Effect of sample size on solvent extraction for detecting cocontinuity in polymer blends

The effect of sample size on the results of solvent extraction measurements for detecting cocontinuity in polymer blends was investigated. Poly(ethylene oxide)/polystyrene (PEO/PS) blend samples of several thicknesses were analyzed by removing the PEO phase using water extraction. The experimental degree of continuity was shown to have a linear dependence on the reciprocal of sample thickness. A model is proposed to explain this dependence and to allow the bulk or true degree of continuity to be determined. Measurement of the bulk degree of continuity is useful for understanding properties of cocontinuous polymer blends such as electrical conductivity, impact strength, or tensile strength.     

Cellulose-binding domains: potential for purification of complex proteins

The endoglucanase CenA and the exoglucanase Cex from Cellulomonasfimi each contain a discrete cellulose-binding domain (CBD),at the amino-terminus or carboxyl-terminus respectively. Thegene fragment encoding the CBD can be fused to the gene of aprotein of interest. Using this approach hybrid proteins canbe engineered which bind reversibly to cellulose and exhibitthe biological activity of the protein partner. Alkaline phosphatase(PhoA) from Escherichia coli, and a ß-glucosidase(Abg) from an Agrobacterium sp. are dimeric proteins. The fusionpolypeptides CenA-PhoA and Abg-CBC_cex are sensitive to proteolysisat the junctions between the fusion partners. Proteolysis resultsin a mixture of homo- and heterodimers; these bind to celluloseif one or both of the monomers carry a CBD, e.g. CenA-PhoA/CenA-PhoAand CenA-PhoA/PhoA. CBD fusion polypeptides could be used inthis way to purify polypeptides which associate with the fusionpartner.     

Characterization of polymer‐layered silicate (clay) nanocomposites by transmission electron microscopy and X‐ray diffraction: A comparative study

Several polymer‐layered silicate (clay) nanocomposites (PLSNs) were analyzed by transmission electron microscopy (TEM) and wide‐angle X‐ray diffraction (XRD) in an effort to characterize the nanoscale dispersion of the layered silicate. The PLSNs investigated included thermoset (cyanate esters) and thermoplastic polymers (polystyrene, nylon 6, and polypropylene‐g‐maleic anhydride). The results of this study reveal that the overall nanoscale dispersion of the clay in the polymer is best described by TEM, especially when mixed morphologies are present. XRD is useful for the measurement of d‐spacings in intercalated systems but cannot always observe low clay loadings (<5%) or be used as a method to identify an exfoliated nanocomposite where no XRD peaks are present (constituting a negative result). Most importantly, the study showed that XRD is not a stand‐alone technique, and it should be used in conjunction with TEM. Our studies suggest that new definitions, or a clarification of existing definitions, are needed to properly describe the diversity of PLSN nanostructures seen in various materials. Published 2002 Wiley Periodicals, Inc. J Appl Polym Sci 87: 1329–1338, 2003     

A model for studying LCAT reaction: In vitro cholesterol esterification in pig ovarian follicular fluid

Phosphatidylcholine acyltransferase (lecithin:cholesterol acyltransferase or LCAT; EC 2.3.1.43) activity was found to be present in pig ovarian follicular fluid (POFF), in addition to pig serum (PS). The cholesterol esterification rate in both POFF and PS is linear with incubation time up to 2 hr. The mean absolute rate of POFF-cholesterol esterification was 8.1±0.4 nmoles per ml per hr approximately one-fourth of that in PS. However, the fractional rate (percent of labeled cholesterol esterified per hr) of POFF-cholesterol esterification was similar to that observed in PS. There was little variation of absolute rate of cholesterol esterification in the fluid obtained from different sizes of follicles. Fatty acid or triacylglycerol did not participate in the reaction of cholesterol esterification in POFF. No appreciable change in enzymatic activity was found from storing POFF at 4 C for periods of time up to 24 hr or at −70 C up to 2 months, but activity was lost thereafter. On the other hand, PS showed a much longer period of stability (5 days at 4 C and 9 months at −70 C). A discrepancy between the fatty acid composition of cholesteryl esters formed by the LCAT reaction and the fatty acid composition at the C-2 position of phosphatidylcholine led us to propose a two-step mechanism for the LCAT reaction. It is concluded that the LCAT of POFF, as well as that of plasma, is specific for individual fatty acids rather than for the fatty acid composition of phosphatidylcholine. The fatty acid concentration of lysophosphatidylcholine decreased during prolonged incubation times (6 to 21 hr) suggesting that the increased lysophosphatidylcholine formed as a product of the LCAT reaction may be reused as substrate for the LCAT reaction or for hydrolysis by lysophosphatidylcholine hydrolase. Presented at the AOCS Meeting, New York, May 1977.     

Functionally substituted tetramethylcyclopentadienes: Synthesis of 1-(p-hydroxyphenyl)-2,3,4,5-tetramethylcyclopentadiene and its use in the synthesis of an organometallic polymer

Reaction of 2,3,4,5-tetramethylcyclopent-2-enone (1) withp-LiC₆H₄OC-Me₂OMe, followed by treatment with aqueous acid afforded 1-(p-hydroxyphenyl)-2,3,4,5-tetramethylcyclopentadiene (2). This new ligand was then used in the synthesis of the functionally substituted organomolybdenum reagent (⁵-C₅Me₄-p-C₆H₅OH)Mo(CO)₂(NO) (3). Treatment of a preformed 1/1 styrene/maleic anhydride copolymer ( ) with 5 mol% 3 led to chemical incorporation of the organometallic species into the polymer. The final product contained 3 mol% of the organometallic moiety.     

Ranking protective coatings: Laboratory vs. field experience

Environmentally protective coatings are used on a wide range of gas turbine components for survival in the harsh operating conditions of engines. A host of coatings are commercially available to protect hot-section components, ranging from simple aluminides to designer metallic overlays and ceramic thermal barrier coatings. A variety of coating-application processes are available, and they range from simple pack cementation processing to complex physical vapor deposition, which requires multimillion dollar facilities. Detailed databases are available for most coatings and coating/process combinations for a range of laboratory tests. Still, the analysis of components actually used in engines often yields surprises when compared against predicted coating behavior from laboratory testing. This paper highlights recent work to develop new laboratory tests that better simulate engine environments. Comparison of in-flight coating performance as well as industrial and factory engine testing on a range of hardware is presented along with laboratory predictions from standard testing and from recently developed cyclic burner-rig testing.     

Monitoring delamination of plasma-sprayed thermal barrier coatings by reflectance-enhanced luminescence

Plasma-sprayed thermal barrier coatings (TBCs) present a challenge for optical diagnostic methods to monitor TBC delamination, because the strong scattering exhibited by plasma-sprayed TBCs severely attenuates light transmitted through the TBC. This paper presents a new approach that indicates delamination in plasma-sprayed TBCs by utilizing a luminescent sublayer that produces significantly greater luminescence intensity from delaminated regions of the TBC. Freestanding coatings were produced with either a Eu-doped or Er-doped yttria-stabilized zirconia (YSZ) luminescent layer below a plasma-sprayed undoped YSZ layer. A NiCr backing layer was added to represent an attached substrate in some sections. For specimens with a Eu-doped YSZ luminescent sublayer, luminescence intensity maps showed excellent contrast between unbacked and NiCr-backed sections. Discernable contrast between unbacked and NiCr-backed sections was not observed for specimens with a Er-doped YSZ luminescent sublayer, because luminescence from Er impurities in the undoped YSZ layer overwhelmed luminescence originating from the Er-doped YSZ sublayer.     

Rapid consolidation of powdered materials by induction hot pressing

A rapid hot press system in which the heat is supplied by RF induction to rapidly consolidate thermoelectric materials is described. Use of RF induction heating enables rapid heating and consolidation of powdered materials over a wide temperature range. Such rapid consolidation in nanomaterials is typically performed by spark plasma sintering (SPS) which can be much more expensive. Details of the system design, instrumentation, and performance using a thermoelectric material as an example are reported. The Seebeck coefficient, electrical resistivity, and thermal diffusivity of thermoelectric PbTe material pressed at an optimized temperature and time in this system are shown to agree with material consolidated under typical consolidation parameters.     

A high temperature apparatus for measurement of the Seebeck coefficient

A high temperature Seebeck coefficient measurement apparatus with various features to minimize typical sources of error is designed and built. Common sources of temperature and voltage measurement error are described and principles to overcome these are proposed. With these guiding principles, a high temperature Seebeck measurement apparatus with a uniaxial 4-point contact geometry is designed to operate from room temperature to over 1200 K. This instrument design is simple to operate, and suitable for bulk samples with a broad range of physical types and shapes.     

ELCA evaluation for keyword search on probabilistic XML data

As probabilistic data management is becoming one of the main research focuses and keyword search is turning into a more popular query means, it is natural to think how to support keyword queries on probabilistic XML data. With regards to keyword query on deterministic XML documents, ELCA (Exclusive Lowest Common Ancestor) semantics allows more relevant fragments rooted at the ELCAs to appear as results and is more popular compared with other keyword query result semantics (such as SLCAs). In this paper, we investigate how to evaluate ELCA results for keyword queries on probabilistic XML documents. After defining probabilistic ELCA semantics in terms of possible world semantics, we propose an approach to compute ELCA probabilities without generating possible worlds. Then we develop an efficient stack-based algorithm that can find all probabilistic ELCA results and their ELCA probabilities for a given keyword query on a probabilistic XML document. Finally, we experimentally evaluate the proposed ELCA algorithm and compare it with its SLCA counterpart in aspects of result probability, time and space efficiency, and scalability.