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The University of Tennessee Institute of Agriculture ANNUAL REPORTING FORM | |||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||
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Douglas Hayes, Associate Professor Biosystems Engineering & Soil Science Annual Performance Period: January 1, 2007 to December 31, 2007 A. SUMMARY AND IMPACTS. 1. Summary. Provide an overall summary (500 words or less) of your accomplishments during the reporting period. PhD student Javier Gomez del Rio (Chem Engr; thesis defense in February, 2008) has developed 3-phase microemulsion systems containing a pH-degradable surfactant that can effectively recover and purify proteins from aqueous solutions, and a thermodynamic model to describe the partitioning of the surfactants between phases as a function of temperature (manuscript draft written; submission in early 2008). Current researchhas demonstrated the successful recovery of 3 different microemulsion-encapsulated proteins. Manuscripts (2) have been written by Hayes based on former student Dr. Mayson Alkhatib’s thesis (1 submitted, another to be submitted in early 2008; with a 3rd manuscript being planned). Small-Angle Neutron Scattering (SANS) results, obtained at NIST, Gaithersburg, MD in 2006 (upon acceptance of peer-reviewed proposals), in collaboration with Drs. Volker Urban and J.S. Lin of ORNL, have been completed and are included in 3 manuscripts. Additional data was collected in late 2007 (to be analyzed). Proposal(s) will be prepared in 2008, subsequent to completion of Gomez’s thesis. Regarding the lipase-catalyzed environmentally-friendly synthesis of saccharide-fatty acid esters as value-added bio-based products (USDA funding), Dr. Sang-Hyun Pyo, postdoctoral research associate, examined conditions means to maximize solubilization of sugars into oleic acid. His work demonstrated that passage of oleic acid/fructose monooleate stream through a packed column containing ~75% sugar and 25% silica gel maximized solubility. However, the solubility levels obtained were several-fold lower than those achieved previously by our group.; moreover, Pyo’s work demonstrated our group’s previous approach produced suspensions of sugar rather than achieving true solubilization. Pyo constructed bioreactor systems in which oleic acid/saccharide monooleate mixtures were continuously recirculated through saccharide desorption and bioreactor units. The system which performed best consisted of a silica gel/saccharide packed column and a packed-bed bioreactor. A manuscript describing the solubilization of saccharide was submitted; a second manuscript relating to the bioreactors is in preparation. Research on lipase-catalyzed synthesis of polyesters of hydroxy fatty acids has continued, due to an NIH grant being funded (based on the material’s use in drug delivery). Mr. Vinay Mannam, MS student, began work on this project in September, 2007. Ionic liquids (ILs) have been utilized as solubilization agents for ligoncellulosic biomass, which can be applied to improve the wet chemistry analysis of biomass, required for proper feedstock utilization in a biorefinery, and as a means to pre-fractionate cellulose, hemicellulose, and lignin (USDA funding to support Ms. Lindsey Kline, MS completed in 07/07; Sun Grant funding to support MS student Mr. Rajesh Jena Kumar in the Fall of 2007; in collaboration with A. Womac, BESS, and N. Labbe, Tennessee Forest Products Center). Specifically, this approach can be used to quantify the amount of lignin via a colorimetric assay or FTIR spectroscopy. In addition, the cellulose content can be quantified through the biocatalytic hydrolysis of biomass in ILs, a safer and simpler alternative to the standard approach. A manuscript is in preparation; an additional manuscript on the chemical analysis of biomass for different anatomical parts of plants has been submitted by collaborator Dr. P. Ye (BESS). 2. Impacts. List up to three significant impacts of your program. Impact statements should be one to three sentences and should be written in a way that would be meaningful to the public. Purification of proteins from fermentation broths at >95% yield has occurred when employing a novel method based on extraction using 3-phase microemulsion systems and pH-degradable surfactants. This technique can potentially be more cost-effective, easily scaled up, and rapid compared to competing technologies. A bench-scale prototype bioreactor system has been developed and tested that is capable of synthesizing technical-grade biocompatible emulsifiers for food and cosmetic products has been synthesized from agricultural feedstocks, fatty acids and monosaccharides, via biocatalysis in an environmentally-friendly, solvent-free, procedure. A mathematical model was developed which effectively described the chemical reaction data. Poorly-soluble biopolymers derived from biomass, such as cellulose, lignin, and whole corn stover, have been effectively solubilized in ionic liquids. This capability will allow for more simple, rapid and safe methods for analyzing the composition of lignocellulosic biomass. B. PROJECTS AND PROGRAMS (EXTENSION, RESEARCH AND TEACHING). As applicable, list title, names of participants (PIs, Leaders, Co-PIs, Co-leaders, Collaborators etc.), project number, sponsor, your role ( leader/co-leader/collaborator) and your percent effort on the project as stated in the project description or document. 1. pH-Degradable Surfactants for Tunable Water-in-Oil Microemulsions, D. G. Hayes (PI/leader; 10% effort), Volker S. Urban (ORNL, collaborator), J.S. Lin (ONRL, collaborator), J. M. Gomez del Rio (PhD student); NSF funding ended in 2007; proposals will be prepared in 2008. 2. Synthesis of Biosurfactant Fatty Acid Esters and Biolubricant Star Polymers via Biocatalysis, D. G. Hayes (PI / leader, 10% effort), S. H. Pyo (Postdoctoral Research Associate), V. Mannam (M.S. student), USDA-NRI and NIH 3. Wet Chemical Analysis and Pre-Fractionation of Lignocellulosic Biomass via Dissolution Into Ionic Liquids, D. G. Hayes (PI/leader, 10% effort), N. Labbe (FPC, co-leader)A. Womac (collaborator), P. Ye (collaborator), L. Kline (MS student, graduated in 2007), R. Jena Kumar (MS student), USDA/DOE (PI = Womac) and Southeastern SUN Grant C. INSTRUCTION, TEACHING AND EXTENSION EDUCATION. Detail credit and non-credit instruction and teaching activities. 1. College credit instruction. List courses in which you were an instructor or guest lecturer during the current calendar year. Include special topics, independent study and internship courses. Provide course number and title, your involvement, semester(s), credit hours and number of students. Please append a summary of teaching evaluations (student and/or peer) if this information is available.
2. Formal continuing education (certification programs, seminar series, in-service training, field days, faculty and/or staff training, journal club, etc.). Provide descriptive title of activity, your involvement, number of participants or students involved, number and duration of each session.
3. Extension presentations and workshops. Indicate title, type, and scope of presentation; number of times presented; attendance estimates. Include evidence of effectiveness (e.g. evaluation summaries) where applicable.
4. Public addresses to lay audiences (TV/radio presentations, service groups, etc.). Indicate title, type, scope of presentation; number of times presented; attendance estimates. Include evidence of effectiveness (e.g. evaluation summaries) where applicable.
5. Presentations at professional meetings, without published abstracts. List presenter, co-authors (if any), title, date and name of meeting (list scientific oral or poster presentations having published abstracts or proceedings at D5). • Douglas G. Hayes [Speaker], Javier A. Gomez del Rio, Mayson H. Alkhatib, Volker S. Urban, J. S. Lin, Guangming Luo, “Analysis of Microemulsions Containing a pH-Degradable Alkyl Ethoxylate Surfactant by Small-Angle Neutron Scattering,” 81st American Chemical Society Colloids and Surface Science Symposium, Newark, DE, June, 2007 • Javier A. Gomez del Rio, Douglas G. Hayes [speaker], “Partition of a Cleavable, 1,3-Dioxolane, Nonionic Surfactants, sodium bis (2-ethylhexyl) sulfosuccinate and n-octyl-beta-D-glucopyranoside in 2- and 3-Phase Water-Isooctane Microemulsion Systems,” 81st American Chemical Society Colloids and Surface Science Symposium, Newark, DE, June, 2007 • Kline, L.M. [poster presentor], D.G. Hayes, N. Labbe, and A.R. Womac. 2007. Rapid determination of lignin content in lignocellulose biomass through the use of ionic liquids. Abstract, 234th ACS National Meeting, Boston, MA, August 19-23, 2007. • Joshua S. Yuan (speaker), Nathan R. Stewart, Lindsey Kline, Douglas G. Hayes, C. Neal Stewart Jr., Rice as a Model Species for Gene Function Study in Biofuels and Bioenergy Research, 5th International Symposium on Rice Functional Genomics, Tsukuba, Japan, 10/07 • Douglas G. Hayes (Invited), “Packed-Column SFC Analysis of Lipid Modification Reactions: Overview and Applications,” The 1st International Conference on Superceritical Fluid Chromatography (sponsored by the Green Chemistry Group), Pittsburgh, 24 September 2007. • Douglas G. Hayes (Speaker; Invited), Reid R. Gerhardt, and Larry C. Wadsworth, “Long-Lasting Insecticide-Treated Nets for Mosquito Control: Commercial Products and Alternate Approaches to Their Preparation,” AATCC Conference and Exhibition, Charleston, SC, 10/04/07 • Mayson H. Alkhatib, Javier Gomez del Rio, Douglas G. Hayes [speaker], Volker S. Urban, Guangming Luo, and J. S. Lin, “Analysis of Microemulsions Containing a pH-Degradable Alkyl Ethoxylate Surfactant by Small-Angle Neutron Scattering,” AOCS Conf., Quebec City, May, 2007. • J. Gomez del Rio and D. G. Hayes [speaker], “Recovery and Purification of Proteins Using 3-Phase Microemulsion Systems,” AOCS Conf., Quebec City, May, 2007 [Invited]. • Douglas G. Hayes [speaker], “Synthesis of Saccharide-Fatty Acid Ester Biosurfactants via Lipase-Catalyzed Reactions: Overview and Recent Developments,” AOCS Conf., Quebec City, May, 2007 [Invited]. • Oriana O. Obiri, Douglas G. Hayes [speaker], “Solvent-Free Lipase-Catalyzed Synthesis of Saccharide-Fatty Acid Esters Using a Bioreactor System,” AOCS Conf., Quebec City, May, 2007 [Invited]. • Douglas G. Hayes and David L. Compton, “Urea Inclusion Compound-Based Fractionation for the Eco-Friendly Purification of Ethyl Ferulate in a Bio-Based Sunscreen Product Stream, “ AOCS Conf., Quebec City, May, 2007 [Invited]. • Liu L., X. P. Ye, L. Kline, D.G. Hayes, A.R. Womac, and S. Sokhansanj. 2007. Investigation of chemical variability of switchgrass and cornstover using fast near infrared techniques. Paper No. 076006, American Society of Agricultural and Biological Engineers, St. Joseph, MI. 6. Student mentoring. Fill in the boxes to indicate number of students in each category.
7. Student or commodity club activities (e.g. club advisor, team competitions, honor or professional societies, etc.). List the club or group; your role with the club or group; and the activities, honors or awards received by this group under your mentorship. 8. Other instructional and teaching activities. D. PUBLICATIONS. List only publications that were published during the annual reporting period (for #8, submitted during reporting period). Format citations as typical and appropriate for outlet. If a co-author(s) is a student or was working under your direct supervision, place an asterisk after that person's name. 1. Refereed articles or refereed reviews appearing in peer-reviewed professional journals. Raikar, M. E.*, Diaz-Martin, E., Torriggiani, M., Cerro, R. L., Harris, J.M., Rogers, S.E., Eastoe,, J. A. Gomez del Rio*, and D. G. Hayes. 2007. Three-Component Microemulsions Formed Using pH-Degradable 1,3-Dioxolane Alkyl Ethoxylate Surfactants. Colloids and Surfaces A, 301 (1-3), 394-403. Raikar, M. E.*, Harris, J. M., and D. G. Hayes. 2007. Solubilization of Enzymes in Water-in-Oil Microemulsions and Their Rapid and Efficient Release Through Use of a pH-Degradable Surfactant. Biotechnology Letters, 29(5), 767-771. 2. Book chapters or books. 3. Bulletins, reports, circulars, pamphlets, factsheets. 4. Popular press, trade, UTIA magazine or newsletter articles. 5. Abstracts from scientific or discipline meetings, papers from conference proceedings, etc. Hayes, D. G., R. R. Gerhardt, and L. C. Wadsworth. 2007. LONG-LASTING INSECTICIDE-TREATED NETS FOR MOSQUITO CONTROL: COMMERCIAL PRODUCTS AND ALTERNATE APPROACHES TO THEIR PREPARATION. Proceedings of the Annual International Conference and Exhibition of the American Association of Textile Chemists and Colorists (AATCC). Kline, L. M.*, D. G. Hayes, N. Labbe, and A. R. Womac. 2007. Rapid determination of lignin content in lignocellulosic biomass through the use of ionic liquids. Abstracts of Papers, 234th ACS National Meeting, Boston, MA, United States, August 19-23, 2007 (2007), IEC-040. Publisher: American Chemical Society, Washington, D. C CODEN: 69JNR2 Conference; Meeting Abstract; Computer Optical Disk written in English. AN 2007:882315. L. Liu, X. P. Ye, L. Kline, D. G. Hayes, A. R. Womac, and S. Sokhansanj. 2007. Investigation of chemical variability of switchgrass and cornstover using fast near infrared techniques. Paper No. 076006, American Society of Agricultural and Biological Engineers, St. Joseph, MI. 6. Theses/Dissertations completed by students that you directed. Kline, L. M.* 2007. IMPROVED METHODOLOGIES FOR BIOMASS WET CHEMICAL ANALYSIS. Master's Thesis. Liu, L., and *. 2007. Applied Fourier-Transform Near-Infrared Techniques for Biomass Compositional Analysis. 7. Other publications. 8. Articles submitted during the reporting period that are in review, in press or rejected. Please do not list articles in preparation. Alkhatib, M. H.*, J. A. Gomez del Rio*, D. G. Hayes, M. E. Diaz-Martin, M. Torriggiani, and R. L. Cerro. 2007. Physicochemical Characterization of Water-in-Oil Microemulsions Formed by a Binary pH-Degradable Alkyl Ethoxylate / Aerosol-OT Surfactant System. (other authors = Volker S. Urban and J.S. Lin), submitted to Langmuir. (in review) Pyo, S., and D. G. Hayes. 2007. On the Desorption of Fructose from a Packed Column to an Oleic Acid / Fructose Oleate Mixture for Employment in a Bioreactor System. Journal of the American Oil Chemists' Society. (in review) Wu, T., S. Zivanovic, D. G. Hayes, and J. Weiss. 2007. Efficient Reduction of Chitosan Molecular Weight by High intensity Ultrasound: Underlying Mechanism and Effect of Process Parameters. Journal of Agricultural and Food Chemistry. (in review) Ye, X. P., L. Liu, D. G. Hayes, A. R. Womac, K.L. Hong, and S. Skhansanj. 2007. Fast Classification and Compositional Analysis of Cornstover Fractions Using Fourier Transform Near-infrared Techniques. (in press) Zhuang, F.*, K. K. Chittur, D. L. Mount, S. C. Smith, and D. G. Hayes. 2007. Simple and Inexpensive Preparation of Long-Lasting Insecticidal Nets Via Co-Adsorption of Pyrethroid and Oligomer. Textile Research Journal. (in press) Obiri, O. O.*, and D. G. Hayes. 2007. Solvent-Free Lipase-Catalyzed Synthesis of Saccharide-Fatty Acid Esters Using a Bioreactor System. submitted to the Journal of the American Oil Chemists' Society. (rejected) E. FUNDING. Format each entry as a citation, include as applicable: investigators (with percent effort shown on grant or contract document), title, source/agency. 1. Grant and contract proposals submitted but not awarded during this reporting period. Indicate date of submission and status (still pending, rejected). Federico Harte (70%), Svetlana Zivanovic (20%), D. G. Hayes (10%). Structure-Function Properties Derived from High-Shear Induced Casein Micelle-Polysaccharide Ionic & . USDA CSREES. 1/17/07. $426,605. (rejected) Nicole Labbe (50%), D. G. Hayes (30%), Joseph John Bozell (10%), Paul D. Frymier (10%). Enhancing the hydrolysis of lignocellulosic biomass through the use of Ionic liquids & engrg.... USDA. 1/17/07. $496,667. (rejected) Hayes, D. G. (40%), Volker Urban (25%), J.S. Lin (25%), J. A. Gomez del Rio (10%). SANS Analy.to Charact. Microemulsion Sys. formed by Binary Surfactant Systems...... NIST Center for Neutron Research. 2/10/07. $1. (rejected) Hayes, D. G. (100%), S. Pyo (%). Improving the "Green" Biocatalytic Synthesis of Biodiesel Through Manipulation of Partial Glyceride . SoutheasternSun Grant. 4/30/07. $60,000. (rejected) Hayes, D. G. (25%), L. C. Wadsworth (15%), Gerhardt, R. R. (10%), Kanath, M. G. (50%). Field-Deployable Treatment of Military Textiles to Provide Long-Term Protection from Biting Arthropo. (pre-proposal)US Army Space and Missile Defense Command, Deployed War-Fighter Protection (DWPF) from Disease-Carrying Insects. Funding Opportunity Number W9113M-07-S-009. 9/13/07. $750,000. (rejected) Hayes, D. G. (100%). Production of Bioethanol and Biodiesel Using a Novel Catalyst (“GRH-C”). Global Resource Holdings, LP, Dallas, TX. 12/31/07. $111,834. (still pending) 2. Grants and contracts awarded during this reporting period. List inclusive period of support (start and end dates) and total amount of award. Hayes, D. G. (70%), Nicole Labbe (30%). Ionic Liquids as Solublization Agents for the Chemical Analysis & Pre-Fractionation of cellulose,etc. Sun Grant Intiative. 7/1/07-6/30/09. $100,000. Hayes, D. G. (100%). Chemo-Enzymatic Synthesis of Unimolecular Micelles for Drug Delivery. National Institutes of Health. 8/15/07-8/14/09. $133,950. 3. Grants and contracts awarded in past years that continued into this reporting period. List inclusive period of support (start and end dates) and total amount of award. Hayes, D. G. (100%). Rapid and Selective Protein Purification via pH-Tunable Water-in-Oil Microemulsions. National Science Foundation. 1/1/03-8/31/07. $331,000. Womac, A. R. (49%), D. G. Hayes (26%), X. P. Ye (26%). Integrated Size Reduction and Separation to Pre-Fractionate Biomass. US DOE. 10/1/04-9/30/08. $717,399. Hayes, D. G. (100%). Comparison of Water Removal Strategies Contained in Bioreactor Sys. Designs for the Green Synthesis . USDA CSREES. 8/15/06-8/14/09. $308,740. 4. Gifts. List recipients, donor, items or amount donated and dollar equivalent received during the reporting period. 5. Grant reports submitted. List authors, title, to whom submitted, date submitted. Hayes, D. G., "Rapid and Selective Protein Purification via pH-Tunable Water-in-Oil Microemulsions," final project report, National Science Foundation, Engineering Division, 08/31/07 Hayes, D. G., "Comparison of Water Removal Strategies Contained in Bioreactor System Designs for the Green" Synthesis of Bio-Based Emulsifiers," USDA/CSREES/NRI (Area 71.1)Annual Progress Report (AD-421), 12/01/07 6. Other (e.g. sales, royalties). F. OTHER CREATIVE ACTIVITIES.
G. SERVICE. List client outreach activities (both public and private sectors) and professional service.
H. PROFESSIONAL DEVELOPMENT (meetings, workshops, classes, trips, etc.). List the event or activity, sponsor, duration of event and your role. I. PERSONNEL SUPERVISION. List the postdoctoral fellows, research associates, research assistants, technicians, extension associates, extension assistants, graduate assistants, undergraduate students, clerical personnel or others that you supervised during the year.
J. HONORS AND AWARDS. List honors and awards received during reporting period, including the name of the organization presenting the award. | |||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||||