Page 1

INSIDE: BENCHTOP FLOW CYTOMETRY POWERS ALGAE DEVELOPMENT September/October 2012

Bullish on Quality A Q&A with Biodiesel Fuel Quality Expert Kent Bullard Page 20

Plus

Solving a Great Biodiesel Mystery Page 28

AND

Comparing Infrared Biodiesel Measurement Methods Page 32

WWW.BIODIESELMAGAZINE.COM


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CONTENTS

SEPTEMBER/OCTOBER 2012 VOLUME 9 ISSUE 5

28

20 Q&A

TESTING TESTIN

Bullish on Biodiesel Quality

Solving a Great Biodiesel Mystery

BY RON KOTRBA

BY RON KOTRBA

Newly retired, Kent Bullard discusses biodiesel use, BQ-9000 and his long career

Advertiser Index 7 2012 Algae Biomass Summit 40 2012 National Advanced Biofuels Conference & Expo 37 2013 Fuel Ethanol Workshop &Expo 35 2013 International Biomass Conference & Expo 9 2013 National Biodiesel Conference 39 BBI Consulting Services 38 Biodiesel Magazine 12 California Biodiesel Alliance 27 Crown Iron Works Company 31 EcoEngineers 23 Eide Bailly, LLP 5 Evonik Degussa Corporation 19 Frazier, Barnes & Associates, LLC 33 French Oil Mill Machinery Company 10 GEA Westfalia Separator 34 Gorge Analytical 11 INTL FCStone Inc. 24 Iowa Central Fuel Testing Lab. 25 Jatrodiesel, Inc. 22 Lindquist & Vennum PLLP 18 Methes Energies 30 National Biodiesel Board 2 Schroeder Industries 13 SGS North America, Inc. 26 Wilks Enterprise, Inc.

Researchers investigate the rare but vexing phenomenon of filter clogging at terminals

CONTRIBUTION 32 ANALYSIS

Comparison of Infrared Biodiesel Measurement Methods Examining existing and potential approaches

BY SANDRA RINTOUL

DEPARTMENTS 4 Editor’s Note

LEADING THE WAY

BY RON KOTRBA 6 Legal Perspectives

Managing Smart Phone Security Issues

BY TERESA THOMPSON AND NORAH OLSON BLUVSHTEIN 8 Talking Point

Benchtop Flow Cytometry Powers Development of Biofuels

BY JIM MULRY 10 Biodiesel Events 12 FrontEnd

Biodiesel News & Trends

14 Inside NBB 18 Business Briefs

Companies, Organizations & People in the News

Biodiesel Magazine: (USPS No. 023-975) September/October 2012, Vol. 9, Issue 5. Biodiesel Magazine is published bi-monthly by BBI International. Principal Office: 308 Second Ave. N., Suite 304, Grand Forks, ND 58203. Periodicals Postage Paid at Grand Forks, North Dakota and additional mailing offices. POSTMASTER: Send address changes to Biodiesel Magazine/Subscriptions, 308 Second Ave. N., Suite 304, Grand Forks, North Dakota 58203.

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EDITOR'S NOTE

LEADING THE WAY www.BiodieselMagazine.com

Ron Kotrba

E D I T O R I A L

Editor Biodiesel Magazine rkotrba@bbiinternational.com

Tom Bryan President & Editor in Chief tbryan@bbiinternational.com Tim Portz Vice President of Content & Executive Editor tportz@bbiinternational.com

In August I had the pleasure of attending the Collective Biofuels Conference in Temecula, Calif., hosted by Promethean Biofuels Cooperative Corp. The mix of speakers and attendees

Ron Kotrba Editor rkotrba@bbiinternational.com Jan Tellmann Copy Editor jtellmann@bbiinternational.com P U B L I S H I N G Mike Bryan Joe Bryan Matthew Spoor Howard Brockhouse

&

S A L E S

Chairman mbryan@bbiinternational.com CEO jbryan@bbiinternational.com Vice President, Sales & Marketing mspoor@bbiinternational.com Executive Account Manager hbrockhouse@bbiinternational.com

Jeremy Hanson

Senior Account Manager jhanson@bbiinternational.com

Marty Steen

Account Manager msteen@bbiinternational.com

Bob Brown

Account Manager bbrown@bbiinternational.com

Andrea Anderson Dave Austin Jessica Beaudry

Account Manager aanderson@bbiinternational.com Account Manager daustin@bbiinternational.com Circulation Manager jbeaudry@bbiinternational.com

Marla DeFoe

Advertising Coordinator mdefoe@bbiinternational.com

John Nelson

Senior Marketing Manager jnelson@bbiinternational.com

Jaci Satterlund Elizabeth Burslie

A R T Art Director jsatterlund@bbiinternational.com Graphic Designer bburslie@bbiinternational.com

Subscriptions Subscriptions to Biodiesel Magazine are free of charge to everyone with the exception of a shipping and handling charge of $49.95 for any country outside the United States, Canada and Mexico. To subscribe, visit www.biodieselmagazine. com or you can send your mailing address and payment (checks made out to BBI International) to: Biodiesel Magazine Subscriptions, 308 Second Ave. N., Suite 304, Grand Forks, ND 58203. You can also fax a subscription form to (701) 746-5367. Reprints and Back Issues Select back issues are available for $3.95 each, plus shipping. Article reprints are also available for a fee. For more information, contact us at (701) 746-8385 or service@bbiinternational.com. Advertising Biodiesel Magazine provides a specific topic delivered to a highly targeted audience. We are committed to editorial excellence and high-quality print production. To find out more about Biodiesel Magazine advertising opportunities, please contact us at 701-7468385 or service@bbiinternational.com. Letters to the Editor We welcome letters to the editor. If you write us, please include your name, address and phone number. Letters may be edited for clarity and/or space. Send to Biodiesel Magazine Letters, 308 Second Ave. N., Suite 304, Grand Forks, ND 58203 or email to rkotrba@ bbiinternational.com.

included some of the greatest recognized minds in biodiesel such as Jon Van Gerpen of University of Idaho, small commercial producers and grease collectors, home brewers, students, and all points in between. Dan Freeman of Dr. Dan’s Biodiesel said he was at the event to reinvigorate his passion for biodiesel. I know the gathering accomplished this for me. The ingenuity and innovation of the small producer should not go unrecognized. Developments by this often-marginalized sector of the biodiesel industry have led to cutting-edge technology improvements over the years, and let’s hope they continue to do so. Biodiesel margins are tight, particularly with small producers, which do not have the balance sheets and bankroll to be anything other than efficient. Riding this edge of financial success and ruin lead small producers to a position in which to survive, they must be innovative. This was seen in Temecula at the Promethean Biofuels plant tour and heard in the open-forum style of questions and answers during the event’s presentations. Speaking of questions and answers, Kent Bullard, the subject of this issue’s Q&A, “Bullish on Biodiesel Quality,” also attended the event. Kent recently retired after serving nearly four decades in the national parks department and is recognized as the longest-serving BQ-9000 auditor. It was great to pick his brain, and watch others do the same. Read about Kent’s introduction to biodiesel years ago, his tireless efforts in promoting sustainability—and his own personal mission to live his life that way—the BQ-9000 program, and Kent’s views on biodiesel’s challenges and opportunities, beginning on page 20 of this issue. I also delve into the pressing phenomenon of filter clogging at fuel terminal storage tanks in this issue. Rare instances of precipitate formation in biodiesel blends with on-spec fuel above the cloud point are thought to result from a combination of several items, including the altered chemical makeup of ultralow sulfur diesel, saturated monoglyceride content in B100, big error bars in the 6584 method and much more. ASTM approved a new No. 1-B grade voluntary spec, which features a 0.4 mono spec and 200-second year-round cold soak filtration time, to address this, but as NREL engineer Robert McCormick says, “It’s not a slam dunk.” NREL began looking into this head-scratcher at the behest of the National Biodiesel Board late last year, well after the No. 1-B grade of biodiesel was originally balloted. Read more on page 28.

Please recycle this magazine and remove inserts or samples before recycling TM

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COPYRIGHT © 2012 by BBI International


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LEGAL PERSPECTIVE

Managing Smart Phone Security Issues BY TERESA THOMPSON AND NORAH OLSON BLUVSHTEIN

IBM’s recent demand that its employees turn off Siri on their iPhones has stirred much debate. IBM feared

that the iPhone’s voice-activated assistant, Siri, “who” uploads your queries and user data to Apple’s servers, could reveal confidential or sensitive business information. While perhaps a bit overhyped, even smaller companies can look at how IBM deals with employee use of personal smart phones and tablets while managing the complexity of corporate security. Here are just a few of the lessons we can learn from IBM’s security policies. Recognize and acknowledge that your employees will use their personal electronic devices for company use. Ignoring this trend may lead to corporate security breaches. Understand that employee use of personal devices will not save company money. The trend simply poses new challenges because personal devices are filled with software not controlled by the company. Understand that your employees know next to nothing about electronic security. IBM surveyed its employees and found many employees were “blissfully unaware” of what popular apps did, and the potential security risk for each. Establish guidelines about which apps employees can use and which to avoid. Do not let employees auto-forward company emails to personal email addresses or let them use their phones for wi-fi hotspots, which poses a potential for unauthorized intrusion and snooping. Educate your employees as to why certain activities are inherently dangerous, and what harm may come to the company and its employees if there are unauthorized intrusions. Treat each individual employee and their devices differently. The higher the risk, the more security protocols required on the smart phone or tablet. It is good prac-

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tice to think about what risks are presented by different employees, and then develop standards for each group. To that end, well-thought-out, and conveyed, standards ultimately give your employees the tools to protect sensitive and secret information. So how does IBM implement its policies? IBM requires each personal device be configured with appropriate security protocols before an employee can use it. If the device is lost or stolen, the IT department can then wipe or erase the device remotely. IBM’s IT department also disables public file sharing platforms and Siri. Disabling these services limits the potential for accidental distribution of sensitive or secret company information. The concern over Siri arises from how Sirilaunched searches, emails, and queries are stored on Apple’s servers, and for how long. Siri also collects other information—names of people from your address book and other unspecified data. While some believe that Siri is not spying on you—but simply “learning” from you—other experts are not so sure. What prevents Apple from trolling important corporate information from competitors, and using it to its advantage in developing new products and services? In the end, employee-owned smart devices are here to stay. Your company’s IT department will ultimately need to address issues of security, privacy, ownership and the like. We recommend addressing these issues proactively rather than after suffering a major breach. Remember the adage about “an ounce of prevention.” Authors: Teresa Thompson, Nora Olson Bluvshtein Attorneys, Fredrikson & Byron tthompson@fredlaw.com nolsonbluvshtein@fredlaw.com


TALKING POINT

Benchtop Flow Cytometry Powers Development of Biofuels BY JIM MULRY

Flow cytometry is used to measure and analyze multiple physical and chemical characteristics of cells as they flow single file, in a fluid stream, through a beam of light. The technology is employed extensively in life-sciences laboratories for counting and sorting cells based on their individual characteristics and for assessing cell viability. It can also be used for complex studies of immune function, apoptosis (programmed cell death), cancer, stem cells, and supporting drug discovery. While flow cytometry is routinely used for life-science and clinical applications, the size, complexity, cost and maintenance requirements of conventional flow cytometry systems have historically confined their use to core facilities and large laboratories with expert users. These factors can limit use of this powerful technology by companies engaged in cutting-edge biofuels R&D as they are unlikely to have access to a central core lab or a flow cytometry expert on staff. The recent development of benchtop flow cytometry instruments, combined with user-friendly software and turnkey assay kits, is now enabling use of this technology right at the lab bench by experts and novices. New microcapillary systems require smaller sample volumes, generate significantly less waste, have lower operating costs, enable high sample throughput, and are easier to set up and run than traditional flow cytometers. The Guava easyCyte 8HT benchtop flow cytometry system by EMD Millipore offers a high-speed, automated, cost-effective method for assessing lipid content and other characteristics of algae cultures including cell numbers and culture densities; relative chlorophyll content with identification of bright, dim, and negative subpopulations; and estimates of potential lipid production. Thousands of strains of algae exist, but there can be significant variations in lipid content between different strains. Identification of high-lipid-producing strains is a prerequisite for sustainable, cost-effective production of algae biofuel. Benchtop flow cytometry offers a high-speed, automated, cost-effective method for assessing lipid content in various algal strains. In addition to identifying which algal strains contain the highest lipid levels, the type of chlorophyll present in the strain must also be considered. Algae strains contain different combinations of chlorophyll molecules, designated A, B and C. Algal strains containing 8

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chlorophyll A produce lipids that are best suited for biofuel development. Some algal strains may have high lipid content but the lipid has not been generated via a process involving chlorophyll A. Therefore, the lipid may not be optimal for biofuel production. Chlorophyll A-positive populations can be identified by flow cytometry by their fluorescence. Applying a gate on chlorophyll A-positive cells allows these cells to be evaluated directly for lipid content. Both chlorophyll A and lipid content can be evaluated in an algal sample in less than three minutes on the Guava easyCyte system. Samples in 96 well plates can be placed in the Guava system allowing for walk-away automation. Benchtop flow cytometry is also used for cell counts and to monitor algal cultures for contamination. The forward scatter function of the flow cytometer can distinguish algal cells from bacteria based on size. The elimination of sheath fluid in benchtop systems, which allows for small instrument footprint, also provides additional benefits. Bard Holdings headquartered in Morrisville, Pa., has developed a unique patent-pending modular system to cultivate algae in a closed-loop, sustainable process. Charles Clerecuzio, chief operating officer, describes flow cytometry as being critical to their operations. One guava flow cytometry system sits in their support lab for R&D and production and is used to adjust feeling requirements and to evaluate biomass levels. “On the R&D level, the system evaluates the strains themselves and tracks the conversion from reproducing to producing lipids and fats for energy storage when the algae is under stress,” Clerecuzio said. “We want to feed the cells of a lot of rich nutrients and grow up as much biomass as possible—build the factories and then you switch conditions to stress the cells out. There’s various ways to stress the cells so we also look at pre- and post-stressing and what methods are effective using the flow cytometer.” Prior to adoption of flow cytometry, more labor intensive, time-consuming techniques such as hemocytometry were used. Clerecuzio noted that the guava system delivers more robust, reproducible results. Bard runs three shifts; with the ease-of-use and automation offered by the system, human error is minimized. Author: Jim Mulry Clinical Development Manager, EMD Millipore (510) 427-4641 Jim_mulry@merckgroup.com


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Biodiesel News & Trends

Looking at biodiesel production in new ways Jon Van Gerpen, a professor at the University of Idaho, wants people to think more fundamentally about biodiesel production. “There are a lot of things we don’t know about the biodiesel process,” he said at the Collective Biofuels Conference. “It’s deceptively simple.” He raised questions that perhaps should have been asked 20 years ago during biodiesel’s infancy, including, “What affects the reaction, and why?” and “Can we guide the reaction in some way?” Methanol’s solubility in oil is limited, so excess methanol is used to facilitate reaction. There’s only 1 percent oil in excess methanol droplets. “The reaction only occurs on the surface of those droplets,” he explained. “The diffusion process moves the oil to reaction zone, and then moves the methyl esters away.” Transesterification is conventionally referred to as a mass transfer limited reaction, but it could be chemical reaction limited. “We usually don’t know which,” he said. “There’s a balance between the relative significance of diffusion and reaction.” Van Gerpen is developing equations to address this. “Diffusion we can do,” he said, “but the piece we’re missing is we don’t know what the chemical reaction rate is in the droplets.” Some calculations have been done by industry but only for specific reactors and parameters. He cited David Boocock’s (Toronto) pioneering work in cosolvent use for biodiesel, used by Biox today. A cosolvent changes a two-phase reaction into one. With a cosolvent there is no longer a mass transfer limitation so, as Van Gerpen said, “The measured rates should be the true chemical reaction rate.” He said modeling can tell us where monos and di’s reside in the droplets. Also, it can help understand how methanol droplets get smaller as the reaction proceeds, and how glycerin behaves in methyl esters. “Can we optimize the timing of agitation and settling for the fastest overall process?” he asked. Ultimately, he said, “This knowledge has to help design a better process, but I’m not sure how just yet.” An important conclusion is that the process should no longer be called mass transfer limited.

Argentina raises export tax, files WTO complaint 40 35

Current soybean export tax

30

percent

FrontEnd

25 20 15 10 5 0

Former biodiesel export tax

Current biodiesel export tax

After Spain closed all imports of biodiesel from Argentina to bolster its own idled industry—until months ago a major outlet for Argentine biodiesel—the South American country raised its national biodiesel blend mandate from 7 to 10 percent. Just recently, the Argentine government increased the biodiesel export tax from 20 percent to 32 percent, a move that has the nation’s biodiesel plants “very upset,” said Georges Breitschmitt of Recup-Oil, a small-scale producer in Argentina. Argentine biodiesel production is expected to hit 3.2 million tons (approximately 961 million gallons) this year, Breitschmitt said, up from 2.4 million tons in 2011 and just 700,000 tons in 2008. In August, Argentina filed a complaint with the World Trade Organization against the European Union about the protectionist Spanish trade barriers.

Representing biodiesel producers, marketers, retailers, feedstock suppliers and stakeholders in California Biodico Sustainable Biorefiner ies

Membership Info: call (916) 583-8015 | www.CaliforniaBiodieselAlliance.org 12

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FRONTEND

US yields 557M gallons of biodiesel through June 150

in millions of gallons

120 90 60 30 0

Jan/Feb

March

April

May

June

The U.S. EPA said 112 million gallons of biodiesel were produced in June, reporting year-to-date production of 557 million gallons through the first six months of the year. Biodiesel production is reported under the EPA’s biomass-based diesel category in the renewable fuel standard (RFS). The EPA numbers show a total of 117.5 million gallons of biomass-based diesel for the month of June, but that figure also includes renewable diesel. Last year, the biodiesel industry set a new production record of nearly 1.1 billion gallons, supporting more than 39,000 jobs across the country.

Plant news from around the globe A new 3 MMly multifeedstock biodiesel plant in Thetford Mines, Quebec, owned by Innoltek, received a $200,000 loan from the Canadian government to purchase and install a distillation system, boiler and reactors, and to finalize layout of the production facility. BDI-BioEnergy International AG was commissioned to build a multifeedstock biodiesel plant in the French port city of Le Havre. The order volume amounts to €16.4 million ($20.1 million). W2 Energy Inc. announced that its recently acquired 650,000 gallon biodiesel plant from Agri-Green Biodiesel Inc. was transported to Guelph, Ontario, and is ready for production. A new biodiesel plant in Cuba using jatropha oil feedstock has begun production. The small refinery located in Guantanamo province is scaled to produce 30,000 gallons per year. Algae.Tec Ltd. held official commissioning of its Shoalhaven One showcase algae production facility in Bomaderry, New South Wales, Australia. Golden Leaf Energy, a 2.2 MMgy multifeedstock biodiesel producer in Harvey, La., plans to expand production with financing help from the New Orleans Startup Fund. Methes Energies Canada Inc. held a grand opening ceremony for its new 50 MMly multifeedstock biodiesel facility in Sombra, Ontario. The California Energy Commission approved $1.86 million in grant funding for the expansion and upgrade of Yokayo Biofuels Inc.’s Ukiah, Calif.-based biodiesel facility, increasing biodiesel production capacity from 1,400 gallons a day to 2,000 gallons a day while retrofitting its process line to enzymatic production. Yokayo is working with Piedmont Biofuels on the enzymatics. Genuine Bio-Fuel Inc. headquartered in Indiantown, Fla., plans building a new biodiesel plant in Lincoln Park, N.J., at the Lincoln Park Airport.

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The Drought is No Reason to Reverse Course on American Fuel For the first time in history, our nation is making meaningful progress in the drive for sustainable energy independence. This is thanks to strong federal policy that has made developing American-made fuels a priority. The federal renewable fuel standard (RFS2) led the U.S. into a record year of biodiesel production and use, more than 1 billion gallons in 2011. This is genuine progress in the quest for energy security, and it brings with it jobs, economic development and additional fuel refining capacity that this nation sorely needs. These benefits are tangible and real, as are the environmental benefits of biodiesel. To be sure, the drought’s grip on the U.S. is also real. Extreme weather conditions and record-breaking heat waves present new challenges to the nation’s farmers and ranchers. Foreseeing fluctuations in crop yields, the biodiesel industry has worked with policymakers through the years to set responsible, attainable goals for biodiesel growth. That includes being ready for unforeseen circumstances, like the current drought. We should not let one year of drought threaten to undo meaningful momentum in the rise of American fuels. To the contrary, we need consistent policy, like RFS2, which reduces volatility. Pulling the plug on domestic energy production leaves us vulnerable to price shocks induced by foreign cartels. As farmers and ranchers struggle with drought conditions across the country, biodiesel producers have continued to stimulate rural economies with domestic energy production. Biodiesel’s feedstock diversity allows for flexibility in times of market instability such as the current drought. This flexibility allows biodiesel production to continue using an optimal blend of feedstocks based on market conditions. On top of a diverse feedstock base, biodiesel demand is also flexible. The RFS2 is built to be flexible. The program is designed to allow up to 20 percent carryover production from one year to the next to avoid supply and demand pressures that could develop. This built-in flexibility means that producers can work within short-term market conditions to meet obligations.

Biodiesel Production Benefits Food Markets All of the feedstocks for biodiesel production come to the market as a byproduct or coproduct of existing food production industries. The utilization of oils and fats in biodiesel production helps add value to underutilized byproducts. This either reduces the consumer cost or increases the producer profit of products like soy protein meal, fried foods and packaged meats. Biodiesel produced from soybean oil benefits many food markets stressed by drought. Since soybean oil-based biodiesel uses only a portion of the soybean, biodiesel production leaves valuable soy protein meal on 14

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the market and reduces the price pressure that the meal portion has to carry. For livestock producers, this means a lower relative price for soybean meal as livestock feed. On the livestock side, an increased demand for animal fats as biodiesel feedstocks improves the value per head for livestock and reduces price pressures on consumer meat and dairy products. Don Scott, Director This is why a number of livestock production of Sustainability, National Biodiesel groups are on record supporting biodiesel. Board From a sustainability perspective, getting more out of one single product is a much better utilization of resources. Using the byproducts and coproducts of existing industries to produce biodiesel means a more sustainable fuel.

Protect Resources, Prevent Future Disasters While much of the drought coverage is focused on the here and now, it is important to look ahead and do all that we can to prevent similar situations in the future. While there is a difference between weather and climate change, it is impossible to deny the frightening number of record weather events in recent history. While these record-setting weather events forebode increasing stresses on our food production systems and society, in general, we must recognize that our industrialized society is pumping millions of tons of carbon dioxide and other greenhouse gases into the atmosphere as a result of reliance on fossil fuels. The same addiction that causes us to pump billions of dollars overseas to buy oil is also choking our atmosphere with carbon from permanent underground stores. One of the most significant environmental benefits of biodiesel is a reduction in greenhouse gas emissions. Biodiesel is the best option for powering our trucks, buses, tractors and diesel cars while minimizing the carbon dioxide and other greenhouse gases that are building up in our atmosphere. Biodiesel also makes wise use of valuable water resources. Biodiesel production reduces wastewater production by 79 percent and reduces hazardous waste production by 96 percent compared to petroleum diesel production. Biodiesel is nontoxic and biodegradable. Preventing contamination is the best way to protect our natural resources. Drought conditions have been difficult this year but the industry must work hard to keep misinformation from derailing the great progress the biodiesel industry has made. Don Scott, Director of Sustainability, National Biodiesel Board


inside

NBB RFS waiver requests and biodiesel As the drought takes its toll across the Midwest, debate over waivers of the renewable fuel standard (RFS) have grown. In recent weeks, a variety of sources have urged the EPA to waive, in whole or in substantial part, the RFS for one year. While many believe that waiving the RFS is not good policy, the National Biodiesel Board has been pleased that biodiesel has not been cited in these waiver requests. In fact, many of the lawmakers and other groups seeking a waiver are biodiesel supporters who have assured NBB that they have no intention of attacking the biodiesel RFS requirement, and we see little impetus for a waiver of the biomass-based diesel category. That said, any effort to waiver or alter the RFS is a potential threat to the program, and NBB’s federal affairs team has been working hard to bolster support for the policy and raise awareness of its critical importance to the biodiesel industry. For example, because the waiver requests have their roots in livestock and poultry states, the team has worked closely with sup-

porters on Capitol Hill and with partners in the livestock industry to ensure that the biodiesel story is accurately portrayed. The following points have been emphasized: • The biodiesel industry uses a diverse mix of feedstocks and has significant flexibility in overcoming production setbacks from drought. Most biodiesel plants can utilize a variety of feedstock and will shift their production accordingly if there is a shortage in any one feedstock, such as soybean oil. • Many livestock groups support the biodiesel industry because we provide a market for animal fats (a leading biodiesel feedstock) and because our production from soybeans stimulates the market for soybean oil—thereby boosting supplies of soybean-meal livestock feed and reducing its cost. NBB continues to monitor the situation closely in Washington, D.C., and urges all biodiesel supporters to spread the word that biodiesel is the only feedstock-diverse, EPA-designated advanced biofuel being produced on a commercial scale across the country.

NBB works to continually improve specs as petrodiesel, diesel engines change Fuel quality and a strong set of standards remain one of the highest priorities for the biodiesel industry. This is especially true as refiners optimize still relatively new ultra-low sulfur diesel (ULSD) fuel and diesel engine makers implement new technology that makes diesel engines 90 percent cleaner than just a few short years ago. Over the past two years, a handful of cases occured where ULSD/biodiesel blends experienced unexpected filter clogging above the cloud point. This led to interest in creating a No. 1-B specification for biodiesel. The new grade maintains the same parameters as the current standard, and provides more stringent controls for minor components, which have been implicated in rare filter clogging in the field with ULSD. “We are committed as an industry to being proactive so biodiesel continues to be the highest quality, most proven advanced biofuel on the market,” said Kyle Anderson, technical projects manager for the National Biodiesel Board. NBB encourages stakeholders to become ASTM members to provide input in the setting of industry specifications.

“Participating in the process that sets the standards your industry must operate under is extremely critical and simply makes sense for biodiesel producers,” Anderson said. “As a trade association, we do everything we can to make it easy for our members to be involved. At the end of the day we need specs that give customers confidence in the fuel that is being produced and used across the country.” For more information on fuel quality specifications and becoming more active in maintaining and setting specifications, contact Kyle Anderson at kanderson@biodiesel.org or (800) 841-5849. SEPTEMBER | OCTOBER 2012

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insideNBB

OEM support for B20 reaches all-time high 2012 is proving to be another big year for biodiesel in a number of ways, but possibly one of the most exciting areas of growth has been the number of original equipment manufacturers (OEMs) supporting the use of B20 in their vehicles and equipment. So far in 2012, 10 more OEM brands have been added to the list of manufacturers supporting B20 or higher blends in at least some of their equipment. With these new additions, now more than 77 percent of the overall U.S. diesel vehicle market supports B20, a 17 percent increase over last year. Great progress was made with the medium-/heavy-duty truck and bus manufacturers this year, as seven of the new B20 supporters come from that category: Volvo Trucks, Mack Trucks, and the Daimler Trucks North America family of brands including Freightliner, Freightliner Custom Chassis, Detroit Diesel, Western Star, and Thomas Built Buses. With these new announcements, now more than 95 percent of the medium- and heavy-duty truck markets support B20. The other three new B20-plus supporters are in the offroad equipment category and include Buhler, Kubota and Deutz, a German OEM that announced its support for the use of B100 in its Tier IIIb Agripower equipment. The National Biodiesel Board’s OEM Outreach and Education Program has been working with these and all major manufacturers for several years, educating them on the latest biodiesel industry advancements and addressing their technical concerns as necessary to help foster their support for B20. These ongoing educational efforts, along with growing biodiesel availability, robust fuel quality specifications and practices under the industry’s BQ-9000 program,

and the OEMs’ own successful B20 research efforts have all led to this remarkable growth in market acceptance for B20 biodiesel blends. It should also be noted that all major OEMs selling diesel equipment in the U.S. support at least B5 and lower blends, provided they are made with biodiesel meeting ASTM D6751specifications. Most OEMs are also recommending use of a BQ-9000 supplier. For a complete detailed listing of OEM position statements on biodiesel, as well as the current U.S. diesel vehicles list, visit: www. biodiesel.org/using-biodiesel/oem-information.

NBB members invited to help lead, set direction for their association The upcoming National Biodiesel Board membership meeting Nov. 12-14 in St. Louis is one of three major membership meetings at which industry participants can help set the direction for the future of the biodiesel industry. “Any successful industry association is made up of actively engaged members who are educated about our issues and volunteer their time to execute the membership’s vision for the future,” said NBB Chairman Gary Haer. “There are many opportunities throughout the year for members to network through committee participation or at membership meetings.” This year, an election committee appointed by Haer is seeking nominations to fill seven board positions created by term expirations. “If you are considering a committee leadership or board position, I, or the staff, am happy to facilitate introductions to others in that group who can help you learn more about leadership roles,” said Haer.

NBB welcomes new members JP Morgan Ventures Energy Corp.—New York, N.Y. 16

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“These leadership positions are critical to our industry and manageable in your current job.” The annual review and update to the organization’s Resolutions and Position Handbook also takes place in the fall. NBB members have an opportunity prior to the November board meeting to review the current industry positions. The agenda at the board meeting then offers time for committee considerations and, ultimately, a governing board vote on potential changes to existing resolutions and the adoption of new resolutions. “We know that our industry is full of passionate individuals with great ideas for moving our industry forward,” Haer said. “We want to hear from you about those ideas or help answer your questions. Please do not hesitate to send an email or call me or the other board members. And, as always, our dedicated staff is always available to help the membership.”

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insideNBB

Sneak peek: 2013 National Biodiesel Conference captures new momentum

Twenty years of momentum has brought biodiesel to record production, but where do we go from here? Make sure you’re a part of the next wave by attending the 2013 National Biodiesel Conference & Expo Feb. 4-7 at the Mirage Resort & Casino in Las Vegas. NBB members can receive the best available rate by registering before the Sept. 30 early-bird deadline. 2013 marks a momentous occasion for the biodiesel industry as we celebrate the 20th anniversary of the National Biodiesel Board, and of the U.S. biodiesel industry itself. During this conference we will look back at how far we have come, while maintaining our focus on how we get to where we want to go. Working educational sessions currently planned include: • How Big, How Soon? “All-in” with Biodiesel Feedstock • Update on Third-Party Approvals for Tanks, Storage and Dispensers • The Future of the Renewable Fuel Standard • Biodiesel: The Most Sustainable Fuel on the Planet • You Say You Want an Evolution? How a Bioheat Campaign Created Change

In 2013, we also celebrate the 10th National Biodiesel Conference & Expo. This conference has grown from a small gathering at our first event in Palm Springs, Calif., in 2004, to a powerful platform that drives biodiesel business all year long. We routinely hear from exhibitors and attendees that the deals made at this event affect their balance sheets all year long. This conference is the only event to gather biodiesel leaders and decision makers from throughout the U.S. and the world. Las Vegas is an important city in the history of biodiesel, and is home to many pioneers who have made a lasting impact on our industry. We’ll hear from some of those champions. We’re betting this is our best event yet, and that you will find it worth your while to join us. See you in Las Vegas! www.biodieselconference.org

No summer doldrums in Washington, DC Although Congress has been in recess for weeks, Washington has been a busy place for the NBB team as a variety of issues percolate through the federal process. A quick update on the issues about which the most frequent meetings with lawmakers and the executive branch include: • Regarding the 2013 RFS volume, it is expected that a final decision will be announced by the time this magazine is published, but as of press time there is still no announcement. The intense focus on the drought and the RFS, NBB believes, has already diverted federal resources from resolving this issue and that could continue. In addition to the 2013 volume, the EPA is also working to finalize future year volumes for other categories of the RFS, a new pathway for camelina, a new processing pathway for biodiesel esterification, and a rule modifying the definition of heating oil under the RFS. • NBB continues to work closely with the EPA and petro-

leum industry groups to find solutions for addressing RIN fraud. On that front, NBB has expanded its work with the law firm of Bingham McCutchen to help navigate the process and fight for the biodiesel industry’s priorities. Bingham McCutchen has experience in this area as they helped NBB win a series of RFS-related lawsuits in recent years. • Congress adjourned without passing a farm bill, but the industry was successful in getting some biodiesel priorities included in the House and Senate versions of the bill. NBB continues to push for final passage. • The Senate Finance Committee on Aug. 2 passed a bipartisan package of tax extensions that includes the biodiesel tax incentive. This represents significant progress on this front and puts the industry in a good position to win an extension if Congress can come together to pass tax legislation later this year.

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BusinessBriefs

BP Connect Hoon Hay offers both BP biodiesel blend and petroleum diesel throughout the trial, both at the same price. PHOTO: BP P.L.C.

Renewable Energy Group Inc. announced its financial results for the quarter ending June 30. Revenue for the second quarter was $271.9 million, an increase of 39 percent compared to revenues of $196.3 million for the same period in 2011. Second quarter 2012 adjusted EBITDA was $26.5 million, an increase of 3 percent compared to $25.8 million for the same period in 2011. The balance sheet remained strong with cash of $87.1 million at the close of the quarter, compared to $75.2 million at March 31. REG produced 43 million gallons of biodiesel in the second quarter of 2012, compared to 33 million gallons in the same period in 2011. REG sold 54 million gallons of biodiesel in the second quarter, an increase of 63 percent compared to the same period in 2011, excluding tolled gallons. The year-over-year increase in gallons sold was primarily due to increased production capacity online and an increase in biodiesel demand compared to the same period in 2011.

Companies, Organizations & People in the News

BP announced that it is offering a BP biodiesel blend to Christchurch, New Zealand, retail customers at BP Connect Hoon Hay. The new product will be trialed for a six-month period with a potential rollout planned for other sites around the country, should it prove popular with customers. BP has partnered with local Christchurch company, Biodiesel New Zealand, to produce the BP biodiesel blend. The product is a blend of normal mineral diesel and up to 5 percent biodiesel, the maximum amount of biodiesel allowed in a blend under current New Zealand legislation. The biodiesel component is sourced from Biodiesel New Zealand and is produced from locally grown canola oilseed and premium used cooking oil.

Ultra Green Energy Services held a ribbon-cutting ceremony and operational demonstration of its new transload facility at Brookhaven Rail Terminal in Long Island, N.Y. The terminal operations will make biodiesel more readily available across Long Island and supply fuel for the New York City Bioheat mandate that goes into effect in October. The company will receive railcar shipments of B100 and says it can store up to 250,000 gallons at the facility. UGES supplies biodiesel through the largest network of wholesale terminals in the metropolitan region. Its principals were among the first to market biodiesel in 1999 and have been blending Bioheat since 2001. The company now operates rail transload facilities and product supply terminals in New York and New Jersey, and has supply positions in Connecticut, Pennsylvania, Massachusetts, New Hampshire, Vermont and Maine.


BUSINESSBRIEFS Sponsored by International Procurement Tools LLC of Reno, Nev., and Incbio of Trofa, Portugal, signed of a memorandum of understanding to form a joint venture to cooperate in the sale, marketing, distribution design and installation of Incbio’s breakthrough ultrasonic cavitation technology worldwide. The new cavitation systems offer much more flexibility in the selection of oil-bearing feedstock from higher FFA greases to complex acceptance of the new algae that are starting to appear. The new facilities’ returns on investment promise to be shorter and production cycles simpler. The new systems are available for installation in any existing biodiesel facility that produces either ASTM or EN quality fuel. Pricing and quotes are available on signing of an NDA/NCA with either IncBio or IPT. Neste Oil and Stora Enso have decided not to progress with their plans to build a renewable diesel plant, for which the two companies had applied for funding under the EU’s NER 300 program. The European Commis-

sion recently published a review on its website of projects that have applied for NER funding, and Neste Oil and Stora Enso’s project is not among those listed as scheduled to receive this funding. Executives say even if they did receive funding, the project would have been shelved. The trials carried out by Neste Oil and Stora Enso at a pilot plant in Varkaus between 2009 and 2011 on the entire chain needed for the planned plant—from wood biomass to biowax suitable for use as a raw material for producing renewable diesel—proved successful. Aemetis Inc. signed a license agreement with Chevron Lummus Global for the inexpensive, rapid production of renewable jet and diesel fuel by the conversion of existing biofuels and petroleum refineries. The license agreement grants Aemetis Advanced Fuels Inc., a wholly owned subsidiary of Aemetis, the use of the Biofuels Isoconversion Process for the production of 100 percent drop-in renewable jet fuel and diesel in Aemetis biorefineries throughout North America. The process

utilizes patented catalytic hydrothermolysis reactor technology, developed by Applied Research Associates, which utilizes water as a catalyst to quickly and inexpensively convert plant oils into stable intermediate oil products that are very similar to petroleum crude oil. The intermediate oils are processed with hydrogen using CLG’s Isoconversion catalysts to produce drop-in jet fuel and diesel. Unlike most other process technologies, the renewable fuels produced by this process are 100 percent replacements for petroleum-based jet and diesel fuel. CLG licenses refining hydroprocessing technologies and catalyst systems worldwide, and is a 50/50 joint venture between Chevron Products Co., a wholly owned subsidiary of Chevron Corp., and Lummus Technology Inc., a CBI Company. SHARE YOUR BUSINESS BRIEFS To be included in Business Briefs, send information (including photos, illustrations or logos, if available) to: Business Briefs, Biodiesel Magazine, 308 Second Ave. N., Suite 304, Grand Forks, ND 58203. You may also fax information to (701) 746-5367, or email it to rkotrba@ bbiinternational.com. Please include your name and telephone number in each correspondence.

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Q&A

'WALKING THE TALK': Kent Bullard, standing next to his B100-powered Dodge truck, was instrumental in getting 23 U.S. National Parks turned on to biodiesel.

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Q&A

Bullish on Biodiesel Quality A sit-down with fuel quality assurance expert Kent Bullard QUESTIONS BY RON KOTRBA PHOTOS BY WAYNE SMITH

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Q&A Kent Bullard wears many hats, but in this industry of biodiesel he is commonly referred to as the longest-serving auditor for the BQ-9000 quality assurance program. Bullard says he was raised with a respect for the environment while growing up in several Western National Parks, as his father was a park ranger. After graduating from high school, he served three years in the U.S. Army as an electrician. Afterwards, his federal career of nearly four decades began with a seasonal position in northern California, a career appointment in Montana and then he transferred to Rocky Mount National Park in Colorado. After a couple of years, while faced with another winter of shoveling snow at 8,000feet, Bullard opted for a transfer to AUDIT DETAILS: As the National Biodiesel Accreditation Commission's longest-serving BQ-9000 auditor, an island off the coast of southern Bullard says the most common noncompliance issues he sees with BQ-9000 are record maintenance and semantics with program requirements. California at Channel Islands National Park. Once there, he was also able to complete his bachelor’s degree in occupational education from Southern Illinois University, with installing more than 50 photovoltaic installations in Channel Islands National Park and, as a result, received an individual Federal Port Hueneme, Calif. “Working on islands tends to get one in tune with conserva- Energy Management Award in recognition for his work. Bullard’s decision for graduate school with a concentration in tion, renewable energy and doing the right thing,” Bullard tells Biodiesel Magazine. Since the early 1980s, Bullard has been involved quality management was, as he says, “a harmonious blend of local

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Q&A school availability and a desire to do things better.” While working full-time, he completed his master’s in Quality Assurance from California State University in Dominguez, Calif. Q: How and when did you first get involved in biodiesel? A: In 1996, I read an article in “Solar Today” about the Sunrider’s trip around the world using biodiesel. A light went off. Since 1997, I’ve had a bottle of biodiesel setting on my desk. In 1998, while attending a Green Energy Parks workshop, I proposed the utilization of biodiesel for the National Park Service that resulted in a pilot project with 23 parks across the country starting on biodiesel in 2000. Channel Islands’ involvement in the project was to run a 56-foot research vessel and Anacapa Island on B100, making it petroleum-free in conjunction with solar. Being an advocate also involves “walking the talk,” so it is for that same reason that I chose to live in a 100 percent solar-powered home. I bought a 1984 Mercedes 300D and began running B100. My fleet eventually included a Volkswagen Golf and Dodge 2500, both also running on B100. My efforts in the utilization and promotion of biodiesel resulted in my receiving the first Eye on Biodiesel Award for Inspiration and a second Federal Energy Management Award. Q: You are often recognized as the longest-serving BQ9000 auditor, but you do much more than that. What other employment do you hold, and what additional biodiesel-related ventures are you involved in? A: I performed my first BQ-9000 audit in August 2005, and since that date I have audited producers, marketers and laboratories across the country and Canada. In addition, I have provided BQ-9000 training at various regional and international venues. Also

in 2005, I co-founded the Los Angeles Biodiesel Cooperative to provide B100 to dedicated users. I have served on the board of directors of the Sustainable Biodiesel Alliance since 2007. I founded the Southern California Biodiesel Users Group in response to California Division of Measurement Standards requirements for the purchase of blends higher than B20 in the state. Currently, membership in the Los Angeles Biodiesel Cooperative stands at around 4,500. For the past two years, I have worked with Lee Enterprises as the team’s BQ-9000 consultant and quality assurance specialist. This January, I retired from the National Park service after 36 years of federal service. Q: You not only work with renewable energy such as biodiesel, but you also live your life that way. Could you share your view on sustainability and what you do in your personal life to be so? I gave a PowerPoint presentation in San Diego in 2005. I was able to present just prior to Tad Patzek (of the infamous Cornell/ Berkley Report). Now, granted some things have changed since then, but my philosophy on sustainability shows through. Sustainability is about leaving this earth to future generations in as good or better condition as when we took responsibility. It's about living within the limits of the earth as we limit our utilization of finite resources. Think of the earth as an island with limited resources. Sustainability is adapting our needs to fit the environment with the minimum impact, and not using it all for ourselves. It’s leaving the next generation the ability to live a quality life. Sustainability is about making educated choices regarding our use of energy resources. Biodiesel is one fuel option we have that reduces our impacts on finite resources. My home is powered 100 percent by solar electricity, which also has provided the power to run our 100 percent electric Nis-

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Q&A

GOOD TIMING: Bullard recommends BQ-9000-accredited organizations perform their yearly internal audits six months out from the official program surveillance audit in which the BQ-9000 auditor pays an on-site visit.

san Leaf for more than 10,000 miles in the past year. Water conservation at my home includes dual-flush toilets, drip irrigation, rainwater collection and short showers. I have served as a member of the board of directors for the Sustainability Council of Ventura County since 1997. Projects I have led include forming the Green Building coalition of Ventura County and serving as the chairman of the Green Team for Habitat for Humanity of Ventura County. Q: Take me through a day in your working life―what is your typical day like? A: Retirement is good. It allows me time to do some household chores. My auditing duties are part time, so there is a mix of dealing with existing clients in closing audits, clarifying positions and answering questions throughout the month. I also have new audits that require thorough document review and a desk audit prior to performing the on-site registration audit. As a one-person shop, I also am a travel agent, 24

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accountant and administrative clerk in completing monthly reports. In performing registration and surveillance audits, I travel to the organization’s location and spend one to two days on site performing the audit and then travel back home. Once any audit findings are closed, I complete a final audit report for the National Biodiesel Accreditation Commission’s approval. Q: For those who don’t know, please briefly describe the BQ-9000 program. How has it changed over the years, and why? A: The BQ-9000 program is a Quality Assurance Program based on process control. It is modeled after ISO 9000. The BQ-9000 accreditation is for the organization’s quality assurance program, not the product. Just as ASTM does not certify fuel, nor does BQ-9000. Thus, when you see someone representing to sell “ASTMand BQ-9000-certified fuel,” you will know that they are unsure of the concept of quality assurance and, as a consumer, you


Q&A should be unsure about the quality of their product. As with any quality assurance program, change is a good thing as it involves continuous improvement. Since the original BQ-9000 program guidelines were written, change has occurred to redefine the process, clarify requirements, and respond to regulatory change and external requirements such as ASTM. Q: Could you explain the program differences for producers, marketers and laboratories? A: There is really very little change between the three program requirements. Remember, this is a program requirement so elements such as record keeping, training, and document control and management responsibility are similar. Operational elements and beyond are specific to the program being audited.

SKEPTICAL EYE: Bullard says if someone tries to sell “ASTM and BQ-9000-certified fuel,” be wary whether they understand the concept of quality assurance.

Q: While 80 percent of U.S. biodiesel volume is BQ-9000-certified, only 40 plants hold accreditation, meaning about 160 U.S. plants, mostly smaller producers, do not. Why do you think smaller producers are disinclined to pursue BQ-9000, and what efforts have the organization taken to reverse that trend? A: Customer demand is key in pushing an organization to seek BQ-9000 accreditation. Scale of operation makes it easier for larger operations to afford the resources to obtain accreditation. Smaller organizations are often on the edge of operational success; fiscal resources are not always available for BQ-9000 registration. That does not mean that they should or do not have a quality assurance program (often modeled on BQ-9000) in place. I as a biodiesel consumer do tend to ask about quality assurance and what’s going on. An answer like occasionally they visually check the fuel for “gickies” is not good enough. I want some program elements in place, something as simple as a quality manual, for instance. I may not have many options of my fuel source, but I do have the final say. The BQ-

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Q&A 9000 program is self-supporting and costs are kept low. Program costs primarily are to cover the auditor’s travel and time. There is really no way to have a blue-light special on quality. Q: What all does a BQ-9000 audit entail? A: An audit begins with the organization developing a quality program that meets the specific BQ-9000 program requirements.

The BQ-9000 accreditation lasts three years. After the initial accreditation audit, organizations are required to perform annual internal audits, and they are also subject to surveillance audits annually by the BQ-9000 auditor. Essentially a surveillance audit is not a full bore audit, but the auditor still goes through the checklist and records. When I come to perform a surveillance audit, I review their internal report and review any corrective actions and the minutes of the report. I also recommend that the organiza-

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Q: How often does an audit turn up program infractions? A: To maintain impartiality, auditors do not see others auditors’ work. Thus, any answers I give in this area are based on my biased views. I do know that auditors can interpret things differently. Also, it is the auditor’s job to verify compliance with program requirements, not to find program infractions. When noncompliance items are found, corrective action is implemented and the audit cannot be closed until all items are closed.

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tion does its internal audits six months out from the surveillance audit. For example, if an organization has their first audit in August, they will be subject to a surveillance audit the following August. But I recommend that in February they complete their internal audit so when I come again in August, they didn’t just complete their internal audit a few weeks prior.

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SEPTEMBER | OCTOBER 2012

Q: What are the typical remedies to those? A: Editing corrections and organizational change. Q: Of the three categories, which (producer, marketer, lab) yields more noncompliance? It is pretty much the same, but it varies with the organization’s quality background. Q: Biodiesel fuel quality has improved greatly over the years, what do you attribute this to? A: The quality of biodiesel has improved as specifications have evolved to


Q&A address individual items, such as the need to address sulfur content and metals in the fuel, which has helped build OEM acceptance, or the introduction of the cold soak filtration test to improve cold weather performance, or the accelerated (three-hour) oxidative stability test to ensure the fuel won’t oxidize too quickly in storage or a vehicle fuel tank. It has taken great work by the ASTM committee and organizations to implement new requirements. What BQ9000 does is help ensure conformance to the latest standard. Q: You are a consultant with Lee Enterprises, which merged elements of its RIN verification program (RIN 9000), such as fuel sampling to ensure quality, with Genscape’s NBB-supported RIN Integrity Network, established as one of many programs to provide obligated parties due diligence in RIN purchasing and to help avoid future cases of biodiesel RIN fraud. Could you explain your role under this program arrangement? A: Although there can be some parallels with recordkeeping and testing, the two programs are different and carry different compliance accreditations. At this time I am not involved in RIN verification programs. Q: What do you think of the new No.1-B grade of biodiesel that has been under development now for a couple of years, which ASTM just recently sanctioned? A: The new ASTM specification for No. 1-B biodiesel is important, as with petroleum diesel it addresses fuel utilization in varying climatic conditions. Q: In your opinion, what are the biggest challenges facing the biodiesel industry today? How might those challenges best be addressed? A: The biggest challenge for the indus-

try today will be the competition for feedstock. The current drought conditions and low crop yields will make it difficult for row crop feedstock to remain competitive. There will again be a great uproar over food costs, availability and the concept of using crops for fuel. It always will be difficult for biodiesel to chase the swings in petroleum costs.

The RFS requirements will continue to move biofuels into mainstream use. Adding additional feedstock options will make biodiesel and biofuels competitive and acceptable for the consumer. Author: Ron Kotrba Editor, Biodiesel Magazine (701) 738-4942 rkotrba@bbiinternational.com

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TESTING

DETECTIVE WORK: Robert McCormick and Teresa Alleman of NREL study why, on rare occasions, on-spec biodiesel blended with ULSD leads to precipitate formation and filter clogging above the cloud point. PHOTO: DENNIS SCHROEDER, NREL

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TESTING

Solving a Great Biodiesel Mystery The best researchers scratch their heads at rare, isolated cases of storage tank filter clogging with biodiesel blends BY RON KOTRBA

The introduction of ultra-low sulfur fuel for on-road diesel in 2006-’07 brought unexpected consequences for biodiesel blending. Refiners began hydrotreating diesel fuel to reduce sulfur to 15 parts per million and, in doing so, changed the solubility characteristics of diesel fuel by removing aromatics and other compounds. “Aromatic compounds are good at making relatively polar things soluble,” says Robert McCormick, a principal engineer at National Renewable Energy Labs. “So when you take them out, that could become an issue.” Sporadic issues with biodiesel blends clogging filters, both vehicle and dispenser, above the cloud point with on-spec B100 arose, recounts Steve Howell, National Biodiesel Board technical director. In general, clogged filters were found to have high levels of sterol gluccosides and saturated monoglycerides. “That prompted the development of the cold soak filtration test,” Howell says, “as a performance test on B100 to pick up any minor biodiesel components that were precipitating out in the field that were not showing up in the cloud point test.” A performance test was desired over measurement of individual components since more than one or two minor components were found on the sampled filters. The CSFT was designed so the cloud point can still be used as a conservative indicator of cold flow operability for blends in the field if the B100 met the CSFT prior to blending. Two CSFT values were adopted by ASTM in 2008 after being implemented first by industry on a voluntary basis: a year-round 360 seconds maximum filtration time for 300 milliliters of B100; a 200-second maximum CSFT value for B100 destined for use in winter weather (below minus 12 degrees Cel-

sius). After full implementation, reports of vehicle filter clogging with biodiesel blends ceased by all accounts, but rare, isolated instances of storage tank filter clogging at terminals—above the cloud point—continue to haunt the industry. And this wasn’t just a cold-weather-state problem. While Minnesota has waived its biodiesel mandate for No. 1 ULSD the past few years as the issue is addressed, it’s not clear, according to McCormick, that this is only a problem with biodiesel blends in No. 1 ULSD. “I don’t know you can say one way or another,” he says. “There is a possibility that certain impurities in biodiesel will be less soluble in colder temperatures in No. 1 mainly because No. 1 contains significantly less aromatic compounds than No. 2, in most cases.” Terminals in Washington state, Minnesota and Texas, to name a few, experienced this problem. No fuel can be expected to perform below its cloud point, but seemingly random precipitate formation above cloud point with on-spec fuel using wintertime CSFT values is a mystery, one the industry cannot ignore. “While the 2008 changes worked for the vast majority of the biodiesel and petrodiesel on the market, it was evident there was some small portion of the market that might need additional controls,” Howell says. “Several refiners and terminals began implementing internal biodiesel purchase specifications controlling monoglycerides at levels in the 0.4 to 0.5 (percent by mass) range, even though there was no official ASTM test method for monoglycerides.” Howell chairs the ASTM Biodiesel Task Force and formed a cold flow working group to investigate the phenomenon and make recommendations how best to address it. “The efforts furthered the understanding of the phenom-

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TESTING enon, with several root causes potentially identified, Howell says, but “with very few problematic samples from the field, it was difficult to pin down specific cause and effect.” As a result, a useful nonmandatory cold flow appendix was added to the D6751 specification, Howell says, to give users more advice and guidance on when the phenomenon might occur and the potential causes. “With no clear-cut answer, NBB led efforts to involve the leading petrodiesel and biodiesel fuel technical specialists to design a larger set of experiments that could provide a more definitive cause and effect,” Howell says. “That would take some time to design the protocols

and secure buy-in, and then secure the samples and funding to execute the work. This work is now in progress, and is estimated to cost over $200,000.” Before NBB approached NREL to conduct this work late last year, the mono limit implemented by select petroleum companies seemed to be working, Howell says, adding that the cold flow working group had several choices. “After some deliberation,” Howell says, “it was generally agreed … that ASTM should move forward now with the best information available, rather than waiting.” The result was two years of balloting the No. 1-B grade of biodiesel, a volun-

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tary spec developed as an interim measure that features a 0.4 percent by mass monoglyceride limit and a 200-second year-round CSFT. The spec finally passed and at press time awaited publication. Howell says it was developed and passed with the understanding that additional study is ongoing and if more information or better test methods are found, there could be changes to the No. 1-B spec to reflect new information. “I think one of the topics of research is to not just understand what these impurities are in biodiesel that come out,” says McCormick, “but try understand exactly what the properties are of diesel fuel—what diesel fuels are exhibiting the same compatibility with biodiesel because it’s a pretty rare problem, there’s a lot of blending in No. 1 ULSD and other low cloud point diesel fuels in the winter months without these problems.” He says NREL looked at biodiesels implicated in this problem, “and they all looked like high-quality material,” he says. “They’re not running up against the top edge of the limits of 6751. That’s the surprise. That is what makes this difficult to solve. We’re looking at the fuel, saying, ‘We don’t see a reason why this stuff should cause problems.’” He says there is not an obvious research path to solving this mystery. NREL has spent the past 10 months talking to industry and deciding what to do, “rather than going off half-cocked,” McCormick says, “doing a research project and, at the end, not really having solved the problem.” NREL has developed a test matrix that uses a couple of really low cloud point No. 1 diesel fuels as the diesel component and up to eight B100 samples with varying cloud points (feedstocks) and levels of monoglyceride content. “There is some evidence that saturated monoglycerides are the culprit here,” McCormick says, “although they by themselves may not be the culprit. It may be a combination of things, or maybe we will complete this project and find out that’s completely wrong.” Biodiesels from different process technologies are another variable. For example, Teresa Alleman, a senior researcher with NREL, says different ways to deal with free fatty acids in feedstock may play a role and, therefore, this information is of value to the investigation. “It’s very difficult for me to say what the production process technology has to do with this problem,” Alleman tells Biodiesel Magazine, “but we’re trying to cover our


TESTING bases.” There are also different techniques for removing the monoglycerides and impurities from crude biodiesel coming out of the reactor. Some of these may have unintended consequences. The first phase of testing (B5 blends) is slated for completion this autumn. Testing all the samples is one thing, but interpreting massive amounts of data is another. “It takes a while to really absorb that and really understand what’s there,” McCormick says. “What we’d like to do is identify some properties of biodiesel and say, ‘If it’s above or below some level, there’s a problem.’ Or identify a test we can do with a blend that would reveal that the cloud point is not going to predict the operability temperature, so we would need to pick some other temperature.” All D6751 requirements, plus a number of additional analytical chemistry tests on B100, will be run. For blends, NREL will look at cloud points, cold filter plugging points and the low temperature flow test (LTFT). “There were some indications from our study that with cold soak filtration, samples with high times would also give you an LTFT result in a blend that was significantly above cloud point,” McCormick says, “so I think we have some preliminary indications that even samples that pass cold soak can sometimes give you, in a blend, a high LTFT result relative to the cloud point. Maybe that’s a test that could be used to identify samples with a problem, even if you don’t know what’s causing the problem.” They are also holding samples for days at temperatures slightly above cloud point to measure precipitate formation. “Not that anyone would want to do a four-day hold on their biodiesel to see if it will work,” McCormick says, “but maybe that long of a hold will identify that this type of B100 or this particular B100 is going to have a lot of precipitates, and then we can go back and look at all the other data and see if there’s some more practical test that predicts it.” Another consideration is that the error bars on the bound glycerin part of the free and total glycerin test method, D6584, “are kind of big,” McCormick says. “We are working on that,” says Alleman, who chairs the task force working to improve the 6584 method. “It is something that the industry has needed to address, and it is something that we are well aware of and are trying to improve.”

Jeff Fetkenhour, owner of Gorge Analytical, says he thinks 6584 is a fine analytical method. “Where we need to see improvement is in how people correctly interpret the chromatography,” Fetkenhour says, adding that rather than using the reference material as an appendix recommendation, ASTM should make it a part of how the method is applied. “Just relying on retention time indices, there can be a number of reasons you have variability from the tabled values and could lead to selection of the wrong peak. This could be overcome by proper application of the method.” As for the new No. 1-B grade voluntary

biodiesel spec, “It’s not a slam dunk,” McCormick says. “We’re hopeful it will work, but we’re not 100 percent sure. The problem is not that widespread, and it’s kind of hard to get your arms around, so that’s why I think ASTM members including myself are hopeful, but we’re also worried that it’s not going to do it.” Author: Ron Kotrba Editor, Biodiesel Magazine (701) 738-4942 rkotrba@bbiinternational.com

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ANALYSIS

PHOTO: WILKS ENTERPRISE INC.

CONTRIBUTION

Comparison of Infrared Biodiesel Measurement Methods An overview of ASTM-approved methods and those under consideration BY SANDRA RINTOUL

There are several options for measuring the amount of biodiesel in diesel fuel. Methods EN 14078 and ASTM D7371 are more amenable to laboratory testing although waiting for an off-site laboratory to perform the test can take several hours to several days. For a driver whose truck has just been loaded for a delivery, any wait is too long. Other options for more simplified on-site testing that will track the official methods are available for those who need a quick verification check of the blend accuracy.

Official Biodiesel Methods As biodiesel’s presence in the marketplace increased over the past 10 years, standards for verifying the amount of biodiesel

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blended into diesel fuel were needed. The first standard, which came out in November 2003, was EN 14078, developed by the European Committee for Standardization (CEN). ASTM International published a method for biodiesel content in diesel fuel in 2007, method D7371.

Why Infrared? Both of these methods employ midinfrared (IR) analysis as the measurement technology. Infrared is a common spectroscopic technique used for quantitative and qualitative analysis. In the biodiesel measurement, the fatty acid methyl ester (FAME) has a characteristic absorption at 1745 cm-1 (5.73 micrometers) due to the carbonyl group (see

Figure 1). Both the EN and ASTM methods specify this wavelength for the biodiesel measurement.

EN14078 Method EN 14078 uses a transmission sampling cell typically with a 0.5 mm pathlength cell. The cell is filled with the biodiesel/diesel mix, then the IR light passes directly through the fluid and the amount of light absorbed by the biodiesel in the sample is measured (see Figure 2). The absorbance increases and decreases with the biodiesel concentration so the IR absorbance can be correlated with a concentration in percent. Because a sample of biodiesel is completely absorbing with the 0.5 mm transmission

The claims and statements made in this article belong exclusively to the author(s) and do not necessarily refl ect the z

views of Biodiesel Magazine or its advertisers. All questions pertaining to this article should be directed to the author(s). SEPTEMBER | OCTOBER 2012


ANALYSIS

FIGURE 2: Schematic of a transmission sample system

FIGURE 1: Infrared spectra of biodiesel

cell, the samples need to be diluted with cyclohexane prior to analysis in order to be below the saturation point. For concentrations up to 11.4 percent, it is a 1:10 dilution. From 11.4 to 22.7 percent, it is a 1:20 dilution. Above 22.7 percent, the EN method states “adequate dilution ratios should be used in order to bring the absorption in the specified absorbance range of the calibration.”1 One challenge in this dilution process is the need to know the concentration of the biodiesel before testing the concentration. There is also an added chance for operator error in performing the dilution. Determining the “adequate dilution” for the “specified absorbance range of the calibration” would not be a straightforward task for operators at a fuel loading dock, which would make this method more amenable to a laboratory setting with trained technicians. The short pathlength cell is also difficult to clean as stated in the EN method, “Because of the viscosity of FAME solutions, cleaning the cells used for measurement is of great importance.”1 Residual fuel in the cell could lead to errors in subsequent analyses. The calibration procedure for EN 14078 is a relatively simple one that uses five standards of biodiesel blended in cyclohexane for a linear regression calibration. One concern with this calibration method is some diesel fuels have infrared absorbance in the region used for the biodiesel measurement that could offset the reading and is not accounted for in the calibration.

ASTM D7371 Method As previously mentioned, with any IR analysis the diesel fuel formulation can have some interference in the reading. This is clearly stated in the interferences section of D7371, “The hydrocarbon composition of

diesel fuel has a significant impact on the calibration model. Therefore, for a robust calibration model, it is important that the diesel fuel in the biodiesel fuel blend is represented in the calibration set.” 2 D7371 utilizes a chemometric partial least squares (PLS) calibration to try to reduce the baseline offset that could come from different diesel fuels. To avoid an unwieldy number of samples, the reasonable decision uses three diesels with varying aromatic contents to span the potential variation. The calibration

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ANALYSIS

FIGURE 3: Infrared ATR sample system schematic

requires 70 calibration standards. In addition to the carbonyl band, this method uses a second infrared absorption region (1371-1060 cm-1) for blend concentrations above 10 percent that has a less intense absorption from biodiesel. ASTM D7371 uses an attenuated total reflection (ATR) sample system to overcome the limited measurement range of a transmission sample system. With ATR, infrared light is focused onto one end of a crystal (such as zinc selenide or diamond) and the light

bounces through the crystal penetrating about 1 micrometer into the sample that is placed on the ATR crystal. The light reflects back into the crystal and is focused back onto a detector for the absorbance measurement (see Figure 3). The short effective pathlength of the ATR crystal allows for a sampling range as low as 0.2 percent up to 100 percent biodiesel. The exposed ATR crystal is easy to clean, reducing the possibility of contamination in future samples.

Alternative Measurements The apparatus specified in both ASTM D7371 and EN 14078 is either an FTIR (Fourier transform IR spectrometer) or dispersive mid-IR spectrometer. FTIR spectrometers are

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relatively expensive and usually operated in a laboratory by technicians who have had some formal training. For those individuals needing a quick blend check for distribution operations or blending audits, filter-based mid-IR systems (like the one pictured on page 32) are an option. These analyzers typically have no moving parts, making them rugged enough to be located at the loading rack at a fuel terminal or for operation out of a truck for testing at a fuel pump. Presently, there are no approved methods for filter-based infrared analyzers although two methods are currently in the ASTM process and could be approved by the beginning of next year. One proposed method incorporates the most trouble-free portions of the current methods. It includes a calibration similar to the EN 14078 and uses the exposed ATR crystal from D7371. The ATR system allows for easy introduction and cleaning of the sample, as well as the extended measurement range from 0.2 to 100 percent without the need for sample dilution.

Conclusion The method and analysis equipment you select will depend on regulations, possible concentration ranges for the biodiesel and where the measurement is needed. FTIR spectrometers have the analysis capability to do much more than a simple biodiesel blend and can comply with either the EN or current ASTM methods. Along with the increased capabilities, however, is added cost and complexity for the user. Filter-based infrared analyzers offer a simplified test method that allows for on-site biodiesel measurements by nontechnical personnel and is well-suited for applications that require a quick routine blend check. Whether you need a laboratory measurement or an onsite test, there is an infrared analysis method to suit your needs. 1. European Standard EN 14078: Liquid petroleum products–Determination of fatty acid methyl esters (FAME) in middle distillates 2. ASTM International D7371-07: Standard Test Method for Determination of Biodiesel (Fatty Acid Methyl Esters) Content in Diesel Fuel Oil Using Mid InfraredSpectroscopy Author: Sandra Rintoul President, Wilks Enterprise Inc. srintoul@wilksir.com


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