title: Examination of glass transitions in CO(2)-processed, peracetylated sugars using sum frequency generation spectroscopy.
abstract: The present study utilizes vibrational sum frequency generation (SFG) spectroscopy to study changes in the surface crystallinity of various peracetylated sugars, a class of materials that have a high affinity for carbon dioxide (CO(2)). Studies of the solid-air interface of acetylated beta-cyclodextrin (Ac-beta-CD) and sucrose octaacetate (SOA) show that diffuse reflectance SFG spectroscopy is sensitive to changes in crystallinity from processing with either heat or solvation in CO(2), due to the loss of signal after glassification occurs. beta-d-Glucose pentaacetate (Ac-beta-GLC) was used as a control for this experiment due to the fact that it does not undergo a crystalline phase transition, regardless of processing conditions. The crystalline to amorpohous transitions of these bulk materials were verified using differential scanning calorimetry (DSC) as a function of thermal and CO(2) processing. In addition, preliminary results suggest that the SFG technique is sensitive in detecting the degree of crystallinity at the interface as a result of incomplete processing and presents new opportunities for the examination and detection of surface crystallinity changes.
authors.affiliation: Department of Chemistry and the NSF Science and Technology Center for Environmentally Responsible Solvents and Processes, Kenan and Venable Laboratories, The University of North Carolina, Chapel Hill, North Carolina 27599-3290, USA.
authors.forename: Michael L
authors.initials: ML
authors.lastname: Hurrey
authors.forename: Scott L
authors.initials: SL
authors.lastname: Wallen
mesh_terms: D000107:Acetylation; D002152:Calorimetry, Differential Scanning; D002245:Carbon Dioxide / Q000737:chemistry*; D003460:Crystallization; D015394:Molecular Structure; D044367:Phase Transition; D013057:Spectrum Analysis / Q000295:instrumentation* / Q000379:methods*; D013395:Sucrose / Q000031:analogs & derivatives* / Q000737:chemistry; D013499:Surface Properties; D013816:Thermodynamics; D014732:Vibration; D047392:beta-Cyclodextrins / Q000737:chemistry*
chemical_list: D047392:beta-Cyclodextrins; C026879:sucrose octaacetate; D002245:Carbon Dioxide; D013395:Sucrose