Progress 09/01/07 to 08/31/11
Outputs
OUTPUTS: This project has resulted in two invention disclosures: one for the gel-spinning of carrageenan fibers, and a second for the electro-spinning of pure starch fibers. The results were disseminated at the annual Project Directors' meetings held in conjunction with the Annual Meeting of the Institute of Food Technologists (June 27-28, 2008, New Orleans, LA, July 16-17, 2010, Chicago, IL, and June 10-11, 2011, New Orleans, LA). Results were disseminated at two international conferences, a paper titled "Spherulite formation in kappa-carrageenan dispersions" was presented at the 10th International Hydrocolloids Conference in Shanghai, China held June 20-24, 2010, and a second titled "Fabrication of kappa-carrageenan fibers by wet spinning: addition of iota-carrageenan" was presented at the 4th Delivery of Functionality in Complex Food Systems symposium held in Guelph, Ontario, Canada, August 22, 2011. The results of research were shared locally at a seminar to the Department of Materials Science at Penn State on October 8, 2009. A further presentation is proposed for the 11th International Hydrocolloids Conference to be held at Purdue University, West Lafayette, IN in 2012, and several more manuscripts are in preparation. PARTICIPANTS: This project trained two post-doctoral scholars: Xiaoyong Wang and Rajesh Bhosale. Dr. Wang is currently employed in the School of Chemistry and Molecular Engineering, East China University of Science and Technology, and Dr. Bhosale is Development Manager, Unilever Research Center, Unilever Hindustan.Debie W. Blair earned both her B.S. with Honors in Food Science and her M.S. in Food Science while working on the project and is now employed by Kraft Foods. Lingyan Kong is currently pursuing his Ph.D. on fiber spinning initiated under this project. In-kind support was obtained during the project from FMC Biopolymers and National Starch. TARGET AUDIENCES: The target audience is the scientific community, both academic and industrial, interested in the production of biopolymer fibers. This would include those using fibrous materials in the biomedical community. PROJECT MODIFICATIONS: As a result of turnover in project personnel, a one-year, no-cost extension had been requested and granted. Due to novel and unforeseen results obtained during the investigation, the original fundamental investigation of the effects of non-equilibrium and non-quiescent conditions on mixed carrageenan-starch gels was replaced by a more practical application of those conditions on spinning and resultant morphology of carrageenan and starch fibers.
Impacts
For the first time, fibers of pure carrageenan and pure starch have been successfully spun using a gel-spinning and electro-spinning techniques, respectively. These carrageenan microfibers and starch nanofibers, being made from biodegradable and biorenewable biopolymers, may find applications in biomedicine, e.g. as wound dressings or tissue scaffolds, and contribute to a sustainable materials industry. During the course of this research it was determined that kappa-carrageenan can template the crystallization of calcium sulfate. Equilibrium phase diagrams for the iota-carrageenan/maltodextrin/water system were established at varying KCl concentrations and temperatures, validating the phase-volume-ratio method for determining phase diagrams in mixed biopolymer systems, and extending our understanding of interactions between charged and neutral biopolymers.
Publications
- Kong, L. and G. R. Ziegler. 2011. Fabrication of κ-Carrageenan Fibers by Wet Spinning: Spinning Parameters. Materials 4(10)1805-1817. http://dx.doi.org/10.3390/ma4101805.
- Blair, B. W. 2010. Ues of starch inclusion complexes for improved devlivery of dietary polyphenols to the oral cavity by chewing gum. M.S. Thesis. The Pennsylvania State University, University Park, PA. 70 pp.
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Progress 09/01/09 to 08/31/10
Outputs
OUTPUTS: The Ph.D. candidate, Lingyan Kong, presented the paper titled "Spherulite formation in k-carrageenan dispersions" at the 10th International Hydrocolloids Conference in Shanghai, China, on June 20-24, 2010, and a similarly titled poster at the Annual Meeting of the IFT, Project Director's meeting in Chicago, IL, July 16-17,2010. PARTICIPANTS: Debie W. Blair earned her B.S. with honors in Food Science by completing an honors thesis related to this project. She continues the work for her M.S. degree. Currently she is employed by Kraft Foods. TARGET AUDIENCES: Nothing significant to report during this reporting period. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
The formation of spherulites was observed on drying of aqueous solutions in some commercial samples of kappa-carrageenan but not others. The size of the spherulites formed was dependent on the drying rate. An investigation into this phenomenon was made by first purifying the carrageenan samples. purified samples, or commercial samples low in calcium did not form spherulites. The addition of calcium chloride to these samples did not restore their ability to form spherulites. However, the addition of both calcium and sulfate ions did. It was determined by FTIR and ESEM/EDS that both calcium and sulfur accumulated in the spherulites. Isolated spherulites comprised calcium sulfate. Under the same conditions, but in the absence of carrageenan calcium sulfate did not form spherulitic morphology. It was concluded that the observed phenomenon was an example of biomineralization, where the morphology of the calcium sulfate crystals was influenced by the presence of carrageenan.
Publications
- No publications reported this period
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Progress 09/01/08 to 08/31/09
Outputs
OUTPUTS: Significant results of this year's research were presented to about 150 attendees in a seminar sponsored by the Department of Materials Science and Engineering, Penn State University, October 8, 2009. PARTICIPANTS: This project provided post-doctoral experience for Dr. Rajesh Bhosale. Dr. Bhosale has returned to India to a position with Unilever Hindustan. This project is presently being pursued by Ph.D. candidate Lingyan Kong, with help from M.S. candidate Debie Blair. In-kind support has been provided by FMC Biopolymers and National Starch. TARGET AUDIENCES: The target audience is the scientific community, both academic and industrial, interested in the production and applications of biopolymer fibers. PROJECT MODIFICATIONS: As a result of turnover in personnel, a one-year, no-cost extension has been requested. The original goal of investigating the effects of non-equilibrium and non-quiescent conditions on mixed carrageenan-starch gels will be replaced with an investigation of the effects of those conditions on the morphology of mixed carrageenan-starch fibers spun from those gels. For objective 5, the investigation of compatibilizers, we have begun an evaluation of the potential use of starch-guest inclusion complexes.
Impacts
While pursuing Objective 2, show that different morphological and rheological product characteristics are obtained by varying the kinetics of phase separation relative to gelation, we observed the formation of spherulitic morphology in carrageenan solutions. Based on similarities to our previous research on spherulitic crystallization of starch, we hypothesized that this resulted from the formation of a liquid crystalline phase, and that consequently, we could spin highly-oriented, crystalline fibers of carrageenan. Subsequently, we built an apparatus to wet-spin (gel-spin) fibers from this carrageenan dope, and successfully spun microfibers of high crystallinity. We followed this by constructing a system for the electrospinning of nanofibers, and have tested this apparatus by successfully spinning nanofibers of pullulan and PVOH.
Publications
- Kong, L., G.R. Ziegler, and R. Bhosale. 2009. Fibers Spun from Polysaccharides. Nova Science Publishers, Inc. Hauppauge, NY. (Accepted for Publication)
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Progress 09/01/07 to 08/31/08
Outputs
OUTPUTS: Results of the initial year's research were disseminated at the annual Project Director's Meeting held June 27 and 28, 2008 in conjunction with the Institute of Food Technologists' Annual Meeting in New Orleans, LA. PARTICIPANTS: This project provided one year's post-doctoral experience for Dr. Xiaoyong Wang. Dr. Wang has returned to China to assume a faculty position there. TARGET AUDIENCES: Nothing significant to report during this reporting period. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
Equilibrium phase diagrams of the iota-carrageenan/maltodextrin/water system have been established at potassium chloride (KCl) concentrations of 0.1, 0.2 and 0.3 M and 80, 85 and 90 degrees C. All pseudo-binary phase diagrams of iota-carrageenan/maltodextrin mixtures suggested classic segregative phase separation. The binodal was heavily skewed toward the maltodextrin axis. The high asymmetry of the iota-carrageenan/maltodextrin/water phase diagram determined by the phase-volume-ratio method was consistent with the compositional analysis of phase-separated iota-carrageenan/maltodextrin samples, and can be explained in terms of the Flory-Huggins interaction parameter, reflecting a higher water binding ability of the charged iota-carrageenan than neutral maltodextrin. Increasing the concentration of iota-carrageenan-gel-promoting KCl from 0.1 to 0.3 M at 80 degrees C enlarged the two-phase domain, whereas increasing temperature from 80 to 90 degrees C at 0.3 M KCl enhanced biopolymer compatibility. The effects of salt concentration and temperature have been related to the differences in the Flory-Huggins interaction parameters of the two biopolymers with water, as well as, the helix formation of iota-carrageenan in the presence of KCl through the changes in the slopes of tie-lines of phase-separated samples. These results validate the applicability of the phase-volume-ratio method, a relatively inexpensive technique, for determining phase diagrams in mixed biopolymer systems, and extend understanding of interactions between charged and neutral polymers as influenced by salts.
Publications
- Wang, X. and G.R. Ziegler. 2008. Phase Behavior of the iota-Carrageenan/Maltodextrin/Water System at Different Potassium Chloride Concentrations and Temperatures. Food Biophysics. (Pending).
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