Perspective On: A Biofuel Research Laboratory

Despite funding challenges, tow biofuel R&D labs continue to optimize methods and service the market.

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Even before the current cloudier tax incentive climate cast its shadow on biofuel production, the budding industry faced the slings and arrows of environmentalists, food producers and even applied economists. The renewability of biomass stock feeds once ignited hopes that biofuels could replace large amounts of fossil fuels, reduce greenhouse gas (GHG) emissions, and generate substantial economic and environmental gains. The reality now is that claims of GHG benefits are constantly challenged, as food security experts blame scarcities of certain consumer items on the diversion of quantities of grains and oil seeds to biofuel production. Further tarnishing the luster of biofuels is the current heightened interest in hydraulic fracturing (fracking) of oil and shale sands to produce oil and natural gas, the recent decisions to expand offshore oil drilling and renewed interest in nuclear power generation.

Still, a hardy band of biofuel research and service laboratory managers and their teams are pressing on to find ways to improve production techniques and cost-effectiveness. By and large, these managers seem unperturbed by the less rosy macro picture. They acknowledge that their customers are affected differently by the changing government incentives and note that while some potential start-ups find entry barriers insurmountable, this could well be a function of our current tough economic setting.

For the past 10 years, Christopher Perkins has served as laboratory director at the Center for Environmental Sciences and Engineering at the University of Connecticut. In response to strong faculty interest in biofuel production from waste vegetable oil and other nonagricultural stock, the scope of the lab was broadened during the past three to five years to encompass both environmental and biofuel analyses. A grant from the state of Connecticut’s Center for Advanced Technologies helped to fund a pilot facility for biofuel production, the acquisition of scale-up and automated instrumentation, and the creation of a biofuel testing program for biodiesel (B100) and blends (B5-B20). “This helped to make our research and laboratory testing services available, at a reduced cost, to Connecticut and regional biofuel producers,” Perkins says.

“Our center has a full-time business office that handles budgeting, billing and invoicing for our services to clients,” he says. Perkins explains that the center works alongside the university, and it directly bills its clients for services very much as a commercial entity does for fee-for-service work. “From our mandated work to support and help incubate biofuel production facilities, we generate revenue that helps to support our activities. Unlike several other areas of the university, the analytical and support staff members here are maintained with our funds, which means that we have to pay overhead, salaries, fringes and other operating expenses from the revenue we generate.”


Biodiesel production prototype in support of UConn’s biofuel R&D (Richard Parnas, Ph.D.), which is housed within the center.

The lab handles about 15 to 20 biofuel samples per week and is capable of conducting tests on all the ASTM D6751 standard specifications for biodiesel fuel blends. It does not conduct cetane number analyses in-house, but it does offer tests that are not part of ASTM requirements, including Karl Fisher moisture analysis. Currently it has one full-time staffer, three part-time professionals and other support personnel for specialized tests. Perkins says that interested students assist with analyses and benefit from training and mentoring as they pursue certification.

“We are not a big service entity, nor do we want to be,” says Perkins, who pointed out that the lab operates only one shift. He says that the cost structure in university labs, which often have M.S.- and Ph.D.-level scientists, is different from that of pure service operations. “Most university labs won’t be able to offer a total acid number for $5 to $10,” he says. There are other barriers that prevent university labs from competing with full-service, external facilities. University labs are not accustomed to acquiring and maintaining the necessary service and quality management, such as that required by the National Biodiesel Board, to enable them to operate in the commercial arena.


Elemental analysis of biodiesel by ICP (EN14538).

Perkins notes that his lab’s background in the environmental area allowed it to become a state-certified analytical facility. This was quite useful when the decision was taken to provide biofuel testing services. “We participate in the quarterly ASTM biofuel cross-check program, and we collaborate with a lot of companies,” says Perkins. Analytical testing of samples from these companies helps to assess how their products will measure up to ASTM standards. He says that because of the lab’s expertise on the production side, it is able to help manufacturers resolve production problems. “If they fail, we work to help them to decide whether they want to continue further—to tweak their processes and resubmit their samples,” he says.

Perkins says that on a number of occasions, the lab works with new producers whose needs have research as well as quality-testing dimensions. “We have individualized interactions with our clients. This is an important part of the value that we add, over and above typical service operations. We offer direct consultations to solve their production issues. This is not a case where they send us their samples and we send them a results report with an invoice; it is much more interactive.”


UPLC-MS-MS analysis in support of biofuel R&D.

Today, the laboratory features testing and pilot production facilities, both of which are used for contract and research work. Perkins says that they use instrumentation from multiple vendors. Waters UPLC, MS-MS, fluorescence and characterization tools help to subject biofuel testing to high-throughput techniques and adjust some of the associated R&D processes. Some PerkinElmer (PE) tools are used for elemental analyses, he says, explaining that some biofuel production methods require the use of catalysts. “So we use PE’s inductively coupled plasma mass spectrometry (ICP-MS) instruments to quantify the catalytic materials in samples.” He says that the lab uses Metrohm’s oxidative stability and titration equipment and Agilent’s GC systems for assessing both methanol and total glycerin in biofuel samples. The lab relies on Kohler products for distillation and temperature analysis.


GC-FID analysis of free and total glycerin (ASTM D6584).

Perkins would like to see more automation in biofuel labs. He says that his lab’s distillation unit is manual, which requires watching over hour-long distillation processes. “Automation could go a far way toward increasing our operational efficiencies,” he says. “We would like to move into more automated systems within the next six months to two years.”

Finding and retaining personnel with the correct mix of skills and temperament represent one of the leading managerial challenges, according to Perkins. To begin with, the lab requires staff with high levels of training and expertise to conduct research. But it also requires them to go into production mode on the service side. This is not easy because the skill sets may be mutually exclusive for the two areas. “Our operating paradigm requires both, and as a result, finding staff with both skill sets is an ongoing challenge. We have to deal with quality, production and multiple other requirements, and we have to do a lot of training because this combination does not necessarily come out of universities or training institutions.”


Dr. Trupia in the fermentation lab with Advanced Microscopy Group’s EVOS fl digital inverted fluorescence microscope and New Brunswick Scientific’s incubator shaker behind her.

For Perkins, one of the critical challenges going forward is “making sure that you have the strategic investments for the future, to ensure that as the science, methods and requirements change, we will have the resources available to stay the course and grow.” Despite such challenges as financial failures among customers, fewer start-ups coming online and competition for scarce dollars from other energy alternatives, Perkins is focused on optimizing the methodologies used in his area. He sees considerable opportunity in the development of high-throughput methods to characterize oils, including algae oil, which may be used to produce not only biofuel but also higher-value products such as cosmetics, pharmaceuticals and aviation fuel. “Not all feed stocks will be applicable, so there is a big opportunity for new methods that match biofuels to their most appropriate applications.”

Also operating in a university environment but in a different geographic locale and with different types of biofuels is Dr. Sabrina Trupia, assistant director of biological research at the National Corn to Ethanol Research Center (NCERC) in Edwardsville, Ill. NCERC has been in operation on the campus of Southern Illinois University Edwardsville since 2003. “We are self-funded; we conduct projects that are funded through competitive grants or for a variety of private clients on a feefor- service basis, [thereby generating] the vast majority of our revenues,” says Trupia.

Despite its name, the center works with feed stocks beyond grain and with other biofuels besides ethanol. Trupia says that the center works with several kinds of grains; it is engaged in grant-funded cellulosic ethanol research and conducts projects for clients that go beyond corn. “We have two laboratories; one is for fermentation, while the other is an analytical lab for QA/QC that also supports our pilot plant, which is used for a number of studies.” Trupia says the pilot plant, one of the center’s proudest accomplishments, is solidly booked until February 2013. “It allows us to scale up production processes, and we are now getting outfitted so that we can go from lab to pilot plant through the intermediate sizes and prove concepts that our private clients and grantees want us to address.” Because of budget constraints, Trupia coordinates a number of projects both in the fermentation lab and the pilot plant, in addition to serving as lab manager.

The center works with clients to clarify the objectives of their experiments and if necessary helps them to evaluate the demands of their experimental designs. Trupia says that when the center’s staff believes it is possible to improve the design, a proposal with cost estimates is drafted and presented to the client. Proposals are also used as the bases of protocols, which guide future project implementation. “Internally, we have vendor operating procedures, including QA/QC plans, which are implied in the protocol.”

“In our lab, we have three full-time analysts, me, and a colleague who conducts research and project management and provides general leadership. I am also involved in the scheduling and reviewing of projects. Altogether, the facility has about 20 employees; in the pilot plant there are four research engineers and three operating coordinators who run the plant and other operations,” says Trupia. She says the plant is capable of running six to 10 different types of analyses, and this is typically done several times per day with one person on shift. Throughput is generally driven by client needs, and when necessary the facility can run once-perhour HPLC samples or microscopy or microbiology samples, according to Trupia. The laboratory is equipped with three HPLC systems from Shimadzu, which are used routinely. It also has an IC system and an LC/MS/MS for research purposes, as well as two GC/FIDs.

Trupia, who is involved in the lab’s equipment acquisition decisions, says, “What we need, even though we do research, is equipment that is well-built and will last for some time. We do not necessarily acquire the fanciest equipment available on the market. For our routine analyses we want reliable, goodquality equipment that at the same time is not too expensive, because we operate with a limited budget.” She says that support services are very important. “We try to gauge the quality of vendors’ tech support service capabilities before we decide to buy equipment,” she says. Equipment acquisition must be done in accordance with the procurement systems of the university; however, if preferred vendors do not have specific instrumentation or accessories, the lab is free to source from elsewhere, according to Trupia.

The center is engaged in both research and service laboratory activities for its outside clients. “With our private clients, the projects are shorter in duration because the clients typically want results within a few weeks. That is helpful, because research is the other way around. It takes a long time to get a grant, and this provides more wiggle room. As a result, we are able to schedule our research to work around the projects we do for our external clients.” She adds that the combination of research and service work also lends itself well to the allocation and distribution of lab personnel.

Relatively speaking, the biofuel industry is fairly new, and the required skills need some level of flexibility, which makes onthe- job training very important, according to Trupia. “Here at NCERC we do a lot of training. We have an internship program, and have conducted training for the staff of private clients and obtained grants to retrain automotive workers. So while it is helpful to have a strong analytical scientific background, it is very beneficial to have our on-the-job training because it is varied and changes with time to meet the needs of the field.”

Turning to future prospects in the biofuel sector, Trupia notes that the tough economic climate and adjustments in tax incentives have changed the mix of private clients seeking the center’s services. “There are a lot fewer start-ups now, although I think this goes in waves,” she says. Even so, she says, “We are always trying to expand our capabilities, but there is great demand for our services, and sometimes we can’t fulfill it fast enough—while that is a challenge, it is also a great opportunity.”

She says that NCERC started out in 2003 as a governmentand state-funded entity. “About four years ago we switched it around completely to be self-sufficient. We are proud of this accomplishment because we have managed to become an asset to the biofuels field and be a self-sustaining functioning research and service laboratory at the same time.”

Published In

Saving Energy, Saving Money Magazine Issue Cover
Saving Energy, Saving Money

Published: April 1, 2012

Cover Story

Saving Energy, Saving Money

In 2002, when Lawrence Berkeley National Laboratory (LBNL) in Berkeley, California, decided to build the Molecular Foundry laboratory, they employed the help of Steve Greenberg, an in-house energy management engineer.