ASTM: Gasoline Today and Tomorrow – An Executive Report

A Hart Energy Publication 

ASTM: Gasoline Today and Tomorrow – An Executive Report 

Constantly changing and ever-tightening 

gasoline quality standards mean that refiners 

increasingly rely on the American Society for Technical 

Measurement. Various committees and subcommittees 

of ASTM members have had the responsibility of 

devising tests and protocols for the measurement of 

fuel sulfur, gasolineʼs corrosion to silver and ethanolʼs 

impact on sulfates and driveability. 

Automakers, refiners, blenders and ethanol interests 

watch these ASTM actions closely. The results are 

going to determine the lifespan of equipment the costs 

of compliance. 

Readers of Octane Week have long had this 

information. Weʼve decided to bring some of the most 

pertinent articles about ASTM activities to you in this 

special report. 

Editor Carol Cole has painstakingly researched 

these technical issues to provide a depth of coverage is 

unmatched. This collection of articles cannot even be 

found in a technical journal outside of the ASTM itself. 

As gasoline gets cleaner, the instrumentation for 

sulfur measurement is becoming as important as the spec 

itself. Knowledge of sulfur concentration is necessary 

for refining as well as for certifying compliance with 

federal and state fuel sulfur regulations. 

Meanwhile, sodium sulfate salts began plugging 

service station filters a few years ago as ethanol entered 

the gasoline pool, and ASTM was able to jump on 

the problem. Subcommittee members were asked if 

they favored a sulfate specification for ethanol, and 

responded with approval of a 4 ppm sulfate limit to 

D4806, ASTMʼs denatured fuel ethanol specification. 

Around the same time, awareness was growing 

that adding an ethanol term to the ASTM Driveability 

Index (DI) equation might be in the best interest of the 

industry. Members of ASTMʼs D 02.A subcommittee 

on gasoline were also asked if they supported adding to 

the DI equation a term that would multiply the volume 

of ethanol in a particular blend by 2.4ºF. Consensus on 

this issue was less likely than on sulfates. 

Corrosive gasoline appeared in the U.S. Southeast 

in 2004, and a Silver Corrosion Task Force began work. 

The group has been searching for funding and soliciting 

labs to participate in round robin testing of methods to 

determine gasolineʼs corrosiveness to silver. 

Among the other issues on ASTMʼs docket is 

RFG. Industry-wide collaboration that results in an 

RFG Research Report will establish a list of the most 

recent ASTM, EPA and California Air Resources Board 

test methods in one document. 

These issues do not comprise all of ASTMʼs 

activities surrounding gasoline standards, nor is it the 

only issue we cover in Octane Week. But we think you 

will find this special report invaluable. 

© 2007 Hart Energy Publishing, LP. Unauthorized reproduction or distribution of Hartʼs Octane Week is strictly prohibited and subject to fines.

Octane Week | ASTM: Gasoline Today and Tomorrow - An Executive Report 

ASTM Plans Action on Gasoline DI, 

Ethanol Sulfates and Corrosion Test 

Pittsburgh, Pa. – ASTM members meeting here 

in June of 2005 agreed to take action on a number of 

gasoline quality issues. Members of the section on 

Gasoline and Oxygenated Fuels were to be polled to 

see if a two-thirds majority would support changing the 

Driveability Index (DI) by adding a term to the equation 

that would reflect the impact of ethanol on driveability. 

They also were to get a ballot asking if they would 

support limiting the sulfate content of ethanol. The Silver 

Corrosion Task Force may include as many as four test 

methods in a laboratory “round robin” to determine a 

permanent method for measuring silver corrosion. 

Ben Bonazza, chairman of the D-02.A 

Subcommittee, said the issues reflect membersʼ 

responsiveness to marketplace influences on D-4814, 

ASTMʼs comprehensive gasoline specification. 

“A specification is a living document. It is never 

finished,” Bonazza told Octane Week. “There is always 

something you havenʼt thought about, some property that 

you learn from real-world experience you need to have 

in the specification. Silver corrosion is one example. 

There will be things that werenʼt contemplated. The 

real world has told us we need them.” 

There is some dispute about the justification for 

changing the DI equation and limiting the sulfate 

content of ethanol. Subcommittee members argued 

for and against the proposals, but despite objections, 

a majority agreed both should be “balloted,” ASTMʼs 

term for polling membersʼ opinions. 

Driveability Task Force Chairman Win Gardner 

of ExxonMobil proposed changing the DI equation to 

include an ethanol term and apply the equation at retail, 

rather than at the refinery gate. Supporters at the Task 

Force and Subcommittee levels approved the motion 

to ballot the changes to the broader membership, 

overcoming arguments that the DI change is unnecessary 

for vehicle performance and will increase the cost of 

producing gasoline. 

There is no 

dispute about the need 

for a permanent silver 

corrosivity test in D- 

4814. Silver corrosion 

has been a hot-button 

issue since sulfurtainted 

gasoline turned 

Existing: DI = 1.5*T10 + 

3.0*T50 + 1.0*T90 

Proposed: DI = 1.5*T10 + 

3.0*T50 + 1.0*T90 + 1.33oC 

(2.4ºF)* Ethanol vol% 

up in the marketplace last year and damaged vehicles 

by the thousands. ASTM approved a modified D- 

130 copper strip test as an emergency method until a 

permanent method is finalized. 

Silver Corrosion Task Force Chairman Kevin Bly 

of ExxonMobil updated attendees about the methods 

that are being considered for round-robin testing. They 

include: 

• A modified D-130, measured with and without 

pressure during testing; 

• A modified D-130 using a disposable thin silver strip 

in a novel suspension system; and 

• A modified IP 227 from the Energy Institute in the 

U.K. 

The round robin might also include a fourth test, 

Petro-Canadaʼs PCM 1005, a rapid ultrasonic test using 

silver wool. Petro-Canada has had nearly two years 

of lab and field experience with the method, which is 

faster and less expensive that the other tests, said the 

companyʼs David Surette. 

– Carol Cole 

2 February 2007


Silver Corrosion Methodologies Ready for Round Robin 

This story appeared on November 21, 2005. 

ASTMʼs Silver Corrosion Task Force is 

searching for funding and soliciting labs to participate in 

round robin testing of methods to determine gasolineʼs 

corrosiveness to silver. Until recently, D 4814, the 

comprehensive gasoline specification, did not contain a 

silver test method, a shortcoming that proved significant 

when corrosive gasoline entered the U.S. marketplace 

in spring 2004 and damaged the silver alloy found on 

some vehiclesʼ fuel sensors. 

Task force members have readied three test methods 

that have been under development since mid-2004. The 

goal is to have round robin results in time for D02.Aʼs 

June 2006 meeting. 

“Weʼre trying to line up the necessary participants,” 

Task Force Chairman Kevin Bly told Octane Week. “We 

donʼt have a sufficient number of labs right now that 

have signed up for the three methods plus the fourth 

that involves silver wool.” 

The three proposed methods, along with a fourth 

utilizing silver wool developed and currently used by 

Petro-Canada, will be round-robin tested if funds and 

labs become available. 

Episodes of fuel sensor failures have been reported 

in Canada and Europe prior to 2004. Petro-Canada was 

one of the first companies to encounter incompatibility 

between gasoline and certain fuel gauge sensors. 

In May 2004, incompatibility issues appeared in 

the U.S. Sulfur-tainted gasoline appeared in Kentucky 

and was traced back to a terminal owned by Marathon 

Ashland Petroleum (MAP) LLC. 

Later that month, a similar problem was discovered 

in the states of Florida and Louisiana and traced back to 

the Motiva refinery at Norco, La. 

The incident caused widespread damage to vehicles 

in those markets and led to costly repairs. Class action 

lawsuits by vehicle owners are still pending against 

Shell and its affiliate Motiva. 

Shortly thereafter, the state of Florida amended 

its gasoline regulations to compensate for the lack of 

a silver methodology in D 4814. The ASTM standardʼs 

test methods only address copper corrosion. 

Floridaʼs temporary rule required that fuel 

suppliers test gasoline for silver corrosiveness using a 

method based on IP227, developed by the Institute of 

Petroleum, now the Energy Institute in the U.K. 

Incorporating an IP method into an ASTM 

specification is not ideal, and the method itself is not 

entirely appropriate for gasoline, having been designed 

for aviation turbine fuel. 

Task Force Charged with Tough Mission 

ASTM sprang into action, and in June 2004, the 

D02.A subcommittee on gasoline established a silver 

corrosion task force. The charge – develop a safe, 

suitable, stand alone ASTM test method or methods 

to accurately detect the silver corrosion properties of 

gasoline. 

The task force was quite active between last June 

and December. Since its formation, members have 

worked with a sense of urgency. Certain sulfur species in 

gasoline, alone or in combination, can become corrosive 

to vehicle fuel sending units that rely on silver alloy. A 

corroded fuel gauge will cause some units to read full 

when, in fact, the tank is not. 

At the December 2004 meeting, D02.A adopted 

on an emergency basis a test method to serve until the 

silver corrosion task force could complete and develop 

a stand-alone standard or standards that could be 

incorporated by reference into the gasoline standard. 

The temporary method, a modified ASTM D 130, 

Test Method for Corrosiveness to Copper by Copper 

Strip Test, was placed in the Annex to the gasoline 

specification, now cited as version D 4814-04b. 

Bly has coordinated the efforts of the oil companies 

and testing labs that have spearheaded the silver 

methodology research. 

Early in the process, the participants determined 

it would be necessary to suspend the silver coupons or 

strips, which were based on the physical dimensions of 

the silver coupons derived from the IP227 method and 

carried into the D 4814-04b test method, in the fuel. 

Bly explained that allowing the silver coupons or 

strips to rest on the bottom of the test tube could lead 

to differences in corrosion ratings between the top and 

bottom faces. 

Two of the proposed methods are based on 

modifications to D 130, and a third is based on testing 

IP227 with gasoline. 

Sonia Bain of MAP LLC and (continued on p4) 

February 2007 3


(from p3) Imran Hussami of Frontier Oil Corp. have 

developed silver methodologies based on modifications 

to D-130, most obviously, substituting a silver strip for 

the copper strip. Their separate processes have many 

similarities and critical differences. Both use 30 ml 

samples of gasoline that are heated to 50oC. Bainʼs test 

method specifies heating the sample for three hours 

while Hussamiʼs test method requires only two hours. 

At the end of the heating period in either method, the 

silver strip is removed and washed, and the color and 

tarnish level is ranked. 

Both Bain and Hussami have developed methods 

having procedures for testing with and without a 

pressure vessel. Method A uses a pressure vessel and 

method B involves the use of a vented test tube. Both 

have designed innovative devices for suspending a 

silver strip. 

“In the D-130 method, the copper strip was not 

suspended,” Bain said. “We had to study how to use the 

cable tie that was developed for suspending the silver 

strip, which is a little longer than the copper strip.” 

The underlying issue is one of incompatibility, 

she explained. “The metallurgy of certain fuel sensors 

is an issue when certain naturally occurring sulfur 

compounds in gasoline interact with silver. Automobile 

manufacturers are replacing silver sensors with a more 

robust metallurgy to remedy this problem,” she said. 

Bain reminded us that in 2000, Audi of America, 

Inc. voluntarily recalled 50,000 vehicles to replace 

the existing fuel sending units inside the fuel tank 

because they could cause the fuel gauge to read full 

while the fuel tank may not in fact be full or could be 

empty. Audi attributed interactions of certain reactive 

sulfur on contact points of any of the three fuel level 

sending units causing them to send an erroneous signal 

to the fuel gauge. Audi replaced the sending units with 

sturdier alloys. 

Suspension Devices Differ 

“Gasoline might not need the pressure 

vessel,” Bain told us. When using a pressure 

vessel (method A), the gasoline sample is placed 

in a clean and dry test tube. A prepared silver strip 

measuring 0.7 in. long, 0.5 inches wide and 0.1 

inches thick is placed inside the assembly (see 

fi gure right, Silver Strip Suspension Assembly, 

Method A), which is then placed in the test tube. 

The sample tube and suspension 

assembly are then placed in 

the pressure vessel. After 

three hours, plus or minus five 

minutes in the bath, the pressure 

vessel is to be withdrawn and 

immersed for a few minutes 

in cool water. The technician 

is advised to open the pressure 

vessel carefully as contents may 

be under pressure. 

The strip is to be withdrawn 

from the suspension assembly 

with forceps and immersed in 

2,2,4-trimethylpentane, dried with ashless filter paper or 

cotton ball and inspected for tarnishing or corrosion. 

A silver corrosion interlaboratory study conducted 

by Marathon indicated that Method A and Method B yield 

equivalent results. Method B is advantageous because 

labs can use the same bath used in copper corrosion 

testing of finished gasoline. Another advantage is that 

labs do not need pressure cylinder vessels for testing 

silver corrosion. 

When testing without pressure (method B), the 

technician is to secure the silver strip as with a cable 

tie lanyard (see fi gure above, Silver Strip Suspension 

Assembly, Procedure B). The cable should hold the strip 

securely at the four corners but it should not contact any 

of the other surfaces. The assembly is to be placed in 

a test tube, and the test tube in a water bath for three 

hours. The silver strip is cleaned and compared in the 

same way as in the previous procedure. 

Thinner Strip Tested 

“Frontierʼs Hussami has also developed a modified 

D 130 test method, but it employs thinner, longer, 

reusable silver strips. This method suggests that strips be 

discarded when their original shape becomes deformed 

or the surface shows pitting, scratches or corrosion that 

cannot be removed by the specified polishing 

procedure. Polishing of unused, fresh strips is 

done with a 400-grit scouring-pad, while used 

strips are first polished with a piece of 150-grit 

roll, followed by the 400-grit pad. 

“At 1.5 inches long, 0.5 inch wide and 0.021 

inch thick, itʼs a fat-free silver strip,” Hussami 

quipped. This size has (continued on p5) 

4 February 2007


(from p4) the advantage 

of providing a greater surface 

area, not only to facilitate the 

strip polishing process but also 

to allow greater exposure of the 

strip to the sample in the overall 

corrosion process. 

Hussami has designed and 

gotten fabricated a silver strip 

centering device that differs 

significantly from Bainʼs design 

by securely gripping only the top 

edge of the strip. The upper part 

of this same device functions as 

a test-tube stopper and sample vent (see fi gure, right). 

In Procedure A, with pressure vessel, 30 mL of 

sample is placed in a test tube and stoppered with a 

cork. 

Within one minute after completing its surface 

preparation, the solvent-washed/dipped silver strip is 

to be secured in the centering device, and placed into 

the test tube containing the gasoline sample. Test tube 

is placed in the pressure vessel which is then placed in 

the liquid or solid heating bath. After two hours, the 

pressure vessel is removed from the bath, immersed in 

cool water for a few minutes before opening to remove 

the test tube with forceps inserted into the vent holes of 

the centering device. Centering device is removed from 

the test tube, strip immersed completely in iso-octane, 

removed immediately, solvent allowed to dry off before 

inspection of strip for tarnishing or corrosion. 

Procedure B, without pressure vessel, uses a 

vented test tube containing the silver strip mounted 

in the centering device. Test tube is placed directly in 

the 50oC liquid or solid bath for two hours, removed 

from bath, allowed to cool slightly, before removal of 

centering device from the test tube, and continuation as 

outlined in Procedure A. 

Silver strips are to be rated as per the Classifications 

and Color Chart employed in the IP227 method. The 

Chart consists of five pictures of tarnished silver, 

ranked 0 to 4, in accordance with the severity of tarnish 

or corrosion. Strips rated 0 for no tarnish or 1 for slight 

tarnish indicate a passing sample. Any sample ranking 

between 2 and 4 indicates a corrosive gasoline. 

Hussami told us that part of the “experience 

gained from the success of the Rapid Copper Corrosion 

Test, using thin copper strips, is being applied to the 

development of this silver strip corrosion test method.” 


Task Force Details Scope of Inter Laboratory Study 

This story appeared on November 28, 2005. 

The chairman of ASTMʼs Silver Corrosion Task 

Force prepared a broadcast message soliciting labs 

outside the group to participate in the ASTM Silver 

Corrosion in Gasoline Inter Laboratory Study (ILS) 

involving four methodologies. The Task Force expects 

participating labs to run 16 samples in duplicate. Task 

Force Chairman Kevin Bly hopes that labs would not 

pay to participate if ASTM provides the necessary 

funding. 

ASTM members meeting in Norfolk, Va. in 

December 2005 will get an update on the Task Forceʼs 

activities. The group has readied four methods for 

determining the silver corrosion capability of gasoline. 

Task Force member Scott Fenwick of Intertek Caleb 

Brett has concentrated on a silver corrosion method that 

utilizes the IP227 test and applies it to gasoline. IP227 

is a copper corrosion test developed by the Institute of 

Petroleum, now the Energy Institute in the UK. 

Caleb Brett became involved when corrosive 

gasoline appeared in the U.S. Southeast in 2004, and 

since that time, Fenwick has become an advocate for 

the modified IP227 test method. 

“Rather than trying to create something, we went 

with an established method, and we didnʼt have to do 

much to modify it,” he told us. Gasoline was outside 

the scope of the original method, and there was concern 

gasolineʼs vapor pressure might have caused the glass 

to shatter. “Weʼve made modifications to apply it to 

gasoline, and we slightly increased the cooling water 

flow to ensure it wouldnʼt build up too much pressure. 

Weʼve run more than 1,000 samples, and nothing like 

that has happened,” Fenwick said. 

The modified IP-based method utilizes 250 mL of 

sample in a 350 mL capacity test tube of heat-resistant 

amber glass. A single ended condensed hollow tube, 

called a cold finger, is fitted through a glass stopper 

at the top of the test tube. Through the tube circulates 

cooling water. At the bottom (continued on p6) 

February 2007 5


(from p5) of the cold finger is a glass hook from 

which is suspended a glass cradle that holds the silver 

strip. The silver coupon is 0.50 in. by 0.10 in. by 0.71 

in. Samples are tested at 50°C for four hours. 

ʻWhen trying to address a real-world issue by 

developing a new scientific method, we try to replicate 

as many of the issues as possible,” Fenwick explained. 

“The method IP227 seems to control more similar 

variables than some of the other proposed methods. We 

are concerned that the ratio of gasoline to silver might 

have an impact upon the results. 

“As with a carʼs fuel tank, at any given time there 

are usually several gallons of gasoline to react with 

the small amount of silver within the fuel sensor unit. 

IP227 has this greater ratio than do the other proposed 

methods. 

“Our other concern stems from the use of open 

containers within some of the other proposed methods. 

A carʼs fuel tank is a closed system. The apparatus used 

in IP227 is also a closed system that contains any volatile 

vapors that may contribute to increased corrosion.” 

While it is still unclear what levels and types of 

sulfur produce the greatest effects, Fenwick said that 

there are some synergistic effects at relatively low 

levels. “We are looking forward to increased studies to 

help determine what might be the best predictor to help 

prevent future situations,” he said. 

Petro-Canadaʼs Method to be Included 

The Silver Corrosion Task Force has also agreed 

to include Petro-Canadaʼs silver wool method fin the 

round-robin. The Canadian oil company has generated 

a lot of interest in its rapid ultrasonic silver wool 

method, PCM 1005-03, and now that issues pertaining 

to its deployment have been resolved, the method will 

go forward for testing. 

“Petro-Canada agreed to make the method 

public, but we will retain the copyright on our original 

method,” explained David Surette, Petro-Canadaʼs 

manager-Quality Strategies and Systems. “The method 

is available for the ILS, and if it is chosen as a method 

to develop, it will be available at no cost.” 

Petro-Canada has had more than two years 

experience with the method and data on thousands of 

actual gasoline samples. It is a step out from the IP227, 

Surette told us. 

The modified test exposes a small amount of fresh 

silver wool to 180 mL of fuel sample in a pre-cleaned 

disposable glass test cell for one hour at 50°C in an 

ultrasonic bath. After the test, the silver wool is removed 

from the sample, rinsed with wash solvent and dried. 

The wool is then pressed into a disk slightly smaller 

than a dime and rated according to a color scale. 

The rating scale is expanded beyond the five 

classifications in the IP227 test method. The silver 

wool disk produces so many color variations that it is 

possible to distinguish 16 distinct classifications. 

The elimination of cleaning glassware or preparing 

the silver strip inherently produced a superior, 

more robust test method with no sample-to-sample 

contamination to worry about, Surette explained. “The 

use of the ultrasonic bath reduces the analysis time 

considerably while ensuring a high degree of agitation, 

such that the reaction is not diffusion-limited and the 

corrosion is uniform.” 

Petro-Canadaʼs PCM 1005-03 method offers 

many advantages over the use of silver strips, Surette 

continued. “Firstly, the silver wool has an extremely 

uniform surface as compared with the cleaned silver 

strip and that leads to uniform corrosion and the 

resolution of the individual colors, the expanded rating 

scale. Secondly the wool is only used once, reducing any 

chance of sample to sample contamination. Thirdly the 

small amount of wool used makes the test economically 

attractive.” 

PCM 1005-03 gains additional robustness and 

precision from the use of inexpensive pre-cleaned 

test cells that are used only once. This eliminates all 

contamination from cleaning agents or residual solvents 

or the cross contamination from sample to sample if 

the cleaning is not well done. ”This is important if 

some samples contain silver corrosion inhibitors since 

these additives have been found difficult to remove 

completely from glass surfaces,” he advised. 

The ultrasonic bath reduces the test time from four 

hours to one hour. “In addition, it provides a high degree 

of agitation such that the reaction is not diffusionlimited,” 

he emphasized. It also eliminates completely 

the “streaking” effect found in the IP227 method and 

leads to uniform corrosion rates at the silver surface 

which yield the resolution of the various “corrosion 

colors.” 


6 February 2007


ASTM Task Force Wrestles with Hydrogen Sulfide 

in Sample Quality Control Issue 

This story appeared on July 31, 2006. 

Because of sample stability concerns, the ASTMʼs 

Silver Corrosion Task Force will delay a round robin 

of silver corrosion test methods and instead conduct a 

ruggedness study to see if a small sample set can be 

blended, shipped and tested. That decision, announced 

at the July 2006 D02.05.C Subcommittee meeting in 

Toronto, Ontario, Canada, might answer some critical 

questions but it sets back the timetable for finalizing 

a test method and adding it to D4814, a process 

subcommittee D02.A members had hoped to complete 

by the upcoming ASTM meeting in December. 

The decision to conduct a small ruggedness study 

stemmed from growing evidence that sample stability 

could not be controlled during the course of the round 

robin. That suspicion first emerged at the D02.05.C 

Subcommittee meeting last December, when round 

robin designers noted that some of the gasoline samples 

would contain hydrogen sulfide, which would oxidize 

over time, making it difficult, if not impossible to 

ensure that participating labs were sampling and testing 

the “same” material. 

Since then, Silver Corrosion Task Force Chairman 

Kevin Bly has probed the issue of hydrogen sulfide 

oxidation. “The problem is keeping the sample stable 

long enough to ensure all labs receive the same material 

in the Inter Laboratory Study,” Bly told the recent 

meeting. “How long can samples containing hydrogen 

sulfide be expected to be stable after preparation?” 

Knowing that, ILS designers could determine 

whether it would be possible to blend, package and ship 

samples, as well as have labs perform tests, within that 

timeframe. 

Blyʼs group considered an alternative strategy 

– excluding hydrogen sulfide as a blending component 

and replacing it with other active components that yield 

corrosion – but that was discounted. 

“We decided to keep hydrogen sulfide because 

thatʼs representative of whatʼs out there in the real 

world,” said Bly. 

Hydrogen sulfide is critical to the round robin, a 

task force member told Octane Week. “The species of 

interest is elemental sulfur, and hydrogen sulfide is the 

catalyst. Elemental sulfur on its own is not corrosive. 

There have been samples with very high levels of 

elemental sulfur, 20-30 ppm, and they still pass the test. 

Elemental sulfur needs to be activated.” 

Another alternative would be to prepare samples 

with varying levels of elemental sulfur and ship them 

to labs, where operators would add a fixed amount of 

hydrogen sulfide just prior to testing. This suggestion 

was appealing to the members at the meeting as a 

means to address the hydrogen sulfide stability issue, 

provided the appropriate guidance and procedure could 

be given to the labs to safely dose each sample with 

a fixed quantity of hydrogen sulfide. David Surette, 

Bob Falkiner and Weldon Cappel agreed to work as 

a separate Action Team to develop such a procedure 

that could subsequently be tested by several labs to 

determine suitability and address potential safety 

concerns involving the proper handling of hydrogen 

sulfide. 

To assess the stability of hydrogen sulfide in 

gasoline, the laboratory at Lyondell-Citgo prepared 

a blend of light cat cracked gasoline mixed with an 

untreated naphtha stream containing 30.8 ppm of 

hydrogen sulfide in liquid to yield a sample containing 

5.9 ppm of hydrogen sulfide. The material was split 

and stored in three separate quart bottles for analysis 

over a three week period. Samples were tightly closed 

and stored in a cold room. Each week for three weeks, 

a sample was tested along with the previous weekʼs 

sample to determine the corresponding hydrogen sulfide 

concentration. During that time, hydrogen sulfide levels 

dropped to 0. 8 ppm relative to the 5.9 ppm concentration 

in the original blend. In short, the conclusion was that 

maintaining a stable solution of hydrogen sulfide in a 

gasoline matrix would be difficult for more than a short 

period of time, less than one week. 

The decline in hydrogen sulfide was believed to 

be due to two main reasons. First, hydrogen sulfide 

might simply have escaped when the sample bottle 

was opened. Second, hydrogen sulfide can change 

chemically over time through polymerization to 

polysulfides, which tends to be more corrosive than 

hydrogen sulfide. Unfortunately, the hydrogen sulfide 

study did not include a sulfur (continued on p8) 

February 2007 7


(from p7) 

speciation study to determine if a portion 

of the hydrogen sulfide concentration had in fact been 

converted to other sulfur species. So while Lyondell- 

Citgo observed hydrogen sulfide levels declining 

over time, it is possible that the samples became more 

corrosive. 

“Based on the results of the Lyondell-Citgo study, 

a decision was made to do a ruggedness study prior 

to going forward with the ILS,” Bly told task force 

members. “The goal is to prepare and ship four samples 

to four separate labs to evaluate replicate results from 

the same bottle using each of the four methods, where 

results will need to be tested within a week of samples 

being prepared.” 

When it gets underway, the ILS will test four silver 

corrosion methods, two based on a modified ASTM 

D130 copper strip test, substituting silver for copper; 

one based on a modified IP227; and Petro-Canadaʼs 

rapid ultrasonic silver wool method 1005-03. The four 

leaders, Sonia Bain of Marathon, Imran Hussami of 

Frontier Oil, Scott Fenwick of Intertek Caleb Brett 

and Petro-Canadaʼs David Surette, will conduct the 

ruggedness study. 

The extra step throws the Silver Corrosion Task 

Force off schedule for completing its work in time 

for a silver method or methods to be added to D4814 

by December. The group had hoped to conduct and 

complete the ILS this spring and report results at the 

recently held ASTM meeting in Toronto. That would 

have enabled D02.A. to prepare a ballot polling 

member support for replacing D4814ʼs temporary 

silver corrosion test method, a modified D-130, with 

one or more of the proposed methods. The ballot 

process would have been conducted this summer and 

would have enabled the group to complete its task in 

two years, a goal established by D02.A Chairman Ben 

Bonazza when D02.05.C had initially convened the 

silver corrosion task force in December 2004. 

“Silver corrosion is a very tricky issue,” 

acknowledged a Toronto meeting attendee. 

ASTM Sulfur Methodology Studied as ULSD, 

New Tier 2 Limits Approach 

In December 2005, ASTM took up sulfur 

methodology. A task group had been working to improve 

ASTM D 2622-03, which measures fuel sulfur by 

wavelength dispersive X-ray fluorescence spectrometry. 

There were questions about the methodʼs capability to 

measure fuel sulfur at the low levels required by the 

U.S. EPAʼs clean fuels rules next year. 

ASTM members were to have a chance to see what 

was termed “sweeping revisions” to D 2622-03, as well 

as a separate Standard Practice document developed 

around the revised method. 

In 2001, ASTM conducted an extensive round-robin 

test of sulfur methods, which determined the precision 

of older, lower-power as well as newer, higher-power 

instruments. The round robin revealed that the pooled 

limit of quantitation is in the range of 15 – 20 ppm. 

That means, even at its best, D 2622-03 might not 

be up to the task of measuring the new, ultra-low sulfur 

diesel levels, said a refiner we spoke with. ULSD with 

a 15 ppm sulfur cap will be required beginning in June 

2006. 

The effort to revise the method will be useful not 

only for ULSD but also for the tightening of the Tier 2 

gasoline rule to a 30 ppm annual average sulfur level, 

which takes effect in January 2006. 

The task group is proposing a round robin, which 

will also reportedly test D 4294 Standard Test Method 

for Sulfur in Petroleum and Petroleum Products by 

Energy-Dispersive X-Ray Fluorescence Spectrometry. 


8 February 2007


EPA Updates Fuel Regulations With Latest ASTM Standards 

This story appeared in the April 10, 2006, edition of 

Octane Week. 

The U.S. EPAʼs gasoline and diesel fuel regulations 

are getting updated with the latest ASTM test methods. 

The federal environmental agency issued a Direct 

Final Rule in April 2006 that updates several aspects 

of regulations and adds a new section on rounding 

practices. 

One of the most significant results is the decision to 

add ASTM D7039-04 as an additional, alternative test 

method for determining the sulfur content of gasoline. 

X-Ray Optical Systems (XOS) requested that EPA 

make its technology the designated test method. 

“EPA has evaluated XOSʼs request on this test 

method and agrees,” the agency said. EPA will allow 

ASTM D7039-04 as an alternative test method, provided 

that results are correlated to ASTM D2622, which is 

currently a designated test method for measuring sulfur 

in gasoline. 

XOS manufactures the SINDIE 7039 bench top 

analyzer, which uses monochromatic, wavelengthdispersive 

X-ray fluorescence spectrometry. According 

to the company, the unit detects sulfur to 0.4 ppm. XOS 

also makes an on-line SINDIE analyzer. 

Several gasoline and diesel fuel test methods are 

being updated as a result of the American Petroleum 

Instituteʼs (API) urging that EPA use the most current 

ASTM methods. Currently, 

• D2622 is a designated test method for measuring sulfur 

in gasoline, and D3120 and D5453 are alternatives, 

• D1319 is the designated method for measuring 

olefins in gasoline and aromatics in diesel and it is an 

alternative for measuring aromatics in gasoline, and 

• D4815 is an alternative test method for measuring 

oxygenate content in gasoline. 

API asked EPA to use the year 2003 versions of 

the test methods. D2622-03, API pointed out, includes an 

updated precision statement determined by recent round 

robin testing. EPA agreed with that and APIʼs other 

recommendations. The other updated methods will be 

D3120-03a, D5453-03a, D1319-03 and D4815-03. 

D1319 and D4815 were to be sunset in 2004, 

but EPA allowed their continued use until the end of 

2006. EPA is withdrawing the sunset provision for the 

test methods. Use of these two methods can continue 

until EPA develops a performance-based test method 

(PBTM) for qualifying alternatives. At that time, these 

and other alternatives may qualify as alternative test 

methods under the BPTM. 

ASTM D6428-99 is also getting an update. It is 

currently the designated test method for measuring 

sulfur in on-road diesel at 15 ppm, an alternative test 

method at 500 ppm and an alternative for measuring 

sulfur in gasoline. The 2003 version contains a precision 

statement that was lacking in the 1999 version. The 

method including the precision statement is D6920-03, 

which will replace the earlier version. 

Another method getting an update is that for 

detecting sulfur in butane. Currently, ASTM D3246-96 

is the designated method. API asked EPA to designate 

D667-01 and allow D3246-96 as an alternative. The 

agency will make D667-01 the designated test method 

for measuring sulfur in butane, and D3246-96 will 

continue to be allowed as an alternative, provided 

results are correlated to D667-01. 

Finally, EPA is adding a new section to the fuels 

regulations that will reference the rounding method 

used in ASTM. The number of significant digits in an 

EPA specification can differ from that in an ASTM test 

method. The standard practice in ASTM E29-02 should 

be followed in this situation. 

February 2007 9


Industry Awaits News of ASTMʼs Sulfur Test Method Round Robin 

This story appeared on June 19, 2006. 

Stakeholders in the fuel industry have suspected for 

some time that D2622, ASTMʼs Standard Test Method for 

Sulfur in Petroleum Products by Wavelength Dispersive 

X-ray Fluorescence Spectrometry (WDXRF), could 

perform better than its published precision statement 

indicates. 

With fuel sulfur levels plunging this year, it became 

imperative that D2622ʼs measurement capability 

be improved, and that a new precision statement be 

developed for one of the most widely used sulfur test 

methods going. That effort has been underway in earnest 

since the beginning of the year, and an update from the 

ASTM work group may be forthcoming at the ASTM 

D02.A Subcommittee on Gasoline and Oxygenated 

Fuelsʼ June meeting in Toronto, Ontario, Canada. 

The sulfur test method review has been undertaken 

by the D02.03 Subcommittee on Elemental Analysis. 

Method D2622 is a critical compliance method for fuels 

certification, but it does not reflect the state-of-the-art 

WDXRF technology. A significant revision to the test 

method is needed to do that. 

Although there are other test methods for 

determining sulfur content of fuels, D2622 provides 

rapid and precise measurement of total sulfur in 

petroleum and petroleum products with a minimum of 

sample preparation. A typical analysis time is one to 

two minutes per sample. 

Knowledge of sulfur concentration is necessary for 

refining as well as for certifying compliance with federal 

and state fuel sulfur regulations. Sulfur regulations 

tightened June 1, when the U.S. EPAʼs 15 ppm sulfur 

limit for highway diesel took effect. The tightening of 

the diesel spec follows the implementation Jan. 1 of a 

30 ppm annual average sulfur cap under EPAʼs Tier 2 

gasoline rules. 

The pooled limit of quantitation for D2622 is in 

the range of 15-20 ppm sulfur, making the test nearly 

obsolete in the ultra-low sulfur environment taking 

shape in 2006. 

“Equipment vendors and users realized the test 

had to do better, and they believed that it could,” said a 

source familiar with the research. 

A Task Group reviewing D2622 planned a roundrobin 

test program. A status update may be available in 

time for the D02.A meeting in Toronto June 26-27. For 

more information about the meeting, log on to www. 

astm.org. 

ASTM Members Consider 1-PPM Sulfate Spec for Ethanol 

This story appeared in July 2005. 

Pittsburgh, Pa. – ASTM subcommittee members 

will be asked whether they favor establishing a sulfate 

specification for ethanol. The D-02 A subcommittee voted 

to poll members by ballot to determine whether they favor 

modifying D-4806, ASTMʼs Standard Specification for 

Denatured Fuel Ethanol, to include a 1-ppm sulfate limit. 

The vote to “ballot” the issue came just hours 

after presentations from oil, auto and ethanol industry 

representatives on the issue of fuel injector damage, 

which has been tied to high sulfate content gasoline. 

The problem first surfaced in 2003 with equipment 

failures at service stations in Minnesota, St. Louis, Mo., 

Los Angeles, Chicago and the Pacific Northwest. 

“We have seen widespread and prolonged 

service station filter plugging,” said Mitch Oliver of 

ConocoPhillips. Filters failed in a matter of days or weeks, 

rather than the months of useful life they ordinarily have. 

An investigation revealed sodium sulfate salts. 

There were no issues with conventional fuels 

or sulfuric acid alkylation by-products, Oliver said. 

Detergents were also ruled out as a source, although 

they play a role. 

“The common denominator was fuel ethanol,” 

he said, and the presence of sodium sulfate salt was 

confirmed by a Bar Chart Haze test. 

ConocoPhillips surveyed its ethanol suppliers in the 

affected regions. The company performed 300 analyses 

using ion chromatography (IC), which showed sodium 

sulfate content ranged from non-detectible levels to 23 

ppm in the worst sample. The average was 2-4 ppm. 

“Sulfates greater than 1 ppm cause severe problems 

on filter performance,” Oliver (continued on p11) 

10 February 2007


(from p10) continued. Detergents impact the rate at 

which sulfates agglomerate on or pass through filters, 

“neither one a good option,” he added. 

ConocoPhillips worked with ethanol suppliers in a 

cooperative fashion and established a joint industry task 

force with other oil companies, automobile manufacturers 

and ethanol makers, Oliver told attendees at ASTMʼs D- 

02 Committee meeting here. Since then, there has been 

little resolution of the issue, in part because there is no 

established test method. The IC method is thought to be 

impractical on an industry-wide basis. 

Decision on Ethanol Sulfate Detection 

With the cooperation of Flint Hills Resources, the 

two oil companies determined that a modified D-6174 test 

method could determine ethanol sulfate concentrations 

as low as 0.05 ppm. The modified test method results 

could also be correlated with the IC test results. 

“We need a sulfate spec in 4806,” Oliver said, 

referring to the standard specification for denatured 

ethanol. The industry investigation established a 

modified D 6174, the Standard Test Method for Inorganic 

Sulfate in Surfactants by Potentiometric Lead Titration, 

as an alternative to IC, he said. “We are asking that the 

industry support the method weʼve put forward.” 

Four presentations later, the morning meeting 

adjourned. At the afternoon roundtable that followed, 

Dave Harvey of Citgo made a motion to ballot whether 

to add a 1-ppm sulfate limit in ASTMʼs D-4806 ethanol 

specification, and to allow either test method, the IC 

D-6827, or the modified D-6174, the titration method, 

until a test method is finalized. 

Although supportive of the ASTM process, 

Bob Reynolds, representing the Renewable Fuels 

Association (RFA), objected to “fast tracking” the 

ballot. The modified titration test was only identified 

two weeks earlier and the correlation to the IC test only 

revealed hours earlier, he pointed out. “Weʼd be putting 

in spec controlled by a test method thatʼs not approved,” 

he told subcommittee members. 

“I would like to see it on a fast track,” countered 

Citgoʼs Harvey. While there are reasons to take the 

“more prudent” route and resolve the problem through 

ASTMʼs normal, deliberative process, Harvey argued, 

“The fact is, we have a problem now.” 

In 2004, drivers in Milwaukee, Wis., started 

reporting vehicle operating problems. Fuel from 

Citgo, a major marketer in the region, was implicated 

as a possible cause. After investigation, Citgo also 

discovered troublesome levels of sulfates in ethanol. 

Owners face “thousands of dollars of repairs” to 

out-of-warranty vehicles that might become affected, 

Harvey and others told roundtable participants. 

For and Against 

Members debated the issue extensively, raising 

numerous concerns. “Weʼve been shown clearly that 

high levels of sulfates, around 5 ppm, lead to a rise 

in field problems,” said Ronald Tharby of Tharby & 

Associates. “Seasonal use of ethanol has been tied in 

with a significant increase in field complaints, which 

are serious to drivers. What if there is a big breakout of 

this problem this winter?” 

Concerned that a 1-ppm sulfate spec might exclude 

a majority of ethanol from the gasoline pool, BPʼs Jim 

McGetrick sounded another alarm. As much as 75% 

of U.S. ethanol production is thought to exceed the 

proposed 1-ppm maximum sulfate standard. “Weʼve got 

mandates for ethanol,” he said, referring to California, 

New York and Connecticut, where MTBE is banned. 

“If we take 75% of supply away, weʼve got problems.” 

“Thatʼs right, if everyone sits back and does 

nothing,” Harvey responded. With a rapidly expanding 

ethanol industry and more “mom and pop” producers, 

“this problem only gets worse,” Harvey warned. 

Sulfates must be addressed, he said, “so that we can 

expand the use of ethanol.” 

One observer suggested that the ethanol industry 

is just going through typical growing problems. 

“Technology exists to remove sulfates from methanol, 

and the ethanol industry is just electing not to use them. 

They may be reluctant to do that, but we all have to 

improve our processes,” the commenter said. 

Ethanol producersʼ actual sulfate levels are far from 

certain, RFAʼs Reynolds said. Survey results are based on 

self-reporting using a variety of test methods. “We need to 

find out what our numbers are,” he admitted. “We support 

work on a test method,” he said, and RFA would favor 

making the modified titration test part of a round robin. 

After the debate, subcommittee members voted 23- 

13 in favor of Harveyʼs motion to ballot the issue. By the 

time of D-02Aʼs December meeting, it should be known 

whether the subcommittee members favor the addition 

of a sulfate limit to ASTMʼs ethanol specification. 

— Carol Cole 

February 2007 11


Ethanol, Oil, Autos Ready for Ethanol Sulfate Round Robin 

This story appeared in January 2006. 

Ethanol, oil and auto companies are fast-tracking 

a round robin that will evaluate three test methods for 

determining sulfate concentrations in ethanol. Fuel 

samples have been prepared and are to be delivered 

in January to the labs participating in the effort, which 

has alternatively engendered cooperation and sparked 

tension among the representatives. 

Dispute over test methods nearly scuttled an 

agreement to set a 4 ppm sulfate limit in D-4806, ASTMʼs 

ethanol specification. After a fierce test method debate 

at ASTMʼs recent winter meeting, oil, ethanol and auto 

industry representatives agreed to initiate a round robin 

this month with the aim of establishing a 4 ppm ethanol 

sulfate specification later this year. 

The Renewable Fuels Association (RFA) has 

endorsed the new specification and is encouraging their 

membership to do the same. 

“The cooperation between automakers, gasoline 

marketers and ethanol producers in supporting this 

specification demonstrates that all facets of the gasoline 

industry understand the need for such a specification to 

protect their mutual customers,” said Citgo Petroleumʼs 

Dave Harvey, who has spearheaded the effort within 

ASTM. 

“With new federal legislation requiring increased 

use of ethanol as a component of automotive fuel, it 

is important to ensure that gasoline blend components 

conform to stricter standards, thereby providing the 

motoring public with a continued reliable energy 

source.” 

Although most ethanol producers do endorse a 4 

ppm sulfate limit, few supported the lead potentiometric 

titration test that had seemed so promising. Ethanol 

industry representatives attending ASTMʼs December 

meeting blasted the method, but their objections were 

not sufficient to halt the entire “ballot,” the method 

ASTM uses to determine member support for changing 

or adopting specifications. The ballot to add a 4 ppm 

sulfate limit to D-4806 passed the D02.A subcommittee 

on gasoline and will be sent to the full D02 Committee 

in time for results to be available at ASTMʼs June 

meeting. 

To resolve the test method grievances, the D03.03 

subcommittee on elemental analysis will conduct a 

round robin on three sulfate detection test methods – the 

lead titration method and two ion chromatography (IC) 

procedures. There too, the aim is to have test method 

results back in time for possible approval of both spec 

and test method at the next D02 meeting, which is 

scheduled for June. 

“The round robin will get started next week,” a 

source close to ASTM told Octane Week. “Fuel samples 

have been obtained and prepared.” 

Although the timetable is very short, the schedule 

should leave room for statistical analysis, which is 

central to the precision statement, the source said. 

Assuming the 4 ppm ballots with test method pass 

the appropriate ASTM committees in June, when might 

the spec take effect? “Sometime in the fall,” ASTM 

members say, but the exact timing depends on the 

date of publication, which can be several months after 

committee approval. 

That doesnʼt leave much time for ethanol producers 

to make plant modifications if any are needed to meet 

the new specification. A survey of ethanol producers 

revealed several plants produced ethanol containing 

more than 4 ppm sulfate. 

“If the spec takes effect in October, thatʼs only 

nine months for producers to design, build and install 

equipment if more than a process change is needed. 

Earlier is worse,” the source continued. 

The ballot faces its toughest test of support at 

the D02 Committee, where new ethanol producermembers 

will be voting in June. If the spec and the 

test method donʼt satisfy that growing population of 

ASTM members, the weight of their votes could spell 

trouble for the “unprecedented display of industry-wide 

cooperation” marshaled by Citgoʼs Harvey. 


12 February 2007


Fuel Ethanol Sulfate Specification Advances 

Despite Lacking Test Method 

This story appeared in July 2006. 

Members of ASTMʼs gasoline subcommittee 

voted to add a 4 ppm sulfate limit to D4806, ASTMʼs 

denatured fuel ethanol specification. The vote signaled 

acceptance by the ethanol industry, which had wavered 

in its support of a sulfate specification at any level. 

The vote is notable for another reason – it advances 

a specification that currently lacks an approved test 

method. 

A round robin on three sulfate detection test 

methods was conducted this spring but failed because 

of sample-related problems, and will be repeated this 

summer. 

The addition of a specification without an approved 

test method is unusual, but nothing has been usual in the 

effort to get a sulfate restriction into the ethanol standard. 

Since the beginning of the debate 18 months ago, oil 

and ethanol company representatives have hammered 

away at the issue, often with opposite goals. 

After resolving disputes over the need for a 

specification, the level and the placement – in the 

ethanol or the gasoline specification – one big issue 

remains unsettled – the test method. 

ASTMʼs D02.03 Subcommittee on Elemental 

Analysis conducted an inter laboratory study (ILS) 

of a lead potentiometric titration method and two ion 

chromatography (IC) procedures in support of the 

ethanol sulfate specification. Unfortunately, the sulfate 

results were disappointing due to problems with the 

samples used in the round robin. The IC methods are 

also capable of detecting chlorides, which are a concern 

to ethanol producers, and the chloride data were 

excellent. 

“The sulfate data were not usable by any method,” 

said a member of the D02.03 subcommittee which 

organized the round robin. “The methods are robust. 

Round robin sample stability was the problem.” 

The ILS utilized 16 samples, all were prepared 

in denatured ethanol with varying amounts of sodium 

sulfate and sodium chloride dissolved in water. Samples 

varied between 0 – 20 mg/kg total sulfate and 0 – 50 

mg/kg total chloride. Unfortunately, the added sodium 

sulfate precipitated out of the samples during the duration 

of the round robin, rendering their results useless, while 

the sodium chloride remained in solution. 

“Concentrations of sulfates may change over 

time,” explained a D02.A member. “Through an 

oxidation reduction process, sulfates can change to 

sulfites or sulfides, which may not be detected by the 

test methods.” 

A second round robin will be conducted, and it 

will include an oxidation step in the IC methods to 

stabilize the sulfate in the ethanol samples. Hydrogen 

peroxide will be added to samples, which will convert 

other species to sulfate prior to testing, providing a 

measurement of “potential sulfate.” 

The procedure not adding the hydrogen peroxide 

will be retained for a total sulfate measurement. Because 

hydrogen peroxide will damage the lead sensor used in 

the lead titration method, the oxidation step will not be 

used in samples tested by the titration method. 

Despite the failure of the first ILS to yield useful 

sulfate precision data, DO2.A voted to accept a 4 ppm 

sulfate limit in D4806, with the understanding that a 

second round robin will be conducted and will likely 

produce useful data. 

The same labs agreed to participate in the second 

round robin, which could start as soon as next month. If 

the data are returned in time, the three methods will be 

balloted for approval with full precision statements in 

D02 at the December meeting. 

February 2007 13


ASTM Issues Ethanol Sulfate Test Method Ballots 

This story appeared on October 23, 2006. 

ASTM members are considering three ballots, 

each proposing a different test method in support of the 

4 ppm sulfate limit recently added to D-4806, ASTMʼs 

denatured fuel ethanol specification. If one or more 

of the test methods is acceptable, fuel providers will 

have solved a difficult issue that threatened to divide 

the subcommittee's ethanol, refiner and auto company 

representatives. 

The methods - two ion chromatography (IC) 

procedures and a lead potentiometric titration method - 

have been round-robin tested twice, and the latest results 

are solid, sources close to the effort told Octane Week. 

The goal is to have ASTM D0.2 Committee and 

subcommittee members review the latest data, and 

if negative votes are cast, “adjudicate” them using 

ASTMʼs mediation process prior to the ASTM winter 

meeting, which begins Dec. 4. 

ASTMʼs D02 Committee on Petroleum Fuels 

issued numerous ballots Friday afternoon. A quick 

scan prior to Octane Weekʼs press time indicated two of 

the three methods – potentiometric titration and direct 

injection IC – were included among the ballots. The 

standard is to be published next month. The balloting 

will close Nov. 20. 

Subcommittee members are feeling pressure 

to complete the standard-setting process. Sulfate 

contamination can cause filter plugging in the fuel 

distribution system and in vehicle fuel injectors. That was 

the case in 2003, when widespread vehicle fuel injector 

plugging was reported. The events triggered the start of 

the ethanol sulfate debate within D02.A a year later. 

Despite the need to limit fuel sulfate content, it 

took more than another year of delicate negotiations to 

bring D02.A subcommittee members into agreement on 

the appropriate level. After much debate, subcommittee 

members voted last June to approve the 4 ppm sulfur 

limit, overcoming limited support for a 1 ppm standard. 

At the time of the vote, test method data was 

lacking. It was expected that an ASTM Inter Laboratory 

Study (ILS) conducted prior to the meeting would have 

provided results demonstrating the adequacy of one or 

more of the test methods. Instead, the ILS failed because 

of sample-related problems. Sodium sulfate precipitated 

out of the samples, and test results were not useful. 

A second round robin was conducted this summer. 

This latest round robin included a sample composition 

that solved the earlier problem and an oxidation step 

in the IC methods to convert any sulfate that may have 

been reduced over time back to sulfate. 

This time around, both the aqueous injection and 

direct injection IC methods produced “good data” from 

a dozen or so participants, a source familiar with the 

round robin told Octane Week. 

The lead titration method, which did not include an 

oxidation step, also produced “very good results from 

about 10 participants.” 

Some 21 labs participated in the direct injection IC 

tests, the source said. “The statistician tried to pool the 

data and could not get convergence. Instead, there was 

a bimodal result.” 

The two leading IC devices, manufactured by 

Metrohm and Dionex, use different column suppression 

configurations (tri-chamber and continuous), and that 

may account for the majority of difference in results. 

“The instruments are different and give different 

responses. Both are in use, so there is an effort to get 

an idea of how the results will appear so that both 

instruments will be allowed in the test method with 

their own precision statements,” our source told us. 

The precision correlation was reworked and now 

there is “different but good convergence for each of the 

two suppressor configurationsʼ data.” 

Ballots for the aqueous injection IC method and 

the potentiometric titration method were submitted to 

ASTM in September. ASTM also extended the ballot 

deadline so ILS leaders could submit the revised 

direct injection IC method for ballot. That method will 

have two precision statements for the two types of IC 

suppression configurations that were tested. 

“From the results of our round robin, I am fully 

confident any of the three methods will support the 4 

ppm sulfate specification. They all will also support a 1 

ppm specification,” he said. 

That doesnʼt mean the test method ballots will pass 

easily, ASTM sources warn. If the negatives cannot be 

adjudicated successfully, the ballot could fail in December. 

In that event, the methods would need to be reworked to 

address the negatives and reballoted in the spring. 

14 February 2007


ASTM Committee Reaches Agreement 

on Ethanol Sulfate Specification 

This story appeared on December 11, 2006. 

After nearly two years of debate, the ASTM D02 

committee on petroleum fuels has approved three new 

test methods in support of a 4 ppm sulfate specification 

in D 4806, ASTMʼs denatured fuel ethanol specification. 

The final discussions at the Committeeʼs winter meeting 

in Orlando, Fla., were characterized as congenial and 

cooperative, as ethanol producers joined with refiners 

to make the new methods possible. 

ASTM will assign identifying numbers to the 

new methods probably sometime in December, and 

the specification containing the test methods should be 

published by ASTM in February, sources tell Octane 

Week. “The specification becomes effective when it is 

available to the general public,” our source told us. 

The three methods, two by ion chromatography 

(IC) and one by a lead potentiometric titration, 

underwent extensive round-robin testing by the D02.03 

Subcommittee on Elemental Analysis. One set of tests 

conducted this spring failed because of sample stability 

problems. Sodium sulfate can precipitate out of ethanol 

and ethanol-blended gasoline, making accurate sulfate 

measurements impossible. But the first round robin did 

produce acceptable data for measuring up to 50 ppm 

total chloride in fuel ethanol using the IC methods, 

which is also included in the specification. 

Eager to proceed, the 4 ppm specification was 

approved by the D02.A Subcommittee on Gasoline 

and Oxygenated Fuels in June, pending approval of 

one or more of the methods in December. That was 

accomplished, so no time was lost by the shortcomings 

of the first round robin. 

Another ASTM inter-laboratory study (ILS) 

that corrected for the sulfate stability problems was 

conducted over the summer. That study included an 

oxidation step in the IC methods to convert sulfate that 

may have been reduced back to sulfate prior to testing. 

This gives a “potential” sulfate result along with the 

total sulfate result. 

The summer ILS produced positive results, 

but study organizers faced another challenge in 

compiling a precision statement for one of the IC 

methods. Direct injection IC devices utilize different 

column suppression configurations – tri-chamber and 

continuous. Statisticians could not get all of the data 

from the different devices to converge into a single 

precision statement for the method. Under intense time 

pressure this fall, they reworked the data in a way that 

yielded acceptable convergence for the two suppressor 

configurations, and two precision statements were 

added to the method. 

By late November, D02 Committee members had 

completed balloting of the three methods, all backed by 

solid ILS results. 

The ballots yielded only three negative votes that 

were successfully resolved at last weekʼs meeting. 

Two involved a procedural misunderstanding and were 

withdrawn. 

The other negative vote challenged the data pooling 

technique for the direct injection IC method, which had 

confounded statisticians this fall. “The negative voter 

had no problem with the test method, only the way 

the data for the precision statement were pooled,” our 

source explained. “There is a possible different way of 

grouping data in the precision statement, and that will 

be considered for a method revision this spring.” 

With all negatives successfully adjudicated, the 

full committee approved the three sulfate test methods 

for use in D 4806, bringing a controversial issue to a 

successful resolution. 

“Ethanol producers are pleased,” said one attendee. 

“They were extremely cooperative, participated in the 

round robins and provided good data. None of them 

voted against the ballots.” 

Now it is up to Subcommittee A to determine how 

the test methods will be listed. Members could make one 

test the “primary” method and the others “alternative” 

methods, or they could say that any of the methods is 

acceptable. 

All three methods are capable of measuring total 

sulfate in concentrations as low as 1 ppm. 

The debate over the level of the sulfate specification, 

1 ppm versus 4 ppm, was one of the early and most 

divisive fights among Subcommittee A members. 

Refining and auto groups support a 1 ppm sulfate limit, 

ethanol producers have not to this time. Given ethanol 

producersʼ increased membership (continued on p16) 

February 2007 15


(from p15) in ASTM and thus their greater voting 

power, Subcommittee D02.A leaders wisely garnered 

support around a 4 ppm spec and brought the issue to 

closure last week. 

“Weʼve got a number, 4 ppm, and we have test 

methods. Thatʼs a great accomplishment,” said Ben 

Bonazza, D02 Committee chairman. 

Refining and auto groups will now try to move the 

specification limit lower. Most of the ethanol that is 

produced and marketed in the U.S. can easily meet the 

4 ppm spec, our source told us. It is only the occasional 

batch of domestic ethanol and some imported material 

than can have trouble meeting the new specification. 

Will the spec move lower? Maybe, but not now. 

“The current specification is a triumph of testing 

and compromise, and deserves support”, our source 

continued. “But anything that will reduce the levels 

of impurities in refining fuel feedstocks is good. And 

ethanol producers are doing the right thing. They are 

working with refiners to facilitate the use of their 

product.” 


Busy ASTM Agenda Includes Debates On DI, Ethanol Sulfates 

From the June 13, 2005 edition. 

ASTM members gathering in Pittsburgh, Pa., in 

June 2005 will be facing an agenda full of gasoline 

quality issues, some familiar, some new. The D02 

Committee on Petroleum Products will investigate 

particulate contamination in gasoline and diesel to 

determine whether a retail spec should be set. Committee 

members also will delve into the issue of ethanol sulfate 

content, now that individual refiners are setting their 

own specs to control sulfates. 

Ethanol is creeping into ASTM discussions 

more frequently. As the fuels industry prepares for 

a possible renewable fuels standard, which will 

mandate substantially more ethanol use, questions 

about the additiveʼs quality and blending traits become 

increasingly important. 

Some ASTM members are concerned that the 

ASTM Subcommittee Wrestles With DI Change; 

Retail Spec Proposed 

existing Distillation Index (DI) equation needs an 

ethanol term. The current T10, T50 and T90 terms 

do not adequately reflect a blendʼs distillation when 

ethanol is present, they say. CRC test results will be 

evaluated in an effort to determine whether an ethanol 

term is needed. 

Committee members also will return to more 

familiar territory, such as whether to apply the test DI 

at the retail level rather than at the refinery, where it is 

currently applied. DI is the only ASTM specification 

that is not applied at retail. 

Silver corrosion is also on the ASTM agenda. The 

emergency test method that was adopted last year will 

be reviewed, and members will evaluate whether more 

round robin testing is needed before a permanent test 

method is selected. 


Coverage of the ASTM Subcommittee meeting appeared 

in the July 5, 2005 issue. 

Adding an ethanol term to the ASTM Driveability 

Index (DI) equation will more accurately reflect the effect 

of ethanol on gasoline cold-start and warm-up driveability, 

supporters of the change said. An ethanol term is not 

needed and will make gasoline more costly to produce, 

opponents countered. This controversial issue was to be 

“balloted” to determine whether members of ASTMʼs D- 

02.A gasoline subcommittee support the change. 

ASTM considered adding an ethanol term to DI 

for years, and various offsets had been discussed. The 

Coordinating Research Council (CRC) has participated 

in the effort to quantify the impact of ethanol on fuels 

and vehicle operation. Early CRC studies showed that 

equal DI, ethanol blends generally have been shown 

not to perform as well. 

The latest CRC research indicated an offset for 

ethanol was needed in the DI equation, said Driveability 

Task Group Chairman Win Gardner of ExxonMobil. 

“CRC data supports the addition (continued on p17) 

16 February 2007


(from p16) 

of an offset,” he told ASTM members 

meeting in Pittsburgh. “The DI change addresses a 

technical issue that arose out of CRC studies. The 

secondary aspect, to have it apply at retail, grew out of 

state positions in the past.” 

The most recent CRC study, completed in 2004, 

was “probably the best cold-start driveability program 

run,” said Task Group member Lew Gibbs of Chevron. 

Vehicles were screened for responsiveness, raters were 

trained and calibrated and procedural changes were 

made to the program. “The result showed a high degree 

of statistical correlation between driveability and an 

adjusted DI index.” 

In contrast, previous CRC tests included older cars 

and a larger ethanol offset, Gibbs explained. “The latest 

test had the best representation of modern vehicles 

on the road,” he told Octane Week. After meeting in 

Naperville, Ill., to discuss the results, Task Group 

members determined to propose balloting a DI change 

to the entire group. 

Specific Proposal Language 

The proposal to be balloted was as follows: 

Change Table 1, footnote C, to read 

“Driveability Index (DI) = 1.5 T10 + 3.0 T50 + 

1.0 T90 + 1.33 o C (2.4 o F) * Ethanol Volume% 

where T10 = distillation temperature, o C 

( o F) at 10% evaporated, T50 = distillation 

temperature, o C ( o F) at 50% evaporated, and 

T90 = distillation temperature, o C ( o F) at 90% 

evaporated.” 

Change footnote D with the following: 

“During spring and fall transitions into and 

out of the federal vapor pressure control 

period, the Driveability Index requirement 

of the volatility class specified in Table 4 is 

waived so long as the DI meets that of the 

volatility class corresponding to the measured 

vapor pressure of the retail sample.” 

Refiners might have to tighten the base fuel 

properties in order to accommodate DI with an ethanol 

offset. A 2.4ºF *10 vol% translates to a 24-point more 

stringent spec. 

Task Group members expressed concern about the 

impact on conventional gasoline. At that time, refiners 

did not know whether ethanol would be added to CG 

downstream of the refinery, which would create a noncomplying 

blend. 

But as Gibbs pointed out, when ethanol is added at 

10 vol%, it lowers the 10% and 50% evaporated points, 

which in turn, lowers DI about 60 points, on average. 

The ethanol adjustment for 10 vol% is only about 24 

points. Since the upward adjustment is smaller than the 

downward blending effect, the blends will always be in 

compliance, he said. 

A 24-point more stringent spec will mean 

additional manufacturing costs for refiners, one fuels 

industry representative said. “This is going to cost more 

to produce,” said Bob Schaefer of BP. 

The DI change is coming at a time when refineries 

are running at maximum, Schaefer pointed out. In the 

future, refiners will have to make additional amounts 

of low-Rvp fuels due to the implementation of the U.S. 

EPAʼs 8-hour ozone standard. That will probably lead 

to fuel quality changes. “States will need emissions 

reductions, and fuels will be on the list.” 

Schaefer observed that the latest CRC study utilized 

a fuel set of 10 fuels, eight of which had a DI in excess 

of the current ASTM maximum of 1250. “The majority 

of the fuel set contains fuels that are non-compliant,” 

he noted. 

A correlation was developed between the effect 

observed on high-DI fuels and applied to the on-spec 

fuels. 

CRCʼs research was “good science” Schaefer said, 

“but the application of the correlation would not be 

good science.” 

Testing a broad range of fuels is common at CRC. 

Two of the test fuels had DIs below the 1250 maximum 

and four were around 1265, Chevronʼs Gibbs countered. 

Previous tests included fuels with DI as low as 1160, 

and they showed an offset for ethanol was needed. “We 

expanded the envelope to get a scale so you can see 

an effect. Thatʼs common practice and accepted good 

science. 

“The relationship between the adjusted DI and 

driveability demerits was linear on a log basis, indicating 

applicability at lower DI levels,” Gibbs said. “Members 

of the auto, oil and ethanol industry all agree that this 

offset has applicability.” (continued on p18) 

February 2007 17


(from p17) 

Applicability Where – Refinery or Retail? 

Just where the spec will be applied is another 

contentious question. There has been a move at ASTM 

to apply DI at retail, where all other ASTM standards 

are applied. The issue is on the table again. 

The large reproducibility of DI tests, some 48 

points, creates problems. Pipelines have indicated they 

would likely require that refiners ship 1202 DI fuels if 

the spec is applied at retail, not 1250 DI fuels which are 

currently allowed with the spec applied upstream at the 

refinery. 

Would a tighter, 1202 DI be justified? Some 

Task Group members think not. Actual fuel industry 

sampling shows more than 99% of in-use fuel comply 

with DI, and reports of drivability problems are few, 

if any. One gasoline subcommittee member observed, 

“Out of 4,000 retail samples, 20 failed. Thatʼs one-half 

of one percent.” 

After the arguments for and against, members in 

attendance voted in favor of balloting the issue to the 

subcommittee to determine support for the DI equation 

change. 

–Carol Cole 

ASTM Members Vote to Retain DI Enforcement at the Refinery 

This story appeared in December 2005. 

Norfolk, Va. — Oil industry representatives to 

ASTMʼs gasoline subcommittee narrowly defeated a 

proposal to shift enforcement of the Driveability Index 

(DI) from the refinery to retail. The vote on the measure, 

taken at the ASTMʼs December 2005 meeting, was the 

narrowest victory opponents could muster, 51%. 

The proposal to shift the enforcement point was 

half of a ballot polling ASTM membersʼ support for 

changing the DI equation. Members of ASTMʼs D 

02.A subcommittee on gasoline were also asked if they 

supported adding to the DI equation a term that would 

reflect the impact of ethanol on vehicle driveability. 

The term would multiply the volume of ethanol in a 

particular blend by 2.4ºF. A 2.4ºF *10 vol% translates to 

a 24-point more stringent spec, some members argued. 

The Driveability Task Force received negative 

comments on both segments of the ballot. Task Force 

Chairman Win Gardner led a discussion of the negative 

comments at last weekʼs meeting. 

Opponents claimed the ethanol offset is not 

supported by recent data. The Coordinating Research 

Council (CRC) conducted a DI test that relied on fuels 

that were not representative of current fuels, they said. 

Only two of the 10 fuels studied had a DI below the 

compliance limit of 1250. The other eight fuels exceeded 

the 1250 DI standard, meaning 80% of the fuels in the 

study were noncompliant. 

Critics also took aim at the vehicle set, saying they 

were not representative of the U.S. vehicle population. 

Despite the objections, task force members did 

not find the arguments “persuasive,” and the proposal 

advanced to the full D 02.A subcommittee for further 

consideration. 

ʻUnacceptable and Irresponsibleʼ 

Shifting enforcement to retail is also unsupported, 

opponents continued. Applying the standard at the 

refinery has already resulted in essentially complete 

compliance — 99.5% — at retail, they argued. 

Furthermore, the move could prompt pipelines to 

adjust the input DI limit lower. The large reproducibility 

of DI tests, some 48 points could lead pipelines to 

require 1202, not 1250, DI fuels. 

“To try to cut back another 50 degrees would be 

unacceptable and irresponsible,” said one refiner. “This 

is our biggest concern.” 

Previously released data from the National 

Petroleum Council indicated the cost of shifting DI 

enforcement downstream could be as much as a 7 c/gal 

increase in the cost of producing gasoline, said another 

commenter. 

“It is important to protect our customers, but 

data suggest cars are protected if DI is enforced at the 

refinery gate.” 

Those arguments were determined to be persuasive, 

and the effort to shift DI to retail ended with the narrow 

failed vote at the D 02.A subcommittee meeting. 


18 February 2007


Major ASTM Argument Lurks in EPA ʻSub Simʼ Reference 

This story appeared on July 10, 2006. 

A tiny reference in a U.S EPA regulation threatens 

to generate a dispute so big it could divide members 

of ASTMʼs D02.A Subcommittee – again. Stated 

simply, the question is whether EPA should update a 

reference in its “Substantially Similar” rule to reflect 

the latest version of D4814, ASTMʼs comprehensive 

gasoline standard. But, according to some ASTM 

members, an update of the reference would change a 

key measure of driveability, a thorny issue that has split 

the subcommittee in the past. 

The current version of EPAʼs “Sub Sim” rule 

has been on the books since 1991. It prohibits the 

introduction of fuels or fuel additives that are not 

substantially similar to fuels or additives used to certify 

1975 or subsequent-year passenger vehicles. Sub Sim 

allowed the blending of oxygenates, rarely used before 

1975, but required that finished blends still meet the 

characteristics of gasoline specified by D4814-88, the 

1988 and then-current version. 

Some in ASTM now suggest that Sub Sim should 

reference the current version, D4814-06. What would 

appear to be a simple matter of updating a reference 

really opens the door to a potentially divisive debate 

about driveability. Oil and auto members see the 

issue differently, and there is even division among the 

subcommitteeʼs oil company, or producer members, as 

they are known. 

D4814-88 references a wintertime T50 of 170 o F. 

D4814-06 references a wintertime T50 of 150 o F. The 

addition of ethanol tends to depress T50, meaning if 

ethanol is added downstream to a gasoline with a T50 

of 150, automakers argue vehicle performance could 

suffer. Auto company members of D02.A, and there are 

only a few, want T50 held at the old 170 o F. 

Some refiners say the issue is not important. “There 

have been a number of spec changes since 1988. If you 

donʼt meet the 1988 version, it doesnʼt mean youʼre not 

substantially similar,” said one. 

Thatʼs what EPA says, too. In fact, EPA stated 

that Sub Sim is an interpretive rule, guidance, not a 

regulation. EPA also stated verbally that gasoline is not 

necessarily out of compliance if it doesnʼt fall under 

Sub Sim. Some refiner members feel thatʼs too vague. 

But on another Sub Sim matter, EPA has been 

crystal clear: Without consensus from ASTM, the 

federal agency will not even take up the issue. 

“We need to come up with a consensus opinion 

before we go to EPA and ask them to update Sub 

Sim,” said BPʼs Jim Simnick, who chairs the Balanced 

Technical Advisory Panel, a high-level working group 

handling the Sub Sim discussion in D02.A. 

Consensus on T50 is unlikely, to put it mildly. 

Itʼs the issue that sparked so much division that auto 

company representatives resigned en masse from D02. 

A in 1997, leaving Honda as the subcommitteeʼs sole 

user member, as automakers are known. 

After the implementation of a more representative 

voting system, autos drifted back to ASTM. But now, 

the explosive issue of T50 is back, this time wrapped 

in a seemingly harmless discussion about a Sub Sim 

reference. 

Subcommittee to Revise RFG Research Report to Reflect EPA, 

EPAct 2005 Directives 

This story appeared on June 26, 2006. 

The Reformulated Gasoline (RFG) Research 

Report got the attention of ASTMʼs Subcommittee 

D02.A on Gasoline and Oxygenated Fuels at a July 

2006 meeting in Toronto. The report was going to have 

to reflect a number of changes in gasoline regulations 

resulting from enactment of the Energy Policy Act 

(EPAct) of 2005 and from activity at the U.S. EPA. 

During the D02.A meeting in December 2005, 

members agreed that a letter ballot should be prepared 

to revise and update Research Report D02: 1347, 

Research Report on Reformulated Spark-Ignition 

Engine Fuel to incorporate changes in federal and state 

RFG programs. 

“There are a number of major (continued on p20) 

February 2007 19


(from p19) developments at the federal and state level 

affecting RFG, and these actions need to be incorporated 

into the RFG Research Report,” said Marilyn Herman, 

president of Herman & Associates, which maintains the 

comprehensive document for ASTM. 

Subcommittee members consider the RFG 

Research Report immensely helpful to their work 

because it maintains a list of the most recent ASTM, 

EPA and California Air Resources Board test methods 

in one document. 

EPAct 2005 makes significant revisions to the 

Federal RFG program and establishes a Renewable 

Fuels Standard requiring the use of renewable fuel 

components such as ethanol and biodiesel in gasoline 

and diesel fuel beginning in 2006. Key provisions of 

the energy bill include elimination of the minimum 2 

wt% oxygen requirement in RFG, both nationally and 

for California, and establishment of a Renewable Fuels 

Standard. The law also consolidates VOC Control 

Regions, establishes small refiner provisions, modifies 

the mobile source air toxics program and adjusts other 

fuel-related programs. 

The RFG Research Report will be updated to reflect 

all those changes, as well as others changes that were 

issued by the U.S. EPA. In April, the agency revised a 

number of gasoline and diesel fuel test methods to allow 

use of more recent ASTM D02 analytical test methods. 

Those changes, including many sulfur test methods are 

also on the ballot. 

Subcommittee members received the proposed 

changes and voted to pass the ballot prior to the D02.A 

meeting June 26 and 27 in Toronto, Ontario, Canada. 

Update after Update, ASTMʼs RFG Research Report Expands 

This story appeared in November 2006. 

ASTMʼs comprehensive RFG Research Report has 

been revised to include a number of changes balloted and 

approved at the last ASTM meeting in June of 2006. With 

the ink barely dry, the document is being readied for a 

new round of changes, author Marilyn Herman, chair of 

the ASTM D02.A Reformulated Gasoline Task Group, 

told us. 

The just-completed RFG Research Report 

incorporates the Energy Policy Act of 2005, including the 

Renewable Fuels Standard and removal of the oxygen 

content requirement in RFG, updates ASTM, EPA, and 

CARB test methods, expands and updates CARB Phase 

3 standards, moves CARB Phase 2 standards to the 

Appendix, and makes other conforming changes. 

The document has become so large that a table of 

contents has been added. 

“This is a completely new version. There were 

massive changes,” said Herman, president of Herman 

& Associates. 

Because the document requires constant updating 

when test methods and state and federal gasoline 

regulations change, new revisions are currently being 

balloted to members of the D02.A subcommittee on 

gasoline and oxygenated fuels. Balloting closes Nov. 24. 

Subcommittee members are considering two 

proposed changes. First, to update the table summarizing 

ASTM, EPA, and CARB test methods with the latest 

versions: 

D 1319 aromatics 

D 3606 benzene 

D 1319 olefins 

D 4953 vapor pressure, and 

D 5191 also vapor pressure. 

Second, the ballot proposes adding a CARB 

Equivalent Test Method for Sulfur. In September, 

the California Air Resources Board determined that 

ASTM D 7039-04 is equivalent to ASTM D 5453- 

93 for detecting the sulfur content of CARB gasoline 

and diesel fuel. This action allows the use of ASTM D 

7039-04 as an alternative to the adopted test method, 

ASTM D 5453-93. 

The reproducibility of D 7039-04 would also 

be added to the RFG Research Report if the ballot is 

approved at the next meeting in December. 

20 February 2007


Range of Ethanol Blending Volumes Signals More Work for ASTM 

This story appeared on December 4, 2006. 

The increased use of ethanol in gasoline at varying 

concentrations is expanding the work load for ASTM. 

The testing body is preparing to update a number of test 

methods to cover the entire possible range of ethanol 

blending. 

Ben Bonazza, chairman of Subcommittee D02. 

A on Gasoline and Oxygenated fuels sent letters to 

a half dozen ASTM analytical subcommittees last 

month, requesting that certain test methods be revised 

or developed to accommodate all ranges of ethanol. 

The test methods include vapor pressure, gum, sulfur, 

sulfate and chloride, lead and phosphorus and gas 

chromatograph (GC) test methods, Bonazza told Octane 

Week. 

This effort may result in changes to D 4814, 

ASTMʼs gasoline specification; D 4806, ASTMʼs 

denatured ethanol specification; and D 5798, Standard 

Specification for Fuel Ethanol for Automotive Spark- 

Ignition Engines. Bonazzaʼs D02.A subcommittee 

is responsible for the three ethanol-containing 

specifications. D02.A is requesting: 

• Development of (GC) test methods and/or 

modification of ASTM D 5501, ASTM’s standard 

test method of determining the ethanol content of 

denatured fuel ethanol by GC, to accommodate all 

ranges of ethanol. 

• Modification of gum test method ASTM D 381 to 

accommodate all ranges of ethanol. 

• Modification of ASTM D 3231 for phosphorus and D 

5059 for lead to accommodate all ranges of ethanol. 

• Modification of applicable ASTM test methods for 

sulfate and chloride in ethanol to accommodate all 

ranges of ethanol. 

• Modification of sulfur test methods to accommodate 

E85 and all ranges of ethanol. 

• Modification of vapor pressure test methods to 

accommodate all ranges of ethanol. 

In a series of letters to the analytical subcommittee 

chairs, Bonazza lays out the rationale for the updates 

this way: 

ASTM Subcommittee D02.A is 

responsible for three ethanol containing 

specifications: D 4814, D 4806, and D 5798. 

In that regard, we believe it is important to 

have appropriate test methods to determine 

compliance for the properties specified which 

list the products in the scope and provide 

a precision statement for all the products. 

Some properties are specified in all three 

specifications. If possible, we would like to 

use the same test methods to measure common 

properties across the three products. The test 

methods may be listed in our specifications, 

but the scopes of the test methods do not 

necessarily identify D 4806 or D 5798 covered 

products. For the product lines for common 

test methods we need to cover 0 - 10 vol % 

ethanol, 70 - 85 vol % ethanol, and 93 - 97 vol 

% ethanol. 

That amounts to a substantial amount of updating, 

urged by the recently formed E85 Task Group, Marilyn 

Herman, president of Herman & Associates told us. 

The E85 Task Group was formed at the June 

2006 D02.A meeting. It was organized in response to 

increased E85 use and the need to review D 5798. 

Andy Buczynsky, of GM, serves as the chair of 

the E 85 Task Group. The E 85 Task Group reports to 

Herman, chair of the Fuel Oxygenates Task Group of 

Subcommittee D02.A. 

February 2007 21


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22 February 2007

ASTM: Gasoline Today and Tomorrow – An Executive Report

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