-4870-F) 

Durability Fuel 

(EM-4873-F) 

Emissions Fuel 

(EM-4904-F) 

API Gravity 33±1 32.2 33.5 33.3 

Sulfur, wt% 0.05±0.0025 0.0508 0.0425 0.0447 

Cetane Number 45.2±2 43.5 40.8 45.4 

Cetane Index 45.7±2 43.7 42.6 45.1 

Aromatics, vol % 38.4±2.7 38.1 37.2 37.6 

Olefins, vol % 1.5±0.4 1.7 1.8 2.2 

Saturates, vol % 60.1±2.0 60.2 53.3 53.1 

Distillation Parameters 

10%, °F 433±5 428 173 172 

50%, °F 516±5 520 507 512 

90%, °F 606±5 601 601 608 

Additives 

Corrosion Inhibitor, ptba Required 4.5 –b 

Demulsifier, ptb Required 2 

Anti-oxidant, ptb Required 2 

Metal Deactivator, ptb Required 2 

a

ptb-pounds per thousand barrels b

Concentration not increased over the amount in the base fuel 

Table 8. Lubricity Measurements 

ASTM Method Property Base Fuel O2DieselTM 

D6078 BOCLE, g 4150 6050 

D6079 HFRR, mm 0.37 0.214 

Each injector was reassembled and reinstalled in the engine with Injector 4, 5, and 6 being placed in 

positions 1, 2, and 3 to see if a similar loss in engine power was observed in the new positions. This 

installation showed the same loss in total engine power except that the error codes shifted with the 

injectors rather than the location. New injectors were ordered and installed. In a conference call between 

Jim Peeples, O2Diesel, Inc., and with Dave Kortum from the EPA, it was determined that, under the 

regulations, a post-maintenance emissions test was not required if engine maintenance was conducted 

10
during the 125-hour engine break-in. However, if the maintenance was required during the emissions 

testing part of the program, then a post-maintenance emissions test would be required. Engine durability 

was continued at 29.8 hours with the new injectors to complete a total of 125 hours of engine operation. 

At that point, the engine was placed in a transient-capable test cell for emissions testing. 

11
III. Description of Analytical Methods 

Regulated and unregulated emission measurements conducted for this program, as required by the 

Environmental Protection Agency (EPA), included the following items: 

• Measurement of regulated emissions including total hydrocarbons (THC), carbon monoxide 

(CO), oxides of nitrogen (NOx), and total particulate 

• Speciation of vapor-phase and semi-volatile hydrocarbon compounds, alcohols, ethers, 

aldehydes, and ketones conducted for the first cold- and hot-start segment of the FTP 

• Measurement of semi-volatile (vapor- and particulate-bound) PAH and NPAH. PAH compounds 

included: benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, 

chrysene, dibenzo[a,h]anthracene, and indeno[1,2,3-cd]pyrene; and NPAH compounds included: 

7-nitrobenzo[a]anthracene, 6-nitrobenzo[a]pyrene, 6-nitrochrysene, 2-nitrofluorene, and 1-

nitropyrene. 

Regulated emissions (THC, CO, NOx, and particulate) and carbon dioxide (CO2) were analyzed 

according to Code of Federal Regulations (CFR) Title 40 specifications, and all applicable accuracy and 

calibration requirements were met. Analyses of unregulated emissions were conducted according to 

CRC, EPA, and SwRI analytical procedures. Applicable SwRI Standard Operating Procedures are listed 

in References 1 through 20. Table 9 presents the sampling requirements for each of the measured 

emissions. 

A. Regulated Emissions 

Regulated emissions were quantified in a manner consistent with EPA protocols for heavy-duty 

emissions testing as given in 40 CFR Part 86, Subpart D. Proportional exhaust gas samples were 

collected in Tedlar bags and analyzed for CO and CO2 using non-dispersive infrared (NDIR) instruments, 

THC and NOx were monitored continuously using a flame ionization detector and a chemiluminescent 

instrument, respectively. Wet absorption techniques were employed to collect alcohols, ethers, aldehydes 

and ketones. These wet absorption techniques are discussed in more detail below. 

Two sizes of filters were used to collect particulate samples. These filters included the following: 

• One set of 90-mm Pallflex (fluorocarbon-coated glass fiber) filters for determination of total 

particulate mass 

• 20×20-inch Pallflex (fluorocarbon-coated glass fiber) filters for total dilute exhaust filtration of 

particulate; all filters were extracted individually for PAH and NPAH analyses. 

12
Table 9. Sample Collection 

Test 

Code 

Test 

Day 

Regulated 

THC, CO, NOx, Part. 

Speciation 

C1 - C12 

Aldehydes/ 

Ketones 

Alcohols 

and 

Ethers 

PAH/NPAH 

Vapor Particulate 

O2DieselTM 

4904-C1 

1 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF 

Traps 

1 20×20 Filter 

4904-H1 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 Filter 

4904-H12 

4904-H13 

4904-H14 

4904-H15 

4904-H16 

4904-C2 

2 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF Traps 

1 20×20 Filter 

4904-H21 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 Filter 

4904-H22 

4904-H23 

4904-H24 

4904-H25 

4904-H26 

4904-C3 

3 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF Traps 

1 20×20 Filter 

4904-H31 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 Filter 

4904-C32 

4904-H33 

4904-H34 

4904-H35 

4904-H36 

211b Baseline Fuel 

4870-C1 

4 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF Traps 

1 20×20 Filter 

4870-H11 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 Filter 

4870-H12 

4870-H13 

4870-H14 

4870-H15 

4870-H16 

Blank 1 4 PUF Traps 1 20×20 Filter 

13
Table 9 (Cont’d). Sample Collection 

Test Code Test 

Day 

Regulated 

THC, CO, NOx, Part. 

Speciation 

C1 - C12 

Aldehydes/ 

Ketones 

Alcohols 

and 

Ethers 

PAH/NPAH 

Vapor Particulate 

4870-C2 

5 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF Traps 

1 20×20 

Filter 

4870-H21 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 

Filter 

4870-H22 

4870-H23 

4870-H24 

4870-H25 

4870-H26 

4870-C3 

6 

Cont., Bag, 90mm Filter Bag Bubbler Bubbler 

4 PUF Traps 

1 20×20 

Filter 

4870-H31 Cont., Bag, 90mm Filter Bag Bubbler Bubbler 1 20×20 

Filter 

4870-H32 

4870-H33 

4870-H34 

4870-H35 

4870-H36 

All filters were conditioned and weighed in accordance with the appropriate sections of the CFR for 

heavy-duty engines. 

B. Speciation of Volatile Hydrocarbon Compounds 

Volatile hydrocarbon compounds were determined by hydrocarbon speciation. Analytical procedures for 

conducting the hydrocarbon speciation (C1 to C12 hydrocarbons, aldehydes, and ketones) were similar to 

the CRC Auto/Oil Phase II methods. With these methods, exhaust emissions samples are analyzed for the 

presence of more than 200 different exhaust species. Four gas chromatography (GC) procedures and one 

High Performance Liquid Chromatograph (HPLC) procedure were used to identify and quantify specific 

compounds. One GC is used for the measurement of methane, a second for C2-C4 species, and a third for 

C5-C12 species including two ethers (methyl tertiary butyl ether - MTBE and ethyl tertiary butyl ether -

ETBE). A fourth GC was used to measure 1-methylcyclopentane, benzene, toluene, and 2,3,3-

trimethylpentane, which co-elute and cannot be accurately quantified by other methods. In general, all 

emission “sample” bags were analyzed before the “background” bags, so that reactive exhaust 

compounds could be analyzed as quickly as possible. A brief description of these procedures is given 

below. 

14
1. Methane Speciation

Methane levels were determined using proportional exhaust gas samples collected in Tedlar bags. A GC

equipped with an FID was utilized for the analyses, and was used in accordance with SAE J1151

procedures. The GC system was equipped with a packed column to resolve methane from other

hydrocarbons in the sample. Samples were introduced into a 5-mL sample loop via a diaphragm pump.

For analysis, the valve was switched to the inject position, and the helium carrier gas swept the sample

from the loop toward the detector through a 61 cm × 0.3 cm Porapak N column in series with a 122 cm ×

0.3 cm molecular sieve 13X column. As soon as the methane peak passed into the molecular sieve

column, the helium flow was reversed through the Porapak N column to vent. For quantification, sample

peak areas were compared to those of external calibration standards.

2. C2-C4 Species

With the aid of a DB-WAX pre-column and a 10-port switching valve, the second GC procedure allows

the separation and determination of exhaust concentrations of C2-C4 individual hydrocarbon species,

including: ethane; ethylene; acetylene; propane; dimethylpropane; propyne; 1,3-butadiene; 2-

methylpropane; 1-butyne; and cis-2-butene. Bag samples were analyzed with a GC system which utilizes

a Hewlett-Packard Model 5890 Series II GC with an FID, two pneumatically operated and electrically

controlled valves, and two analytical columns. The carrier gas was helium. One column is utilized to

separate the C2-C4 hydrocarbons from the higher molecular weight hydrocarbons and the polar

compounds. These higher molecular weight hydrocarbons (and water and alcohols) are retained on the

pre-column while the C2-C4 hydrocarbons are passed through to the analytical column. While the C2-C4

hydrocarbons are separated on the analytical column, the pre-column is back-flushed with helium to

prepare for the next run. The column flow was set by fine-tuning the column head pressure to give butane

a retention time of 5.25 ± 0.05 minutes. The GC was calibrated daily using a CRC Auto/Oil 23-

component calibration mixture. Detection limits for the procedure were on the order of 5 ppbC in dilute

exhaust for all compounds.

3. C5-C12 Species

The third GC procedure provides separation and exhaust concentrations for more than 100 C5-C12

individual hydrocarbon compounds. Bag samples were analyzed using a gas chromatograph equipped

with an FID. The GC system utilizes a Hewlett-Packard Model 5890 Series II GC with an FID, a

pneumatically operated and electrically controlled valve, and a DB-1 fused silica open tubular column

(FSOT). The carrier gas was helium. Gaseous samples are pumped from the bag through a sample loop

and then introduced into a liquid nitrogen cooled column. The column oven was then programmed to a

maximum temperature of 200°C. The analog signal from the FID was sent to a networked computer

system via a buffered analog to digital converter. Column flow was set by fine-tuning the column head

pressure to give propane a retention time of 5.40 ± 0.10 minutes using a temperature program. The GC

was calibrated daily using a CRC Auto/Oil 23-component calibration mixture. Detection limits for the

procedure are on the order of 10 ppbC in dilute exhaust for all compounds.

4. Benzene and Toluene

The fourth GC procedure uses a separate system configured similarly to the third GC method (but

utilizing a DB-5 analytical column instead of a DB-1 FSOT column) to resolve individual concentrations

of benzene and toluene according to the CRC Auto/Oil Phase II Protocols. Separation of benzene and

toluene from co-eluting peaks was carried out by fine-tuning the column head pressure to give benzene a

retention time of 22 to 23 minutes. The GC was calibrated daily using a CRC 7-component calibration

mixture.

5. Aldehydes and Ketones

An HPLC procedure was utilized for the analysis of aldehydes and ketones. Samples were collected by

bubbling dilute exhaust at a nominal flowrate of 4 L/min through chilled glass impingers containing an

15
acetonitrile solution of 2,4-DNPH and perchloric acid. For analysis, a portion of the acetonitrile solution 

was injected into a liquid chromatograph equipped with a UV detector. External standards of the 

aldehyde and ketone DNPH derivatives were used to quantify the results. The aldehydes and ketones 

measured were: formaldehyde, acetaldehyde, acrolein, acetone, propionaldehyde, crotonaldehyde, 

isobutyraldehyde/methylethylketone (not resolved from each other during normal operating conditions, 

and so split equally between the two compounds), benzaldehyde, valeraldehyde, o-tolualdehyde, mtolualdehyde/p-tolualdehyde (not resolved from each other during normal operating conditions, and so 

reported together), and hexanaldehyde. Detection limits for this procedure are on the order of 0.005 ppm 

aldehyde or ketone in dilute exhaust. 

C. Alcohols and Ethers 

The measurement of alcohols and ethers in exhaust was accomplished by bubbling the exhaust through 

glass impingers containing deionized water. Two glass impingers in series, with each containing 25 mL 

of deionized water were used to collect exhaust samples for the analysis. The two glass impingers collect 

99+ percent of the lower molecular weight alcohols which are soluble in water. Table 10 lists a number 

of alcohols and ethers that range in solubility from miscible to slightly soluble in water. The temperature 

of the collection impingers was maintained at 0-5°C with an ice water bath, and the flow rate through the 

impingers was maintained at 4 L/minute by the sample pump. A dry gas meter was used to determine the 

total flow through the impingers. The temperature of the gas stream was monitored by a thermocouple 

immediately prior to the dry gas meter. A drier was included in the system to prevent condensation in the 

pump, flowmeter, dry gas meter, etc. The flowmeter in the system allowed continuous monitoring of the 

sample to ensure proper flowrates during the sampling. The Teflon line connecting the CVS and the 

solenoid valve was heated to approximately 235°F in order to prevent water from condensing in the 

sample line. 

The exhaust sample was collected continuously during the test cycle. Upon completion of each transient 

cycle, the impingers were removed, and the contents were transferred to a 30 mL polypropylene bottle 

and capped. For analysis, a 1.0 μL portion of the aqueous solution was injected into a Hewlett-Packard 

5890 GC equipped with a FID and a 7673 auto sampler. The analytical column was a 0.32 mm X 30 m 

DB-WAX column with a 1.0 μm film thickness. The carrier gas was helium and was set to give optimum 

separation (20 mL/minute). To quantify the results, the sample peak areas were compared to the peak 

areas of standard solutions. External standards containing methanol and ethanol in deionized water were 

used to quantify the results. In addition, 1-propanol, 2-propanol, and tertiary butanol were analyzed for 

retention time identification should they have appeared. No other compounds were detected in the water 

samples and, if present, were below the detection limits for the procedure. Detection limits for the lower 

molecular weight alcohols with this procedure are on the order of 0.06 ppm in dilute exhaust. 

16
Table 10. Selected C1 to C6 Alcohols and Ethers That Have Some Solubility in Water 

Compound Empirical Formula 

Alcohols 

Methanol CH4O 

Ethanol C2H6O 

2-Propyn-1-ol C3H4O 

Allyl alcohol C3H6O 

Isopropanol C3H8O 

n-Propanol C3H8O 

Crotyl alcohol C4H8O 

n-Butanol C4H10O 

sec-Butanol C4H10O 

tert-Butanol C4H10O 

Isobutanol C4H10O 

Furfuryl alcohol C5H6O2 

2-Methyl-3-butyn-2-ol C5H8O 

Cyclopentanol C5H10O 

Tetrahydrofurfuryl alcohol C5H10O2 

Isopentanol C5H12O 

2-Methyl-1-butanol C5H12O 

3-Methyl-2-butanol C5H12O 

Neopentanol C5H12O 

1-Pentanol C5H12O 

2-Pentanol C5H12O 

3-Pentanol C5H12O 

tert-Pentanol C5H12O 

Phenol C6H6O 

3-Methyl-1-pentyn-3-ol C6H10O 

17
Table 10 (Cont.) Selected C1 to C6 Alcohols and Ethers That Have Some Solubility in 

Water 

Compound Empirical Formula 

Cyclohexanol C6H12O 

4-Hydroxy-4-methyl-2-pentanone C6H12O2 

2,2-Dimethyl-1,3-dioxolane-4-methanol C6H12O3 

2,5-Tetrahydrofurandimethanol C6H12O3 

1-Hexanol C6H14O 

Ethers 

Methyl ether C2H6O 

Methyl ethyl ether C3H8O 

Vinyl ether C4H6O 

Cyclopropyl methyl ether C4H8O 

Ethyl ether C4H10O 

Methyl propyl ether C4H10O 

Isopropyl ether C6H14O 

Propyl ether C6H14O 

D. PAH and NPAH 

In addition to the regulated and C1 to C12 hydrocarbon exhaust emissions, semi-volatile (vapor- and 

particulate-phase) PAH and NPAH compounds were also determined for each fuel. Seven PAH 

compounds were quantified: benzo[a]anthracene, benzo[b]fluoranthene, benzo[k]fluoranthene, 

benzo[a]pyrene, chrysene, dibenzo[a,h]anthracene, and indeno[1,2,3-cd]pyrene; and five NPAH 

compounds: 7-nitrobenzo[a]anthracene, 6-nitrobenzo[a]pyrene, 6-nitrochrysene, 2-nitrofluorene, and 1-

nitropyrene. A 400 in2

 fluorocarbon-coated glass fiber filter (20×20-inch Pallflex filter) was used to 

collect the particulate-phase PAH and NPAH, and a PUF/XAD/PUF sandwich adsorbent trap was used to 

collect the vapor-phase PAH and NPAH. The PUF/XAD/PUF traps contained a layered sampling media 

consisting of a 1.25 inch deep layer of polyurethane foam (PUF), a 0.5 inch deep layer of XAD-2 resin, 

and a second 1.25 inch deep layer of PUF. The XAD-2 resin was incorporated to improve the trapping 

efficiency for NPAH compounds, which were potentially present in much lower levels than PAH 

compounds. 

Both XAD-2 and PUF sample media were cleaned prior to use as described below. The XAD-2 was 

cleaned by siphoning four times with water using a Soxhlet followed by the residual water being 

vacuumed off, Soxhlet extracted with methanol for 24 hours, Soxhlet extracted with toluene for 48 hours, 

and finally Soxhlet extracted with methylene chloride for 48 hours. The residual methylene chloride was 

removed as much as possible and then totally removed by purging with heated nitrogen. For PUF 

cleaning, each foam disk was Soxhlet extracted for 24 hours with acetone, for 48 hours with 

hexane/ether, and finally for 24 hours with acetone. 

18
Vapor- and particulate-phase PAH and NPAH samples were obtained using a separate secondary dilution 

tunnel, which was operated in parallel with a smaller secondary dilution tunnel used to obtain the 90-mm 

filter samples for particulate mass determinations. The PAH and NPAH tunnel was considerably larger 

than the one with 90-mm filter to allow for the use of 20×20-inch Pallflex sampling media for the 

particulate-phase PAH and NPAH compounds and the use of the four specially designed PUF/XAD/PUF 

traps for the vapor-phase PAH and NPAH compounds. Filter samples were generated during the coldstart and the six hot-start tests, although only samples from the cold-start and the first hot-start were 

analyzed individually. PUF/XAD/PUF trap samples were collected during the entire test sequence (one 

cold- and six hot-starts combined). 

Vapor-phase PAH and NPAH samples presented a particular problem for heavy-duty sampling because 

conventional sampling techniques would not allow for sufficient sample to be gathered to meet EPA 

detection requirements. Commercially available sampling media and hardware were of insufficient size 

to allow for the collection of sample volumes needed to meet these detection limits. Sampling media size 

was also limited by the ability to extract and concentrate samples obtained. Therefore, an approach was 

devised involving both custom built sampling hardware and a modified sampling plan. The 

PUF/XAD/PUF traps were sized to allow a media diameter of 4 inches, rather than the conventional 2.5 

inches. This larger diameter allowed a much higher flowrate to be used, while maintaining the face 

velocity within recommended levels for the smaller, conventional sampling media. 

The combination of using four larger sample media cartridges and the collection of samples over multiple 

test runs allowed for the accumulation of a sample volume similar to that passing through a 20×20-inch 

filter during a single test (roughly 3000 standard cubic feet of dilute exhaust). This volume of dilute 

exhaust sample was sufficient for the analysis to meet the required detection threshold of 1 ng/hp-hr. A 

sample set for a given test day consisted of a cold-start filter sample, a hot-start filter sample, and a set of 

four PUF/XAD/PUF traps for the vapor-phase PAH and NPAH. Background PAH and NPAH sample 

sets were obtained by operating the sampling systems with sampling media loaded, but without the 

engine operating, for about two hours. 

Following testing, sample sets were delivered to the laboratory for analysis. In cases where immediate 

extraction was not possible, samples were stored at 4°C. Filters and PUF/XAD/PUF traps were extracted 

separately. Prior to extraction of the filters, each filter was spiked with a surrogate solution containing 

100 ng each of six deuterated PAH: benzo[a]anthracene-d12, chrysene-d12, benzo[b]fluoranthene-d12, 

benzo[k]fluoranthene-d12, benzo[a]pyrene, and dibenzo[a,h]anthracene-d14 in order to verify recovery 

during the extraction process. The samples were then Soxhlet extracted for 8 hours with ethanol/toluene 

(70/30 v/v). Prior to extraction, each PUF/XAD/PUF trap was spiked with a surrogate solution 

containing 200 ng each of six deuterated PAH: benzo[a]anthracene-d12, chrysene-d12, 

benzo[b]fluoranthene-d12, benzo[k]fluoranthene-d12, benzo[a]pyrene, and dibenzo[a,h]anthracene-d14 

in order to verify recovery during the extraction process. The trap samples were then extracted for at least 

8 hours with methylene chloride. At this point, both filter and trap samples were treated similarly. One 

half of each filter or trap extract was cleaned using dilute sulfuric acid and an activated silica gel column. 

The extracts were then reduced to 500 μL in toluene; and just prior to analysis, 100 μL of the extract was 

spiked with 30 ng of benzo[e]pyrene-d12 for PAH and 10 ng each of 2-nitrofluorene-d9, 1-nitropyrened9, 6-nitrochrysene-d11, and 6-nitrobenzo[a]pyrene-d11 for NPAH. 

Samples for both the vapor- and the particulate-phase PAH and NPAHs were analyzed by GC/MS (gas 

chromatograph/mass spectroscopy) using an Agilent 5973N MSD with a 30 m X 0.32 mm i.d. DB-5 

column and a 0.25 μm film thickness. For each analysis, a 2 μL aliquot of the sample extract was injected 

into the instrument. A calibration curve consisting of at least five points was obtained prior to sample 

analysis to ensure linearity, and a mid-point continuing calibration was performed each day after the 

19
initial five point calibration. Analysis of NPAH compounds was performed using the negative ion 

chemical ionization (NI/CI) mode and for PAH compounds using the positive ion electron impact (PI/EI) 

mode. Two or three characteristic ions for each PAH and NPAH were monitored. Separate GC/MS 

analyses were necessary to acquire both the PAH and NPAH data. Each target compound met the 

criterion of a 30 percent relative response (RRF) factor and 30 percent deviation in relation to the mean 

RRF obtained in the initial and continuing calibration. 

20
IV. Quality Control and Quality Assurance 

In order to demonstrate SwRI’s constant goal to provide quality emissions data in our project efforts, the 

Department of Emissions Research maintains accreditation to ISO 9002 and ISO/IEC Guide 25 

standards. Standard operating procedures and routine instrument calibration and calibration records are 

included in these standards. Based on the successful completion of laboratory audits, the SwRI 

Department of Emissions Research is able to maintain registration under ISO 9002, “Model for Quality 

Assurance in Production and Installation,” and accreditation by ISO/IEC Guide 25, General 

Requirements for the Competence of Calibration and Testing Laboratories.” Presented below is the 

SwRI Department of Emissions Research Quality Policy Statement: 

SwRI Department of Emissions Research Quality Policy Statement 

“A key dimension of the services we provide is high quality that is selfevident to our clients and the technical community. Every individual 

contribution to our research, development, evaluation, and certification 

projects is intended to further our clients’ success and to fulfill the 

mission of the Institute. Our commitment is to continuously improve our 

ability to meet changing needs in our discipline and deliver all we have 

agreed to do, or more, while sustaining a climate of consideration and 

adherence to ethical standards in our workplace. Implementation of our 

quality program will be relied on for maintaining our market position, 

our personal growth and satisfaction, and the long-term expansion of 

our activity.” 

Throughout this project, SwRI implemented our QA/QC plan in a manner consistent with the program 

objectives, including spot-checking of records, accuracy/precision charts, notebooks, calibration tags, and 

other quality control elements including chain of custody of samples. Listed below are a few of the 

regular procedures that ensure the quality standards are maintained. 

• Senior Scientist/Technician Review - A system for formal data review is in place in the SwRI 

DER. All technicians review their work prior to submitting it to the data computations laboratory 

for calculation of final concentrations. The Project Leader reviews the results before a test is 

accepted. 

• Interlaboratory Comparisons/Round Robins - SwRI has participated in numerous Round 

Robin exercises to correlate the results of our laboratory with other accepted facilities. Those 

Round Robin studies which are directly related to this project include: CRC Round Robin 

Analysis of Alcohol and Carbonyl Synthetic Exhaust Samples (results published in SAE Paper 

No. 941944); and CRC Round Robin Hydrocarbon Speciation Analysis of Synthetic Exhaust Gas 

(results not yet published). 

• Lab Audits - Internal audits are conducted by the DER Quality Coordinator as specified in DER 

Quality Policy and Program 12, "Internal Audits." 

• Project Records - Documents directly associated with a technical project, such as: 

correspondence, proposals, contracts, work orders, cost sheets, invoices, interim and final 

reports, and follow-up contacts are maintained. All records come under Standard Operating 

Procedure (SOP), document SOP-14-001, "Storage and Maintenance of DER Records" 

(Reference 21). 

• Calibration Records - Data sheets, chart recordings, computer printouts, log books, calibration 

and maintenance logs, and spreadsheets associated with the calibration of measurement 

equipment are maintained. Also includes calibration results from external suppliers. 

• Engine and Vehicle Testing Records - Data sheets, chart recordings, log books, start/stop logs, 

21
and computer printouts associated with evaluation and testing of engines and vehicles are 

retained. 

• Chemistry Calibration and Analysis Records - Data sheets, log books, and spreadsheets 

associated with calibration and analyses performed in the chemistry areas are retained. 

• Data Reduction and Test Result Records - Computed results, tables, and spread sheets 

generated using information obtained from emissions testing and chemical analysis are 

maintained. Records developed in the areas specified in SOP 14-001 are retained for a period of 

ten years. 

22
V. Test Results 

Emission testing was performed on the exhaust from a 2002 Detroit Diesel heavy-duty diesel engine. 

Tests with O2DieselTM were performed after a total of 125 hours of engine operation with the fuel. Three 

cold- and eighteen hot-start tests were utilized for the emissions characterizations. The fuel was changed 

to the 211b baseline fuel, durability operation was performed for about five hours, and an additional set 

of emissions tests were conducted. 

A. Regulated Emissions 

After the 125 hours of engine operation, the average composite regulated emissions were lower than or 

equal to the corresponding 2002 emission standards with both fuels, except for particulate. When CO, 

NOx, and particulate emissions with the O2DieselTM were compared to the 211b baseline fuel, the 

O2DieselTM was found to produce about 6 percent lower CO and NOx emissions and about 7 percent 

lower particulate emissions. The THC emissions were increased by about 40 percent when compared to 

the 211b baseline fuel. Table 11 summarizes the regulated emissions with each fuel. Appendix A 

contains the individual and composite emission test results. 

B. Speciation of Volatile Hydrocarbon Compounds 

Speciation of the volatile hydrocarbon compounds with carbon numbers from C1 to C12 plus aldehydes, 

ketones, and two ethers (methyl tertiary butyl ether - MTBE and ethyl tertiary butyl ether - ETBE) was 

performed for each cold- and hot-segment of the EPA transient cycle. More than 200 compounds were 

checked for their presence in the dilute exhaust. Data for the individual compounds, corrected for 

background dilution air contributions, are included in Appendix B. A composite result for the triplicate 

tests is also included in Appendix B. 

In general, all compounds found in the exhaust with the O2DieselTM were also found in the exhaust with 

the 211b baseline diesel fuel. One exception was with an unidentified C8 compound that was detected at 

very low concentrations in only two of the three hot-start tests with the O2DieselTM. No additional 

compounds were found in the exhaust from the O2DieselTM as compared to the 211b baseline fuel at or 

above the detection limits for the analytical procedures. 

23
Table 11. Summary of Regulated Emissions 

Test 

Emissions Results, g/bhp-hr 

THC CO NOx Particulate 

2002 Standard 1.3 16 4.0 0.10 

O2DieselTM 

4904 C1 0.32 1.9 3.9 0.17 

4904 H11 0.26 1.4 3.4 0.13 

Composite 0.27 1.5 3.4 0.13 

4904 C2 0.29 1.8 4.0 0.17 

4904 H21 0.27 1.5 3.5 0.13 

Composite 0.27 1.5 3.6 0.13 

4904 C3 0.37 1.9 4.0 0.15 

4904 H31 0.30 1.5 3.6 0.13 

Composite 0.31 1.6 3.6 0.13 

Average of Three Composites 0.28 1.5 3.6 0.13 

211b Baseline Fuel 

4870 C1 0.23 1.9 4.0 0.15 

4870 H11 0.15 1.5 3.7 0.13 

Composite 0.16 1.6 3.8 0.13 

4870 C2 0.34 2.0 4.1 0.17 

4870 H21 0.22 1.5 3.8 0.13 

Composite 0.24 1.6 3.8 0.14 

4870 C3 0.36 2.1 4.0 0.17 

4870 H31 0.19 1.6 3.7 0.14 

Composite 0.21 1.7 3.7 0.15 

Average of Three Composites 0.20 1.6 3.8 0.14 

24
While no additional compounds which could be identified were found with the O2DieselTM, some 

differences did occur in the individual concentrations. Six compounds were detected in the 211b baseline 

diesel fuel that were not detected with the O2DieselTM. These compounds included: 

• butane 

• trans-2-butene 

• 3-methyl-1-butene 

• hexane 

• 2,4-dimethylhexane 

• trans-4-octene. 

In addition, five aldehydes (formaldehyde, acetaldehyde, acrolein, acetone, and benzaldehyde) were 

detected at 27, 54, 72, 54, and 85 percent higher concentration, respectively, in the O2DieselTM than in 

the exhaust of the 211b baseline diesel fuel. Some compounds were also found in either one or more of 

the cold- or one or more of the hot-starts during the triplicate test sequence. In other cases, some 

compounds were detected at less than two times the detection limit for the compound when calculated as 

a composite value or as an average. These compounds are labeled as “trace” in the Appendix tables. 

C. Alcohols and Ethers 

The only alcohols or ethers up to C6 that were detected with either of the two fuels were methanol, 

ethanol, and isopropanol. Methanol was detected in the exhaust from the O2DieselTM at about the same 

concentration as levels found in the exhaust from the 211b baseline fuel. Isopropanol was detected in 

trace amounts with both fuels. Ethanol was detected at about an order of magnitude greater in the exhaust 

from the O2DieselTM when compared to the levels found in the exhaust from the 211b baseline fuel. 

These results were expected because ethanol is a component of the fuel formulation for the O2DieselTM. 

While the other water soluble alcohols and ethers were below the detection limit, one cannot conclude 

that these compounds were present or not present; but if present, they were below the limits of detection. 

Table 12 lists the results for these analyses. 

D. PAH and NPAH 

Vapor- and particulate-phase semi-volatile PAH and NPAH compounds were also determined for each 

fuel. The seven PAH compounds included: benzo[a]anthracene, benzo[b]fluoranthene, 

benzo[k]fluoranthene, benzo[a]pyrene, chrysene, dibenzo[a,h]anthracene, and indeno[1,2,3-cd]pyrene; 

and the five NPAH compounds included: 7-nitrobenzo[a]anthracene, 6-nitrobenzo[a]pyrene, 6-

nitrochrysene, 2-nitrofluorene, and 1-nitropyrene. The analytical procedure used to measure these 

compounds was able to detect less than 1 ppm (equivalent to 1 ng/mg organic extract) for this analysis. 

Values were reported in terms of ng/bhp-hr. Samples were collected from the vapor- and particulatephases of exhaust. Table 13 presents the vapor-phase PAH and NPAH results, and Table 14 presents the 

particulate-phase results. 

25
Table 12. Vapor Phase Alcohol Results 

Compound 

Cold Hot Composite Cold Hot Composite Cold Hot 

mg/hp-hr mg/hp-hr mg/hp-hr mg/hp-hr mg/hp-hr mg/hp-hr mg/hp-hr mg/hp-hr 

O2DieselTM 

Methanol 2.6 2.4 2.4 4.7 4.1 4.2 6.0 7.1 

Ethanol 29 28 28 27 29 29 35 35 

1-Propanol NDa ND ND ND ND ND ND ND 

2-Propanol Traceb Trace Trace Trace Trace Trace Trace Trace 

t-Butanol ND ND ND ND ND ND ND ND 

211b Baseline Fuel 

Methanol 6.3 4.2 4.5 3.4 1.8 2.0 4.6 4.4 

Ethanol 5.2 2.8 3.1 13.1 2.4 3.9 1.9 1.4 

1-Propanol ND ND ND ND ND ND ND ND 2-Propanol Trace ND Trace Trace ND Trace ND Trace 

t-Butanol ND ND ND ND ND ND ND ND 

aND - None detected. bTrace - Value not quantifiable. 

Note: No other alcohols were detected at the limits of detection for this procedure. 

26

Table 13. Vapor Phase Semi-Volatile PAH and NPAH Results 

Compound 

O2DieselTM, ng/hp-hr 211b Baselin

Composite 

C1 

Composite 

C2 

Composite 

C3 

Average Composite 

C1 

Composite 

C2 

2-Nitrofluorenea NDb ND ND ND ND ND 

1-Nitropyrenec ND ND ND ND ND ND 

7-Nitrobenz(a)anthracene 5.6 6.8 6.4 6.3 5.5 5.8 

6-Nitrochrysenec ND ND ND ND ND ND 

6-Nitrobenz(a)pyrenec ND ND ND ND ND ND 

Benzo(a)anthracene 10 16 13 13 5.1 5 

Chrysene 17 16 19 17 2.7 4.1 

Benzo(b)fluoranthene 2.4 4.5 4.1 3.7 1.2 1.2 

Benzo(k)fluoranthene 3.2 5.2 4.4 4.3 3.5 3.9 

Benzo(a)pyrene 3.9 4.7 4.8 4.5 1.9 2.6 

Indeno[1,2,3-cd]pyrene 2.3 3.5 3.6 3.1 1.5 1.1 

Dibenz(a,h)anthracenec ND ND ND ND ND ND 

aDetection limit in ng/hp-hr calculated using the minimum value that could be quantified by the analytical procedure; if pres

concentration less than 0.4 ng/hp-hr. 

bND - None detected; calculated detection indicated. cDetection limit in ng/hp-hr calculated using the minimum value that could be quantified by the analytical procedure; if pres

concentration less than 0.8 ng/hp-hr. 

27

Table 14. Particulate Phase Semi-Volatile PAH and NPAH Results 

Compound 

C1, ng/hp-hr C2, ng/hp-hr C3, ng/hp-hr 

Cold Hot Composite Cold Hot Composite Cold Hot Co

O2DieselTM 

2-Nitrofluorene 19 9.9 11 14 10 11 9.8 20 

1-Nitropyrene 168 94 105 150 77 87 105 68 

7-Nitrobenz(a)anthracene 9.5 9.9 9.8 9.6 5 5.7 20 20 

6-Nitrochrysenea traceb trace trace NDc trace trace trace ND 

6-Nitrobenz(a)pyrenea ND ND ND ND ND ND ND trace 

Benzo(a)anthracene 6200 4900 5100 4400 3500 3600 4400 4000 

Chrysene 12300 10300 10600 8800 7800 7900 8200 6000 

Benzo(b)fluoranthene 3400 2300 2400 2800 2900 2700 3200 2800 

Benzo(k)fluoranthene 3500 3400 3400 2600 2300 2300 2900 2200 

Benzo(a)pyrene 4700 4000 4100 4000 3900 3900 3900 3600 

Indeno[1,2,3-cd]pyrene 2300 2100 2200 1900 2100 2000 2100 1800 

Dibenz(a,h)anthracene 208 136 146 118 124 123 141 95 

aDetection limit in ng/hp-hr calculated using the minimum value that could be quantified by the analytical procedure; if pres

was at a concentration less than 5.0 ng/hp-hr. 

bTrace - Value not quantifiable cND - None detected; calculated detection indicated. 

28

Table 14 (Cont’d). Particulate-Phase Semi-Volatile PAH and NPAH Results 

Compound 

C1, ng/hp-hr C2, ng/hp-hr C3, ng/hp-hr 

Cold Hot Composite Cold Hot Composite Cold Hot Comp

211b Baseline Fuel 

2-Nitrofluorene 48 9.8 15 9.4 29 26 38 15 18 

1-Nitropyrene 107 118 117 197 100 114 210 75 94 

7-Nitrobenz(a)anthracene 43 34 35 9.4 33 30 9.5 9.8 9.7 

6-Nitrochrysenea traceb NDc trace ND trace trace trace trace trac

6-Nitrobenz(a)pyrenea ND ND ND trace ND trace ND ND ND 

Benzo(a)anthracene 3700 3500 3500 4100 4500 4500 4000 3800 380

Chrysene 7300 5300 5600 8000 6600 6800 7100 6300 640

Benzo(b)fluoranthene 2200 1900 1900 2600 2700 2700 2700 2300 230

Benzo(k)fluoranthene 2300 1800 1900 2500 1900 2000 2400 2000 200

Benzo(a)pyrene 3300 2700 2800 3400 2900 3000 3000 3000 300

Indeno[1,2,3-cd]pyrene 1300 1200 1200 1800 1400 1500 1400 1500 150

Dibenz(a,h)anthracene 94 57 62 115 84 88 112 68 73 

aDetection limit in ng/hp-hr calculated using the minimum value that could be quantified by the analytical procedure; if pres

was at a concentration less than 5.0 ng/hp-hr. 

bTrace - Value not quantifiable. cND - None detected; calculated detection indicated. 

29

No vapor-phase PAH or NPAH compounds were detected with the O2DieselTM that were not found with 

the 211b baseline fuel. The vapor-phase PAHs were between 2 and 6 times higher with the O2DieselTM, 

except for benzo(k)fluoranthene and for dibenz(a,h) anthracene which was not detected in any of the 

vapor-phase samples at the limits of detection. For the vapor-phase NPAH compounds, only 7­

nitrobenz(a)anthracene was detected with either fuel. 

For the particulate-phase, all PAH and NPAH compounds were present at quantifiable levels except 6-

nitrochrysene and 6-nitrobenz(a)pyrene which were only detected at trace quantities. All NPAH 

compounds were about two orders of magnitude lower in concentration than the PAH compounds for 

both fuels. 

As a means of comparing the PAH and NPAH results, the vapor- and particulate-phases were combined 

to obtain a total value for both fuels. These total values were obtained by averaging the results for the 

three individual tests with each sample and adding the two values together. Table 15 summarizes the 

results in terms of the combined phases for each compound. As can be seen from the table, the 

particulate-phase compounds were detected at much higher rates that the vapor-phase results. 

Table 15. Combined Vapor- and Particulate-Phase 

PAH and NPAH Results 

Compound 

O2DieselTM, μg/hp-hr 211b Baseline Fuel, μg/hp-hr 

Vapor Particulate Total Vapor Particulate Total 

2-Nitrofluorene NDa 0.014 0.01 

4 

ND 0.02 0.020 

1-Nitropyrene ND 0.088 0.08 

8 

ND 0.108 0.108 

7-

Nitrobenz(a)anthracene 

0.006 0.012 0.01 

8 

0.006 0.025 0.031 

6-Nitrochrysene ND traceb trace ND trace trace 

6-Nitrobenz(a)pyrene ND trace trace ND trace trace 

Benzo(a)anthracene 0.01 4.20 4.21 0.01 3.90 3.91 

Chrysene 0.02 8.40 8.42 0.00 6.30 6.30 

Benzo(b)fluoranthene 0.00 2.60 2.60 0.00 2.30 2.30 

Benzo(k)fluoranthene 0.00 2.70 2.70 0.00 2.00 2.00 

Benzo(a)pyrene 0.01 3.80 3.81 0.00 2.90 2.90 

Indeno[1,2,3-cd]pyrene 0.00 2.00 2.00 0.00 1.40 1.40 

Dibenz(a,h)anthracene ND 0.13 0.13 ND 0.07 0.07 

a

ND - None detected at detection limit. b

Trace - Value not quantifiable. 

30
VI. Summary 

Testing was performed on a heavy-duty engine to provide O2Diesel, Inc. with data in support of the EPA 

requirements for registration of a designated F/FA as stipulated by section 211 (b) and 211 (e) of the 

CAA. A 2002 Detroit Diesel engine was tested according to procedures established in 40 CFR 79.57 and 

40 CFR 86 Subpart D. Emissions characterization was performed on the engine after 125 hours of 

operation with O2DieselTM. The fuel was changed to the 211b baseline fuel, and the engine was operated 

for about five hours. At this point, tests were once again conducted to characterize the emissions. 

In general, the composite regulated emissions were lower than or equal to the 2002 emission standards 

except for particulate. When the CO, NOx, and particulate emissions from O2DieselTM were compared to 

the emissions from the 211b baseline fuel, the O2DieselTM produced about 6 percent less CO and NOx 

emissions, and about 7 percent less particulate emissions (See Table 16). The THC emissions were 

increased by about 40 percent when compared to the 211b baseline fuel. Speciation of the C1 to C12 

hydrocarbons including C1 to C6 alcohols and ethers, aldehydes, and ketones was performed during each 

cold- and hot-segment of the EPA transient cycle. In general, compounds measured in the exhaust with 

the O2DieselTM were also present in the exhaust with the 211b baseline fuel, except for an unidentified C8 

compound which was detected in only two hot-start tests with the O2DieselTM. Ethanol, formaldehyde, 

acetaldehyde, acrolein, acetone, and benzaldehyde were found at higher concentrations than in the 

exhaust of the 211b baseline fuel. No additional compounds, which could be attributed to the use of 

O2DieselTM, were found in the exhaust at the detection limits for the analytical procedures. 

In addition, vapor- and particulate-phase PAH and NPAH compounds were measured in the exhaust with 

both fuels. Some vapor-phase PAH compounds with the O2DieselTM were detected at about two to six 

times the levels detected in the exhaust from the 211b baseline fuel. However, the vapor-phase PAH 

compounds for both fuels were about two orders of magnitude lower than the particulate-phase 

compounds for both fuels. No PAH or NPAH compounds were detected with the O2DieselTM that were 

not found in the 211b baseline fuel. While selected individual C1 to C12 hydrocarbons and selected C1 to 

C6 alcohols and ethers were determined to be below the detection limit, one cannot necessarily conclude 

that these compounds were present or not present; however if present, the compounds were below the 

limits of detection. 

31
Table 16. Summary of Composite Regulated Emissions 

Test 

Emissions Results, g/bhp-hr 

THC CO NOx Particulate 

2002 Standard 1.3 16 4.0 0.10 

O2DieselTM 

Composite C1-H11 0.27 1.5 3.4 0.13 

Composite C2-H21 0.27 1.5 3.6 0.13 

Composite C3-H31 0.31 1.6 3.6 0.13 

Average of Three Composites 0.28 1.5 3.6 0.13 

211b Baseline Fuel 

Composite C1-H11 0.16 1.6 3.8 0.13 

Composite C2-H21 0.24 1.6 3.8 0.14 

Composite C3-H31 0.21 1.7 3.7 0.15 

Average of Three Composites 0.20 1.6 3.8 0.14 

32
References 

1. DER SwRI SOP 06-001 “Traceability to Standards.”

2. DER SwRI SOP 06-002 “NOx Converter Efficiency Determination.”

3. DER SwRI SOP 06-003 “Linearity Verification of Gas Dividers.”

4. DER SwRI SOP 06-010 “Barometric Pressure Verification.”

5. DER SwRI SOP 06-011 “Propane Recovery Check.”

6. DER SwRI SOP 06-013 “Temperature Calibration and Verification.”

7. DER SwRI SOP 06-016 “Wet CO2 Interference Check for CO Analyzers.”

8. DER SwRI SOP 06-020 “Pressure Calibration and Verification.”

9. DER SwRI SOP 06-022 “CVS Blower Calibration.”

10. DER SwRI SOP 06-023 “Calibration of Analyzers Using Digital Readout.”

11. DER SwRI SOP 07-023 “Operation of Bag Cart.”

12. DER SwRI SOP 07C-002 “Methane Quantitative Analysis.”

13. DER SwRI SOP 07C-006 “Analysis of Aldehydes and Ketones in Exhaust by Liquid

Chromatography.”

14. DER SwRI SOP 07C-010 “Impinger Sampling of Exhaust Emissions.”

15. DER SwRI SOP 07C-011 “Preparation of Impingers Used in Collection of Unregulated

Emissions.”

16. DER SwRI SOP 07C-013 “Hydrocarbon Speciation.”

17. DER SwRI SOP 08-003 “Data Transfers and Calculations - HD, LD, and NR.”

18. DER SwRI SOP 08-006 “Calculation of Aldehyde and Ketone Results.”

19. DER SwRI SOP 08-007 “Calculation of Methane Results.”

20. DER SwRI SOP-14-001, "Storage and Maintenance of DER Records.”

33
1

2

3

4

5

6

7

8

9

Appendix A 

Heavy-Duty Emission Test Results 

Page Test No. 

O2DieselTM 

A- 4904 C1 

A- 4904 H11 

A- 4904 C1/4904 H11 Composite 

A- 4904 C2 

A- 4904 H21 

A- 4904 C2/4904 H21 Composite 

A- 4904 C3 

A- 4904 H31 

A- 4904 C3/4904 H31 Composite 

211b Baseline Fuel 

A-10 4870 C1 

A-11 4870 H11 

A-12 4870 C1/4870 H11 Composite 

A-13 4870 C2 

A-14 4870 H21 

A-15 4870 C2/4870 H21 Composite 

A-16 4870 C3 

A-17 4870 H31 

A-18 4870 C3/4870 H31 Composite 

34

Appendix B 

HYDROCARBON SPECIATION DATA 

Table Page Title 

B-1 B-1 Cold- and Hot-Start Hydrocarbon Speciation Data for 211b 

Baseline Fuel (Background Corrected) 

B-2 B-6 Cold- and Hot-Start Hydrocarbon Speciation Data for 

O2DieselTM (Background Corrected) 

B-3 B-11 

Comparison of Hydrocarbon Speciation Composite 

Emissions Data for O2DieselTM to 211b Baseline Fuel 

(Background Corrected) 

35

Appendix C 

Test Substance Information 

OCTIMAXTM 4931 

containing 

proprietary surfactants 

and 

2-ethylhexyl nitrate 

MANUFACTURER 

O2Diesel, Inc. 

200 Executive Drive 

Newark, Delaware 19702 

CONTACT PERSON 

Jim Peeples

Phone: (703) 256-4497

The O2Diesel, Inc. additive technology is an ethanol-based diesel fuel containing up to 7.7 percent 

ethanol as the primary additive and OCTIMAXTM 4931 as the blending additive. OCTIMAXTM 4931, a 

proprietary additive technology of O2Diesel, Inc., is produced by Octel Starreon LLC and is based on the 

chemistry of proprietary surfactants. These proprietary surfactants are blended at a concentration greater 

than 75 percent with 2-ethylhexyl nitrate (CAS No. 27247-96-7) at a concentration of less than 25 

percent to produce the blending additive OCTIMAXTM 4931. OCTIMAXTM 4931 is blended with the 

diesel and alcohol at concentrations up to 1.0 percent. When OCTIMAXTM 4931 is blended with diesel 

fuel and 7.7 percent ethanol, the product is referred to as O2DieselTM. This 211b test protocol was 

employed to test for a 7.7 percent ethanol and diesel fuel blend utilizing 1.0 percent concentration of the 

OCTIMAXTM 4931 additive technology. Material Safety Data Sheets (MSDS) for OCTIMAXTM 4931 

and O2DieselTM are included in Appendix C. 

36

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1. AGENCY USE ONLY (Leave blank) 2. REPORT DATE 

February 2004 

3. REPORT TYPE AND DATES COVERED 

Subcontractor Report 

4. TITLE AND SUBTITLE 

Fuel and Fuel Additive Registration Testing of Ethanol-Diesel Blend for O2Diesel, Inc. 5. FUNDING NUMBERS 

ZCL-3-32068-01 

BBA3.5110 6. AUTHOR(S) 

E. Robert Fanick, Southwest Research Institute 

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 

AAE Technologies Inc 

200 Executive Drive 

Newark DE 19702 

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National Renewable Energy Laboratory 

1617 Cole Blvd. 

Golden, CO 80401-3393 

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NREL/SR-540-35334 

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NREL Technical Monitor: R. McCormick 

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13. ABSTRACT (Maximum 200 words) 

O2 Diesel Inc. (formerly AAE Technologies Inc.) tested a heavy duty engine with O2Diesel (diesel fuel with 7.7% ethanol and 

additives) for regulated emissions and speciation of vapor-phase and semi-volatile hydrocarbon compounds. This testing was 

performed in support of EPA requirements for registering designated fuels and fuel additives as stipulated by sections 211(b) 

and 211(e) of the Clean Air Act. 

14. SUBJECT TERMS 

O2Diesel; ethanol-diesel 

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