Direct Ca2+-dependent Heterophilic Interaction between Desmosomal Cadherins, Desmoglein and Desmocollin, Contributes to Cell–Cell Adhesion

PubMed Central

Chitaev, Nikolai A.; Troyanovsky, Sergey M.

1997-01-01

Human fibrosarcoma cells, HT-1080, feature extensive adherens junctions, lack mature desmosomes, and express a single known desmosomal protein, Desmoglein 2 (Dsg2). Transfection of these cells with bovine Desmocollin 1a (Dsc1a) caused dramatic changes in the subcellular distribution of endogenous Dsg2. Both cadherins clustered in the areas of the adherens junctions, whereas only a minor portion of Dsg2 was seen in these areas in the parental cells. Deletion mapping showed that intact extracellular cadherin-like repeats of Dsc1a (Arg1-Thr170) are required for the translocation of Dsg2. Deletion of the intracellular C-domain that mediates the interaction of Dsc1a with plakoglobin, or the CSI region that is involved in the binding to desmoplakin, had no effect. Coimmunoprecipitation experiments of cell lysates stably expressing Dsc1a with anti-Dsc or -Dsg antibodies demonstrate that the desmosomal cadherins, Dsg2 and Dsc1a, are involved in a direct Ca2+-dependent interaction. This conclusion was further supported by the results of solid phase binding experiments. These showed that the Dsc1a fragment containing cadherin-like repeats 1 and 2 binds directly to the extracellular portion of Dsg in a Ca2+-dependent manner. The contribution of the Dsg/ Dsc interaction to cell–cell adhesion was tested by coculturing HT-1080 cells expressing Dsc1a with HT-1080 cells lacking Dsc but expressing myc-tagged plakoglobin (MPg). In the latter cells, MPg and the endogenous Dsg form stable complexes. The observed specific coimmunoprecipitation of MPg by anti-Dsc antibodies in coculture indicates that an intercellular interaction between Dsc1 and Dsg is involved in cell–cell adhesion. PMID:9214392

Implementation of DSC model and application for analysis of field pile tests under cyclic loading

NASA Astrophysics Data System (ADS)

Shao, Changming; Desai, Chandra S.

2000-05-01

The disturbed state concept (DSC) model, and a new and simplified procedure for unloading and reloading behavior are implemented in a nonlinear finite element procedure for dynamic analysis for coupled response of saturated porous materials. The DSC model is used to characterize the cyclic behavior of saturated clays and clay-steel interfaces. In the DSC, the relative intact (RI) behavior is characterized by using the hierarchical single surface (HISS) plasticity model; and the fully adjusted (FA) behavior is modeled by using the critical state concept. The DSC model is validated with respect to laboratory triaxial tests for clay and shear tests for clay-steel interfaces. The computer procedure is used to predict field behavior of an instrumented pile subjected to cyclic loading. The predictions provide very good correlation with the field data. They also yield improved results compared to those from a HISS model with anisotropic hardening, partly because the DSC model allows for degradation or softening and interface response.

Effects of particle reinforcement and ECAP on the precipitation kinetics of an Al-Cu alloy

NASA Astrophysics Data System (ADS)

Härtel, M.; Wagner, S.; Frint, P.; F-X Wagner, M.

2014-08-01

The precipitation kinetics of Al-Cu alloys have recently been revisited in various studies, considering either the effect of severe plastic deformation (e.g., by equal-channel angular pressing - ECAP), or the effect of particle reinforcements. However, it is not clear how these effects interact when ECAP is performed on particle-reinforced alloys. In this study, we analyze how a combination of particle reinforcement and ECAP affects precipitation kinetics. After solution annealing, an AA2017 alloy (initial state: base material without particle reinforcement); AA2017 + 10 vol.-% Al2O3; and AA2017 + 10 vol.-% SiC were deformed in one pass in a 120° ECAP tool at a temperature of 140°C. Systematic differential scanning calorimetry (DSC) measurements of each condition were carried out. TEM specimens were prepared out of samples from additional DSC measurements, where the samples were immediately quenched in liquid nitrogen after reaching carefully selected temperatures. TEM analysis was performed to characterize the morphology of the different types of precipitates, and to directly relate microstructural information to the endo- and exothermic peaks in our DSC data. Our results show that both ECAP and particle reinforcement are associated with a shift of exothermic precipitation peaks towards lower temperatures. This effect is even more pronounced when ECAP and particle reinforcement are combined. The DSC data agrees well with our TEM observations of nucleation and morphology of different precipitates, indicating that DSC measurements are an appropriate tool for the analysis of how severe plastic deformation and particle reinforcement affect precipitation kinetics in Al-Cu alloys.

Biodiesel: Characterization by DSC and P-DSC

NASA Astrophysics Data System (ADS)

Chiriac, Rodica; Toche, François; Brylinski, Christian

Thermal analytical methods such as differential scanning calorimetry (DSC) have been successfully applied to neat petrodiesel and engine oils in the last 25 years. This chapter shows how DSC and P-DSC (pressurized DSC) techniques can be used to compare, characterize, and predict some properties of alternative non-petroleum fuels, such as cold flow behavior and oxidative stability. These two properties are extremely important with respect to the operability, transport, and long-term storage of biodiesel fuel. It is shown that the quantity of unsaturated fatty acids in the fuel composition has an important impact on both properties. In addition, it is shown that the impact of fuel additives on the oxidative stability or the cold flow behavior of biodiesel can be studied by means of DSC and P-DSC techniques. Thermomicroscopy can also be used to study the cold flow behavior of biodiesel, giving information on the size and the morphology of crystals formed at low temperature.

Media Coverage of FDA Drug Safety Communications about Zolpidem: A Quantitative and Qualitative Analysis.

PubMed

Woloshin, Steve; Schwartz, Lisa M; Dejene, Sara; Rausch, Paula; Dal Pan, Gerald J; Zhou, Esther H; Kesselheim, Aaron S

2017-05-01

FDA issues Drug Safety Communications (DSCs) to alert health care professionals and the public about emerging safety information affecting prescription and over-the-counter drugs. News media may amplify DSCs, but it is unclear how DSC messaging is transmitted through the media. We conducted a content analysis of the lay media coverage reaching the broadest audience to characterize the amount and content of media coverage of two zolpidem DSCs from 2013. After the first DSC, zolpidem news stories increased from 19 stories/week in the preceding 3 months to 153 following its release. Most (81%) appeared in the lay media, and 64% focused on the DSC content. After the second DSC, news stories increased from 24 stories/week in the preceding 3 months to 39 following. Among the 100 unique lay media news stories, at least half correctly reported three key DSC messages: next-day impairment and drowsiness as common safety hazards, lower doses for some but not all zolpidem products, and women's higher risk for impairment. Other DSC messages were reported in fewer than one-third of stories, such as the warning that impairment can happen even when people feel fully awake. The first-but not the second-zolpidem DSC generated high-profile news coverage. The finding that some messages were widely reported but others were not emphasizes the importance of ensuring translation of key DSC content.

Characterization of cure kinetics and physical properties of a high performance, glass fiber-reinforced epoxy prepreg and a novel fluorine-modified, amine-cured commercial epoxy

NASA Astrophysics Data System (ADS)

Bilyeu, Bryan

Kinetic equation parameters for the curing reaction of a commercial glass fiber reinforced high performance epoxy prepreg composed of the tetrafunctional epoxy tetraglycidyl 4,4-diaminodiphenyl methane (TGDDM), the tetrafunctional amine curing agent 4,4'-diaminodiphenylsulfone (DDS) and an ionic initiator/accelerator, are determined by various thermal analysis techniques and the results compared. The reaction is monitored by heat generated determined by differential scanning calorimetry (DSC) and by high speed DSC when the reaction rate is high. The changes in physical properties indicating increasing conversion are followed by shifts in glass transition temperature determined by DSC, temperature-modulated DSC (TMDSC), step scan DSC and high speed DSC, thermomechanical (TMA) and dynamic mechanical (DMA) analysis and thermally stimulated depolarization (TSD). Changes in viscosity, also indicative of degree of conversion, are monitored by DMA. Thermal stability as a function of degree of cure is monitored by thermogravimetric analysis (TGA). The parameters of the general kinetic equations, including activation energy and rate constant, are explained and used to compare results of various techniques. The utilities of the kinetic descriptions are demonstrated in the construction of a useful time-temperature-transformation (TTT) diagram and a continuous heating transformation (CHT) diagram for rapid determination of processing parameters in the processing of prepregs. Shrinkage due to both resin consolidation and fiber rearrangement is measured as the linear expansion of the piston on a quartz dilatometry cell using TMA. The shrinkage of prepregs was determined to depend on the curing temperature, pressure applied and the fiber orientation. Chemical modification of an epoxy was done by mixing a fluorinated aromatic amine (aniline) with a standard aliphatic amine as a curing agent for a commercial Diglycidylether of Bisphenol-A (DGEBA) epoxy. The resulting cured network was tested for wear resistance using tribological techniques. Of the six anilines, 3-fluoroaniline and 4-fluoroaniline were determined to have lower wear than the unmodified epoxy, while the others showed much higher wear rates.

DSC and EPR investigations on effects of cholesterol component on molecular interactions between paclitaxel and phospholipid within lipid bilayer membrane.

PubMed

Zhao, Lingyun; Feng, Si-Shen; Kocherginsky, Nikolai; Kostetski, Iouri

2007-06-29

Differential scanning calorimetry (DSC) and electron paramagnetic resonance spectroscopy (EPR) were applied to investigate effects of cholesterol component on molecular interactions between paclitaxel, which is one of the best antineoplastic agents found from nature, and dipalmitoylphosphatidylcholine (DPPC) within lipid bilayer vesicles (liposomes), which could also be used as a model cell membrane. DSC analysis showed that incorporation of paclitaxel into the DPPC bilayer causes a reduction in the cooperativity of bilayer phase transition, leading to a looser and more flexible bilayer structure. Including cholesterol component in the DPPC/paclitaxel mixed bilayer can facilitate the molecular interaction between paclitaxel and lipid and make the tertiary system more stable. EPR analysis demonstrated that both of paclitaxel and cholesterol have fluidization effect on the DPPC bilayer membranes although cholesterol has more significant effect than paclitaxel does. The reduction kinetics of nitroxides by ascorbic acid showed that paclitaxel can inhibit the reaction by blocking the diffusion of either the ascorbic acid or nitroxide molecules since the reaction is tested to be a first order one. Cholesterol can remarkably increase the reduction reaction speed. This research may provide useful information for optimizing liposomal formulation of the drug as well as for understanding the pharmacology of paclitaxel.

Glass Reinforcement of Various Epoxy Resins-Polyurea Systems

NASA Astrophysics Data System (ADS)

Joshi, Medha; Jauhari, Smita

2012-07-01

Polyureas (PUs) were prepared by the polycondensation reaction of disperse dyes containing -NH2 group and toluene 2, 4-diisocyanate. The disperse dyes have been prepared by coupling of various 2-diazobenzothiazoles with 1,3-benzenediamine. All the PUs were characterized by elemental analysis, spectral studies, number average molecular weight ( {overline{{Mn}} } ), and thermogravimetry. Further reaction of PUs was carried out with an epoxy resin (i.e., DGEBA). The curing study of prepared resins was monitored by differential scanning calorimeter (DSC). Based on DSC, thermograms glass fiber-reinforced composites have been laminated and characterized by chemical, mechanical, and electrical properties. The unreinforced cured resins were subjected to thermogravimetric analysis (TGA). The laminated composites showed excellent resistance properties against chemicals and good mechanical and electrical properties.

Calorimetric analysis points out the physical-chemistry of organic olive oils and reveals the geographical origin

NASA Astrophysics Data System (ADS)

Mallamace, Domenico; Vasi, Sebastiano; Corsaro, Carmelo; Naccari, Clara; Clodoveo, Maria Lisa; Dugo, Giacomo; Cicero, Nicola

2017-11-01

The thermal properties of many organic extra Virgin Olive Oils (eVOOs) coming from different countries of the world were investigated by Differential Scanning Calorimetry (DSC). This technique, through a series of heating and cooling cycles, provides a specific curve, i.e., a thermogram, which represents the fingerprint of each eVOO sample. In fact, variations due to the different cultivars, geographical origin or chemical composition can be highlighted because they produce changes in the corresponding thermogram. In particular, in this work, we show the results of an unsupervised multivariate statistical analysis applied to the DSC thermograms of many organic eVOOs. This analysis allows us to discriminate the geographical origin of the different studied samples in terms of the peculiar features shown by the melting profiles of the triacylglycerol moieties.

Brain Gliomas: Multicenter Standardized Assessment of Dynamic Contrast-enhanced and Dynamic Susceptibility Contrast MR Images.

PubMed

Anzalone, Nicoletta; Castellano, Antonella; Cadioli, Marcello; Conte, Gian Marco; Cuccarini, Valeria; Bizzi, Alberto; Grimaldi, Marco; Costa, Antonella; Grillea, Giovanni; Vitali, Paolo; Aquino, Domenico; Terreni, Maria Rosa; Torri, Valter; Erickson, Bradley J; Caulo, Massimo

2018-06-01

Purpose To evaluate the feasibility of a standardized protocol for acquisition and analysis of dynamic contrast material-enhanced (DCE) and dynamic susceptibility contrast (DSC) magnetic resonance (MR) imaging in a multicenter clinical setting and to verify its accuracy in predicting glioma grade according to the new World Health Organization 2016 classification. Materials and Methods The local research ethics committees of all centers approved the study, and informed consent was obtained from patients. One hundred patients with glioma were prospectively examined at 3.0 T in seven centers that performed the same preoperative MR imaging protocol, including DCE and DSC sequences. Two independent readers identified the perfusion hotspots on maps of volume transfer constant (K trans ), plasma (v p ) and extravascular-extracellular space (v e ) volumes, initial area under the concentration curve, and relative cerebral blood volume (rCBV). Differences in parameters between grades and molecular subtypes were assessed by using Kruskal-Wallis and Mann-Whitney U tests. Diagnostic accuracy was evaluated by using receiver operating characteristic curve analysis. Results The whole protocol was tolerated in all patients. Perfusion maps were successfully obtained in 94 patients. An excellent interreader reproducibility of DSC- and DCE-derived measures was found. Among DCE-derived parameters, v p and v e had the highest accuracy (are under the receiver operating characteristic curve [A z ] = 0.847 and 0.853) for glioma grading. DSC-derived rCBV had the highest accuracy (A z = 0.894), but the difference was not statistically significant (P > .05). Among lower-grade gliomas, a moderate increase in both v p and rCBV was evident in isocitrate dehydrogenase wild-type tumors, although this was not significant (P > .05). Conclusion A standardized multicenter acquisition and analysis protocol of DCE and DSC MR imaging is feasible and highly reproducible. Both techniques showed a comparable, high diagnostic accuracy for grading gliomas. © RSNA, 2018 Online supplemental material is available for this article.

Potential for differentiation of pseudoprogression from true tumor progression with dynamic susceptibility-weighted contrast-enhanced magnetic resonance imaging using ferumoxytol versus gadoteridol: A pilot study

PubMed Central

Gahramanov, Seymur; Raslan, Ahmed; Muldoon, Leslie L.; Hamilton, Bronwyn E.; Rooney, William D.; Varallyay, Csanad G.; Njus, Jeffrey M.; Haluska, Marianne; Neuwelt, Edward A.

2010-01-01

Purpose We evaluated dynamic susceptibility-weighted contrast-enhanced magnetic resonance imaging (DSC-MRI) using gadoteridol in comparison to the iron oxide nanoparticle blood pool agent, ferumoxytol in patients with glioblastoma multiforme (GBM) who received standard radiochemotherapy (RCT). Methods and Materials Fourteen patients with GBM received standard RCT and underwent 19 MRI sessions that included DSC-MRI acquisitions with gadoteridol on day 1 and ferumoxytol on day 2. Relative cerebral blood volume (rCBV) values were calculated from DSC data obtained from each contrast agent. T1-weighted acquisition post-gadoteridol administration was used to identify enhancing regions. Results In 7 MRI sessions of clinically presumptive active tumor, gadoteridol-DSC showed low rCBV in 3 and high rCBV in 4, while ferumoxytol-DSC showed high rCBV in all 7 sessions (p=0.002). After RCT, 7 MRI sessions showed increased gadoteridol contrast enhancement on T1-weighted scans coupled with low rCBV without significant differences between contrast agents (p=0.9). Based on post-gadoteridol T1-weighted scans, DSC-MRI, and clinical presentation four patterns of response to RCT were observed: 1) regression, 2) pseudoprogression, 3) true progression, and 4) mixed response. Conclusion We conclude that DSC-MRI with a blood-pool agent such as ferumoxytol may provide a better monitor of tumor rCBV than DSC-MRI with gadoteridol. Lesions demonstrating increased enhancement on T1-weighted MRI coupled with low ferumoxytol rCBV, are likely exhibiting pseudoprogression, while high rCBV with ferumoxytol is a better marker than gadoteridol for determining active tumor. These interesting pilot observations suggest that ferumoxytol may differentiate tumor progression from pseudoprogression, and warrant further investigation. PMID:20395065

Comparative kinetic analysis on thermal degradation of some cephalosporins using TG and DSC data

PubMed Central

2013-01-01

Background The thermal decomposition of cephalexine, cefadroxil and cefoperazone under non-isothermal conditions using the TG, respectively DSC methods, was studied. In case of TG, a hyphenated technique, including EGA, was used. Results The kinetic analysis was performed using the TG and DSC data in air for the first step of cephalosporin’s decomposition at four heating rates. The both TG and DSC data were processed according to an appropriate strategy to the following kinetic methods: Kissinger-Akahira-Sunose, Friedman, and NPK, in order to obtain realistic kinetic parameters, even if the decomposition process is a complex one. The EGA data offer some valuable indications about a possible decomposition mechanism. The obtained data indicate a rather good agreement between the activation energy’s values obtained by different methods, whereas the EGA data and the chemical structures give a possible explanation of the observed differences on the thermal stability. A complete kinetic analysis needs a data processing strategy using two or more methods, but the kinetic methods must also be applied to the different types of experimental data (TG and DSC). Conclusion The simultaneous use of DSC and TG data for the kinetic analysis coupled with evolved gas analysis (EGA) provided us a more complete picture of the degradation of the three cephalosporins. It was possible to estimate kinetic parameters by using three different kinetic methods and this allowed us to compare the Ea values obtained from different experimental data, TG and DSC. The thermodegradation being a complex process, the both differential and integral methods based on the single step hypothesis are inadequate for obtaining believable kinetic parameters. Only the modified NPK method allowed an objective separation of the temperature, respective conversion influence on the reaction rate and in the same time to ascertain the existence of two simultaneous steps. PMID:23594763

DSC of human hair: a tool for claim support or incorrect data analysis?

PubMed

Popescu, C; Gummer, C

2016-10-01

Differential scanning calorimetry (DSC) data are increasingly used to substantiate product claims of hair repair. Decreasing peak temperatures may indicate structural changes and chemical damage. Increasing the DSC, wet peak temperature is, therefore, often considered as proof of hair repair. A detailed understanding of the technique and hair structure indicates that this may not be a sound approach. Surveying the rich literature on the use of dynamic thermal analysis (DTA) and differential scanning calorimetry (DSC) for the analyses of human hair and the effect of cosmetic treatments, we underline some of the problems of hair structure and data interpretation. To overcome some of the difficulties of data interpretation, we advise that DSC acquired data should be supported by other techniques when used for claim substantiation. In this way, one can provide meaningful interpretation of the hair science and robust data for product claims support. © 2016 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Center Variation and Outcomes Associated with Delayed Sternal Closure Following Stage 1 Palliation for Hypoplastic Left Heart Syndrome

PubMed Central

Johnson, Jason N.; Jaggers, James; Li, Shuang; O’Brien, Sean M.; Li, Jennifer S.; Jacobs, Jeffrey P.; Jacobs, Marshall L.; Welke, Karl F.; Peterson, Eric D.; Pasquali, Sara K.

2009-01-01

Objectives There is debate whether primary or delayed sternal closure (DSC) is the best strategy following Stage 1 palliation (S1P) for hypoplastic left heart syndrome (HLHS). We describe center variation in DSC following S1P and associated outcomes. Methods Society of Thoracic Surgeons Congenital Database participants performing S1P for HLHS from 2000–2007 were included. We examined center variation in DSC, and compared in-hospital mortality, prolonged length of stay (LOS >6wks), and postoperative infection in centers with low (≤25% of cases), middle (26%–74% of cases), and high (≥75% of cases) DSC utilization, adjusting for patient and center factors. Results There were 1283 patients (45 centers) included. Median age and weight at surgery were 6d (IQR4-9d) and 3.2 kg (IQR2.8–3.5kg); 59% were male. DSC was used in 74% (range 3–100% of cases/center). In centers with high (n=23) and middle (n=17) vs. low (n=5) DSC utilization, there was a greater proportion of patients with prolonged LOS and infection, and a trend toward increased in-hospital mortality in unadjusted analysis. In multivariable analysis, there was no difference in mortality. Centers with high and middle DSC utilization had prolonged LOS [OR (95%CI): 2.83(1.46–5.47) p=0.002 and 2.23(1.17–4.26) p=0.02] and more infection [2.34(1.20–4.57) p=0.01 and 2.37(1.36–4.16) p=0.003]. Conclusions Utilization of DSC following S1P varies widely. These observational data suggest more frequent use of DSC is associated with longer LOS and higher postoperative infection rates. Further evaluation of the risks and benefits of DSC in the management of these complex infants is necessary. PMID:20167337

Thermal Analysis of Plastics

ERIC Educational Resources Information Center

D'Amico, Teresa; Donahue, Craig J.; Rais, Elizabeth A.

2008-01-01

This lab experiment illustrates the use of differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) in the measurement of polymer properties. A total of seven exercises are described. These are dry exercises: students interpret previously recorded scans. They do not perform the experiments. DSC was used to determine the…

Thermal degradation and morphological studies on raw and reinforced polyacrylic rubbers

NASA Astrophysics Data System (ADS)

Sasikala, A.; Kala, A.

2017-05-01

Poly acrylate rubbers (ACM) of today are saturated copolymers of monomeric acrylic esters and reactive cure site monomers. ACM elastomer have also found use in vibration damping due to its excellent resilience. Other applications include textiles, adhesives, and coatings. Two state of Poly acrylic raw and reinforced Rubber are analyzed using FTIR spectroscopy, Optical Microscopy, DSC and TGA measurements. With the objective of determined the mechanical strength, Thermal analysis on TGA and DSC studies show that, the thermal degradation temperature Tg of the sample material is obtained and activation energy is also calaulated by Broido, Horowitz - Metzger, Piloyan-Novikova and Coats Redfern methods which are found.

Chitosan pretreatment for cotton dyeing with black tea

NASA Astrophysics Data System (ADS)

Campos, J.; Díaz-García, P.; Montava, I.; Bonet-Aracil, M.; Bou-Belda, E.

2017-10-01

Chitosan is used in a wide range of applications due to its intrinsic properties. Chitosan is a biopolymer obtained from chitin and among their most important aspects highlights its bonding with cotton and its antibacterial properties. In this study two different molecular weight chitosan are used in the dyeing process of cotton with black tea to evaluate its influence. In order to evaluate the effect of the pretreatment with chitosan, DSC and reflection spectrophotometer analysis are performed. The curing temperature is evaluated by the DSC analysis of cotton fabric treated with 15 g/L of chitosan, whilst the enhancement of the dyeing is evaluated by the colorimetric coordinates and the K/S value obtained spectrophotometrically. This study shows the extent of improvement of the pretreatment with chitosan in dyeing with natural products as black tea.

Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry.

PubMed

Pan, Xiaohong; Julian, Thomas; Augsburger, Larry

2006-02-10

Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system.

Synthesis and Characterization of Novel Fluorine-Containing Water-Based Antirust Coating

NASA Astrophysics Data System (ADS)

Wang, Huiru; Wang, Xin; Zhao, Xiongyan

2018-01-01

A fluorine-containing polyacrylate copolymer emulsion was synthesized by a seed emulsion polymerization method, in which styrene(St) and butyl acrylate (BA) were used as main monomers and dodecafluoroheptyl methacrylate(DFMA) as fluorine-containing monomer. The structure and properties were characterized by Fourier transform infrared spectrum (FT-IR), scanning electron microscopy (SEM), particle size analysis, differential scanning calorimetry (DSC). The FTIR results showed that DFMA was effectively involved in the emulsion copolymerization, and the formed emulsion particles had a narrow particle size distribution. From the results salt spray test presented, it seems when the content of DFMA was 5wt% anti-rust performance of emulsion is relatively better. DSC and TGA also showed that their film exhibited higher thermal stability than that of fluorine-free emulsion.

Is It Necessary to Dry Primary Standards before Analysis?

ERIC Educational Resources Information Center

Spraggins, Jeffrey M., II; Williams, Theodore R.

2005-01-01

The thermal gravimetric analysis (TGA) data suggests that the quantity of volatile components in primary standards is less than 1% of the initial weight and differential scanning calorimetry (DSC) data shows that water present in the same chemicals is below the limit of detection of the instrumentation. This suggests that the 1-2 hour drying…

Determination of microplastic polyethylene (PE) and polypropylene (PP) in environmental samples using thermal analysis (TGA-DSC).

PubMed

Majewsky, Marius; Bitter, Hajo; Eiche, Elisabeth; Horn, Harald

2016-10-15

Microplastics are increasingly detected in the environment and the consequences on water resources and ecosystems are not clear to date. The present study provides a cost-effective and straightforward method to determine the mass concentrations of polymer types using thermal analysis. Characteristic endothermic phase transition temperatures were determined for seven plastic polymer types using TGA-DSC. Based on that, extracts from wastewater samples were analyzed. Results showed that among the studied polymers, only PE and PP could be clearly identified, while the phase transition signals of the other polymers largely overlap each other. Subsequently, calibration curves were run for PE and PP for qualitative measurements. 240 and 1540mg/m(3) of solid material (12µm to 1mm) was extracted from two wastewater effluent samples of a municipal WWTP of which 34% (81mg/m(3)) and 17% (257mg/m(3)) could be assigned to PE, while PP was not detected in any of the samples. The presented application of TGA-DSC provides a complementary or alternative method to FT-IR analyses for the determination of PE and PP in environmental samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Assessment of accuracy and efficiency of atlas-based autosegmentation for prostate radiotherapy in a variety of clinical conditions.

PubMed

Simmat, I; Georg, P; Georg, D; Birkfellner, W; Goldner, G; Stock, M

2012-09-01

The goal of the current study was to evaluate the commercially available atlas-based autosegmentation software for clinical use in prostate radiotherapy. The accuracy was benchmarked against interobserver variability. A total of 20 planning computed tomographs (CTs) and 10 cone-beam CTs (CBCTs) were selected for prostate, rectum, and bladder delineation. The images varied regarding to individual (age, body mass index) and setup parameters (contrast agent, rectal balloon, implanted markers). Automatically created contours with ABAS(®) and iPlan(®) were compared to an expert's delineation by calculating the Dice similarity coefficient (DSC) and conformity index. Demo-atlases of both systems showed different results for bladder (DSC(ABAS) 0.86 ± 0.17, DSC(iPlan) 0.51 ± 0.30) and prostate (DSC(ABAS) 0.71 ± 0.14, DSC(iPlan) 0.57 ± 0.19). Rectum delineation (DSC(ABAS) 0.78 ± 0.11, DSC(iPlan) 0.84 ± 0.08) demonstrated differences between the systems but better correlation of the automatically drawn volumes. ABAS(®) was closest to the interobserver benchmark. Autosegmentation with iPlan(®), ABAS(®) and manual segmentation took 0.5, 4 and 15-20 min, respectively. Automatic contouring on CBCT showed high dependence on image quality (DSC bladder 0.54, rectum 0.42, prostate 0.34). For clinical routine, efforts are still necessary to either redesign algorithms implemented in autosegmentation or to optimize image quality for CBCT to guarantee required accuracy and time savings for adaptive radiotherapy.

Influence of Processing Conditions on the Mechanical Behavior and Morphology of Injection Molded Poly(lactic-co-glycolic acid) 85:15

PubMed Central

Fancello, Eduardo Alberto

2017-01-01

Two groups of PLGA specimens with different geometries (notched and unnotched) were injection molded under two melting temperatures and flow rates. The mechanical properties, morphology at the fracture surface, and residual stresses were evaluated for both processing conditions. The morphology of the fractured surfaces for both specimens showed brittle and smooth fracture features for the majority of the specimens. Fracture images of the notched specimens suggest that the surface failure mechanisms are different from the core failure. Polarized light techniques indicated birefringence in all specimens, especially those molded with lower temperature, which suggests residual stress due to rapid solidification. DSC analysis confirmed the existence of residual stress in all PLGA specimens. The specimens molded using the lower injection temperature and the low flow rate presented lower loss tangent values according to the DMA and higher residual stress as shown by DSC, and the photoelastic analysis showed extensive birefringence. PMID:28848605

Synthesis and characterization of starch-poly(methyl acrylate) graft copolymers using horseradish peroxidase.

PubMed

Wang, Su; Wang, Qiang; Fan, Xuerong; Xu, Jin; Zhang, Ying; Yuan, Jiugang; Jin, Heling; Cavaco-Paulo, Artur

2016-01-20

Horseradish peroxidase (HRP)-mediated graft polymerization in the presence of hydrogen peroxide (H2O2) and acetylacetone (Acac) has been successfully applied to the synthesis of starch-poly(methyl acrylate) (PMA). The graft copolymer was characterized by Fourier transform infrared (FT-IR), elemental analysis, nuclear magnetic resonance ((1)H NMR and (13)C NMR), and differential scanning calorimetry (DSC). FT-IR, elemental analysis and NMR confirmed that methyl acrylate (MA) was grafted onto starch successfully. DSC results showed the graft reaction had changed the crystalline regions of the gelatinized starch. The effects of pH, MA content, HRP dosage, incubation temperature and time on grafting percentage (GP) and grafting efficiency (GE) were also investigated. The GP and GE under optimal conditions reached 30.21% and 45.13%, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Applications of high pressure differential scanning calorimetry to aviation fuel thermal stability research

NASA Technical Reports Server (NTRS)

Neveu, M. C.; Stocker, D. P.

1985-01-01

High pressure differential scanning calorimetry (DSC) was studied as an alternate method for performing high temperature fuel thermal stability research. The DSC was used to measure the heat of reaction versus temperature of a fuel sample heated at a programmed rate in an oxygen pressurized cell. Pure hydrocarbons and model fuels were studied using typical DSC operating conditions of 600 psig of oxygen and a temperature range from ambient to 500 C. The DSC oxidation onset temperature was determined and was used to rate the fuels on thermal stability. Kinetic rate constants were determined for the global initial oxidation reaction. Fuel deposit formation is measured, and the high temperature volatility of some tetralin deposits is studied by thermogravimetric analysis. Gas chromatography and mass spectrometry are used to study the chemical composition of some DSC stressed fuels.

Investigation of surface-modified solid lipid nanocontainers formulated with a heterolipid-templated homolipid.

PubMed

Attama, A A; Müller-Goymann, C C

2007-04-04

There is increasing interest in the search for improved drug delivery systems with greater versatility. Consequently, many drug delivery systems have been studied. In this study, surface-modified lipid nanocontainers were formulated with a homolipid from Capra hircus (goat fat) templated with a heterolipid (Phospholipon 90G) which was also the surface modifier. The solid lipid nanocontainers (SLN) were formulated by hot high pressure homogenisation using increasing concentrations of polysorbate 80 as the mobile surfactant. Prior to SLN preparation, the templated homolipid was formulated by fusion to obtain a homogeneous lipid matrix, which was characterized using differential scanning calorimetry (DSC), polarized light microscopy (PLM) and wide angle X-ray diffraction (WAXD) to obtain its thermal and crystal characteristics. Isothermal heat conduction microcalorimetry (IMC) and freeze-fracture transmission electron microscopy (FFTEM) studies were carried out on the templated homolipid and SLN containing 1.0% (w/w) of polysorbate 80 to study their in situ crystallization kinetics and morphology, respectively. The formulated SLN were also subjected to time-resolved DSC, WAXD and particle size analyses for one month. The thermal and crystal characteristics were compared with those of the bulk lipid matrix (templated homolipid). Result of the particle size analysis indicated that the particles size remained roughly within the lower nanometer range after one month. FFTEM micrograph of the lipid matrices revealed lamellar sheets for Phospholipon 90G and layered triglyceride structures for the homolipid and Phospholipon 90G-templated homolipid. FFTEM micrograph of SLN revealed anisometric structures. PLM of the templated homolipid did not show, but goat fat (homolipid) alone showed slight growth in crystals with time. WAXD and DSC studies revealed minor increase in crystallinity of the new lipid matrix after one month and DSC also detected templation of homolipid by the heterolipid noted by the disappearance of the lower melting peak of the homolipid. However, for the SLN, WAXD results showed low crystalline particles while DSC only showed a very little endothermic process after one month of storage at 20 degrees C. The implication of this finding is that progression of the SLN to highly ordered particles over time would not occur. This will be favourable for any incorporated drug as drug expulsion, due to increase in crystallinity, will not occur. Result obtained from analysis of the isothermal crystallization exotherms indicated that the templated homolipid and SLN1 containing 1.0% polysorbate 80 possess similar nucleation mechanisms and growth dimensions different from the pure homolipid. The SLN containing 0.5 and 1.0% polysorbate 80 possessed good properties and could prove to be good delivery systems for drugs for parenteral or ocular administration. The result of this study also shows a method of improving natural lipids for use in particulate drug delivery systems.

The liquid wood heat flow and material properties as a function of temperature

NASA Astrophysics Data System (ADS)

Mazurchevici, Simona; Quadrini, Fabrizio; Nedelcu, Dumitru

2018-03-01

There are three types of ‘liquid wood’, Arbofill, Arboblend and Arboform and will replace plastics materials in the near future taking into account the biodegradability and higher properties versus common used plastics materials. In order to get more information about the materials properties of ‘liquid wood’ the granules and samples obtained by injection molding were studied using Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) for Arboform L,V3 Nature-‘liquid wood’ (A-LW) and Arboform L, V3 Nature reinforced with Aramid Fibers (A-LWAF).In case of A-LW granule studied, the DSC analysis presents that at 97 °C appears an endoderm peak which represents the crystallization of the material, at 175 °C the exoderm peak which means the melting point of the material. After the tested granule cooling period of time this one was tested again and the endoderm peak disappears, which means that crystallization of material disappeared. The melting point of the second test decreases slightly at 174.6 °C. Also, the new test shows that at 61.7 °C the glass transition temperature appears and the melting point slightly decreases. In case of A-LW samples the DSC analyses shows that the melting point increased by 2.77 °C compared to the melting point of Arboform granule. The material behavior is more or less the same without the crystallization area.

Use of differential scanning calorimetry to detect canola oil (Brassica napus L.) adulterated with lard stearin.

PubMed

Marikkar, Jalaldeen Mohammed Nazrim; Rana, Sohel

2014-01-01

A study was conducted to detect and quantify lard stearin (LS) content in canola oil (CaO) using differential scanning calorimetry (DSC). Authentic samples of CaO were obtained from a reliable supplier and the adulterant LS were obtained through a fractional crystallization procedure as reported previously. Pure CaO samples spiked with LS in levels ranging from 5 to 15% (w/w) were analyzed using DSC to obtain their cooling and heating profiles. The results showed that samples contaminated with LS at 5% (w/w) level can be detected using characteristic contaminant peaks appearing in the higher temperature regions (0 to 70°C) of the cooling and heating curves. Pearson correlation analysis of LS content against individual DSC parameters of the adulterant peak namely peak temperature, peak area, peak onset temperature indicated that there were strong correlations between these with the LS content of the CaO admixtures. When these three parameters were engaged as variables in the execution of the stepwise regression procedure, predictive models for determination of LS content in CaO were obtained. The predictive models obtained with single DSC parameter had relatively lower coefficient of determination (R(2) value) and higher standard error than the models obtained using two DSC parameters in combination. This study concluded that the predictive models obtained with peak area and peak onset temperature of the adulteration peak would be more accurate for prediction of LS content in CaO based on the highest coefficient of determination (R(2) value) and smallest standard error.

Thermal analysis of hydroxypropylmethylcellulose and methylcellulose: powders, gels and matrix tablets.

PubMed

Ford, J L

1999-03-15

This review focuses on the thermal analysis of hydroxypropylmethylcellulose (HPMC) and methylcellulose. Differential scanning calorimetry (DSC) of their powders is used to determine temperatures of moisture loss (in conjunction with thermogravimetric analysis) and glass transition temperatures. However, sample preparation and encapsulation affect the values obtained. The interaction of these cellulose ethers with water is evaluated by DSC. Water is added to the powder directly in DSC pans or preformed gels can be evaluated. Data quality depends on previous thermal history but estimates of the quantity of water bound to the polymers may be made. Water uptake by cellulose ethers may be evaluated by the use of polymeric wafers and by following loss of free water, over a series of timed curves, into wafers in contact with water. Cloud points, which assess the reduction of polymer solubility with increase of temperature, may be assessed spectrophotometrically. DSC and rheometric studies are used to follow thermogelation, a process involving hydrophobic interaction between partly hydrated polymeric chains. The advantages and disadvantages of the various methodologies are highlighted. Copyright.

Thermal properties of polyethylene reinforced with recycled–poly (ethylene terephthalate) flakes.

NASA Astrophysics Data System (ADS)

Ruqiyah Nik Hassan, Nik; Mazni Ismail, Noor; Ghazali, Suriati; Nuruzzaman, Dewan Muhammad

2018-04-01

In this study, recycled plastic bottles (RPET) were used as a filler in high density polyethylene (HDPE) thermoplastic. The plastic sheet of RPET/HDPE was prepared by using hot and cold press machine. The effects of RPET addition and hot press process to the thermal properties of the composite RPET/HDPE were investigated using differential scanning calorimetry (DSC) and thermogravimetric (TGA). Results from DSC analysis show that the melting point of HDPE slightly shifted to a higher temperature for about 2°C to 4°C with the addition of RPET as a filler. The starting degradation temperature of RPET/HDPE composite examined from TGA analysis also seen to be slightly increased. It was observed that the incorporation of recycled PET flakes into HDPE is achievable using hot press process with slight improvement seen in both melting point and thermal stability of the composite compared to the neat HDPE.

Differentiating between Central Nervous System Lymphoma and High-grade Glioma Using Dynamic Susceptibility Contrast and Dynamic Contrast-enhanced MR Imaging with Histogram Analysis.

PubMed

Murayama, Kazuhiro; Nishiyama, Yuya; Hirose, Yuichi; Abe, Masato; Ohyu, Shigeharu; Ninomiya, Ayako; Fukuba, Takashi; Katada, Kazuhiro; Toyama, Hiroshi

2018-01-10

We evaluated the diagnostic performance of histogram analysis of data from a combination of dynamic susceptibility contrast (DSC)-MRI and dynamic contrast-enhanced (DCE)-MRI for quantitative differentiation between central nervous system lymphoma (CNSL) and high-grade glioma (HGG), with the aim of identifying useful perfusion parameters as objective radiological markers for differentiating between them. Eight lesions with CNSLs and 15 with HGGs who underwent MRI examination, including DCE and DSC-MRI, were enrolled in our retrospective study. DSC-MRI provides a corrected cerebral blood volume (cCBV), and DCE-MRI provides a volume transfer coefficient (K trans ) for transfer from plasma to the extravascular extracellular space. K trans and cCBV were measured from a round region-of-interest in the slice of maximum size on the contrast-enhanced lesion. The differences in t values between CNSL and HGG for determining the most appropriate percentile of K trans and cCBV were investigated. The differences in K trans , cCBV, and K trans /cCBV between CNSL and HGG were investigated using histogram analysis. Receiver operating characteristic (ROC) analysis of K trans , cCBV, and K trans /cCBV ratio was performed. The 30 th percentile (C30) in K trans and 80 th percentile (C80) in cCBV were the most appropriate percentiles for distinguishing between CNSL and HGG from the differences in t values. CNSL showed significantly lower C80 cCBV, significantly higher C30 K trans , and significantly higher C30 K trans /C80 cCBV than those of HGG. In ROC analysis, C30 K trans /C80 cCBV had the best discriminative value for differentiating between CNSL and HGG as compared to C30 K trans or C80 cCBV. The combination of K trans by DCE-MRI and cCBV by DSC-MRI was found to reveal the characteristics of vascularity and permeability of a lesion more precisely than either K trans or cCBV alone. Histogram analysis of these vascular microenvironments enabled quantitative differentiation between CNSL and HGG.

Effect of additives on mineral trioxide aggregate setting reaction product formation.

PubMed

Zapf, Angela M; Chedella, Sharath C V; Berzins, David W

2015-01-01

Mineral trioxide aggregate (MTA) sets via hydration of calcium silicates to yield calcium silicate hydrates and calcium hydroxide (Ca[OH]2). However, a drawback of MTA is its long setting time. Therefore, many additives have been suggested to reduce the setting time. The effect those additives have on setting reaction product formation has been ignored. The objective was to examine the effect additives have on MTA's setting time and setting reaction using differential scanning calorimetry (DSC). MTA powder was prepared with distilled water (control), phosphate buffered saline, 5% calcium chloride (CaCl2), 3% sodium hypochlorite (NaOCl), or lidocaine in a 3:1 mixture and placed in crucibles for DSC evaluation. The setting exothermic reactions were evaluated at 37°C for 8 hours to determine the setting time. Separate samples were stored and evaluated using dynamic DSC scans (37°C→640°C at10°C/min) at 1 day, 1 week, 1 month, and 3 months (n = 9/group/time). Dynamic DSC quantifies the reaction product formed from the amount of heat required to decompose it. Thermographic peaks were integrated to determine enthalpy, which was analyzed with analysis of variance/Tukey test (α = 0.05). Isothermal DSC identified 2 main exothermal peaks occurring at 44 ± 12 and 343 ± 57 minutes for the control. Only the CaCl2 additive was an accelerant, which was observed by a greater exothermic peak at 101 ± 11 minutes, indicating a decreased setting time. The dynamic DSC scans produced an endothermic peak around 450°C-550°C attributed to Ca(OH)2 decomposition. The use of a few additives (NaOCl and lidocaine) resulted in significantly less Ca(OH)2 product formation. DSC was used to discriminate calcium hydroxide formation in MTA mixed with various additives and showed NaOCl and lidocaine are detrimental to MTA reaction product formation, whereas CaCl2 accelerated the reaction. Copyright © 2015 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

Calorimetric Studies of Precipitation and Dissolution Kinetics in Aluminum Alloys 2219 and 7075

NASA Astrophysics Data System (ADS)

Papazian, John M.

1982-05-01

Differential scanning calorimetry (DSC) was used to study the kinetics of precipitation and dissolution of metastable and stable phases in aluminum alloys 2219 and 7075. A comparison of DSC scans obtained at heating rates of 1, 5, 10, and 20 K per minute showed that, during a DSC scan, the rates of precipitation of θ' and θ in 2219 and η' and η in 7075 were limited by their reaction kinetics. Likewise, the rates of dissolution of GP zones, θ' and η', were found to be dominated by kinetics. In contrast, the dissolution of θ and η was dominated by the thermodynamic equilibrium between these phases and the matrix. Analysis of the kinetically dominated reaction peaks and their dependence on heating rate and particle size showed that the GP zone dissolution reaction could best be described by a three-dimensional volume diffusion limited rate expression with an activation energy equal to that for diffusion. The rate of formation of θ' was best described by an Avrami expression with n = 1.1, indicating that nucleation was not the rate controlling step. A pronounced dependence of the θ' formation rate on prior plastic deformation was observed and ascribed to the influence of the matrix dislocation density on diffusivity.

Functional characterization of the Dsc E3 ligase complex in the citrus postharvest pathogen Penicillium digitatum.

PubMed

Ruan, Ruoxin; Chung, Kuang-Ren; Li, Hongye

2017-12-01

Sterol regulatory element binding proteins (SREBPs) are required for sterol homeostasis in eukaryotes. Activation of SREBPs is regulated by the Dsc E3 ligase complex in Schizosaccharomyces pombe and Aspergillus spp. Previous studies indicated that an SREBP-coding gene PdsreA is required for fungicide resistance and ergosterol biosynthesis in the citrus postharvest pathogen Penicillium digitatum. In this study, five genes, designated PddscA, PddscB, PddscC, PddscD, and PddscE encoding the Dsc E3 ligase complex were characterized to be required for fungicide resistance, ergosterol biosynthesis and CoCl 2 tolerance in P. digitatum. Each of the dsc genes was inactivated by target gene disruption and the resulted phenotypes were analyzed and compared. Genetic analysis reveals that, of five Dsc complex components, PddscB is the core subunit gene in P. digitatum. Although the resultant dsc mutants were able to infect citrus fruit and induce maceration lesions as the wild-type, the mutants rarely produced aerial mycelia on affected citrus fruit peels. P. digitatum Dsc proteins regulated not only the expression of genes involved in ergosterol biosynthesis but also that of PdsreA. Yeast two-hybrid assays revealed a direct interaction between the PdSreA protein and the Dsc proteins. Ectopic expression of the PdSreA N-terminus restored fungicide resistance in the dsc mutants. Our results provide important evidence to understand the mechanisms underlying SREBP activation and regulation of ergosterol biosynthesis in plant pathogenic fungi. Copyright © 2017 Elsevier GmbH. All rights reserved.

Sodium hydrogen carbonate as an alternative blowing agent in the preparation of palm-based polyurethane foam

NASA Astrophysics Data System (ADS)

Shakir, Amira Shakim Abdul; Badri, Khairiah Haji; Hua, Chia Chin

2016-11-01

An environmental-friendly blowing agent has been used to fabricate flexible polyurethane (PU) foam. Polyurethane foam was prepared from palm kernel oil-based monoester polyol (PKO-p) via prepolymerization method. Acetone has been used as solvent in this study. The developed polyurethane foam was characterized using tensile, differential scanning calorimetry analysis (DSC), thermogravimetric analysis (TGA), optical microscope and drop shape analyzer. The mechanical properties of the PU-reference (PU-R) and PU-NaHCO3 foam was analyzed by tensile using ASTM D 3574-01. From the results, the elongation of PU- NaHCO3 shows reduction to 26.3 % compared to PU-R. The DSC showed two glass transition temperatures in all samples that belonged to the PU-R and PU-NaHCO3. TGA revealed that the incorporation of sodium hydrogen carbonate into the PU system did not show significant difference as compared to the control PU. The morphology of both PU was investigated using optical microscope. Contact angle has been measured to determine the hydrophobicity of the PU. The PU- NaHCO3 exhibited an increase in contact angle (93.1°).

[Preparation of ibuprofen/EC-PVP sustained-release composite particles by supercritical CO2 anti-solvent technology].

PubMed

Cai, Jin-Yuan; Huang, De-Chun; Wang, Zhi-Xiang; Dang, Bei-Lei; Wang, Qiu-Ling; Su, Xin-Guang

2012-06-01

Ibuprofen/ethyl-cellulose (EC)-polyvinylpyrrolidone (PVP) sustained-release composite particles were prepared by using supercritical CO2 anti-solvent technology. With drug loading as the main evaluation index, orthogonal experimental design was used to optimize the preparation process of EC-PVP/ibuprofen composite particles. The experiments such as encapsulation efficiency, particle size distribution, electron microscope analysis, infrared spectrum (IR), differential scanning calorimetry (DSC) and in vitro dissolution were used to analyze the optimal process combination. The orthogonal experimental optimization process conditions were set as follows: crystallization temperature 40 degrees C, crystallization pressure 12 MPa, PVP concentration 4 mgmL(-1), and CO2 velocity 3.5 Lmin(-1). Under the optimal conditions, the drug loading and encapsulation efficiency of ibuprofen/EC-PVP composite particles were 12.14% and 52.21%, and the average particle size of the particles was 27.621 microm. IR and DSC analysis showed that PVP might complex with EC. The experiments of in vitro dissolution showed that ibuprofen/EC-PVP composite particles had good sustained-release effect. Experiment results showed that, ibuprofen/EC-PVP sustained-release composite particles can be prepared by supercritical CO2 anti-solvent technology.

Highly crystalline zinc incorporated hydroxyapatite nanorods' synthesis, characterization, thermal, biocompatibility, and antibacterial study

NASA Astrophysics Data System (ADS)

Udhayakumar, Gayathri; Muthukumarasamy, N.; Velauthapillai, Dhayalan; Santhosh, Shanthi Bhupathi

2017-10-01

Highly crystalline zinc incorporated hydroxyapatite (Zn-HAp) nanorods have been synthesized using microwave irradiation method. To improve bioactivity and crystallinity of pure HAp, zinc was incorporated into it. As-synthesized samples were characterized by Fourier transform-infrared spectroscopy (FT-IR), X-ray diffraction, field-emission scanning electron microscopy (FESEM), energy dispersive X-ray analysis (EDAX), high-resolution transmission electron microscopy (HRTEM), and the thermal and crystallinity behavior of Zn-HAp nanoparticle were studied by thermogravimetry (TGA) and differential scanning calorimetry (DSC). Antibacterial activity of the as-synthesized nanorods was evaluated against two prokaryotic strains ( Escherichia coli and Staphylococcus aureus). The FT-IR studies show the presence of hydroxide and phosphate functional groups. HRTEM and FESEM images showed highly crystalline rod-shaped nanoparticles with the diameter of about 50-60 nm. EDAX revealed the presence of Ca, Zn, P, and O in the prepared samples. The crystallinity and thermal stability were further confirmed by TGA-DSC analysis. The biocompatibility evaluation results promoted that the Zn-HAp nanorods are biologically active apatites and potentially promising bone-substitute biomaterials for orthopaedic application.

A calorimetric study of precipitation in aluminum alloy 2219

NASA Astrophysics Data System (ADS)

Papazian, John M.

1981-02-01

Precipitate microstructures in aluminum alloy 2219 were characterized using transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The DSC signatures of individual precipitate phases were established by comparing the DSC and TEM results from samples that had been aged such that only one precipitate phase was present. These signatures were then used to analyze the commercial tempers. It was found that DSC could readily distinguish between the T3, T4, T6, T8 and O tempers but could not distinguish amongst T81, T851 and T87. Small amounts of plastic deformation between solution treatment and aging had a significant effect on the thermograms. Aging experiments at 130 and 190 °C showed that the aging sequence and DSC response of this alloy were similar to those of pure Al-Cu when the increased copper content is taken into account. Further aging experiments at temperatures between room temperature and 130 °C showed pronounced changes of the GP zone dissolution peak as a function of aging conditions. These changes were found to be related to the effect of GP zone size on the metastable phase boundary and on the GP zone dissolution kinetics.

Differential Scanning Calorimetry and Evolved Gas Analysis at Mars Ambient Conditions Using the Thermal Evolved Gas Analyzer (TEGA)

NASA Technical Reports Server (NTRS)

Musselwhite, D. S.; Boynton, W. V.; Ming, Douglas W.; Quadlander, G.; Kerry, K. E.; Bode, R. C.; Bailey, S. H.; Ward, M. G.; Pathare, A. V.; Lorenz, R. D.

2000-01-01

Differential Scanning Calorimetry (DSC) combined with evolved gas analysis (EGA) is a well developed technique for the analysis of a wide variety of sample types with broad application in material and soil sciences. However, the use of the technique for samples under conditions of pressure and temperature as found on other planets is one of current C development and cutting edge research. The Thermal Evolved Gas Analyzer (MGA), which was designed, built and tested at the University of Arizona's Lunar and Planetary Lab (LPL), utilizes DSC/EGA. TEGA, which was sent to Mars on the ill-fated Mars Polar Lander, was to be the first application of DSC/EGA on the surface of Mars as well as the first direct measurement of the volatile-bearing mineralogy in martian soil.

Thermodynamics of micellization from heat-capacity measurements.

PubMed

Šarac, Bojan; Bešter-Rogač, Marija; Lah, Jurij

2014-06-23

Differential scanning calorimetry (DSC), the most important technique for studying the thermodynamics of structural transitions of biological macromolecules, is seldom used in quantitative thermodynamic studies of surfactant micellization/demicellization. The reason for this could be ascribed to an insufficient understanding of the temperature dependence of the heat capacity of surfactant solutions (DSC data) in terms of thermodynamics, which leads to problems with the design of experiments and interpretation of the output signals. We address these issues by careful design of DSC experiments performed with solutions of ionic and nonionic surfactants at various surfactant concentrations, and individual and global mass-action model analysis of the obtained DSC data. Our approach leads to reliable thermodynamic parameters of micellization for all types of surfactants, comparable with those obtained by using isothermal titration calorimetry (ITC). In summary, we demonstrate that DSC can be successfully used as an independent method to obtain temperature-dependent thermodynamic parameters for micellization. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Non-resonant dynamic stark control of vibrational motion with optimized laser pulses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas, Esben F.; Henriksen, Niels E.

2016-06-28

The term dynamic Stark control (DSC) has been used to describe methods of quantum control related to the dynamic Stark effect, i.e., a time-dependent distortion of energy levels. Here, we employ analytical models that present clear and concise interpretations of the principles behind DSC. Within a linearly forced harmonic oscillator model of vibrational excitation, we show how the vibrational amplitude is related to the pulse envelope, and independent of the carrier frequency of the laser pulse, in the DSC regime. Furthermore, we shed light on the DSC regarding the construction of optimal pulse envelopes — from a time-domain as wellmore » as a frequency-domain perspective. Finally, in a numerical study beyond the linearly forced harmonic oscillator model, we show that a pulse envelope can be constructed such that a vibrational excitation into a specific excited vibrational eigenstate is accomplished. The pulse envelope is constructed such that high intensities are avoided in order to eliminate the process of ionization.« less

Calorimetric evidence for two distinct molecular packing arrangements in stable glasses of indomethacin.

PubMed

Kearns, Kenneth L; Swallen, Stephen F; Ediger, M D; Sun, Ye; Yu, Lian

2009-02-12

Indomethacin glasses of varying stabilities were prepared by physical vapor deposition onto substrates at 265 K. Enthalpy relaxation and the mobility onset temperature were assessed with differential scanning calorimetry (DSC). Quasi-isothermal temperature-modulated DSC was used to measure the reversing heat capacity during annealing above the glass transition temperature Tg. At deposition rates near 8 A/s, scanning DSC shows two enthalpy relaxation peaks and quasi-isothermal DSC shows a two-step change in the reversing heat capacity. We attribute these features to two distinct local packing structures in the vapor-deposited glass, and this interpretation is supported by the strong correlation between the two calorimetric signatures of the glass to liquid transformation. At lower deposition rates, a larger fraction of the sample is prepared in the more stable local packing. The transformation of the vapor-deposited glasses into the supercooled liquid above Tg is exceedingly slow, as much as 4500 times slower than the structural relaxation time of the liquid.

Energetic domains and conformational analysis of human serum albumin upon co-incubation with sodium benzoate and glucose.

PubMed

Taghavi, F; Moosavi-Movahedi, A A; Bohlooli, M; Habibi-Rezaei, M; Hadi Alijanvand, H; Amanlou, M; Sheibani, N; Saboury, A A; Ahmad, F

2014-01-01

Sodium benzoate (SB), a powerful inhibitor of microbial growth, is one of the most commonly used food preservative. Here, we determined the effects of SB on human serum albumin (HSA) structure in the presence or absence of glucose after 35 days of incubation under physiological conditions. The biochemical, biophysical, and molecular approaches including free amine content assay (TNBSA assay), fluorescence, and circular dichroism spectroscopy (CD), differential scanning calorimetry (DSC), and molecular docking and LIGPLOT studies were utilized for structural studies. The TNBSA results indicated that SB has the ability to bind Lys residues in HSA through covalent bonds. The docking and LIGPLOT studies also determined another specific site via hydrophobic interactions. The CD results showed more structural helicity for HSA incubated with SB, while HSA incubated with glucose had the least, and HSA incubated with glucose + SB had medium helicity. Fluorescence spectrophotometry results demonstrated partial unfolding of HSA incubated with SB in the presence or absence of glucose, while maximum partial unfolding was observed in HSA incubated with glucose. These results were confirmed by DSC and its deconvoluted thermograms. The DSC results also showed significant changes in HSA energetic structural domains due to HSA incubation with SB in the presence or absence of glucose. Together, our studies showed the formation of three different intermediates and indicate that biomolecular investigation are effective in providing new insight into safety determinations especially in health-related conditions including diabetes.

Differential Scanning Calorimetry and Evolved Gas Analysis at Mars Ambient Conditions Using the Thermal Evolved Gas Analyser (TEGA)

NASA Technical Reports Server (NTRS)

Musselwhite, D. S.; Boynton, W. V.; Ming, D. W.; Quadlander, G.; Kerry, K. E.; Bode, R. C.; Bailey, S. H.; Ward, M. G.; Pathare, A. V.; Lorenz, R. D.

2000-01-01

Differential Scanning Calorimetry (DSC) combined with evolved gas analysis (EGA) is a well developed technique for the analysis of a wide variety of sample types with broad application in material and soil sciences. However, the use of the technique for samples under conditions of pressure and temperature as found on other planets is one of current development and cutting edge research. The Thermal Evolved Gas Analyzer (TEGA), which was designed, built and tested at the University of Arizona's Lunar and Planetary Lab (LPL), utilizes DSC/EGA. TEGA, which was sent to Mars on the ill-fated Mars Polar Lander, was to be the first application of DSC/EGA on the surface of Mars as well as the first direct measurement of the volatile-bearing mineralogy in martian soil. Additional information is available in the original extended abstract.

Combined use of susceptibility weighted magnetic resonance imaging sequences and dynamic susceptibility contrast perfusion weighted imaging to improve the accuracy of the differential diagnosis of recurrence and radionecrosis in high-grade glioma patients.

PubMed

Kim, Tae-Hyung; Yun, Tae Jin; Park, Chul-Kee; Kim, Tae Min; Kim, Ji-Hoon; Sohn, Chul-Ho; Won, Jae Kyung; Park, Sung-Hye; Kim, Il Han; Choi, Seung Hong

2017-03-21

Purpose was to assess predictive power for overall survival (OS) and diagnostic performance of combination of susceptibility-weighted MRI sequences (SWMRI) and dynamic susceptibility contrast (DSC) perfusion-weighted imaging (PWI) for differentiation of recurrence and radionecrosis in high-grade glioma (HGG). We enrolled 51 patients who underwent radiation therapy or gamma knife surgeryfollowed by resection for HGG and who developed new measurable enhancement more than six months after complete response. The lesions were confirmed as recurrence (n = 32) or radionecrosis (n = 19). The mean and each percentile value from cumulative histograms of normalized CBV (nCBV) and proportion of dark signal intensity on SWMRI (proSWMRI, %) within enhancement were compared. Multivariate regression was performed for the best differentiator. The cutoff value of best predictor from ROC analysis was evaluated. OS was determined with Kaplan-Meier method and log-rank test. Recurrence showed significantly lower proSWMRI and higher mean nCBV and 90th percentile nCBV (nCBV90) than radionecrosis. Regression analysis revealed both nCBV90 and proSWMRI were independent differentiators. Combination of nCBV90 and proSWMRI achieved 71.9% sensitivity (23/32), 100% specificity (19/19) and 82.3% accuracy (42/51) using best cut-off values (nCBV90 > 2.07 and proSWMRI≤15.76%) from ROC analysis. In subgroup analysis, radionecrosis with nCBV > 2.07 (n = 5) showed obvious hemorrhage (proSWMRI > 32.9%). Patients with nCBV90 > 2.07 and proSWMRI≤15.76% had significantly shorter OS. In conclusion, compared with DSC PWI alone, combination of SWMRI and DSC PWI have potential to be prognosticator for OS and lower false positive rate in differentiation of recurrence and radionecrosis in HGG who develop new measurable enhancement more than six months after complete response.

Soil organic matter composition from correlated thermal analysis and nuclear magnetic resonance data in Australian national inventory of agricultural soils

NASA Astrophysics Data System (ADS)

Moore, T. S.; Sanderman, J.; Baldock, J.; Plante, A. F.

2016-12-01

National-scale inventories typically include soil organic carbon (SOC) content, but not chemical composition or biogeochemical stability. Australia's Soil Carbon Research Programme (SCaRP) represents a national inventory of SOC content and composition in agricultural systems. The program used physical fractionation followed by 13C nuclear magnetic resonance (NMR) spectroscopy. While these techniques are highly effective, they are typically too expensive and time consuming for use in large-scale SOC monitoring. We seek to understand if analytical thermal analysis is a viable alternative. Coupled differential scanning calorimetry (DSC) and evolved gas analysis (CO2- and H2O-EGA) yields valuable data on SOC composition and stability via ramped combustion. The technique requires little training to use, and does not require fractionation or other sample pre-treatment. We analyzed 300 agricultural samples collected by SCaRP, divided into four fractions: whole soil, coarse particulates (POM), untreated mineral associated (HUM), and hydrofluoric acid (HF)-treated HUM. All samples were analyzed by DSC-EGA, but only the POM and HF-HUM fractions were analyzed by NMR. Multivariate statistical analyses were used to explore natural clustering in SOC composition and stability based on DSC-EGA data. A partial least-squares regression (PLSR) model was used to explore correlations among the NMR and DSC-EGA data. Correlations demonstrated regions of combustion attributable to specific functional groups, which may relate to SOC stability. We are increasingly challenged with developing an efficient technique to assess SOC composition and stability at large spatial and temporal scales. Correlations between NMR and DSC-EGA may demonstrate the viability of using thermal analysis in lieu of more demanding methods in future large-scale surveys, and may provide data that goes beyond chemical composition to better approach quantification of biogeochemical stability.

pH responsive cross-linked polymeric matrices based on natural polymers: effect of process variables on swelling characterization and drug delivery properties.

PubMed

Naeem, Fahad; Khan, Samiullah; Jalil, Aamir; Ranjha, Nazar Muhammad; Riaz, Amina; Haider, Malik Salman; Sarwar, Shoaib; Saher, Fareha; Afzal, Samrin

2017-01-01

Introduction: The current work was aimed to design and synthesize novel crosslinked pH-sensitive gelatin/pectin (Ge/Pec) hydrogels using different polymeric ratios and to explore the effect of polymers and degree of crosslinking on dynamic, equilibrium swelling and in vitro release behavior of the model drug (Mannitol). Methods: The Ge/Pec based hydrogels were prepared using glutaraldehyde as the crosslinker. Various structural parameters that affect their release behavior were determined, including swelling study, porosity, sol-gel analysis, average molecular weight between crosslinks (Mc), volume fraction of polymer (V2,s), solvent interaction parameter (χ) and diffusion coefficient. The synthesized hydrogels were subjected to various characterization tools like Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and DSC differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Results: The hydrogels show highest water uptake and release at lower pH values. The FTIR spectra showed an interaction between Ge and Pec, and the drug-loaded samples also showed the drug-related peaks, indicating proper loading of the drug. DSC and TGA studies confirmed the thermal stability of hydrogel samples, while SEM showed the porous nature of hydrogels. The drug release followed non-Fickian diffusion or anomalous mechanism. Conclusion: Aforementioned characterizations reveal the successful formation of copolymer hydrogels. The pH-sensitive swelling ability and drug release behavior suggest that the rate of polymer chain relaxation and drug diffusion from these hydrogels are comparable which also predicts their possible use for site-specific drug delivery.

pH responsive cross-linked polymeric matrices based on natural polymers: effect of process variables on swelling characterization and drug delivery properties

PubMed Central

Naeem, Fahad; Khan, Samiullah; Jalil, Aamir; Ranjha, Nazar Muhammad; Riaz, Amina; Haider, Malik Salman; Sarwar, Shoaib; Saher, Fareha; Afzal, Samrin

2017-01-01

Introduction: The current work was aimed to design and synthesize novel crosslinked pH-sensitive gelatin/pectin (Ge/Pec) hydrogels using different polymeric ratios and to explore the effect of polymers and degree of crosslinking on dynamic, equilibrium swelling and in vitro release behavior of the model drug (Mannitol). Methods: The Ge/Pec based hydrogels were prepared using glutaraldehyde as the crosslinker. Various structural parameters that affect their release behavior were determined, including swelling study, porosity, sol-gel analysis, average molecular weight between crosslinks (Mc), volume fraction of polymer (V2,s), solvent interaction parameter (χ) and diffusion coefficient. The synthesized hydrogels were subjected to various characterization tools like Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and DSC differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Results:The hydrogels show highest water uptake and release at lower pH values. The FTIR spectra showed an interaction between Ge and Pec, and the drug-loaded samples also showed the drug-related peaks, indicating proper loading of the drug. DSC and TGA studies confirmed the thermal stability of hydrogel samples, while SEM showed the porous nature of hydrogels. The drug release followed non-Fickian diffusion or anomalous mechanism. Conclusion: Aforementioned characterizations reveal the successful formation of copolymer hydrogels. The pH-sensitive swelling ability and drug release behavior suggest that the rate of polymer chain relaxation and drug diffusion from these hydrogels are comparable which also predicts their possible use for site-specific drug delivery. PMID:29159145

The mechanism of interactions between tea polyphenols and porcine pancreatic alpha‐amylase: Analysis by inhibition kinetics, fluorescence quenching, differential scanning calorimetry and isothermal titration calorimetry

PubMed Central

Sun, Lijun; Gidley, Michael J.

2017-01-01

Scope This study aims to use a combination of biochemical and biophysical methods to derive greater mechanistic understanding of the interactions between tea polyphenols and porcine pancreatic α‐amylase (PPA). Methods and results The interaction mechanism was studied through fluorescence quenching (FQ), differential scanning calorimetry (DSC) and isothermal titration calorimetry (ITC) and compared with inhibition kinetics. The results showed that a higher quenching effect of polyphenols corresponded to a stronger inhibitory activity against PPA. The red‐shift of maximum emission wavelength of PPA bound with some polyphenols indicated a potential structural unfolding of PPA. This was also suggested by the decreased thermostability of PPA with these polyphenols in DSC thermograms. Through thermodynamic binding analysis of ITC and inhibition kinetics, the equilibrium of competitive inhibition was shown to result from the binding of particularly galloylated polyphenols with specific sites on PPA. There were positive linear correlations between the reciprocal of competitive inhibition constant (1/K ic), quenching constant (K FQ) and binding constant (K itc). Conclusion The combination of inhibition kinetics, FQ, DSC and ITC can reasonably characterize the interactions between tea polyphenols and PPA. The galloyl moiety is an important group in catechins and theaflavins in terms of binding with and inhibiting the activity of PPA. PMID:28618113

Degradation of components in drug formulations: a comparison between HPLC and DSC methods.

PubMed

Ceschel, G C; Badiello, R; Ronchi, C; Maffei, P

2003-08-08

Information about the stability of drug components and drug formulations is needed to predict the shelf-life of the final products. The studies on the interaction between the drug and the excipients may be carried out by means of accelerated stability tests followed by analytical determination of the active principle (HPLC and other methods) and by means of the differential scanning calorimetry (DSC). This research has been focused to the acetyl salicylic acid (ASA) physical-chemical characterisation by using DSC method in order to evaluate its compatibility with some of the most used excipients. It was possible to show, with the DSC method, the incompatibility of magnesium stearate with ASA; the HPLC data confirm the reduction of ASA concentration in the presence of magnesium stearate. With the other excipients the characteristic endotherms of the drug were always present and no or little degradation was observed with the accelerated stability tests. Therefore, the results with the DSC method are comparable and in good agreement with the results obtained with other methods.

Investigation of Phase Mixing in Amorphous Solid Dispersions of AMG 517 in HPMC-AS Using DSC, Solid-State NMR, and Solution Calorimetry.

PubMed

Calahan, Julie L; Azali, Stephanie C; Munson, Eric J; Nagapudi, Karthik

2015-11-02

Intimate phase mixing between the drug and the polymer is considered a prerequisite to achieve good physical stability for amorphous solid dispersions. In this article, spray dried amorphous dispersions (ASDs) of AMG 517 and HPMC-as were studied by differential scanning calorimetry (DSC), solid-state NMR (SSNMR), and solution calorimetry. DSC analysis showed a weakly asymmetric (ΔTg ≈ 13.5) system with a single glass transition for blends of different compositions indicating phase mixing. The Tg-composition data was modeled using the BKCV equation to accommodate the observed negative deviation from ideality. Proton spin-lattice relaxation times in the laboratory and rotating frames ((1)H T1 and T1ρ), as measured by SSNMR, were consistent with the observation that the components of the dispersion were in intimate contact over a 10-20 nm length scale. Based on the heat of mixing calculated from solution calorimetry and the entropy of mixing calculated from the Flory-Huggins theory, the free energy of mixing was calculated. The free energy of mixing was found to be positive for all ASDs, indicating that the drug and polymer are thermodynamically predisposed to phase separation at 25 °C. This suggests that miscibility measured by DSC and SSNMR is achieved kinetically as the result of intimate mixing between drug and polymer during the spray drying process. This kinetic phase mixing is responsible for the physical stability of the ASD.

Elemental composition and structural characteristics of as-received TriTaniumTM orthodontic archwire

NASA Astrophysics Data System (ADS)

Ilievska, I.; Petrov, V.; Mihailov, V.; Karatodorov, S.; Andreeva, L.; Zaleski, A.; Mikli, V.; Gueorgieva, M.; Petrova, V.; Stoyanova-Ivanova, A.

2018-03-01

Orthodontic archwires are among the most important devices of fixed orthodontic therapy. Many types of archwires are made available on the market by various manufacturers with different elemental composition and structural characteristics. Knowing this information is important when choosing a suitable archwire for a particular stage of orthodontic treatment. The aim of our study is to characterize a new type orthodontic archwires (TriTaniumTM, American Orthodontics) before their placement in the oral cavity. To achieve the aim, we used modern methods for determining their elemental composition and structural characteristics: laser-induced plasma spectroscopy (LIBS), X-ray diffraction analysis (XRD), scanning electronic microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and differential scanning calorimetry (DSC). The results obtained from the qualitative elemental analysis by LIBS and the quantitative elemental analysis by EDX showed that Ni and Ti are the main elements in the archwire studied. The room-temperature XRD patterns showed peaks typical for a Ni-Ti alloy with an austenite-type structure. Monitoring the phase transitions by means of DSC measurements in the temperature range from –50 °C to +50 °C, we showed that in TriTaniumTM archwires, besides the austenite to martensite transition, there exists a rhombohedral intermediate phase (R phase). This study will be useful in assisting orthodontists in applying appropriate nickel-titanium orthodontic archwires in the clinical practice.

Differential Scanning Calorimetry Techniques: Applications in Biology and Nanoscience

PubMed Central

Gill, Pooria; Moghadam, Tahereh Tohidi; Ranjbar, Bijan

2010-01-01

This paper reviews the best-known differential scanning calorimetries (DSCs), such as conventional DSC, microelectromechanical systems-DSC, infrared-heated DSC, modulated-temperature DSC, gas flow-modulated DSC, parallel-nano DSC, pressure perturbation calorimetry, self-reference DSC, and high-performance DSC. Also, we describe here the most extensive applications of DSC in biology and nanoscience. PMID:21119929

Multivariate analysis of DSC-XRD simultaneous measurement data: a study of multistage crystalline structure changes in a linear poly(ethylene imine) thin film.

PubMed

Kakuda, Hiroyuki; Okada, Tetsuo; Otsuka, Makoto; Katsumoto, Yukiteru; Hasegawa, Takeshi

2009-01-01

A multivariate analytical technique has been applied to the analysis of simultaneous measurement data from differential scanning calorimetry (DSC) and X-ray diffraction (XRD) in order to study thermal changes in crystalline structure of a linear poly(ethylene imine) (LPEI) film. A large number of XRD patterns generated from the simultaneous measurements were subjected to an augmented alternative least-squares (ALS) regression analysis, and the XRD patterns were readily decomposed into chemically independent XRD patterns and their thermal profiles were also obtained at the same time. The decomposed XRD patterns and the profiles were useful in discussing the minute peaks in the DSC. The analytical results revealed the following changes of polymorphisms in detail: An LPEI film prepared by casting an aqueous solution was composed of sesquihydrate and hemihydrate crystals. The sesquihydrate one was lost at an early stage of heating, and the film changed into an amorphous state. Once the sesquihydrate was lost by heating, it was not recovered even when it was cooled back to room temperature. When the sample was heated again, structural changes were found between the hemihydrate and the amorphous components. In this manner, the simultaneous DSC-XRD measurements combined with ALS analysis proved to be powerful for obtaining a better understanding of the thermally induced changes of the crystalline structure in a polymer film.

Increase of dielectric constant in PVDF by incorporating La{sub 1.8}Sr{sub 0.2}NiO{sub 4} into its matrix

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Rajnish, E-mail: rajnish@iitp.ac.in; Goswami, Ashwin M., E-mail: ashwin.nanoplast@gmail.com; Kar, Manoranjan, E-mail: mano-iitg@yahoo.com

2016-05-06

To obtain the material with high dielectric constant and high dielectric strength for the technological applications, nanocomposite of Lanthanum Strontium Nickelete (La{sub 1.8}Sr{sub 0.2}NiO{sub 4}) as nanofiller and polyvinylidene fluoride (PVDF) as polymer matrix has been prepared. The different nanofiler weight concentration varies from 2-8 weight percent. X-ray diffraction technique confirms the phase formation of nanocomposite. Differential scanning calorimeter (DSC) has been employed to study the percentage of crystallinity and Impedance measurement has been carried out to study the dielectric constant. DSC analysis shows decreasing trend of crystallinity whereas impedance analysis gives increasing dielectric constant with increasing La{sub 1.8}Sr{sub 0.2}NiO{submore » 4} concentration in the nanocomposite. Also, these materials can be used as insulator in the transformer as the strength and dielectric behavior of present composite meets the technological requirements.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Keeratitham, Waralee, E-mail: waralee.ke@student.chula.ac.th; Somwangthanaroj, Anongnat, E-mail: anongnat.s@chula.ac.th

Herein, our main objective is to prepare the fast curing epoxy system with high glass transition temperature (T{sub g}) by incorporating the multifunctional epoxy resin into the mixture of diglycidyl ether of bisphenol A (DGEBA) as a major epoxy component and aromatic diamine as a hardener. Furthermore, the curing behavior as well as thermal and thermomechanical properties were investigated by differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and thermomechanical analysis (TMA). It was found that T{sub g} obtained from tan δ of DGEBA/aromatic diamine system increased from 100 °C to 205 °C with the presence of 30 percentage bymore » weight of multifunctional epoxy resin. Additionally, the isothermal DSC results showed that the multifunctional epoxy resin can accelerate the curing reaction of DGEBA/aromatic diamine system. Namely, a high degree of curing (∼90%) was achieved after a few minutes of curing at low temperature of 130 °C, owing to a large number of epoxy ring of multifunctional epoxy resin towards the active hydrogen atoms of aromatic diamine.« less

Synthesis and characterization of cassava starch with maleic acid derivatives by etherification reaction.

PubMed

Clasen, Samuel H; Müller, Carmen M O; Parize, Alexandre L; Pires, Alfredo T N

2018-01-15

Cassava starch was grafted with three different esters by the etherification reaction and its modification was characterized by 1 H NMR, FTIR, DSC, SEM, XDR, contact angle and SLS. The samples grafted with diethyl maleate, dipropyl maleate, and dibutyl maleate showed DS values of 2.3, 1.0 and 2.0, respectively, determined from 1 H NMR analysis and confirmed by FTIR analysis, with the appearance of bands at 1721, 1550 and 1126cm -1 . The FTIR, XRD, SEM and DSC results indicated a change in the intra and intermolecular hydrogen interactions in the grafted starch when compared to native starch. Based on the contact angles, it was observed that the macromolecular starch chain acquired hydrophobic characteristics through the substitution of the hydrogens with di maleate esters. The characteristics acquired by grafted starch allow it to be used for the encapsulation of bioactive molecules for the production of bioactive packages and the production of biodegradable packages. Copyright © 2017 Elsevier Ltd. All rights reserved.

Computational modeling of latent-heat-storage in PCM modified interior plaster

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fořt, Jan; Maděra, Jiří; Trník, Anton

2016-06-08

The latent heat storage systems represent a promising way for decrease of buildings energy consumption with respect to the sustainable development principles of building industry. The presented paper is focused on the evaluation of the effect of PCM incorporation on thermal performance of cement-lime plasters. For basic characterization of the developed materials, matrix density, bulk density, and total open porosity are measured. Thermal conductivity is accessed by transient impulse method. DSC analysis is used for the identification of phase change temperature during the heating and cooling process. Using DSC data, the temperature dependent specific heat capacity is calculated. On themore » basis of the experiments performed, the supposed improvement of the energy efficiency of characteristic building envelope system where the designed plasters are likely to be used is evaluated by a computational analysis. Obtained experimental and computational results show a potential of PCM modified plasters for improvement of thermal stability of buildings and moderation of interior climate.« less

Synthesis and interaction of sterol-uridine conjugate with DMPC liposomes studied by differential scanning calorimetry.

PubMed

Escobar, Jhon Fernando Berrío; Restrepo, Manuel Humberto Pastrana; Fernández, Diana Margarita Márquez; Martínez, Alejandro Martínez; Giordani, Cristiano; Castelli, Francesco; Sarpietro, Maria Grazia

2018-06-01

Differential scanning calorimetry (DSC) is a thermoanalytical technique which provides information on the interaction between drugs and models of cell membranes. Studies on the calorimetric behavior of hydrated phospholipids within liposomes are employed to shed light on the changes in the physico-chemical properties when interacting with drugs. In this report, new potential anti-cancer drugs such as uridine and uridine derivatives (acetonide and its succinate), 3β-5α,8α-endoperoxide-cholestan-6-en-3-ol (5,8-epidioxicholesterol) and conjugate (uridine acetonide-epidioxicholesterol succinate) have been synthesized. Steglich esterification method using coupling agents allowed to obtain the uridine acetonide-sterol conjugate. The study on the interaction between the drugs and dimiristoyl-phophatidilcholine (DMPC) liposomes has been conducted by the use of DSC. The analysis of the DSC curves indicated that the uridine and derivatives (acetonide and its succinate) present a very soft interaction with the DMPC liposomes, whereas the 5,8-epidioxicholesterol and the conjugate showed a strong effect on the thermotropic behavior. Our results suggested that the lipophilic character of uridine acetonide-sterol conjugate improves the affinity with the DMPC liposomes. Copyright © 2018 Elsevier B.V. All rights reserved.

Microstructural characterisation of Al-Si cast alloys containing rare earth additions

NASA Astrophysics Data System (ADS)

Elgallad, E. M.; Ibrahim, M. F.; Doty, H. W.; Samuel, F. H.

2018-05-01

This paper presents a thorough study on the effect of rare earth elements, specifically La and Ce, on the microstructure characteristics of non-modified and Sr-modified A356 and A413 alloys. Several alloys were prepared by adding 1% La and 1% Ce either individually or in combination. Microstructural characterisation was carried out using optical microscopy, scanning electron microscopy and electron probe microanalysis as well as differential scanning calorimetry (DSC) analysis. The results showed that the individual and combined additions of La and Ce did not bring about any modification or even refinement in the eutectic Si structure. Moreover, these additions were found to negate the modification effect of Sr, particularly in the presence of La. The A356 and A413 alloys containing La and/or Ce displayed high phase volume fractions owing to the formation of Al-Si-La/Ce/(La,Ce) and Al-Ti-La/Ce intermetallic phases. DSC analysis revealed that the formation temperatures of these phases varied from 560 to 568 °C and 568 to 574 °C, respectively. This analysis also showed that the addition of La and Ce whether individually or in combination resulted in a depression in the eutectic temperature and a considerable increase in the solidification range, particularly for the A413 alloy.

Effect of egg freshness on texture and baking characteristics of batter systems formulated using egg, flour and sugar.

PubMed

Xing, Liting; Niu, Fuge; Su, Yujie; Yang, Yanjun

2016-04-01

The aim of this work was to evaluate the effects of egg freshness on baking properties and final qualities in batter systems. Batters were made with eggs of different freshness, and the properties of batter systems were studied through rheological analysis, rapid viscosity analysis (RVA), differential scanning calorimetry (DSC), batter density and expansion rate during the baking and cooling processes. Moreover, the qualities of final baked systems were investigated, including specific volume and texture profile analysis (TPA). The flow behavior of batters showed that the consistency index (K) decreased as the Haugh unit (HU) value decreased, while the flow behavior index (n) increased. Both the storage modulus (G') and loss modulus (G″) determined by mechanical spectra at 20 °C decreased with decreasing HU. RVA and DSC determinations revealed that lower-HU samples had a lower viscosity in the baking process and a shorter time for starch gelatinization and egg protein denaturation. Observation of the batter density revealed an increasing change, which was reflected by a decrease in the specific volume of final models. TPA showed significant differences in hardness and chewiness, but no significant differences in springiness and cohesiveness were found. The egg freshness affected the properties of batter systems. © 2015 Society of Chemical Industry.

Thermal and dynamic mechanical properties of hydroxypropyl cellulose films

Treesearch

Timothy G. Rials; Wolfgang G. Glasser

1988-01-01

Differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were used to characterize the morphology of slovent cast hydroxypropyl cellulose (HPC) films. DSC results were indicative of a semicrystalline material with a melt of 220°C and a glass transition at 19°C (T1), although an additional event was suggested by a...

Synthesis, crystal structure and catalytic effect on thermal decomposition of RDX and AP: An energetic coordination polymer [Pb{sub 2}(C{sub 5}H{sub 3}N{sub 5}O{sub 5}){sub 2}(NMP)·NMP]{sub n}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Jin-jian; Yancheng Teachers College, Yancheng 224002; Liu, Zu-Liang, E-mail: liuzl@mail.njust.edu.cn

2013-04-15

An energetic lead(II) coordination polymer based on the ligand ANPyO has been synthesized and its crystal structure has been got. The polymer was characterized by FT-IR spectroscopy, elemental analysis, DSC and TG-DTG technologies. Thermal analysis shows that there are one endothermic process and two exothermic decomposition stages in the temperature range of 50–600 °C with final residues 57.09%. The non-isothermal kinetic has also been studied on the main exothermic decomposition using the Kissinger's and Ozawa–Doyle's methods, the apparent activation energy is calculated as 195.2 KJ/mol. Furthermore, DSC measurements show that the polymer has significant catalytic effect on the thermal decompositionmore » of ammonium perchlorate. - Graphical abstract: An energetic lead(II) coordination polymer of ANPyO has been synthesized, structurally characterized and properties tested. Highlights: ► We have synthesized and characterized an energetic lead(II) coordination polymer. ► We have measured its molecular structure and thermal decomposition. ► It has significant catalytic effect on thermal decomposition of AP.« less

Template occluded SBA-15: An effective dissolution enhancer for poorly water-soluble drug

NASA Astrophysics Data System (ADS)

Tingming, Fu; Liwei, Guo; Kang, Le; Tianyao, Wang; Jin, Lu

2010-09-01

The aim of the present work was to improve the dissolution rate of piroxicam by inclusion into template occluded SBA-15. Our strategy involves directly introducing piroxicam into as-prepared SBA-15 occluded with P123 (EO 20PO 70EO 20) by self assembling method in acetonitrile/methylene chloride mixture solution. Ultraviolet spectrometry experiment and thermogravimetric analysis-differential scanning calorimetry (TG-DSC) profiles show that the piroxicam and P123 contents in the inclusion compound are 12 wt% and 28 wt%, respectively. X-ray powder diffraction and DSC analysis reveal that the included piroxicam is arranged in amorphous form. N 2 adsorption-desorption experiment indicates that the piroxicam has been introduced to the mesopores instead of precipitating at the outside of the silica material. The inclusion compound was submitted to in vitro dissolution tests, the results show that the piroxicam dissolve from template occluded inclusion compound more rapidly, than these from the piroxicam crystalline and template removed samples in all tested conditions. Thus a facile method to improve the dissolution rate of poorly water-soluble drug was established, and this discovery opens a new avenue for the utilization of templates used for the synthesis of mesoporous materials.

Separator Membrane from Crosslinked Poly(Vinyl Alcohol) and Poly(Methyl Vinyl Ether-alt-Maleic Anhydride)

PubMed Central

Rohatgi, Charu Vashisth; Dutta, Naba K.; Choudhury, Namita Roy

2015-01-01

In this work, we report separator membranes from crosslinking of two polymers, such as poly vinyl alcohol (PVA) with an ionic polymer poly(methyl vinyl ether-alt-maleic anhydride) (PMVE-MA). Such interpolymer-networked systems were extensively used for biomedical and desalination applications but they were not examined for their potential use as membranes or separators for batteries. Therefore, the chemical interactions between these two polymers and the influence of such crosslinking on physicochemical properties of the membrane are systematically investigated through rheology and by critical gel point study. The hydrogen bonding and the chemical interaction between PMVE-MA and PVA resulted in highly cross-linked membranes. Effect of the molecular weight of PVA on the membrane properties was also examined. The developed membranes were extensively characterized by studying their physicochemical properties (water uptake, swelling ratio, and conductivity), thermal and electrochemical properties using differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), thermo-gravimetric analysis (TGA) and electrochemical impedance spectroscopy (EIS). The DSC study shows the presence of a single Tg in the membranes indicating compatibility of the two polymers in flexible and transparent films. The membranes show good stability and ion conductivity suitable for separator applications. PMID:28347019

Thermal behavior of gamma-irradiated low-density polyethylene/paraffin wax blend

NASA Astrophysics Data System (ADS)

Abdou, Saleh M.; Elnahas, H. H.; El-Zahed, H.; Abdeldaym, A.

2016-05-01

The thermal properties of low-density polyethylene (LDPE)/paraffin wax blends were studied using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and melt flow index (MFI). Blends of LDPE/wax in ratios of 100/0, 98/2, 96/4, 94/6, 92/8, 90/10 and 85/15 (w/w) were prepared by melt-mixing at the temperature of 150°C. It was found that increasing the wax content more than 15% leads to phase separation. DSC results showed that for all blends both the melting temperature (Tm) and the melting enthalpy (ΔHm) decrease linearly with an increase in wax content. TGA analysis showed that the thermal stability of all blends decreases linearly with increasing wax content. No clear correlation was observed between the melting point and thermal stability. Horowitz and Metzger method was used to determine the thermal activation energy (Ea). MFI increased exponentially by increasing the wax content. The effect of gamma irradiation on the thermal behavior of the blends was also investigated at different gamma irradiation doses. Significant correlations were found between the thermal parameters (Tm, ΔHm, T5%, Ea and MFI) and the amount of wax content and gamma irradiation.

Study of the Thermal Polymerization of Linseed and Passion Fruit Oils

NASA Astrophysics Data System (ADS)

Lopes, R. V. V.; Loureiro, N. P. D.; Fonseca, P. S.; Macedo, J. L.; Santos, M. L.; Sales, M. J.

2008-08-01

Researches involving ecofriendliness materials are growing up, as well as, a current interest in developing materials from inexpensive and renewable resources. Vegetable oils show a number of excellent properties, which could be utilized to produce valuable polymeric materials. In this work is described the synthesis of polymeric materials from linseed oil (Linum usitatissimum L.) and passion fruit oil (Passiflora edulis) and their characterization by thermogravimetry (TG), differential scanning calorimetry (DSC) and Raman spectroscopy. The TG curve shows that those polymeric materials present two stages of decomposition. DSC plots of the vegetable oils showed some endothermic and exothermic transitions which are not present in the DSC curves corresponding to oil-based polymers. The Raman spectra of the polymers indicate declining of absorbance in the region of C = C stretching (˜1600 cm-1). This absorption was used to estimate the degree of polymerization (79% and 67.5% for linseed and passion fruit oils, respectively)

Chain length effect on the structure and stability of antimicrobial peptides of the (RW)n series.

PubMed

Phambu, Nsoki; Almarwani, Bashiyar; Garcia, Arlette M; Hamza, Nafisa S; Muhsen, Amira; Baidoo, Jacqueline E; Sunda-Meya, Anderson

2017-08-01

Three peptides containing (RW) n -NH 2 units (where n=4, 6, and 8) have been chosen to study the effect of the chain length on the structure and stability of the peptide using Fourier transform infrared (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) techniques. Their interactions with Escherichia coli (E. coli) membrane mimetic vesicles are discussed. Infrared results indicate that addition of (RW) n -NH 2 units increases intermolecular H bonds with antiparallel orientation. TGA and DSC results reveal that (RW) 6 -NH 2 shows the optimal chain length in terms of stability and all three peptides show a preferential interaction with one of the anionic lipids in E. coli membranes. SEM images of (RW) 4 -NH 2 present large aggregates while those of (RW) 6 -NH 2 and (RW) 8 -NH 2 present layers of sheet-like structure. In the presence of model membranes, (RW) n -NH 2 show fibrillar peptide superstructures. This study suggests that repeating structures of (RW) n -NH 2 promotes lateral assembly. Copyright © 2017 Elsevier B.V. All rights reserved.

Physical-chemical properties of nanocomposites based on poly(3-hydroxybutyrate-co-3-hydroxyvalerate) and titanium dioxide nanoparticles

NASA Astrophysics Data System (ADS)

Braga, Natália F.; da Silva, Ana Paula; Moraes Arantes, Tatiane; Lemes, Ana Paula; Cristovan, Fernando Henrique

2018-01-01

Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) was reinforced with titanium dioxide (TiO2) in concentrations of 1.0%, 2.5% and 5.0% (m/m) to produce nanocomposites by the solvent casting technique. TiO2 was synthesized by a hydrothermal treatment to produce nanoparticles. The nanostructure of the nanoparticles was studied by x-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The XRD confirmed TiO2 crystalline nanoparticles, with a mixture of anatase and rutile phases. Through TEM analysis, the formation of TiO2 nanorod agglomerates with an average diameter and length of 40 and 12 nm, respectively, was observed. The thermal and mechanical properties of the pure PHBV and nanocomposite films were characterized by differential scanning calorimetry (DSC) and dynamic mechanical analysis. The DSC analysis showed that the glass transition temperature decreased with the inclusion of TiO2 in the PHBV matrix in relation to pure PHBV. The results of biodegradation assays for the PHBV and nanocomposites in an aqueous medium and in soil showed morphological and structural changes for all samples, indicating a high biodegradation rate for this material. The most important conclusion is that the biodegradation of the PHBV was not affected by the addition of nanoparticles, thus enabling the use of nanocomposites in applications requiring biodegradable materials.

Use of thermal analysis techniques (TG-DSC) for the characterization of diverse organic municipal waste streams to predict biological stability prior to land application.

PubMed

Fernández, José M; Plaza, César; Polo, Alfredo; Plante, Alain F

2012-01-01

The use of organic municipal wastes as soil amendments is an increasing practice that can divert significant amounts of waste from landfill, and provides a potential source of nutrients and organic matter to ameliorate degraded soils. Due to the high heterogeneity of organic municipal waste streams, it is difficult to rapidly and cost-effectively establish their suitability as soil amendments using a single method. Thermal analysis has been proposed as an evolving technique to assess the stability and composition of the organic matter present in these wastes. In this study, three different organic municipal waste streams (i.e., a municipal waste compost (MC), a composted sewage sludge (CS) and a thermally dried sewage sludge (TS)) were characterized using conventional and thermal methods. The conventional methods used to test organic matter stability included laboratory incubation with measurement of respired C, and spectroscopic methods to characterize chemical composition. Carbon mineralization was measured during a 90-day incubation, and samples before and after incubation were analyzed by chemical (elemental analysis) and spectroscopic (infrared and nuclear magnetic resonance) methods. Results were compared with those obtained by thermogravimetry (TG) and differential scanning calorimetry (DSC) techniques. Total amounts of CO(2) respired indicated that the organic matter in the TS was the least stable, while that in the CS was the most stable. This was confirmed by changes detected with the spectroscopic methods in the composition of the organic wastes due to C mineralization. Differences were especially pronounced for TS, which showed a remarkable loss of aliphatic and proteinaceous compounds during the incubation process. TG, and especially DSC analysis, clearly reflected these differences between the three organic wastes before and after the incubation. Furthermore, the calculated energy density, which represents the energy available per unit of organic matter, showed a strong correlation with cumulative respiration. Results obtained support the hypothesis of a potential link between the thermal and biological stability of the studied organic materials, and consequently the ability of thermal analysis to characterize the maturity of municipal organic wastes and composts. Copyright © 2011 Elsevier Ltd. All rights reserved.

Melting temperature and enthalpy variations of phase change materials (PCMs): a differential scanning calorimetry (DSC) analysis

NASA Astrophysics Data System (ADS)

Sun, Xiaoqin; Lee, Kyoung Ok; Medina, Mario A.; Chu, Youhong; Li, Chuanchang

2018-06-01

Differential scanning calorimetry (DSC) analysis is a standard thermal analysis technique used to determine the phase transition temperature, enthalpy, heat of fusion, specific heat and activation energy of phase change materials (PCMs). To determine the appropriate heating rate and sample mass, various DSC measurements were carried out using two kinds of PCMs, namely N-octadecane paraffin and calcium chloride hexahydrate. The variations in phase transition temperature, enthalpy, heat of fusion, specific heat and activation energy were observed within applicable heating rates and sample masses. It was found that the phase transition temperature range increased with increasing heating rate and sample mass; while the heat of fusion varied without any established pattern. The specific heat decreased with the increase of heating rate and sample mass. For accuracy purpose, it is recommended that for PCMs with high thermal conductivity (e.g. hydrated salt) the focus will be on heating rate rather than sample mass.

Probing the heat sources during thermal runaway process by thermal analysis of different battery chemistries

NASA Astrophysics Data System (ADS)

Zheng, Siqi; Wang, Li; Feng, Xuning; He, Xiangming

2018-02-01

Safety issue is very important for the lithium ion battery used in electric vehicle or other applications. This paper probes the heat sources in the thermal runaway processes of lithium ion batteries composed of different chemistries using accelerating rate calorimetry (ARC) and differential scanning calorimetry (DSC). The adiabatic thermal runaway features for the 4 types of commercial lithium ion batteries are tested using ARC, whereas the reaction characteristics of the component materials, including the cathode, the anode and the separator, inside the 4 types of batteries are measured using DSC. The peaks and valleys of the critical component reactions measured by DSC can match the fluctuations in the temperature rise rate measured by ARC, therefore the relevance between the DSC curves and the ARC curves is utilized to probe the heat source in the thermal runaway process and reveal the thermal runaway mechanisms. The results and analysis indicate that internal short circuit is not the only way to thermal runaway, but can lead to extra electrical heat, which is comparable with the heat released by chemical reactions. The analytical approach of the thermal runaway mechanisms in this paper can guide the safety design of commercial lithium ion batteries.

Multispectral Image Compression Based on DSC Combined with CCSDS-IDC

PubMed Central

Li, Jin; Xing, Fei; Sun, Ting; You, Zheng

2014-01-01

Remote sensing multispectral image compression encoder requires low complexity, high robust, and high performance because it usually works on the satellite where the resources, such as power, memory, and processing capacity, are limited. For multispectral images, the compression algorithms based on 3D transform (like 3D DWT, 3D DCT) are too complex to be implemented in space mission. In this paper, we proposed a compression algorithm based on distributed source coding (DSC) combined with image data compression (IDC) approach recommended by CCSDS for multispectral images, which has low complexity, high robust, and high performance. First, each band is sparsely represented by DWT to obtain wavelet coefficients. Then, the wavelet coefficients are encoded by bit plane encoder (BPE). Finally, the BPE is merged to the DSC strategy of Slepian-Wolf (SW) based on QC-LDPC by deep coupling way to remove the residual redundancy between the adjacent bands. A series of multispectral images is used to test our algorithm. Experimental results show that the proposed DSC combined with the CCSDS-IDC (DSC-CCSDS)-based algorithm has better compression performance than the traditional compression approaches. PMID:25110741

Multispectral image compression based on DSC combined with CCSDS-IDC.

PubMed

Li, Jin; Xing, Fei; Sun, Ting; You, Zheng

2014-01-01

Remote sensing multispectral image compression encoder requires low complexity, high robust, and high performance because it usually works on the satellite where the resources, such as power, memory, and processing capacity, are limited. For multispectral images, the compression algorithms based on 3D transform (like 3D DWT, 3D DCT) are too complex to be implemented in space mission. In this paper, we proposed a compression algorithm based on distributed source coding (DSC) combined with image data compression (IDC) approach recommended by CCSDS for multispectral images, which has low complexity, high robust, and high performance. First, each band is sparsely represented by DWT to obtain wavelet coefficients. Then, the wavelet coefficients are encoded by bit plane encoder (BPE). Finally, the BPE is merged to the DSC strategy of Slepian-Wolf (SW) based on QC-LDPC by deep coupling way to remove the residual redundancy between the adjacent bands. A series of multispectral images is used to test our algorithm. Experimental results show that the proposed DSC combined with the CCSDS-IDC (DSC-CCSDS)-based algorithm has better compression performance than the traditional compression approaches.

Measuring the glass transition temperature of EPDM roofing materials: Comparison of DMA, TMA, and DSC techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Paroli, R.M.; Penn, J.

1994-09-01

Two ethylene-propylene-diene monomer (EPDM) roofing membranes were aged at 100 C for 7 and 28 days. The T{sub g} of these membranes was then determined by dynamic mechanical analysis (DMA), thermomechanical analysis (TMA), and differential scanning calorimetry (DSC) and the results compared. It was found that: (1) T{sub g} data can be obtained easily using the DMA and TMA techniques. The DSC method requires greater care due to the broad step change in the baseline which is associated with heavily plasticized materials. (2) The closest correspondence between techniques was for TMA and DSC (half-height). The latter, within experimental error, yieldedmore » the same glass transition temperature before and after heat-aging. (3) The peak maxima associated with tan{delta} and E{double_prime} measurements should be cited with T{sub g} values as significant differences can exist. (4) The T{sub g}(E{double_prime}) values were closer to the T{sub g}(TMA) and T{sub g}(DSC) data than were the T{sub g}(tan{delta}) values. Data obtained at 1 Hz (or possibly less) should be used when making comparisons based on various techniques. An assessment of T{sub g} values indicated that EPDM 112 roofing membrane is more stable than the EPDM 111 membrane. The T{sub g} for EPDM 112 did not change significantly with heat-aging for 28 days at 130 C.« less

High-Speed Digital Scan Converter for High-Frequency Ultrasound Sector Scanners

PubMed Central

Chang, Jin Ho; Yen, Jesse T.; Shung, K. Kirk

2008-01-01

This paper presents a high-speed digital scan converter (DSC) capable of providing more than 400 images per second, which is necessary to examine the activities of the mouse heart whose rate is 5–10 beats per second. To achieve the desired high-speed performance in cost-effective manner, the DSC developed adopts a linear interpolation algorithm in which two nearest samples to each object pixel of a monitor are selected and only angular interpolation is performed. Through computer simulation with the Field II program, its accuracy was investigated by comparing it to that of bilinear interpolation known as the best algorithm in terms of accuracy and processing speed. The simulation results show that the linear interpolation algorithm is capable of providing an acceptable image quality, which means that the difference of the root mean square error (RMSE) values of the linear and bilinear interpolation algorithms is below 1 %, if the sample rate of the envelope samples is at least four times higher than the Nyquist rate for the baseband component of echo signals. The designed DSC was implemented with a single FPGA (Stratix EP1S60F1020C6, Altera Corporation, San Jose, CA) on a DSC board that is a part of a high-speed ultrasound imaging system developed. The temporal and spatial resolutions of the implemented DSC were evaluated by examining its maximum processing time with a time stamp indicating when an image is completely formed and wire phantom testing, respectively. The experimental results show that the implemented DSC is capable of providing images at the rate of 400 images per second with negligible processing error. PMID:18430449

Selection of PLA polymers for the development of injectable prilocaine controlled release microparticles: usefulness of thermal analysis.

PubMed

Bragagni, Marco; Beneitez, Cristina; Martín, Cristina; Hernán Pérez de la Ossa, Dolores; Mura, Paola Angela; Gil-Alegre, María Esther

2013-01-30

The use of injectable local anaesthetics for the treatment of severe postoperative pain is limited by the short duration of the painkilling effect. Pre-formulation studies were carried out for the development of an injectable microparticle formulation for controlled release of prilocaine, an amino-amide type local anaesthetic suitable for intravenous, subcutaneous and intramuscular administration. To the best of our knowledge, the encapsulation of prilocaine into microparticles has not been investigated yet. Three different poly-lactic-acid (PLA) polymers were separately employed for the preparation of the microparticles. Thermal analyses by differential scanning calorimetry (DSC) were carried out for the characterization of the raw materials, to assess the drug-polymer compatibility and miscibility, to investigate the effects of the production process on the components. Empty and prilocaine loaded microparticles were prepared by double emulsion method. All formulations were fully characterized in terms of drug content, morphology, size and in vitro drug release. The preliminary value of PRL solubility in the polymer material determined by DSC was evaluated and discussed as a predictive value for encapsulation efficiency and controlled release. DSC analysis turned out to be a usefulness tool for a fast polymer selection. Microparticles prepared with PLA R202 and R203S showed desirable characteristics for subcutaneous administration and could represent two promising formulations for the development of innovative pharmacological tools in the treatment of postoperative pain. Copyright © 2012 Elsevier B.V. All rights reserved.

The Structure of Mother-Child Play: Young Children with Down Syndrome and Typically Developing Children.

ERIC Educational Resources Information Center

Roach, Mary A.; Barratt, Marguerite Stevenson; Miller, Jon F.; Leavitt, Lewis A.

1998-01-01

Compared mothers' play with infants with Down syndrome (DSC) and typically developing children (TDC) matched for mental or chronological age. Found that TDC mothers exhibited more object demonstrations with their developmentally younger children, who showed less object play. DSC mothers were more directive and supportive than mothers of younger…

Dynamic system classifier.

PubMed

Pumpe, Daniel; Greiner, Maksim; Müller, Ewald; Enßlin, Torsten A

2016-07-01

Stochastic differential equations describe well many physical, biological, and sociological systems, despite the simplification often made in their derivation. Here the usage of simple stochastic differential equations to characterize and classify complex dynamical systems is proposed within a Bayesian framework. To this end, we develop a dynamic system classifier (DSC). The DSC first abstracts training data of a system in terms of time-dependent coefficients of the descriptive stochastic differential equation. Thereby the DSC identifies unique correlation structures within the training data. For definiteness we restrict the presentation of the DSC to oscillation processes with a time-dependent frequency ω(t) and damping factor γ(t). Although real systems might be more complex, this simple oscillator captures many characteristic features. The ω and γ time lines represent the abstract system characterization and permit the construction of efficient signal classifiers. Numerical experiments show that such classifiers perform well even in the low signal-to-noise regime.

Solid state characterization of dehydroepiandrosterone.

PubMed

Chang, L C; Caira, M R; Guillory, J K

1995-10-01

Three polymorphs (forms I-III), a monohydrate (form S2), and three new solvates [4:1 hydrate (form S1), monohydrate (form S3), and methanol half-solvate (form S4)] were isolated and characterized by X-ray powder diffractometry (XRPD), IR spectroscopy, differential scanning calorimetry (DSC), hot stage microscopy, solution calorimetry, and their dissolution rates. A new polymorph, designated as form V, melting at 146.5-148 degrees C, was observed by hot stage microscopy. Our results indicate that only forms I and S4 exhibit reproducible DSC thermograms. Five of the isolated modifications undergo phase transformation on heating, and their DSC thermograms are not reproducible. Interpretation of DSC thermograms was facilitated by use of hot stage microscopy. The identification of each modification is based on XRPD patterns (except forms S3 and S4, for which the XRPD patterns are indistinguishable) and IR spectra. In the IR spectra, a significant difference was observed in the OH stretching region of all seven modifications. In a purity determination study, 5% of a contaminant modification in binary mixtures of several modifications could be detected by use of XRPD. To obtain a better understanding of the thermodynamic properties of these modifications, a series of increasing heating rates and different pan types were used in DSC. According to Burger's rule, forms I-III are monotropic polymorphs with decreasing stability in the order form I > form II > form III. The melting onsets and heats of fusion for forms I-III are 149.1 degrees C, 25.5 kJ/mol; 140.8 degrees C, 24.6 kJ/mol; and 137.8 degrees C, 24.0 kJ/mol, respectively. For form III the heat of fusion was calculated from heat of solution and DSC data. In the case of form S1 the melting point, 127.2 degrees C, was obtained by DSC using a hermetically sealed pan. The relative stabilities of the six modifications stored under high humidity conditions were predicted to be, on the basis of the heat of solution and thermal analysis data, from S2 > form S3 > form S1 > form I > form II > form III. However, the results of the dissolution rate determination were inconsistent with the heat of solution data. The stable form I shows a higher initial dissolution rate than the metastable form II and unstable form III. All modifications were converted into the stable monohydrate, form S2, during the dissolution study, suggesting that the moisture level in solid formulations should be carefully controlled.

Calorimetric analysis of fungal degraded wood

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blankenhorn, P.R.; Baldwin, R.C.; Merrill, W. Jr.

1980-01-01

Endothermic transition and gross heat of combustion of aspenwood subjected to degradation by Lenzites trabea and Polyporus versicolor were determined by using differential scanning calorimetry (DSC) and an adiabatic O bomb. Endothermic peak areas of undegraded and fungi-degraded wood differed from each other at all levels of weight loss. The regression analysis of the DSC data vs. weight loss revealed a significant relations, although not highly correlated, for P. versicolor-degraded specimens and a nonsignificant relation for L. trabea-degraded specimens; weight loss and gross heat of combustion values of degraded specimens were significantly correlated.

Solid state of CG-400549, a novel FabI inhibitor: characterization, dissolution, transformation.

PubMed

Kim, Bo-Yeon; Sohn, Young-Taek

2011-05-01

The polymorphic and pseudopolymorphic forms of CG-400549, a novel FabI inhibitor with potent in vivo activity were prepared and characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). Seven crystal forms of CG-400549, one anhydrate and six solvates, have been isolated by recrystallization and the DSC and PXRD patterns of the seven crystal forms of CG-400549 were different respectively. The dissolution patterns of these seven crystal forms of CG-400549 were studied and they showed significant differences in the dissolution rate. After storage of 1 month at 0% RH (silica gel, 20°C), 52% RH (saturated solution of Na(2)Cr(2)O(7)2H(2)O/20°C) and 95% RH (saturated solution of Na(2)HPO(4)/20°C), all crystal forms were not transformed.

Time-series modeling and prediction of global monthly absolute temperature for environmental decision making

NASA Astrophysics Data System (ADS)

Ye, Liming; Yang, Guixia; Van Ranst, Eric; Tang, Huajun

2013-03-01

A generalized, structural, time series modeling framework was developed to analyze the monthly records of absolute surface temperature, one of the most important environmental parameters, using a deterministicstochastic combined (DSC) approach. Although the development of the framework was based on the characterization of the variation patterns of a global dataset, the methodology could be applied to any monthly absolute temperature record. Deterministic processes were used to characterize the variation patterns of the global trend and the cyclic oscillations of the temperature signal, involving polynomial functions and the Fourier method, respectively, while stochastic processes were employed to account for any remaining patterns in the temperature signal, involving seasonal autoregressive integrated moving average (SARIMA) models. A prediction of the monthly global surface temperature during the second decade of the 21st century using the DSC model shows that the global temperature will likely continue to rise at twice the average rate of the past 150 years. The evaluation of prediction accuracy shows that DSC models perform systematically well against selected models of other authors, suggesting that DSC models, when coupled with other ecoenvironmental models, can be used as a supplemental tool for short-term (˜10-year) environmental planning and decision making.

Preparation and Evaluation of Multiple Nanoemulsions Containing Gadolinium (III) Chelate as a Potential Magnetic Resonance Imaging (MRI) Contrast Agent.

PubMed

Sigward, Estelle; Corvis, Yohann; Doan, Bich-Thuy; Kindsiko, Kadri; Seguin, Johanne; Scherman, Daniel; Brossard, Denis; Mignet, Nathalie; Espeau, Philippe; Crauste-Manciet, Sylvie

2015-09-01

The objective was to develop, characterize and assess the potentiality of W1/O/W2 self-emulsifying multiple nanoemulsions to enhance signal/noise ratio for Magnetic Resonance Imaging (MRI). For this purpose, a new formulation, was designed for encapsulation efficiency and stability. Various methods were used to characterize encapsulation efficiency ,in particular calorimetric methods (Differential Scanning Calorimetry (DSC), thermogravimetry analysis) and ultrafiltration. MRI in vitro relaxivities were assessed on loaded DTPA-Gd multiple nanoemulsions. Characterization of the formulation, in particular of encapsulation efficiency was a challenge due to interactions found with ultrafiltration method. Thanks to the specifically developed DSC protocol, we were able to confirm the formation of multiple nanoemulsions, differentiate loaded from unloaded nanoemulsions and measure the encapsulation efficiency which was found to be quite high with a 68% of drug loaded. Relaxivity studies showed that the self-emulsifying W/O/W nanoemulsions were positive contrast agents, exhibiting higher relaxivities than those of the DTPA-Gd solution taken as a reference. New self-emulsifying multiple nanoemulsions that were able to load satisfactory amounts of contrasting agent were successfully developed as potential MRI contrasting agents. A specific DSC protocol was needed to be developed to characterize these complex systems as it would be useful to develop these self-formation formulations.

Preparation, optimisation and characterisation of novel wound healing film dressings loaded with streptomycin and diclofenac.

PubMed

Pawar, H V; Tetteh, J; Boateng, J S

2013-02-01

Streptomycin (STP) and diclofenac (DLF) loaded film dressings were prepared by blending Polyox(®) (POL) with four hydrophilic polymers [hydroxypropylmethylcellulose (HPMC), carrageenan (CAR), sodium alginate (SA) or chitosan (CS)] using glycerol (GLY) as plasticiser. The films were characterised by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy, texture analysis (tensile and swelling characteristics) and in vitro dissolution profiles using Franz diffusion cell. SEM showed homogeneous morphology for both blank (BLK) and drug loaded (DL) films. Films prepared by blending of POL with the other polymers showed a reduction in the crystallisation of POL in descending order of SA>CS>HPMC>CAR respectively. DSC and XRD showed no crystalline peaks of STP and DLF suggesting molecular dispersion of both drugs as well as possible drug interaction with negatively charged sulphate ions present in CAR. The DL films did not show any IR bands of both drugs, confirming the DSC and XRD results. POL-CAR-BLK films showed higher tensile strength (12.32±1.40 MPa) than the POL-CAR-DL films (9.52±1.12 MPa). DL films plasticised with 25%w/w GLY revealed soft and tough (tensile strength 1.02±0.28 MPa, % elongation 1031.33±16.23) formulations. The swelling capacities of POL-CAR-BLK and POL-CAR-DL films were (733.17±25.78%) and (646.39±40.39%), increasing to (1072.71±80.30%) and (1051±86.68%) for POL-CAR-BLK-25% GLY and POL-CAR-DL-25% GLY respectively. POL-CAR-DL films showed significantly (n=3, p<0.0318) lower cumulative release of STP and DLF (52.11±1.34, 55.26±2.25) compared to POL-CAR-DL-25% GLY films (60.07±1.56, 63.39±1.92) respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Automatic segmentation of invasive breast carcinomas from dynamic contrast-enhanced MRI using time series analysis.

PubMed

Jayender, Jagadaeesan; Chikarmane, Sona; Jolesz, Ferenc A; Gombos, Eva

2014-08-01

To accurately segment invasive ductal carcinomas (IDCs) from dynamic contrast-enhanced MRI (DCE-MRI) using time series analysis based on linear dynamic system (LDS) modeling. Quantitative segmentation methods based on black-box modeling and pharmacokinetic modeling are highly dependent on imaging pulse sequence, timing of bolus injection, arterial input function, imaging noise, and fitting algorithms. We modeled the underlying dynamics of the tumor by an LDS and used the system parameters to segment the carcinoma on the DCE-MRI. Twenty-four patients with biopsy-proven IDCs were analyzed. The lesions segmented by the algorithm were compared with an expert radiologist's segmentation and the output of a commercial software, CADstream. The results are quantified in terms of the accuracy and sensitivity of detecting the lesion and the amount of overlap, measured in terms of the Dice similarity coefficient (DSC). The segmentation algorithm detected the tumor with 90% accuracy and 100% sensitivity when compared with the radiologist's segmentation and 82.1% accuracy and 100% sensitivity when compared with the CADstream output. The overlap of the algorithm output with the radiologist's segmentation and CADstream output, computed in terms of the DSC was 0.77 and 0.72, respectively. The algorithm also shows robust stability to imaging noise. Simulated imaging noise with zero mean and standard deviation equal to 25% of the base signal intensity was added to the DCE-MRI series. The amount of overlap between the tumor maps generated by the LDS-based algorithm from the noisy and original DCE-MRI was DSC = 0.95. The time-series analysis based segmentation algorithm provides high accuracy and sensitivity in delineating the regions of enhanced perfusion corresponding to tumor from DCE-MRI. © 2013 Wiley Periodicals, Inc.

Reproducibility of dynamic contrast-enhanced MRI and dynamic susceptibility contrast MRI in the study of brain gliomas: a comparison of data obtained using different commercial software.

PubMed

Conte, Gian Marco; Castellano, Antonella; Altabella, Luisa; Iadanza, Antonella; Cadioli, Marcello; Falini, Andrea; Anzalone, Nicoletta

2017-04-01

Dynamic susceptibility contrast MRI (DSC) and dynamic contrast-enhanced MRI (DCE) are useful tools in the diagnosis and follow-up of brain gliomas; nevertheless, both techniques leave the open issue of data reproducibility. We evaluated the reproducibility of data obtained using two different commercial software for perfusion maps calculation and analysis, as one of the potential sources of variability can be the software itself. DSC and DCE analyses from 20 patients with gliomas were tested for both the intrasoftware (as intraobserver and interobserver reproducibility) and the intersoftware reproducibility, as well as the impact of different postprocessing choices [vascular input function (VIF) selection and deconvolution algorithms] on the quantification of perfusion biomarkers plasma volume (Vp), volume transfer constant (K trans ) and rCBV. Data reproducibility was evaluated with the intraclass correlation coefficient (ICC) and Bland-Altman analysis. For all the biomarkers, the intra- and interobserver reproducibility resulted in almost perfect agreement in each software, whereas for the intersoftware reproducibility the value ranged from 0.311 to 0.577, suggesting fair to moderate agreement; Bland-Altman analysis showed high dispersion of data, thus confirming these findings. Comparisons of different VIF estimation methods for DCE biomarkers resulted in ICC of 0.636 for K trans and 0.662 for Vp; comparison of two deconvolution algorithms in DSC resulted in an ICC of 0.999. The use of single software ensures very good intraobserver and interobservers reproducibility. Caution should be taken when comparing data obtained using different software or different postprocessing within the same software, as reproducibility is not guaranteed anymore.

Automatic Segmentation of Invasive Breast Carcinomas from DCE-MRI using Time Series Analysis

PubMed Central

Jayender, Jagadaeesan; Chikarmane, Sona; Jolesz, Ferenc A.; Gombos, Eva

2013-01-01

Purpose Quantitative segmentation methods based on black-box modeling and pharmacokinetic modeling are highly dependent on imaging pulse sequence, timing of bolus injection, arterial input function, imaging noise and fitting algorithms. To accurately segment invasive ductal carcinomas (IDCs) from dynamic contrast enhanced MRI (DCE-MRI) using time series analysis based on linear dynamic system (LDS) modeling. Methods We modeled the underlying dynamics of the tumor by a LDS and use the system parameters to segment the carcinoma on the DCE-MRI. Twenty-four patients with biopsy-proven IDCs were analyzed. The lesions segmented by the algorithm were compared with an expert radiologist’s segmentation and the output of a commercial software, CADstream. The results are quantified in terms of the accuracy and sensitivity of detecting the lesion and the amount of overlap, measured in terms of the Dice similarity coefficient (DSC). Results The segmentation algorithm detected the tumor with 90% accuracy and 100% sensitivity when compared to the radiologist’s segmentation and 82.1% accuracy and 100% sensitivity when compared to the CADstream output. The overlap of the algorithm output with the radiologist’s segmentation and CADstream output, computed in terms of the DSC was 0.77 and 0.72 respectively. The algorithm also shows robust stability to imaging noise. Simulated imaging noise with zero mean and standard deviation equal to 25% of the base signal intensity was added to the DCE-MRI series. The amount of overlap between the tumor maps generated by the LDS-based algorithm from the noisy and original DCE-MRI was DSC=0.95. Conclusion The time-series analysis based segmentation algorithm provides high accuracy and sensitivity in delineating the regions of enhanced perfusion corresponding to tumor from DCE-MRI. PMID:24115175

Homoacetogenesis in Deep-Sea Chloroflexi, as Inferred by Single-Cell Genomics, Provides a Link to Reductive Dehalogenation in Terrestrial Dehalococcoidetes

PubMed Central

Sewell, Holly L.; Kaster, Anne-Kristin

2017-01-01

ABSTRACT The deep marine subsurface is one of the largest unexplored biospheres on Earth and is widely inhabited by members of the phylum Chloroflexi. In this report, we investigated genomes of single cells obtained from deep-sea sediments of the Peruvian Margin, which are enriched in such Chloroflexi. 16S rRNA gene sequence analysis placed two of these single-cell-derived genomes (DscP3 and Dsc4) in a clade of subphylum I Chloroflexi which were previously recovered from deep-sea sediment in the Okinawa Trough and a third (DscP2-2) as a member of the previously reported DscP2 population from Peruvian Margin site 1230. The presence of genes encoding enzymes of a complete Wood-Ljungdahl pathway, glycolysis/gluconeogenesis, a Rhodobacter nitrogen fixation (Rnf) complex, glyosyltransferases, and formate dehydrogenases in the single-cell genomes of DscP3 and Dsc4 and the presence of an NADH-dependent reduced ferredoxin:NADP oxidoreductase (Nfn) and Rnf in the genome of DscP2-2 imply a homoacetogenic lifestyle of these abundant marine Chloroflexi. We also report here the first complete pathway for anaerobic benzoate oxidation to acetyl coenzyme A (CoA) in the phylum Chloroflexi (DscP3 and Dsc4), including a class I benzoyl-CoA reductase. Of remarkable evolutionary significance, we discovered a gene encoding a formate dehydrogenase (FdnI) with reciprocal closest identity to the formate dehydrogenase-like protein (complex iron-sulfur molybdoenzyme [CISM], DET0187) of terrestrial Dehalococcoides/Dehalogenimonas spp. This formate dehydrogenase-like protein has been shown to lack formate dehydrogenase activity in Dehalococcoides/Dehalogenimonas spp. and is instead hypothesized to couple HupL hydrogenase to a reductive dehalogenase in the catabolic reductive dehalogenation pathway. This finding of a close functional homologue provides an important missing link for understanding the origin and the metabolic core of terrestrial Dehalococcoides/Dehalogenimonas spp. and of reductive dehalogenation, as well as the biology of abundant deep-sea Chloroflexi. PMID:29259088

Biomass pyrolysis and combustion integral and differential reaction heats with temperatures using thermogravimetric analysis/differential scanning calorimetry.

PubMed

Shen, Jiacheng; Igathinathane, C; Yu, Manlu; Pothula, Anand Kumar

2015-06-01

Integral reaction heats of switchgrass, big bluestem, and corn stalks were determined using thermogravimetric analysis/differential scanning calorimetry (TGA/DSC). Iso-conversion differential reaction heats using TGA/DSC pyrolysis and combustion of biomass were not available, despite reports available on heats required and released. A concept of iso-conversion differential reaction heats was used to determine the differential reaction heats of each thermal characteristics segment of these materials. Results showed that the integral reaction heats were endothermic from 30 to 700°C for pyrolysis of switchgrass and big bluestem, but they were exothermic for corn stalks prior to 587°C. However, the integral reaction heats for combustion of the materials followed an endothermic to exothermic transition. The differential reaction heats of switchgrass pyrolysis were predominantly endothermic in the fraction of mass loss (0.0536-0.975), and were exothermic for corn stalks (0.0885-0.850) and big bluestem (0.736-0.919). Study results provided better insight into biomass thermal mechanism. Published by Elsevier Ltd.

Sol-Gel transition behavior of pure iota-carrageenan in both salt-free and added salt states.

PubMed

Hossain, K S; Miyanaga, K; Maeda, H; Nemoto, N

2001-01-01

This paper describes how strongly the gelation process of iota-carrageenan is affected by addition of metallic ions from the creep and creep recovery, dynamic viscoelasticity (DVE) and DSC measurements. Creep results at T = 25 degrees C indicate that below a polymer concentration C of 3.0 wt % the salt-free system behaves as a viscous solution, and it starts to exhibit viscoelasticity as C exceeds 3.0 wt %. In the range C = 5.0-7.0 wt %, the salt-free system shows gellike behavior whereas the added salt system, measured in the low C range 1.0-2.5 wt %, showed gellike behavior at the same temperature. The sol-gel transition temperature T(c) was determined using Winter's criterion as the temperature at which both G'(omega) and G' '(omega) follow power law behavior with the same exponent n. DSC measurements reveal that salt-free and added salt systems take different types of thermal behavior within the same temperature range. The temperature T(c) is quite close to the gelation temperature T(m) determined from DSC measurement. The Eldrige-Ferry plot was performed to estimate activaton enthalpy, which shows that physical cross-links in the salt-free iota-carrageenan is not strong in comparison with those of samples which contains metal ions. We conclude from the data analysis of C dependence of the plateau modulus using the theory developed by Jones and Marques for rigid networks based on the fractal theories that addition of metallic ions gives rise to a rigid fiber like structure even at low C of iota-carrageenan in contrast to the salt-free system for which a flexible structure has been maintained at higher C.

Characterization and evaluation of 5-fluorouracil-loaded solid lipid nanoparticles prepared via a temperature-modulated solidification technique.

PubMed

Patel, Meghavi N; Lakkadwala, Sushant; Majrad, Mohamed S; Injeti, Elisha R; Gollmer, Steven M; Shah, Zahoor A; Boddu, Sai Hanuman Sagar; Nesamony, Jerry

2014-12-01

The aim of this research was to advance solid lipid nanoparticle (SLN) preparation methodology by preparing glyceryl monostearate (GMS) nanoparticles using a temperature-modulated solidification process. The technique was reproducible and prepared nanoparticles without the need of organic solvents. An anticancer agent, 5-fluorouracil (5-FU), was incorporated in the SLNs. The SLNs were characterized by particle size analysis, zeta potential analysis, differential scanning calorimetry (DSC), infrared spectroscopy, atomic force microscopy (AFM), transmission electron microscopy (TEM), drug encapsulation efficiency, in vitro drug release, and in vitro cell viability studies. Particle size of the SLN dispersion was below 100 nm, and that of redispersed lyophilizates was ~500 nm. DSC and infrared spectroscopy suggested that the degree of crystallinity did not decrease appreciably when compared to GMS. TEM and AFM images showed well-defined spherical to oval particles. The drug encapsulation efficiency was found to be approximately 46%. In vitro drug release studies showed that 80% of the encapsulated drug was released within 1 h. In vitro cell cultures were biocompatible with blank SLNs but demonstrated concentration-dependent changes in cell viability to 5-FU-loaded SLNs. The 5-FU-loaded SLNs can potentially be utilized in an anticancer drug delivery system.

[Preparation of curcumin-EC sustained-release composite particles by supercritical CO2 anti-solvent technology].

PubMed

Bai, Wei-li; Yan, Ting-yuan; Wang, Zhi-xiang; Huang, De-chun; Yan, Ting-xuan; Li, Ping

2015-01-01

Curcumin-ethyl-cellulose (EC) sustained-release composite particles were prepared by using supercritical CO2 anti-solvent technology. With drug loading and yield of inclusion complex as evaluation indexes, on the basis of single factor tests, orthogonal experimental design was used to optimize the preparation process of curcumin-EC sustained-release composite particles. The experiments such as drug loading, yield, particle size distribution, electron microscope analysis (SEM) , infrared spectrum (IR), differential scanning calorimetry (DSC) and in vitro dissolution were used to analyze the optimal process combination. The orthogonal experimental optimization process conditions were set as follows: crystallization temperature 45 degrees C, crystallization pressure 10 MPa, curcumin concentration 8 g x L(-1), solvent flow rate 0.9 mL x min(-1), and CO2 velocity 4 L x min(-1). Under the optimal conditions, the average drug loading and yield of curcumin-EC sustained-release composite particles were 33.01% and 83.97%, and the average particle size of the particles was 20.632 μm. IR and DSC analysis showed that curcumin might complex with EC. The experiments of in vitro dissolution showed that curcumin-EC composite particles had good sustained-release effect. Curcumin-EC sustained-release composite particles can be prepared by supercritical CO2 anti-solvent technology.

Physical and molecular changes during the storage of gluten-free rice and oat bread.

PubMed

Hager, Anna-Sophie; Bosmans, Geertrui M; Delcour, Jan A

2014-06-18

Gluten-free bread crumb generally firms more rapidly than regular wheat bread crumb. We here combined differential scanning calorimetry (DSC), texture analysis, and time-domain proton nuclear magnetic resonance (TD (1)H NMR) to investigate the mechanisms underlying firming of gluten-free rice and oat bread. The molecular mobility of water and biopolymers in flour/water model systems and changes thereof after heating and subsequent cooling to room temperature were investigated as a basis for underpinning the interpretation of TD (1)H NMR profiles of fresh crumb. The proton distributions of wheat and rice flour/water model systems were comparable, while that of oat flour/water samples showed less resolved peaks and an additional population at higher T2 relaxation times representing lipid protons. No significant crumb moisture loss during storage was observed for the gluten-free bread loaves. Crumb firming was mainly caused by amylopectin retrogradation and water redistribution within bread crumb. DSC, texture, and TD (1)H NMR data correlated well and showed that starch retrogradation and crumb firming are much more pronounced in rice flour bread than in oat flour bread.

Histogram analysis of T2*-based pharmacokinetic imaging in cerebral glioma grading.

PubMed

Liu, Hua-Shan; Chiang, Shih-Wei; Chung, Hsiao-Wen; Tsai, Ping-Huei; Hsu, Fei-Ting; Cho, Nai-Yu; Wang, Chao-Ying; Chou, Ming-Chung; Chen, Cheng-Yu

2018-03-01

To investigate the feasibility of histogram analysis of the T2*-based permeability parameter volume transfer constant (K trans ) for glioma grading and to explore the diagnostic performance of the histogram analysis of K trans and blood plasma volume (v p ). We recruited 31 and 11 patients with high- and low-grade gliomas, respectively. The histogram parameters of K trans and v p , derived from the first-pass pharmacokinetic modeling based on the T2* dynamic susceptibility-weighted contrast-enhanced perfusion-weighted magnetic resonance imaging (T2* DSC-PW-MRI) from the entire tumor volume, were evaluated for differentiating glioma grades. Histogram parameters of K trans and v p showed significant differences between high- and low-grade gliomas and exhibited significant correlations with tumor grades. The mean K trans derived from the T2* DSC-PW-MRI had the highest sensitivity and specificity for differentiating high-grade gliomas from low-grade gliomas compared with other histogram parameters of K trans and v p . Histogram analysis of T2*-based pharmacokinetic imaging is useful for cerebral glioma grading. The histogram parameters of the entire tumor K trans measurement can provide increased accuracy with additional information regarding microvascular permeability changes for identifying high-grade brain tumors. Copyright © 2017 Elsevier B.V. All rights reserved.

A high-resolution, regional analysis of stormwater runoff for managed aquifer recharge site assessment

NASA Astrophysics Data System (ADS)

Young, K. S.; Fisher, A. T.; Beganskas, S.; Harmon, R. E.; Teo, E. K.; Weir, W. B.; Lozano, S.

2016-12-01

Distributed Stormwater Collection-Managed Aquifer Recharge (DSC-MAR) presents a cost-effective method of aquifer replenishment by collecting runoff and infiltrating it into underlying aquifers, but its successful implementation demands thorough knowledge of the distribution and availability of hillslope runoff. We applied a surface hydrology model to analyze the dynamics of hillslope runoff at high resolution (0.1 to 1.0 km2) across the 350 km2 San Lorenzo River Basin (SLRB) watershed, northern Santa Cruz County, CA. We used a 3 m digital elevation model to create a detailed model grid, which we parameterized with high-resolution geologic, hydrologic, and land use data. To analyze hillslope runoff under a range of precipitation regimes, we developed dry, normal, and wet climate scenarios from historic daily precipitation records (1981-2014). Simulation results show high spatial variability of hillslope runoff generation as a function of differences in precipitation and soil and land use conditions, and reveal a consistent increase in the spatial and temporal variability of runoff under wetter climate scenarios. Our results suggest that there may be opportunities to develop successful DSC-MAR projects that provide benefits during all climate scenarios. In the SLRB, our results indicate that annual hillslope runoff generation achieves a target minimum of 100 acre-ft, per 100 acres of drainage area, in approximately 15% of the region during dry climate scenarios and 60% of the region during wet climate scenarios. The high spatial and temporal resolution of our simulation output enables quantification of hillslope runoff at sub-watershed scales, commensurate with the spacing and operation of DSC-MAR. This study demonstrates a viable tool for screening of potential DSC-MAR project sites and assessing project performance under a range of climate and land use scenarios.

Synthesis of plutonium trifluoride by hydro-fluorination and novel thermodynamic data for the PuF3-LiF system

NASA Astrophysics Data System (ADS)

Tosolin, A.; Souček, P.; Beneš, O.; Vigier, J.-F.; Luzzi, L.; Konings, R. J. M.

2018-05-01

PuF3 was synthetized by hydro-fluorination of PuO2 and subsequent reduction of the product by hydrogenation. The obtained PuF3 was analysed by X-Ray Diffraction (XRD) and found phase-pure. High purity was also confirmed by the melting point analysis using Differential Scanning Calorimetry (DSC). PuF3 was then used for thermodynamic assessment of the PuF3-LiF system. Phase equilibrium points and enthalpy of fusion of the eutectic composition were measured by DSC. XRD analyses of selected samples after DSC measurement confirm that after solidification from the liquid, the system returns to a mixture of LiF and PuF3.

Optimization of DSC MRI Echo Times for CBV Measurements Using Error Analysis in a Pilot Study of High-Grade Gliomas.

PubMed

Bell, L C; Does, M D; Stokes, A M; Baxter, L C; Schmainda, K M; Dueck, A C; Quarles, C C

2017-09-01

The optimal TE must be calculated to minimize the variance in CBV measurements made with DSC MR imaging. Simulations can be used to determine the influence of the TE on CBV, but they may not adequately recapitulate the in vivo heterogeneity of precontrast T2*, contrast agent kinetics, and the biophysical basis of contrast agent-induced T2* changes. The purpose of this study was to combine quantitative multiecho DSC MRI T2* time curves with error analysis in order to compute the optimal TE for a traditional single-echo acquisition. Eleven subjects with high-grade gliomas were scanned at 3T with a dual-echo DSC MR imaging sequence to quantify contrast agent-induced T2* changes in this retrospective study. Optimized TEs were calculated with propagation of error analysis for high-grade glial tumors, normal-appearing white matter, and arterial input function estimation. The optimal TE is a weighted average of the T2* values that occur as a contrast agent bolus transverses a voxel. The mean optimal TEs were 30.0 ± 7.4 ms for high-grade glial tumors, 36.3 ± 4.6 ms for normal-appearing white matter, and 11.8 ± 1.4 ms for arterial input function estimation (repeated-measures ANOVA, P < .001). Greater heterogeneity was observed in the optimal TE values for high-grade gliomas, and mean values of all 3 ROIs were statistically significant. The optimal TE for the arterial input function estimation is much shorter; this finding implies that quantitative DSC MR imaging acquisitions would benefit from multiecho acquisitions. In the case of a single-echo acquisition, the optimal TE prescribed should be 30-35 ms (without a preload) and 20-30 ms (with a standard full-dose preload). © 2017 by American Journal of Neuroradiology.

Kinetics of phase transformation in glass forming systems

NASA Technical Reports Server (NTRS)

Ray, Chandra S.

1994-01-01

The objectives of this research were to (1) develop computer models for realistic simulations of nucleation and crystal growth in glasses, which would also have the flexibility to accomodate the different variables related to sample characteristics and experimental conditions, and (2) design and perform nucleation and crystallization experiments using calorimetric measurements, such as differential scanning calorimetry (DSC) and differential thermal analysis (DTA) to verify these models. The variables related to sample characteristics mentioned in (1) above include size of the glass particles, nucleating agents, and the relative concentration of the surface and internal nuclei. A change in any of these variables changes the mode of the transformation (crystallization) kinetics. A variation in experimental conditions includes isothermal and nonisothermal DSC/DTA measurements. This research would lead to develop improved, more realistic methods for analysis of the DSC/DTA peak profiles to determine the kinetic parameters for nucleation and crystal growth as well as to assess the relative merits and demerits of the thermoanalytical models presently used to study the phase transformation in glasses.

Material Assessment of L97A1/L96A1 Grenades by Fourier Transform Infrared Spectroscopy and Thermogravimetric Analysis

DTIC Science & Technology

2010-12-01

infrared (FTIR) spectroscopy Differential scanning calorimetry ( DSC ) L97A1/L96A1 grenades Thermogravimetric analysis (TGA) 16. SECURITY CLASSIFICATION OF...Spectroscopy The FTIR scan (fig. 3) shows two baseline materials • The blue spectra represent the Nylon 6 sample • The black spectra represent Nylon 6...The black spectra represent a sample taken from the body of the older grenade body • The relative size and location of all the peaks are identical

Peptide conjugated polymeric nanoparticles as a carrier for targeted delivery of docetaxel.

PubMed

Kulhari, Hitesh; Pooja, Deep; Shrivastava, Shweta; V G M, Naidu; Sistla, Ramakrishna

2014-05-01

The aim of this research work was to develop Bombesin peptide (BBN) conjugated, docetaxel loaded nanocarrier for the treatment of breast cancer. Docetaxel loaded nanoparticles (DNP) were prepared by solvent evaporation method using sodium cholate as surfactant. BBN was conjugated to DNP surface through covalent bonding. Both DNP and BBN conjugated DNP (BDNP) were characterized by various techniques such as dynamic light scattering, Fourier transform infrared spectroscopy (FTIR), atomic force microscopy (AFM), powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC) and thermogravimetric analysis. The particle diameter and zeta potential of BDNP were 136±3.95 nm and -10.8±2.7 mV, respectively. The change in surface charge and FTIR studies confirmed the formation of amide linkage between BBN and DNP. AFM analysis showed that nanoparticles were spherical in shapes. In nanoparticles, docetaxel was present in its amorphous form as confirmed by DSC and PXRD analysis and was stable during the thermal studies. The formulations showed the sustained release of DTX over the period of 120 h. During cellular toxicity assay in gastrin releasing peptide receptor positive breast cancer cells (MDA-MB-231), BDNP were found to be 12 times more toxic than pure DTX and Taxotere. The IC50 value for DTX, Taxotere, DNP and BDNP was >375, >375, 142.23 and 35.53 ng/ml, respectively. The above studies showed that Bombesin conjugated nanocarrier system could be a promising carrier for active targeting of anticancer drugs in GRP receptor over expressing cancer cells. Copyright © 2014 Elsevier B.V. All rights reserved.

Raman scattering boson peak and differential scanning calorimetry studies of the glass transition in tellurium-zinc oxide glasses.

PubMed

Stavrou, E; Tsiantos, C; Tsopouridou, R D; Kripotou, S; Kontos, A G; Raptis, C; Capoen, B; Bouazaoui, M; Turrell, S; Khatir, S

2010-05-19

Raman scattering and differential scanning calorimetry (DSC) measurements have been carried out on four mixed tellurium-zinc oxide (TeO(2))(1 - x)(ZnO)(x) (x = 0.1, 0.2, 0.3, 0.4) glasses under variable temperature, with particular attention being given to the respective glass transition region. From the DSC measurements, the glass transition temperature T(g) has been determined for each glass, showing a monotonous decrease of T(g) with increasing ZnO content. The Raman study is focused on the low-frequency band of the glasses, the so-called boson peak (BP), whose frequency undergoes an abrupt decrease at a temperature T(d) very close to the respective T(g) values obtained by DSC. These results show that the BP is highly sensitive to dynamical effects over the glass transition and provides a means for an equally reliable (to DSC) determination of T(g) in tellurite glasses and other network glasses. The discontinuous temperature dependence of the BP frequency at the glass transition, along with the absence of such a behaviour by the high-frequency Raman bands (due to local atomic vibrations), indicates that marked changes of the medium range order (MRO) occur at T(g) and confirms the correlation between the BP and the MRO of glasses.

Activity in the superior colliculus reflects dynamic interactions between voluntary and involuntary influences on orienting behaviour.

PubMed

Bell, Andrew H; Munoz, Douglas P

2008-10-01

Performance in a behavioural task can be influenced by both bottom-up and top-down processes such as stimulus modality and prior probability. Here, we exploited differences in behavioural strategy to explore the role of the intermediate and deep layers of the superior colliculus (dSC) in covert orienting. Two monkeys were trained on a predictive cued-saccade task in which the cue predicted the target's upcoming location with 80% validity. When the delay between cue and target onset was 250 ms, both monkeys showed faster responses to the uncued (Invalid) location. This was associated with a reduced target-aligned response in the dSC on Valid trials for both monkeys and is consistent with a bottom-up (i.e. involuntary) bias. When the delay was increased to 650 ms, one monkey continued to show faster responses to the Invalid location whereas the other monkey showed faster responses to the Valid location, consistent with a top-down (i.e. voluntary) bias. This latter behaviour was correlated with an increase in activity in dSC neurons preceding target onset that was absent in the other monkey. Thus, using the information provided by the cue shifted the emphasis towards top-down processing, while ignoring this information allowed bottom-up processing to continue to dominate. Regardless of the selected strategy, however, neurons in the dSC consistently reflected the current bias between the two processes, emphasizing its role in both the bottom-up and top-down control of orienting behaviour.

SU-F-J-81: Evaluation of Automated Deformable Registration Between Planning Computed Tomography (CT) and Daily Cone Beam CT Images Over the Course of Prostate Cancer Radiotherapy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Matney, J; Hammers, J; Kaidar-Person, O

2016-06-15

Purpose: To compute daily dose delivered during radiotherapy, deformable registration needs to be relatively fast, automated, and accurate. The aim of this study was to evaluate the performance of commercial deformable registration software for deforming between two modalities: planning computed tomography (pCT) images acquired for treatment planning and cone beam (CB) CT images acquired prior to each fraction of prostate cancer radiotherapy. Methods: A workflow was designed using MIM Software™ that aligned and deformed pCT into daily CBCT images in two steps: (1) rigid shifts applied after daily CBCT imaging to align patient anatomy to the pCT and (2) normalizedmore » intensity-based deformable registration to account for interfractional anatomical variations. The physician-approved CTV and organ and risk (OAR) contours were deformed from the pCT to daily CBCT over the course of treatment. The same structures were delineated on each daily CBCT by a radiation oncologist. Dice similarity coefficient (DSC) mean and standard deviations were calculated to quantify the deformable registration quality for prostate, bladder, rectum and femoral heads. Results: To date, contour comparisons have been analyzed for 31 daily fractions of 2 of 10 of the cohort. Interim analysis shows that right and left femoral head contours demonstrate the highest agreement (DSC: 0.96±0.02) with physician contours. Additionally, deformed bladder (DSC: 0.81±0.09) and prostate (DSC: 0.80±0.07) have good agreement with physician-defined daily contours. Rectum contours have the highest variations (DSC: 0.66±0.10) between the deformed and physician-defined contours on daily CBCT imaging. Conclusion: For structures with relatively high contrast boundaries on CBCT, the MIM automated deformable registration provided accurate representations of the daily contours during treatment delivery. These findings will permit subsequent investigations to automate daily dose computation from CBCT. However, improved methods need to be investigated to improve deformable results for rectum contours.« less

Social Media Impact of the Food and Drug Administration's Drug Safety Communication Messaging About Zolpidem: Mixed-Methods Analysis

PubMed Central

Sinha, Michael S; Freifeld, Clark C; Brownstein, John S; Donneyong, Macarius M; Rausch, Paula; Lappin, Brian M; Zhou, Esther H; Dal Pan, Gerald J; Pawar, Ajinkya M; Hwang, Thomas J; Avorn, Jerry

2018-01-01

Background The Food and Drug Administration (FDA) issues drug safety communications (DSCs) to health care professionals, patients, and the public when safety issues emerge related to FDA-approved drug products. These safety messages are disseminated through social media to ensure broad uptake. Objective The objective of this study was to assess the social media dissemination of 2 DSCs released in 2013 for the sleep aid zolpidem. Methods We used the MedWatcher Social program and the DataSift historic query tool to aggregate Twitter and Facebook posts from October 1, 2012 through August 31, 2013, a period beginning approximately 3 months before the first DSC and ending 3 months after the second. Posts were categorized as (1) junk, (2) mention, and (3) adverse event (AE) based on a score between –0.2 (completely unrelated) to 1 (perfectly related). We also looked at Google Trends data and Wikipedia edits for the same time period. Google Trends search volume is scaled on a range of 0 to 100 and includes “Related queries” during the relevant time periods. An interrupted time series (ITS) analysis assessed the impact of DSCs on the counts of posts with specific mention of zolpidem-containing products. Chow tests for known structural breaks were conducted on data from Twitter, Facebook, and Google Trends. Finally, Wikipedia edits were pulled from the website’s editorial history, which lists all revisions to a given page and the editor’s identity. Results In total, 174,286 Twitter posts and 59,641 Facebook posts met entry criteria. Of those, 16.63% (28,989/174,286) of Twitter posts and 25.91% (15,453/59,641) of Facebook posts were labeled as junk and excluded. AEs and mentions represented 9.21% (16,051/174,286) and 74.16% (129,246/174,286) of Twitter posts and 5.11% (3,050/59,641) and 68.98% (41,138/59,641) of Facebook posts, respectively. Total daily counts of posts about zolpidem-containing products increased on Twitter and Facebook on the day of the first DSC; Google searches increased on the week of the first DSC. ITS analyses demonstrated variability but pointed to an increase in interest around the first DSC. Chow tests were significant (P<.0001) for both DSCs on Facebook and Twitter, but only the first DSC on Google Trends. Wikipedia edits occurred soon after each DSC release, citing news articles rather than the DSC itself and presenting content that needed subsequent revisions for accuracy. Conclusions Social media offers challenges and opportunities for dissemination of the DSC messages. The FDA could consider strategies for more actively disseminating DSC safety information through social media platforms, particularly when announcements require updating. The FDA may also benefit from directly contributing content to websites like Wikipedia that are frequently accessed for drug-related information. PMID:29305342

Detection of Collapse and Crystallization of Saccharide, Protein, and Mannitol Formulations by Optical Fibers in Lyophilization

PubMed Central

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg') as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg' and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol, and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitates online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes. PMID:29435445

Detection of Collapse and Crystallization of Saccharide, Protein and Mannitol Formulations by Optical Fibers in Lyophilization

NASA Astrophysics Data System (ADS)

Horn, Jacqueline; Friess, Wolfgang

2018-01-01

The collapse temperature (Tc) and the glass transition temperature of freeze-concentrated solutions (Tg’) as well as the crystallization behavior of excipients are important physicochemical characteristics which guide the cycle development in freeze-drying. The most frequently used methods to determine these values are differential scanning calorimetry (DSC) and freeze-drying microscopy (FDM). The objective of this study was to evaluate the optical fiber system (OFS) unit as alternative tool for the analysis of Tc, Tg’ and crystallization events. The OFS unit was also tested as a potential online monitoring tool during freeze-drying. Freeze/thawing and freeze-drying experiments of sucrose, trehalose, stachyose, mannitol and highly concentrated IgG1 and lysozyme solutions were carried out and monitored by the OFS. Comparative analyses were performed by DSC and FDM. OFS and FDM results correlated well. The crystallization behavior of mannitol could be monitored by the OFS during freeze/thawing as it can be done by DSC. Online monitoring of freeze-drying runs detected collapse of amorphous saccharide matrices. The OFS unit enabled the analysis of both Tc and crystallization processes, which is usually carried out by FDM and DSC. The OFS can hence be used as novel measuring device. Additionally, detection of these events during lyophilization facilitate online-monitoring. Thus the OFS is a new beneficial tool for the development and monitoring of freeze-drying processes.

Use of thermal analysis techniques (TG-DSC) for the characterization of diverse organic municipal waste streams to predict biological stability prior to land application

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fernandez, Jose M., E-mail: joseman@sas.upenn.edu; Plaza, Cesar; Polo, Alfredo

2012-01-15

Highlights: Black-Right-Pointing-Pointer Thermal analysis was used to assess stability and composition of organic matter in three diverse municipal waste streams. Black-Right-Pointing-Pointer Results were compared with C mineralization during 90-day incubation, FTIR and {sup 13}C NMR. Black-Right-Pointing-Pointer Thermal analysis reflected the differences between the organic wastes before and after the incubation. Black-Right-Pointing-Pointer The calculated energy density showed a strong correlation with cumulative respiration. Black-Right-Pointing-Pointer Conventional and thermal methods provide complimentary means of characterizing organic wastes. - Abstract: The use of organic municipal wastes as soil amendments is an increasing practice that can divert significant amounts of waste from landfill, and providesmore » a potential source of nutrients and organic matter to ameliorate degraded soils. Due to the high heterogeneity of organic municipal waste streams, it is difficult to rapidly and cost-effectively establish their suitability as soil amendments using a single method. Thermal analysis has been proposed as an evolving technique to assess the stability and composition of the organic matter present in these wastes. In this study, three different organic municipal waste streams (i.e., a municipal waste compost (MC), a composted sewage sludge (CS) and a thermally dried sewage sludge (TS)) were characterized using conventional and thermal methods. The conventional methods used to test organic matter stability included laboratory incubation with measurement of respired C, and spectroscopic methods to characterize chemical composition. Carbon mineralization was measured during a 90-day incubation, and samples before and after incubation were analyzed by chemical (elemental analysis) and spectroscopic (infrared and nuclear magnetic resonance) methods. Results were compared with those obtained by thermogravimetry (TG) and differential scanning calorimetry (DSC) techniques. Total amounts of CO{sub 2} respired indicated that the organic matter in the TS was the least stable, while that in the CS was the most stable. This was confirmed by changes detected with the spectroscopic methods in the composition of the organic wastes due to C mineralization. Differences were especially pronounced for TS, which showed a remarkable loss of aliphatic and proteinaceous compounds during the incubation process. TG, and especially DSC analysis, clearly reflected these differences between the three organic wastes before and after the incubation. Furthermore, the calculated energy density, which represents the energy available per unit of organic matter, showed a strong correlation with cumulative respiration. Results obtained support the hypothesis of a potential link between the thermal and biological stability of the studied organic materials, and consequently the ability of thermal analysis to characterize the maturity of municipal organic wastes and composts.« less

DSC, X-ray and FTIR studies of a gemfibrozil/dimethyl-β-cyclodextrin inclusion complex produced by co-grinding.

PubMed

Aigner, Z; Berkesi, O; Farkas, G; Szabó-Révész, P

2012-01-05

The steps of formation of an inclusion complex produced by the co-grinding of gemfibrozil and dimethyl-β-cyclodextrin were investigated by differential scanning calorimetry (DSC), X-ray powder diffractometry (XRPD) and Fourier transform infrared (FTIR) spectroscopy with curve-fitting analysis. The endothermic peak at 59.25°C reflecting the melting of gemfibrozil progressively disappeared from the DSC curves of the products on increase of the duration of co-grinding. The crystallinity of the samples too gradually decreased, and after 35min of co-grinding the product was totally amorphous. Up to this co-grinding time, XRPD and FTIR investigations indicated a linear correlation between the cyclodextrin complexation and the co-grinding time. After co-grinding for 30min, the ratio of complex formation did not increase. These studies demonstrated that co-grinding is a suitable method for the complexation of gemfibrozil with dimethyl-β-cyclodextrin. XRPD analysis revealed the amorphous state of the gemfibrozil-dimethyl-β-cyclodextrin product. FTIR spectroscopy with curve-fitting analysis may be useful as a semiquantitative analytical method for discriminating the molecular and amorphous states of gemfibrozil. Copyright © 2011 Elsevier B.V. All rights reserved.

Nitrogen-rich salts based on the energetic [monoaquabis(N,N-bis(1H-tetrazol-5-yl)amine)-zinc(II)] anion: a promising design in the development of new energetic materials.

PubMed

Li, Fugang; Bi, Yangang; Zhao, Wenyuan; Zhang, Tonglai; Zhou, Zunning; Yang, Li

2015-02-16

Nitrogen-rich energetic salts involving various cations (lithium, 1; ammonium, 2; hydrazinium, 3; hydroxylammonium, 4; guanidinium, 5; aminoguanidinium, 6; diaminoguanidinium, 7; and triaminoguanidinium, 8) based on nitrogen-rich anion [Zn(BTA)2(H2O)](2-) (N% = 65.37, BTA = N,N-bis[1H-tetrazol-5-yl]amine anion) were synthesized with a simple method. The crystal structures of all compounds except 1, 2, and 6 were determined by single-crystal X-ray diffraction and fully characterized by elemental analysis and FT-IR spectroscopy. The thermal stabilities were investigated by differential scanning calorimetry (DSC). The DSC results show that all compounds exhibit high thermal stabilities (decomposition temperature >200 °C). Additionally, the heats of formation were calculated on the basis of the experimental constant-volume energies of combustion measured by using bomb calorimetry. Lastly, the sensitivities toward impact and friction were assessed according to Bundesamt für Materialforschung (BAM) standard methods.

Kinetics of Thermal Decomposition of Ammonium Perchlorate by TG/DSC-MS-FTIR

NASA Astrophysics Data System (ADS)

Zhu, Yan-Li; Huang, Hao; Ren, Hui; Jiao, Qing-Jie

2014-01-01

The method of thermogravimetry/differential scanning calorimetry-mass spectrometry-Fourier transform infrared (TG/DSC-MS-FTIR) simultaneous analysis has been used to study thermal decomposition of ammonium perchlorate (AP). The processing of nonisothermal data at various heating rates was performed using NETZSCH Thermokinetics. The MS-FTIR spectra showed that N2O and NO2 were the main gaseous products of the thermal decomposition of AP, and there was a competition between the formation reaction of N2O and that of NO2 during the process with an iso-concentration point of N2O and NO2. The dependence of the activation energy calculated by Friedman's iso-conversional method on the degree of conversion indicated that the AP decomposition process can be divided into three stages, which are autocatalytic, low-temperature diffusion and high-temperature, stable-phase reaction. The corresponding kinetic parameters were determined by multivariate nonlinear regression and the mechanism of the AP decomposition process was proposed.

Physicochemical characterization of chitosan/nylon6/polyurethane foam chemically cross-linked ternary blends.

PubMed

Jayakumar, S; Sudha, P N

2013-03-15

Chitosan/nylon6/polyurethane foam (CS/Ny6/PUF) ternary blend was prepared and chemically cross-linked with glutaraldehyde. Structural, thermal and morphological studies were performed for the prepared ternary blends. Characterizations of the ternary blends were investigated by Fourier transform infrared spectroscopy (FTIR), thermo gravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM). The FTIR results showed that the strong intermolecular hydrogen bonds took place between CS, Ny6 and PUF. TGA and DSC studies reveal that the thermal stability of the blend is enhanced by glutaraldehyde as crosslinking agent. Results of XRD indicated that the relative crystalline of pure CS film was reduced when the polymeric network was reticulated by glutaraldehyde. Finally, the results of scanning electron microscopy (SEM) indicated that the morphology of the blend is rough and heterogeneous, further it confirms the interaction between the functional groups of the blend components. Copyright © 2012 Elsevier B.V. All rights reserved.

Enhanced Thermal Properties of Novel Latent Heat Thermal Storage Material Through Confinement of Stearic Acid in Meso-Structured Onion-Like Silica

NASA Astrophysics Data System (ADS)

Gao, Junkai; Lv, Mengjiao; Lu, Jinshu; Chen, Yan; Zhang, Zijun; Zhang, Xiongjie; Zhu, Yingying

2017-12-01

Meso-structured onion-like silica (MOS), which had a highly ordered, onion-like multilayer; large surface area and pore volume; and highly curved mesopores, were synthesized as a support for stearic acid (SA) to develop a novel shape-stabilized phase change material (SA/MOS). The characterizations of SA/MOS were studied by the analysis technique of scanning electron microscope, infrared spectroscopy, x-ray diffraction, differential scanning calorimeter (DSC), and thermal gravimetry analysis (TGA). The results showed that the interaction between the SA and the MOS was physical adsorption and that the MOS had no effect on the crystal structure of the SA. The DSC results suggested that the melting and solidifying temperature of the SA/MOS were 72.7°C and 63.9°C with a melting latent heat of 108.0 J/g and a solidifying latent heat of 126.0 J/g, respectively, and the TGA results indicated that the SA/MOS had a good thermal stability. All of the results demonstrated that the SA/MOS was a promising thermal energy storage material candidate for practical applications.

Thermal and mechanical analysis of PVA / sulfonated carbon nanotubes composite

NASA Astrophysics Data System (ADS)

Yadav, Vikrant; Sharma, Prem P.; Rajput, Abhishek; Kulshrestha, Vaibhav

2018-04-01

Nanocomposites of polyvinyl alcohol (PVA) and sulfonated carbon nanotubes (s-CNT) with enhanced properties were synthesized successfully. Effect of different amount of sulfonated nanotubes on thermal and mechanical properties of resultant nanocomposites derived from s-CNT and PVA were studied. Structural analysis for functionalization of CNT was done by using FTIR spectra. Thermal and mechanical analysis were done by using TGA, DSC and UTM. Nanocomposite containing s-CNT shows higher elastic moduli, higher melting temperature in consort with lower weight loss at same temperature, compared with pristine PVA. The novelty of this work is to use PVA/s-CNT based composites with improved thermomechanical properties in different nanotechnologies.

Effect of γ-radiation on free radicals formation, structural changes and functional properties of wheat starch.

PubMed

Atrous, Hager; Benbettaieb, Nasreddine; Hosni, Faouzi; Danthine, Sabine; Blecker, Christophe; Attia, Hamadi; Ghorbel, Dorra

2015-09-01

Wheat starch was treated by different γ-radiation doses (3, 5, 10, 20, 35 and 50 kGy). The effects of γ-radiation on structural, thermal, physicochemical, morphological and rheological properties of wheat starch were studied. The presence of free radicals after γ-radiation treatment, which number decreased with time was confirmed. Structural analysis revealed decreases in the intensities of the O-H and C-H stretches and glycosidic linkages indicating the depolymerization of amylose and probably amylopectin into shorter chain molecules, but showed that γ-radiation treatment did not affect the crystalline structure. Differential scanning calorimetric (DSC) thermograms showed the absence of significant differences in the gelatinization temperatures, as well as the corresponding transition enthalpies since the DSC parameters are related to the crystalline ordering within the granules. Apparent amylose content decreased linearly with increasing irradiation dose leading to an increase in water solubility index. An increase in the swelling power was observed after irradiation treatment until 20 kGy, followed by a rapid decrease at higher doses. Microscopic observations showed that the effect of γ-radiation was more visible on starch pastes than on starch granules. Rheological properties of the starch pastes decreased with increasing irradiation dose as a result of glycosidic bond cleavage. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural basis of host recognition and biofilm formation by Salmonella Saf pili

PubMed Central

2017-01-01

Pili are critical in host recognition, colonization and biofilm formation during bacterial infection. Here, we report the crystal structures of SafD-dsc and SafD-SafA-SafA (SafDAA-dsc) in Saf pili. Cell adherence assays show that SafD and SafA are both required for host recognition, suggesting a poly-adhesive mechanism for Saf pili. Moreover, the SafDAA-dsc structure, as well as SAXS characterization, reveals an unexpected inter-molecular oligomerization, prompting the investigation of Saf-driven self-association in biofilm formation. The bead/cell aggregation and biofilm formation assays are used to demonstrate the novel function of Saf pili. Structure-based mutants targeting the inter-molecular hydrogen bonds and complementary architecture/surfaces in SafDAA-dsc dimers significantly impaired the Saf self-association activity and biofilm formation. In summary, our results identify two novel functions of Saf pili: the poly-adhesive and self-associating activities. More importantly, Saf-Saf structures and functional characterizations help to define a pili-mediated inter-cellular oligomerizaiton mechanism for bacterial aggregation, colonization and ultimate biofilm formation. PMID:29125121

A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy

PubMed Central

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Objective: Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. Materials and Methods: The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. Results: The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70–55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 (d10), 3.025 (d50), and 6.712 (d90) μm and average surface area of 2.71 m2/g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed Tmax at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λmax), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn–Cl stretching. Conclusions: These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications. PMID:28405577

A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

PubMed

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guener, M.; Gueler, E.; Aktas, H.

Kinetic, morphological and some thermal properties of thermally induced and deformation-induced martensite were studied in a Fe-32%Ni-0.4%Cr alloy. Scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and compression deformation test techniques were used for these studies. SEM observations revealed the occurrence of both athermal and isothermal martensitic transformation kinetics for producing a lenticular martensite morphology for different homogenization conditions of the prior austenite phase. The DSC measurement results showed a fair agreement with those of previous studies on ferrous alloys.

Radiotherapy volume delineation using 18F-FDG-PET/CT modifies gross node volume in patients with oesophageal cancer.

PubMed

Jimenez-Jimenez, E; Mateos, P; Aymar, N; Roncero, R; Ortiz, I; Gimenez, M; Pardo, J; Salinas, J; Sabater, S

2018-05-02

Evidence supporting the use of 18F-FDG-PET/CT in the segmentation process of oesophageal cancer for radiotherapy planning is limited. Our aim was to compare the volumes and tumour lengths defined by fused PET/CT vs. CT simulation. Twenty-nine patients were analyzed. All patients underwent a single PET/CT simulation scan. Two separate GTVs were defined: one based on CT data alone and another based on fused PET/CT data. Volume sizes for both data sets were compared and the spatial overlap was assessed by the Dice similarity coefficient (DSC). The gross tumour volume (GTVtumour) and maximum tumour diameter were greater by PET/CT, and length of primary tumour was greater by CT, but differences were not statistically significant. However, the gross node volume (GTVnode) was significantly greater by PET/CT. The DSC analysis showed excellent agreement for GTVtumour, 0.72, but was very low for GTVnode, 0.25. Our study shows that the volume definition by PET/CT and CT data differs. CT simulation, without taking into account PET/CT information, might leave cancer-involved nodes out of the radiotherapy-delineated volumes.

Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.

Fabrication of novel GMO/Eudragit E100 nanostructures for enhancing oral bioavailability of carvedilol.

PubMed

Patil, Sharvil S; Roy, Krishtey; Choudhary, Bhavana; Mahadik, Kakasaheb R

2016-08-01

In the present work, novel nanostructures comprising of glyceryl monooleate (GMO) and Eudragit E100 were prepared using high intensity ultrasonic homogenization. 3(2) Factorial design approach was used for optimization of nanostructures. Results of regression analysis revealed that the amount of GMO and Eudragit E100 had a drastic effect on particle size and percent entrapment efficiency. Optimized carvedilol-loaded nanostructures (Car-NS) were characterized by FTIR, TEM, DSC, in vitro drug release study. Pharmacokinetic parameters such as Cmax, Tmax, Ke, Ka, Vd and AUC were estimated for Car-NS upon its oral administration in Sprague-Dawley rats. Particle size of Car-NS was found to be 183 ± 2.43 nm with an entrapment efficiency of 81.4 ± 0.512%. FTIR studies revealed loading and chemical compatibility of carvedilol with the components of nanostructures. DSC thermograms did not show endothermic peak for melting of carvedilol which could be attributed to solubilization of carvedilol in molten GMO during DSC run. The prepared Car-NS released carvedilol in sustained manner over a period of 10 h as suggested by in vitro drug release study. The pharmacokinetic study of Car-NS showed significant improvement in Cmax (two fold, p < 0.001) and AUC (four folds, p < 0.001) of carvedilol when compared to carvedilol suspension. Car-NS were found to be stable for a period of 3 months. Thus, a stable, floating, multiparticulate GMO/Eudragit E100 nanostructures having ability to release the drug in sustained manner with enhanced oral bioavailability can prove to be a promising carrier system for poorly water soluble drugs.

Cocrystal screening of hydroxybenzamides with benzoic acid derivatives: a comparative study of thermal and solution-based methods.

PubMed

Manin, Alex N; Voronin, Alexander P; Drozd, Ksenia V; Manin, Nikolay G; Bauer-Brandl, Annette; Perlovich, German L

2014-12-18

The main problem occurring at the early stages of cocrystal search is the choice of an effective screening technique. Among the most popular techniques of obtaining cocrystals are crystallization from solution, crystallization from melt and solvent-drop grinding. This paper represents a comparative analysis of the following screening techniques: DSC cocrystal screening method, thermal microscopy and saturation temperature method. The efficiency of different techniques of cocrystal screening was checked in 18 systems. Benzamide and benzoic acid derivatives were chosen as model systems due to their ability to form acid-amide supramolecular heterosynthon. The screening has confirmed the formation of 6 new cocrystals. The screening by the saturation temperature method has the highest screen-out rate but the smallest range of application. DSC screening has a satisfactory accuracy and allows screening over a short time. Thermal microscopy is most efficient as an additional technique used to interpret ambiguous DSC screening results. The study also included an analysis of the influence of solvent type and component solubility on cocrystal formation. Copyright © 2014 Elsevier B.V. All rights reserved.

Loss of Desmocollin 3 in Skin Tumor Development and Progression

PubMed Central

Chen, Jiangli; O’Shea, Charlene; Fitzpatrick, James E.; Koster, Maranke I.; Koch, Peter J.

2011-01-01

Desmocollin 3 (DSC3) is a desmosomal cadherin that is required for maintaining cell adhesion in the epidermis as demonstrated by the intra-epidermal blistering observed in Dsc3 null skin. Recently, it has been suggested that deregulated expression of DSC3 occurs in certain human tumor types. It is not clear whether DSC3 plays a role in the development or progression of cancers arising in stratified epithelia such as the epidermis. To address this issue, we generated a mouse model in which Dsc3 expression is ablated in K-Ras oncogene-induced skin tumors. Our results demonstrate that loss of Dsc3 leads to an increase in K-Ras induced skin tumors. We hypothesize that acantholysis-induced epidermal hyperplasia in the Dsc3 null epidermis facilitates Ras-induced tumor development. Further, we demonstrate that spontaneous loss of DSC3 expression is a common occurrence during human and mouse skin tumor progression. This loss occurs in tumor cells invading the dermis. Interestingly, other desmosomal proteins are still expressed in tumor cells that lack DSC3, suggesting a specific function of DSC3 loss in tumor progression. While loss of DSC3 on the skin surface leads to epidermal blistering, it does not appear to induce loss of cell-cell adhesion in tumor cells invading the dermis, most likely due to a protection of these cells within the dermis from mechanical stress. We thus hypothesize that DSC3 can contribute to the progression of tumors both by cell adhesion-dependent (skin surface) and likely by cell adhesion-independent (invading tumor cells) mechanisms. PMID:21681825

Roughness-controlled self-assembly of mannitol/LB agar microparticles by polymorphic transformation for pulmonary drug delivery.

PubMed

Zhang, Fengying; Ngoc, Nguyen Thi Quynh; Tay, Bao Hui; Mendyk, Aleksander; Shao, Yu-Hsuan; Lau, Raymond

2015-01-05

Novel roughness-controlled mannitol/LB Agar microparticles were synthesized by polymorphic transformation and self-assembly method using hexane as the polymorphic transformation reagent and spray-dried mannitol/LB Agar microparticles as the starting material. As-prepared microparticles were characterized by Fourier transform infrared spectra (FTIR), X-ray diffraction spectra (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), thermal gravimetric analysis (TGA), and Andersen Cascade Impactor (ACI). The XRD and DSC results indicate that after immersing spray-dried mannitol/LB Agar microparticles in hexane, β-mannitol was completely transformed to α-mannitol in 1 h, and all the δ-mannitol was transformed to α form after 14 days. SEM shows that during the transformation the nanobelts on the spray-dried mannitol/LB Agar microparticles become more dispersed and the contour of the individual nanobelts becomes more noticeable. Afterward, the nanobelts self-assemble to nanorods and result in rod-covered mannitol/LB Agar microparticles. FTIR indicates new hydrogen bonds were formed among mannitol, LB Agar, and hexane. SEM images coupled with image analysis software reveal that different surface morphology of the microparticles have different drug adhesion mechanisms. Comparison of ACI results and image analysis of SEM images shows that an increase in the particle surface roughness can increase the fine particle fractions (FPFs) using the rod-covered mannitol microparticles as drug carriers. Transformed microparticles show higher FPFs than commercially available lactose carriers. An FPF of 28.6 ± 2.4% was achieved by microparticles transformed from spray-dried microparticles using 2% mannitol(w/v)/LB Agar as feed solution. It is comparable to the highest FPF reported in the literature using lactose and spray-dried mannitol as carriers.

Elaboration, structural, spectroscopy, DSC investigations and Hirshfeld surface analysis of a one-dimensional self-assembled organic-inorganic hybrid compound

NASA Astrophysics Data System (ADS)

Mesbeh, Radhia; Hamdi, Besma; Zouari, Ridha

2017-01-01

The new organic-inorganic hybrid of the formula [H2mela]Cu2Cl6, where mela = 1,3,5-triazine-2,4,6-triamine, has been synthesized by the reaction of 1,3,5-triazine-2,4,6-triamine and copper(II) chloride dihydrate in the presence of hydrochloric acid. This compound has been determined by X-ray diffraction analysis and characterized by FT-IR, Raman, NMR characterization, differential scanning calorimetric (DSC) analysis, dielectric measurements and Hirshfeld surface. 1,3,5-triazinidium-2,4,6-triamine hexachlorodicuprate(II) crystallizes in the monoclinic system with space group P21/c. The final refinement of the structure of the program led to the reliability factors unweighted R1 = 3.53% and weighted WR2 = 8.87%. The observed internal C3sbnd N31sbnd C1 and C3sbnd N23sbnd C2 angle (121.5 and 121.4°) at protanated N-atom are significantly greater the other ring angle C1sbnd N12sbnd C2 (117.1°). The titled compound crystallizes as an organic-inorganic one-dimensional (1D) structure. The crystal structure was stabilized by two types of hydrogen bonding Nsbnd H⋯Cl and Nsbnd H⋯N. The infrared spectra was recorded in the 4000-400 cm-1 frequency region and the Raman spectra was recorded in the external region of the anionic sublattice vibration 4000-50 cm-1 at room temperature. Solid-state 13C and 63Cu MAS-NMR spectroscopies are in agreement with the X-ray structure. The differential scanning calorimetric (DSC) show the presence of a structural phase transition of the title compound at 338 K. Hirshfeld surface analyses for visually analyzing intermolecular interactions in crystal structures employing molecular surface contours and 2D fingerprint plots have been used to examine molecular shapes.

Homoacetogenesis in Deep-Sea Chloroflexi, as Inferred by Single-Cell Genomics, Provides a Link to Reductive Dehalogenation in Terrestrial Dehalococcoidetes.

PubMed

Sewell, Holly L; Kaster, Anne-Kristin; Spormann, Alfred M

2017-12-19

The deep marine subsurface is one of the largest unexplored biospheres on Earth and is widely inhabited by members of the phylum Chloroflexi In this report, we investigated genomes of single cells obtained from deep-sea sediments of the Peruvian Margin, which are enriched in such Chloroflexi 16S rRNA gene sequence analysis placed two of these single-cell-derived genomes (DscP3 and Dsc4) in a clade of subphylum I Chloroflexi which were previously recovered from deep-sea sediment in the Okinawa Trough and a third (DscP2-2) as a member of the previously reported DscP2 population from Peruvian Margin site 1230. The presence of genes encoding enzymes of a complete Wood-Ljungdahl pathway, glycolysis/gluconeogenesis, a Rhodobacter nitrogen fixation (Rnf) complex, glyosyltransferases, and formate dehydrogenases in the single-cell genomes of DscP3 and Dsc4 and the presence of an NADH-dependent reduced ferredoxin:NADP oxidoreductase (Nfn) and Rnf in the genome of DscP2-2 imply a homoacetogenic lifestyle of these abundant marine Chloroflexi We also report here the first complete pathway for anaerobic benzoate oxidation to acetyl coenzyme A (CoA) in the phylum Chloroflexi (DscP3 and Dsc4), including a class I benzoyl-CoA reductase. Of remarkable evolutionary significance, we discovered a gene encoding a formate dehydrogenase (FdnI) with reciprocal closest identity to the formate dehydrogenase-like protein (complex iron-sulfur molybdoenzyme [CISM], DET0187) of terrestrial Dehalococcoides/Dehalogenimonas spp. This formate dehydrogenase-like protein has been shown to lack formate dehydrogenase activity in Dehalococcoides/Dehalogenimonas spp. and is instead hypothesized to couple HupL hydrogenase to a reductive dehalogenase in the catabolic reductive dehalogenation pathway. This finding of a close functional homologue provides an important missing link for understanding the origin and the metabolic core of terrestrial Dehalococcoides/Dehalogenimonas spp. and of reductive dehalogenation, as well as the biology of abundant deep-sea Chloroflexi IMPORTANCE The deep marine subsurface is one of the largest unexplored biospheres on Earth and is widely inhabited by members of the phylum Chloroflexi In this report, we investigated genomes of single cells obtained from deep-sea sediments and provide evidence for a homacetogenic lifestyle of these abundant marine Chloroflexi Moreover, genome signature and key metabolic genes indicate an evolutionary relationship between these deep-sea sediment microbes and terrestrial, reductively dehalogenating Dehalococcoides . Copyright © 2017 Sewell et al.

Social Media Impact of the Food and Drug Administration's Drug Safety Communication Messaging About Zolpidem: Mixed-Methods Analysis.

PubMed

Sinha, Michael S; Freifeld, Clark C; Brownstein, John S; Donneyong, Macarius M; Rausch, Paula; Lappin, Brian M; Zhou, Esther H; Dal Pan, Gerald J; Pawar, Ajinkya M; Hwang, Thomas J; Avorn, Jerry; Kesselheim, Aaron S

2018-01-05

The Food and Drug Administration (FDA) issues drug safety communications (DSCs) to health care professionals, patients, and the public when safety issues emerge related to FDA-approved drug products. These safety messages are disseminated through social media to ensure broad uptake. The objective of this study was to assess the social media dissemination of 2 DSCs released in 2013 for the sleep aid zolpidem. We used the MedWatcher Social program and the DataSift historic query tool to aggregate Twitter and Facebook posts from October 1, 2012 through August 31, 2013, a period beginning approximately 3 months before the first DSC and ending 3 months after the second. Posts were categorized as (1) junk, (2) mention, and (3) adverse event (AE) based on a score between -0.2 (completely unrelated) to 1 (perfectly related). We also looked at Google Trends data and Wikipedia edits for the same time period. Google Trends search volume is scaled on a range of 0 to 100 and includes "Related queries" during the relevant time periods. An interrupted time series (ITS) analysis assessed the impact of DSCs on the counts of posts with specific mention of zolpidem-containing products. Chow tests for known structural breaks were conducted on data from Twitter, Facebook, and Google Trends. Finally, Wikipedia edits were pulled from the website's editorial history, which lists all revisions to a given page and the editor's identity. In total, 174,286 Twitter posts and 59,641 Facebook posts met entry criteria. Of those, 16.63% (28,989/174,286) of Twitter posts and 25.91% (15,453/59,641) of Facebook posts were labeled as junk and excluded. AEs and mentions represented 9.21% (16,051/174,286) and 74.16% (129,246/174,286) of Twitter posts and 5.11% (3,050/59,641) and 68.98% (41,138/59,641) of Facebook posts, respectively. Total daily counts of posts about zolpidem-containing products increased on Twitter and Facebook on the day of the first DSC; Google searches increased on the week of the first DSC. ITS analyses demonstrated variability but pointed to an increase in interest around the first DSC. Chow tests were significant (P<.0001) for both DSCs on Facebook and Twitter, but only the first DSC on Google Trends. Wikipedia edits occurred soon after each DSC release, citing news articles rather than the DSC itself and presenting content that needed subsequent revisions for accuracy. Social media offers challenges and opportunities for dissemination of the DSC messages. The FDA could consider strategies for more actively disseminating DSC safety information through social media platforms, particularly when announcements require updating. The FDA may also benefit from directly contributing content to websites like Wikipedia that are frequently accessed for drug-related information. ©Michael S Sinha, Clark C Freifeld, John S Brownstein, Macarius M Donneyong, Paula Rausch, Brian M Lappin, Esther H Zhou, Gerald J Dal Pan, Ajinkya M Pawar, Thomas J Hwang, Jerry Avorn, Aaron S Kesselheim. Originally published in JMIR Public Health and Surveillance (http://publichealth.jmir.org), 05.01.2018.

Desmocollin 2 is a new immunohistochemical marker indicative of squamous differentiation in urothelial carcinoma.

PubMed

Hayashi, Tetsutaro; Sentani, Kazuhiro; Oue, Naohide; Anami, Katsuhiro; Sakamoto, Naoya; Ohara, Shinya; Teishima, Jun; Noguchi, Tsuyoshi; Nakayama, Hirofumi; Taniyama, Kiyomi; Matsubara, Akio; Yasui, Wataru

2011-10-01

Urothelial carcinoma (UC) with squamous differentiation tends to present at higher stages than pure UC. To distinguish UC with squamous differentiation from pure UC, a sensitive and specific marker is needed. Desmocollin 2 (DSC2) is a protein localized in desmosomal junctions of stratified epithelium, but little is known about its biological significance in bladder cancer. We examined the utility of DSC2 as a diagnostic marker. We analysed the immunohistochemical characteristics of DSC2, and studied the relationship of DSC2 expression with the expression of the known markers uroplakin III (UPIII), cytokeratin (CK)7, CK20, epidermal growth factor receptor (EGFR), and p53. DSC2 staining was detected in 24 of 25 (96%) cases of UC with squamous differentiation, but in none of 85 (0%) cases of pure UC. DSC2 staining was detected only in areas of squamous differentiation. DSC2 expression was mutually exclusive of UPIII expression, and was correlated with EGFR expression. Furthermore, DSC2 expression was correlated with higher stage (P = 0.0314) and poor prognosis (P = 0.0477). DSC2 staining offers high sensitivity (96%) and high specificity (100%) for the detection of squamous differentiation in UC. DSC2 is a useful immunohistochemical marker for separation of UC with squamous differentiation from pure UC. 2011 Blackwell Publishing Limited.

Modification of bone-like apatite nanoparticle size and growth kinetics by alizarin red S

NASA Astrophysics Data System (ADS)

Ibsen, Casper Jon Steenberg; Birkedal, Henrik

2010-11-01

The formation of nanocrystals in biomineralization such as in bone occurs under the influence of organic molecules. Prompted by this fact, the effect of alizarin red S, a dye used in in vivo bone labeling methods, on bone-like carbonated apatite nanocrystal formation was investigated as a function of alizarin red S additive concentration. The obtained nanoparticles were investigated by powder X-ray diffraction (XRD), FTIR as well thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) while the kinetics of nanoparticle formation was investigated by in situ pH and synchrotron XRD measurements. Increasing alizarin red S concentration lead to amorphous particles over a threshold concentration and to smaller crystallites in a dose-dependent fashion. Alizarin red S induced a macroscopic lattice strain that scaled linearly with the alizarin red S concentration; this effect is reminiscent of that seen in biogenic calcium carbonates. TGA showed that the amorphous particles contained significantly more water than the crystalline samples and the DSC data showed that crystallization occurs after loss of most of the included organic material. The in situ studies showed that the formation of apatite goes via the very rapid formation of an amorphous precursor that after a certain nucleation time crystallizes into apatite. This nucleation time increased exponentially with alizarin red S concentration showing that this additive strongly stabilizes the amorphous precursor phase.

In vitro deposition of hydroxyapatite on cortical bone collagen stimulated by deformation-induced piezoelectricity.

PubMed

Noris-Suárez, Karem; Lira-Olivares, Joaquin; Ferreira, Ana Marina; Feijoo, José Luis; Suárez, Nery; Hernández, Maria C; Barrios, Esteban

2007-03-01

In the present work, we have studied the effect of the piezoelectricity of elastically deformed cortical bone collagen on surface using a biomimetic approach. The mineralization process induced as a consequence of the piezoelectricity effect was evaluated using scanning electron microscopy (SEM), thermally stimulated depolarization current (TSDC), and differential scanning calorimetry (DSC). SEM micrographs showed that mineralization occurred predominantly over the compressed side of bone collagen, due to the effect of piezoelectricity, when the sample was immersed in the simulated body fluid (SBF) in a cell-free system. The TSDC method was used to examine the complex collagen dielectric response. The dielectric spectra of deformed and undeformed collagen samples with different hydration levels were compared and correlated with the mineralization process followed by SEM. The dielectric measurements showed that the mineralization induced significant changes in the dielectric spectra of the deformed sample. DSC and TSDC results demonstrated a reduction of the collagen glass transition as the mineralization process advanced. The combined use of SEM, TSDC, and DSC showed that, even without osteoblasts present, the piezoelectric dipoles produced by deformed collagen can produce the precipitation of hydroxyapatite by electrochemical means, without a catalytic converter as occurs in classical biomimetic deposition.

Distinct Roles of the DmNav and DSC1 Channels in the Action of DDT and Pyrethroids

PubMed Central

Rinkevich, Frank D.; Du, Yuzhe; Tolinski, Josh; Ueda, Atsushi; Wu, Chun-Fang; Zhorov, Boris S.; Dong, Ke

2015-01-01

Voltage-gated sodium channels (Nav channels) are critical for electrical signaling in the nervous system and are the primary targets of the insecticides DDT and pyrethroids. In Drosophila melanogaster, besides the canonical Nav channel, Para (also called DmNav), there is a sodium channel-like cation channel called DSC1 (Drosophila sodium channel 1). Temperature-sensitive paralytic mutations in DmNav (parats) confer resistance to DDT and pyrethroids, whereas DSC1 knockout flies exhibit enhanced sensitivity to pyrethroids. To further define the roles and interaction of DmNav and DSC1 channels in DDT and pyrethroid neurotoxicology, we generated a DmNav/DSC1 double mutant line by introducing a parats1 allele (carrying the I265N mutation) into a DSC1 knockout line. We confirmed that the I265N mutation reduced the sensitivity to two pyrethroids, permethrin and deltamethrin of a DmNav variant expressed in Xenopus oocytes. Computer modeling predicts that the I265N mutation confers pyrethroid resistance by allosterically altering the second pyrethroid receptor site on the DmNav channel. Furthermore, we found that I265N-mediated pyrethroid resistance in parats1 mutant flies was almost completely abolished in parats1;DSC1−/− double mutant flies. Unexpectedly, however, the DSC1 knockout flies were less sensitive to DDT, compared to the control flies (w1118A), and the parats1;DSC1−/− double mutant flies were even more resistant to DDT compared to the DSC1 knockout or parats1 mutant. Our findings revealed distinct roles of the DmNav and DSC1 channels in the neurotoxicology of DDT vs. pyrethroids and implicate the exciting possibility of using DSC1 channel blockers or modifiers in the management of pyrethroid resistance. PMID:25687544

Detection of cocrystal formation based on binary phase diagrams using thermal analysis.

PubMed

Yamashita, Hiroyuki; Hirakura, Yutaka; Yuda, Masamichi; Teramura, Toshio; Terada, Katsuhide

2013-01-01

Although a number of studies have reported that cocrystals can form by heating a physical mixture of two components, details surrounding heat-induced cocrystal formation remain unclear. Here, we attempted to clarify the thermal behavior of a physical mixture and cocrystal formation in reference to a binary phase diagram. Physical mixtures prepared using an agate mortar were heated at rates of 2, 5, 10, and 30 °C/min using differential scanning calorimetry (DSC). Some mixtures were further analyzed using X-ray DSC and polarization microscopy. When a physical mixture consisting of two components which was capable of cocrystal formation was heated using DSC, an exothermic peak associated with cocrystal formation was detected immediately after an endothermic peak. In some combinations, several endothermic peaks were detected and associated with metastable eutectic melting, eutectic melting, and cocrystal melting. In contrast, when a physical mixture of two components which is incapable of cocrystal formation was heated using DSC, only a single endothermic peak associated with eutectic melting was detected. These experimental observations demonstrated how the thermal events were attributed to phase transitions occurring in a binary mixture and clarified the relationship between exothermic peaks and cocrystal formation.

Study of the pH-sensitive mechanism of tumor-targeting liposomes.

PubMed

Fan, Yang; Chen, Cong; Huang, Yiheng; Zhang, Fang; Lin, Guimei

2017-03-01

Currently, the phosphatidylethanolamine-based, pH-sensitive, liposome drug-delivery system has been widely developed for efficient, targeted cancer therapy. However, the mechanism of pH sensitivity was unclear; it is a main obstacle in controlling the preparation of pH-sensitive liposomes (PSLs).Therefore, our research is aimed at clarifying the pH-response mechanism of the various molecules that compose liposomes. We chose the small pH-sensitive molecules oleic acid (OA), linoleic acid (LA) and cholesteryl hemisuccinate (CHEMS) and the fundamental lipids cholesterol and phosphatidylethanolamine (PE) as test molecules. The PSLs were prepared using the thin-film hydration method and characterized in detail at various pH values (pH 5.0, 6.0 and 7.4), including particle size, ζ-potential, drug encapsulation efficiency and drug loading. The surface structure was observed by transmission electron microscopy (TEM), and the electrical conductivity of the liposome dispersion was also tested. The calorimetric analysis was conducted by Nano-differential scanning calorimetry (Nano-DSC). The in vitro drug release profile showed that PSLs exhibit good pH sensitivity. At neutral pH, the particle size was approximately 150nm, and it dramatically increased at pH 5.0. The ζ-potential increased as the pH decreased. The Nano-DSC results showed that cholesterol and CHEMS can both increase the stability and phase transfer temperature of PSLs. Conductivity increased to a maximum at pH 5.0 and was rather low at pH 7.4. In conclusion, results show that the three kinds of liposomes have pH responsive release characteristics in acidic pH. The OA-PSLs have a pH sensitive point of 5. Since CHEMS has a cholesterol-like structure, it can stabilizes the phospholipid bilayer under neutral conditions as shown in the Nano-DSC data, and because it has a special steroidal rigid structure, it exhibits better pH response characteristics under acidic conditions. Copyright © 2016 Elsevier B.V. All rights reserved.

47 CFR 80.409 - Station logs.

Code of Federal Regulations, 2010 CFR

2010-10-01

... calling (DSC) equipment has been verified by actual communications or a test call; (ii) The portable... devices which do not have integral navigation receivers, including: VHF DSC, MF DSC, satellite EPIRB and HF DSC or INMARSAT SES. On a ship without integral or directly connected navigation receiver input to...

47 CFR 80.409 - Station logs.

Code of Federal Regulations, 2011 CFR

2011-10-01

... calling (DSC) equipment has been verified by actual communications or a test call; (ii) The portable... devices which do not have integral navigation receivers, including: VHF DSC, MF DSC, satellite EPIRB and HF DSC or INMARSAT SES. On a ship without integral or directly connected navigation receiver input to...

Characterization of organic matter of plants from lakes by thermal analysis in a N2 atmosphere

NASA Astrophysics Data System (ADS)

Guo, Fei; Wu, Fengchang; Mu, Yunsong; Hu, Yan; Zhao, Xiaoli; Meng, Wei; Giesy, John P.; Lin, Ying

2016-03-01

Organic matter (OM) has been characterized using thermal analysis in O2 atmospheres, but it is not clear if OM can be characterized using slow thermal degradation in N2 atmospheres (STDN). This article presents a new method to estimate the behavior of OM in anaerobic environment. Seventeen different plants from Tai Lake (Ch: Taihu), China were heated to 600 °C at a rate of 10 °C min-1 in a N2 atmosphere and characterized by use of differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). DSC chromatograms were compared with 9 standard compounds. Seven peaks were observed in DSC chromatograms, 2 main peaks strongly correlated with biochemical indices, and one main peak was a transitional stage. Energy absorbed by a peak at approximately 200 °C and total organic carbon were well correlated, while energy absorbed at approximately 460 °C was negatively correlated with lignin content. Presence of peaks at approximately 350 and 420 °C varied among plant biomass sources, providing potential evidence for biomass identification. Methods of STDN reported here were rapid and accurate ways to quantitatively characterize OM, which may provide useful information for understanding anaerobic behaviors of natural organic matters.

Thermal Stability and Kinetic Study of Fluvoxamine Stability in Binary Samples with Lactose.

PubMed

Ghaderi, Faranak; Nemati, Mahboob; Siahi-Shadbad, Mohammad Reza; Valizadeh, Hadi; Monajjemzadeh, Farnaz

2017-04-01

Purpose: In the present study the incompatibility of FLM (fluvoxamine) with lactose in solid state mixtures was investigated. The compatibility was evaluated using different physicochemical methods such as differential scanning calorimetry (DSC), Fourier-transform infrared (FTIR) spectroscopy and mass spectrometry. Methods: Non-Isothermally stressed physical mixtures were used to calculate the solid-state kinetic parameters. Different thermal models such as Friedman, Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS) were used for the characterization of the drug-excipient interaction. Results: Overall, the incompatibility of FLM with lactose as a reducing carbohydrate was successfully evaluated and the activation energy of this interaction was calculated. Conclusion: In this research the lactose and FLM Maillard interaction was proved using physicochemical techniques including DSC and FTIR. It was shown that DSC- based kinetic analysis provides fast and versatile kinetic comparison of Arrhenius activation energies for different pharmaceutical samples.

Thermal Stability and Kinetic Study of Fluvoxamine Stability in Binary Samples with Lactose

PubMed Central

Ghaderi, Faranak; Nemati, Mahboob; Siahi-Shadbad, Mohammad Reza; Valizadeh, Hadi; Monajjemzadeh, Farnaz

2017-01-01

Purpose: In the present study the incompatibility of FLM (fluvoxamine) with lactose in solid state mixtures was investigated. The compatibility was evaluated using different physicochemical methods such as differential scanning calorimetry (DSC), Fourier-transform infrared (FTIR) spectroscopy and mass spectrometry. Methods: Non-Isothermally stressed physical mixtures were used to calculate the solid–state kinetic parameters. Different thermal models such as Friedman, Flynn–Wall–Ozawa (FWO) and Kissinger–Akahira–Sunose (KAS) were used for the characterization of the drug-excipient interaction. Results: Overall, the incompatibility of FLM with lactose as a reducing carbohydrate was successfully evaluated and the activation energy of this interaction was calculated. Conclusion: In this research the lactose and FLM Maillard interaction was proved using physicochemical techniques including DSC and FTIR. It was shown that DSC- based kinetic analysis provides fast and versatile kinetic comparison of Arrhenius activation energies for different pharmaceutical samples. PMID:28507936

Final report for tank 241-AP-108, grab samples 8AP-96-1, 8AP-96-2 and 8AP-96-FB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Esch, R.A.

1996-04-19

This document is the final report deliverable for the tank 241-AP-108 grab samples. The samples were subsampled and analyzed in accordance with the TSAP. Included in this report are the results for the Waste Compatibility analyses, with the exception of DSC and thermogravimetric analysis (TGA) results which were presented in the 45 Day report (Part 2 of this document). The raw data for all analyses, with the exception of DSC and TGA, are also included in this report.

Electrical properties of CZTS thin films

NASA Astrophysics Data System (ADS)

Rao, M. C.; Kumar, M. Seshu; Lakshmi, K.; Rao, K. Koteswara; Parimala, M. P. D.; Basha, S. K. Shahenoor

2018-05-01

CZTS (Cu2ZnSnS4) thin films have been coated on to FTO and MO glass substrates by single step electro deposition process. Different characterization techniques were performed on to the prepared samples such as DSC and Raman studies. The Phase transition and weight loss of the precursors can be measured by DSC analysis. Raman spectrum is used to identify the functional groups and chemical structure involved in the materials. Electrical measurements confirm the nature of the film and also depend on the charge concentration present in the samples.

47 CFR 80.359 - Frequencies for digital selective calling (DSC).

Code of Federal Regulations, 2011 CFR

2011-10-01

... 47 Telecommunication 5 2011-10-01 2011-10-01 false Frequencies for digital selective calling (DSC... for digital selective calling (DSC). (a) General purpose calling. The following table describes the calling frequencies for use by authorized ship and coast stations for general purpose DSC. There are three...

DOE Office of Scientific and Technical Information (OSTI.GOV)

Polan, D; Kamp, J; Lee, JY

Purpose: To perform validation and commissioning of a commercial deformable image registration (DIR) algorithm (Velocity, Varian Medical Systems) for numerous clinical sites using single and multi-modality images. Methods: In this retrospective study, the DIR algorithm was evaluated for 10 patients in each of the following body sites: head and neck (HN), prostate, liver, and gynecological (GYN). HN DIRs were evaluated from planning (p)CT to re-pCT and pCTs to daily CBCTs using dice similarity coefficients (DSC) of corresponding anatomical structures. Prostate DIRs were evaluated from pCT to CBCTs using DSC and target registration error (TRE) of implanted RF beacons within themore » prostate. Liver DIRs were evaluated from pMR to pCT using DSC and TRE of vessel bifurcations. GYN DIRs were evaluated between fractionated brachytherapy MRIs using DSC of corresponding anatomical structures. Results: Analysis to date has given average DSCs for HN pCT-to-(re)pCT DIR for the brainstem, cochleas, constrictors, spinal canal, cord, esophagus, larynx, parotids, and submandibular glands as 0.88, 0.65, 0.67, 0.91, 0.77, 0.69, 0.77, 0.87, and 0.71, respectively. Average DSCs for HN pCT-to-CBCT DIR for the constrictors, spinal canal, esophagus, larynx, parotids, and submandibular glands were 0.64, 0.90, 0.62, 0.82, 0.75, and 0.69, respectively. For prostate pCT-to-CBCT DIR the DSC for the bladder, femoral heads, prostate, and rectum were 0.71, 0.82, 0.69, and 0.61, respectively. Average TRE using implanted beacons was 3.35 mm. For liver pCT-to-pMR, the average liver DSC was 0.94 and TRE was 5.26 mm. For GYN MR-to-MR DIR the DSC for the bladder, sigmoid colon, GTV, and rectum were 0.79, 0.58, 0.67, and 0.76, respectively. Conclusion: The Velocity DIR algorithm has been evaluated over a number of anatomical sites. This work functions to document the uncertainties in the DIR in the commissioning process so that these can be accounted for in the development of downstream clinical processes. This work was supported in part by a co-development agreement with Varian Medical Systems.« less

SU-D-18C-02: Feasibility of Using a Short ASL Scan for Calibrating Cerebral Blood Flow Obtained From DSC-MRI

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, P; Chang, T; Huang, K

2014-06-01

Purpose: This study aimed to evaluate the feasibility of using a short arterial spin labeling (ASL) scan for calibrating the dynamic susceptibility contrast- (DSC-) MRI in a group of patients with internal carotid artery stenosis. Methods: Six patients with unilateral ICA stenosis enrolled in the study on a 3T clinical MRI scanner. The ASL-cerebral blood flow (-CBF) maps were calculated by averaging different number of dynamic points (N=1-45) acquired by using a Q2TIPS sequence. For DSC perfusion analysis, arterial input function was selected to derive the relative cerebral blood flow (rCBF) map and the delay (Tmax) map. Patient-specific CF wasmore » calculated from the mean ASL- and DSC-CBF obtained from three different masks: (1)Tmax< 3s, (2)combined gray matter mask with mask 1, (3)mask 2 with large vessels removed. One CF value was created for each number of averages by using each of the three masks for calibrating the DSC-CBF map. The CF value of the largest number of averages (NL=45) was used to determine the acceptable range(< 10%, <15%, and <20%) of CF values corresponding to the minimally acceptable number of average (NS) for each patient. Results: Comparing DSC CBF maps corrected by CF values of NL (CBFL) in ACA, MCA and PCA territories, all masks resulted in smaller CBF on the ipsilateral side than the contralateral side of the MCA territory(p<.05). The values obtained from mask 1 were significantly different than the mask 3(p<.05). Using mask 3, the medium values of Ns were 4(<10%), 2(<15%) and 2(<20%), with the worst case scenario (maximum Ns) of 25, 4, and 4, respectively. Conclusion: This study found that reliable calibration of DSC-CBF can be achieved from a short pulsed ASL scan. We suggested use a mask based on the Tmax threshold, the inclusion of gray matter only and the exclusion of large vessels for performing the calibration.« less

Thermal Analyzer for Planetary Soil (TAPS): an in Situ Instrument for Mineral and Volatile-element Measurements

NASA Technical Reports Server (NTRS)

Gooding, J. L.; Ming, D. W.; Gruener, J. E.; Gibbons, F. L.; Allton, J. H.

1993-01-01

Thermal Analyzer for Planetary Soil (TAPS) offers a specific implementation for the generic thermal analyzer/evolved-gas analyzer (TA/EGA) function included in the Mars Environmental Survey (MESUR) strawman payload; applications to asteroids and comets are also possible. The baseline TAPS is a single-sample differential scanning calorimeter (DSC), backed by a capacitive-polymer humidity sensor, with an integrated sampling mechanism. After placement on a planetary surface, TAPS acquires 10-50 mg of soil or sediment and heats the sample from ambient temperature to 1000-1300 K. During heating, DSC data are taken for the solid and evolved gases are swept past the water sensor. Through ground based data analysis, multicomponent DSC data are deconvolved and correlated with the water release profile to quantitatively determine the types and relative proportions of volatile-bearing minerals such as clays and other hydrates, carbonates, and nitrates. The rapid-response humidity sensors also achieve quantitative analysis of total water. After conclusion of soil-analysis operations, the humidity sensors become available for meteorology. The baseline design fits within a circular-cylindrical volume less than 1000 cm(sup 3), occupies 1.2 kg mass, and consumes about 2 Whr of power per analysis. Enhanced designs would acquire and analyze multiple samples and employ additional microchemical sensors for analysis of CO2, SO2, NO(x), and other gaseous species. Atmospheric pumps are also being considered as alternatives to pressurized purge gas.

Thermal Analyzer for Planetary Soil (TAPS): an in situ instrument for mineral and volatile-element measurements

NASA Astrophysics Data System (ADS)

Gooding, J. L.; Ming, D. W.; Gruener, J. E.; Gibbons, F. L.; Allton, J. H.

Thermal Analyzer for Planetary Soil (TAPS) offers a specific implementation for the generic thermal analyzer/evolved-gas analyzer (TA/EGA) function included in the Mars Environmental Survey (MESUR) strawman payload; applications to asteroids and comets are also possible. The baseline TAPS is a single-sample differential scanning calorimeter (DSC), backed by a capacitive-polymer humidity sensor, with an integrated sampling mechanism. After placement on a planetary surface, TAPS acquires 10-50 mg of soil or sediment and heats the sample from ambient temperature to 1000-1300 K. During heating, DSC data are taken for the solid and evolved gases are swept past the water sensor. Through ground based data analysis, multicomponent DSC data are deconvolved and correlated with the water release profile to quantitatively determine the types and relative proportions of volatile-bearing minerals such as clays and other hydrates, carbonates, and nitrates. The rapid-response humidity sensors also achieve quantitative analysis of total water. After conclusion of soil-analysis operations, the humidity sensors become available for meteorology. The baseline design fits within a circular-cylindrical volume less than 1000 cm3, occupies 1.2 kg mass, and consumes about 2 Whr of power per analysis. Enhanced designs would acquire and analyze multiple samples and employ additional microchemical sensors for analysis of CO2, SO2, NO(x), and other gaseous species. Atmospheric pumps are also being considered as alternatives to pressurized purge gas.

Estimation of Temperature Range for Cryo Cutting of Frozen Mackerel using DSC

NASA Astrophysics Data System (ADS)

Okamoto, Kiyoshi; Hagura, Yoshio; Suzuki, Kanichi

Frozen mackerel flesh was subjected to measurement of its fracture stress (bending energy) in a low temperature range. The optimum conditions for low temperature cutting, "cryo cutting," were estimated from the results of enthalpy changes measured by a differential scanning calorimeter (DSC). There were two enthalpy changes for gross transition on the DSC chart for mackerel, one was at -63°C to -77°C and the other at -96°C to -112°C. Thus we estimated that mackerel was able to cut by bending below -63°C and that there would be a great decrease in bending energy occurring at around -77°C and -112°C. In testing, there were indeed two great decreases of bending energy for the test pieces of mackerel that had been frozen at -40°C, one was at -70°C to -90°C and the other was at -100°C to -120°C. Therefore, the test pieces of mackerel could be cut by bending at -70°C. The results showed that the DSC measurement of mackerel flesh gave a good estimation of the appropriate cutting temperature of mackerel.

Cerebral perfusion alterations in epileptic patients during peri-ictal and post-ictal phase: PASL vs DSC-MRI.

PubMed

Pizzini, Francesca B; Farace, Paolo; Manganotti, Paolo; Zoccatelli, Giada; Bongiovanni, Luigi G; Golay, Xavier; Beltramello, Alberto; Osculati, Antonio; Bertini, Giuseppe; Fabene, Paolo F

2013-07-01

Non-invasive pulsed arterial spin labeling (PASL) MRI is a method to study brain perfusion that does not require the administration of a contrast agent, which makes it a valuable diagnostic tool as it reduces cost and side effects. The purpose of the present study was to establish the viability of PASL as an alternative to dynamic susceptibility contrast (DSC-MRI) and other perfusion imaging methods in characterizing changes in perfusion patterns caused by seizures in epileptic patients. We evaluated 19 patients with PASL. Of these, the 9 affected by high-frequency seizures were observed during the peri-ictal period (within 5hours since the last seizure), while the 10 patients affected by low-frequency seizures were observed in the post-ictal period. For comparison, 17/19 patients were also evaluated with DSC-MRI and CBF/CBV. PASL imaging showed focal vascular changes, which allowed the classification of patients in three categories: 8 patients characterized by increased perfusion, 4 patients with normal perfusion and 7 patients with decreased perfusion. PASL perfusion imaging findings were comparable to those obtained by DSC-MRI. Since PASL is a) sensitive to vascular alterations induced by epileptic seizures, b) comparable to DSC-MRI for detecting perfusion asymmetries, c) potentially capable of detecting time-related perfusion changes, it can be recommended for repeated evaluations, to identify the epileptic focus, and in follow-up and/or therapy-response assessment. Copyright © 2013 Elsevier Inc. All rights reserved.

Design and long-term monitoring of DSC/CIGS tandem solar module

NASA Astrophysics Data System (ADS)

Vildanova, M. F.; Nikolskaia, A. B.; Kozlov, S. S.; Shevaleevskiy, O. I.

2015-11-01

This paper describes the design and development of tandem dye-sensitized/Cu(In, Ga)Se (DSC/CIGS) PV modules. The tandem PV module comprised of the top DSC module and a bottom commercial 0,8 m2 CIGS module. The top DSC module was made of 10 DSC mini-modules with the field size of 20 × 20 cm2 each. Tandem DSC/CIGS PV modules were used for providing the long-term monitoring of energy yield and electrical parameters in comparison with standalone CIGS modules under outdoor conditions. The outdoor test facility, containing solar modules of both types and a measurement unit, was located on the roof of the Institute of Biochemical Physics in Moscow. The data obtained during monitoring within the 2014 year period has shown the advantages of the designed tandem DSC/CIGS PV-modules over the conventional CIGS modules, especially for cloudy weather and low-intensity irradiation conditions.

The interplay between the paracetamol polymorphism and its molecular structures dissolved in supercritical CO2 in contact with the solid phase: In situ vibration spectroscopy and molecular dynamics simulation analysis.

PubMed

Oparin, Roman D; Moreau, Myriam; De Walle, Isabelle; Paolantoni, Marco; Idrissi, Abdenacer; Kiselev, Michael G

2015-09-18

The aim of this paper is to characterize the distribution of paracetamol conformers which are dissolved in a supercritical CO2 phase being in equilibrium with their corresponding crystalline form. The quantum calculations and molecular dynamics simulations were used in order to characterize the structure and analyze the vibration spectra of the paracetamol conformers in vacuum and in a mixture with CO2 at various thermodynamic state parameters (p,T). The metadynamics approach was applied to efficiently sample the various conformers of paracetamol. Furthermore, using in situ IR spectroscopy, the conformers that are dissolved in supercritical CO2 were identified and the evolution of the probability of their presence as a functions of thermodynamic condition was quantified while the change in the crystalline form of paracetamol have been monitored by DSC, micro IR and Raman techniques. The DSC analysis as well as micro IR and Raman spectroscopic studies of the crystalline paracetamol show that the subsequent heating up above the melting temperature of the polymorph I of paracetamol and the cooling down to room temperature in the presence of supercritical CO2 induces the formation of polymorph II. The in situ IR investigation shows that two conformers (Conf. 1 and Conf. 2) are present in the phase of CO2 while conformer 3 (Conf. 3) has a high probability to be present after re-crystallization. Copyright © 2015. Published by Elsevier B.V.

Distinct roles of the DmNav and DSC1 channels in the action of DDT and pyrethroids.

PubMed

Rinkevich, Frank D; Du, Yuzhe; Tolinski, Josh; Ueda, Atsushi; Wu, Chun-Fang; Zhorov, Boris S; Dong, Ke

2015-03-01

Voltage-gated sodium channels (Nav channels) are critical for electrical signaling in the nervous system and are the primary targets of the insecticides DDT and pyrethroids. In Drosophila melanogaster, besides the canonical Nav channel, Para (also called DmNav), there is a sodium channel-like cation channel called DSC1 (Drosophila sodium channel 1). Temperature-sensitive paralytic mutations in DmNav (para(ts)) confer resistance to DDT and pyrethroids, whereas DSC1 knockout flies exhibit enhanced sensitivity to pyrethroids. To further define the roles and interaction of DmNav and DSC1 channels in DDT and pyrethroid neurotoxicology, we generated a DmNav/DSC1 double mutant line by introducing a para(ts1) allele (carrying the I265N mutation) into a DSC1 knockout line. We confirmed that the I265N mutation reduced the sensitivity to two pyrethroids, permethrin and deltamethrin of a DmNav variant expressed in Xenopus oocytes. Computer modeling predicts that the I265N mutation confers pyrethroid resistance by allosterically altering the second pyrethroid receptor site on the DmNav channel. Furthermore, we found that I265N-mediated pyrethroid resistance in para(ts1) mutant flies was almost completely abolished in para(ts1);DSC1(-/-) double mutant flies. Unexpectedly, however, the DSC1 knockout flies were less sensitive to DDT, compared to the control flies (w(1118A)), and the para(ts1);DSC1(-/-) double mutant flies were even more resistant to DDT compared to the DSC1 knockout or para(ts1) mutant. Our findings revealed distinct roles of the DmNav and DSC1 channels in the neurotoxicology of DDT vs. pyrethroids and implicate the exciting possibility of using DSC1 channel blockers or modifiers in the management of pyrethroid resistance. Copyright © 2015 Elsevier Inc. All rights reserved.

Human decidual stromal cells secrete soluble pro-apoptotic factors during decidualization in a cAMP-dependent manner.

PubMed

Leno-Durán, E; Ruiz-Magaña, M J; Muñoz-Fernández, R; Requena, F; Olivares, E G; Ruiz-Ruiz, C

2014-10-10

Is there a relationship between decidualization and apoptosis of decidual stromal cells (DSC)? Decidualization triggers the secretion of soluble factors that induce apoptosis in DSC. The differentiation and apoptosis of DSC during decidualization of the receptive decidua are crucial processes for the controlled invasion of trophoblasts in normal pregnancy. Most DSC regress in a time-dependent manner, and their removal is important to provide space for the embryo to grow. However, the mechanism that controls DSC death is poorly understood. The apoptotic response of DSC was analyzed after exposure to different exogenous agents and during decidualization. The apoptotic potential of decidualized DSC supernatants and prolactin (PRL) was also evaluated. DSC lines were established from samples of decidua from first trimester pregnancies. Apoptosis was assayed by flow cytometry. PRL production, as a marker of decidualization, was determined by enzyme-linked immunosorbent assay. DSCs were resistant to a variety of apoptosis-inducing substances. Nevertheless, DSC underwent apoptosis during decidualization in culture, with cAMP being essential for both apoptosis and differentiation. In addition, culture supernatants from decidualized DSC induced apoptosis in undifferentiated DSC, although paradoxically these supernatants decreased the spontaneous apoptosis of decidual lymphocytes. Exogenously added PRL did not induce apoptosis in DSC and an antibody that neutralized the PRL receptor did not decrease the apoptosis induced by supernatants. Further studies are needed to examine the involvement of other soluble factors secreted by decidualized DSC in the induction of apoptosis. The present results indicate that apoptosis of DSC occurs in parallel to differentiation, in response to decidualization signals, with soluble factors secreted by decidualized DSC being responsible for triggering cell death. These studies are relevant in the understanding of how the regression of decidua, a crucial process for successful pregnancy, takes place. This work was supported by the Consejería de Economía, Innovación y Ciencia, Junta de Andalucía (Grant CTS-6183, Proyectos de Investigación de Excelencia 2010 to C.R.-R.) and the Instituto de Salud Carlos III, Ministerio de Economía y Competitividad, Spain (Grants PS09/00339 and PI12/01085 to E.G.O.). E.L.-D. was supported by fellowships from the Ministerio de Educación y Ciencia, Spain and the University of Granada. The authors have no conflict of interest. © The Author 2014. Published by Oxford University Press on behalf of the European Society of Human Reproduction and Embryology. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Implementation of the Domino Sampling Waveform digitizer in the PIBETA experiment

NASA Astrophysics Data System (ADS)

Wang, Ying

The Domino Sampling Chip(DSC)-Waveform digitization system is a significant addition to electronics arsenal of PIBETA experiment. It is used to digitize waveforms from every photo tube in the detector. Through carefully programmed offline analysis of its raw data collected during regular runtime, better timing and energy resolution are achieved compared with feast's results. And more importantly, the geometric character of the digitized waveform which contains information of energy deposition of particle decays can be utilized for particle identification, a great advantage that regular unit could not possess. In addition to fastbus, incorporate DSC data through its offline analysis including timing and energy offset, scale calibration will contribute a final more precise result of PIBETA experiment.

Temperature-modulated DSC provides new insight about nickel-titanium wire transformations.

PubMed

Brantley, William A; Iijima, Masahiro; Grentzer, Thomas H

2003-10-01

Differential scanning calorimetry (DSC) is a well-known method for investigating phase transformations in nickel-titanium orthodontic wires; the microstructural phases and phase transformations in these wires have central importance for their clinical performance. The purpose of this study was to use the more recently developed technique of temperature-modulated DSC (TMDSC) to gain insight into transformations in 3 nickel-titanium orthodontic wires: Neo Sentalloy (GAC International, Islandia, NY), 35 degrees C Copper Ni-Ti (Ormco, Glendora, Calif) and Nitinol SE (3M Unitek, Monrovia, Calif). In the oral environment, the first 2 superelastic wires have shape memory, and the third wire has superelastic behavior but not shape memory. All wires had cross-section dimensions of 0.016 x 0.022 in. Archwires in the as-received condition and after bending 135 degrees were cut into 5 or 6 segments for test specimens. TMDSC analyses (Model 2910 DSC, TA Instruments, Wilmington, Del) were conducted between -125 degrees C and 100 degrees C, using a linear heating and cooling rate of 2 degrees C per min, an oscillation amplitude of 0.318 degrees C with a period of 60 seconds, and helium as the purge gas. For all 3 wire alloys, strong low-temperature martensitic transformations, resolved on the nonreversing heat-flow curves, were not present on the reversing heat-flow curves, and bending appeared to increase the enthalpy change for these peaks in some cases. For Neo Sentalloy, TMDSC showed that transformation between martensitic and austenitic nickel-titanium, suggested as occurring directly in the forward and reverse directions by conventional DSC, was instead a 2-step process involving the R-phase. Two-step transformations in the forward and reverse directions were also found for 35 degrees C Copper Ni-Ti and Nitinol SE. The TMDSC results show that structural transformations in these wires are complex. Some possible clinical implications of these observations are discussed.

The characterization of copper alloys for the application of fusion reactors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ishiyama, S.; Fukaya, K.; Eto, M.

Three kinds of candidate copper alloys for divertor structural materials of fusion experimental reactors, that is, Oxygen Free High thermal conductivity Copper (OFHC), alumina disperse reinforced copper (DSC) and the composite of W and Cu (W/Cu), were prepared for strength and fatigue tests at temperatures ranging from R.T. to 500 C in a vacuum. High temperature strength of DSC and W/Cu with rapid fracture after peak loading at the temperatures is higher than that of OFHC by factor of 2, but fracture strains of DFC and W/Cu are smaller than that of OFHC. Fatigue life of DSC, which shows themore » same fatigue behavior of OFHC at room temperature, is longer than other materials at 400 C. Remarkable fatigue life reduction of OFHC found in this experiment is to be due to recrystallization of OFHC yielded above 400 C.« less

Preparation, characterization, dielectric properties and diffusion studies of styrene butadiene rubber (SBR)/manganous tungstate (MnWO4) nanocomposites

NASA Astrophysics Data System (ADS)

Jasna, V. C.; Ramesan, M. T.

2017-06-01

Nanocomposites based on SBR with different content of manganous tungstate nanoparticles were prepared and characterized by FTIR, UV-visible spectroscopy, XRD, SEM, TGA, DSC and impedance analysis. The interaction between nanoparticles and the elastomer was clear from the shift in peaks of UV and FTIR. XRD and SEM analysis showed the uniform arrangement of nanoparticles in SBR matrix. Glass transition temperature, thermal stability and dielectric properties of composites were enhanced by the addition of nanoparticles. Sorption studies of nanocomposites were done in aromatic solvents at different temperature. Sorption data obtained were used to estimate the thermodynamic properties.

Preparation, process optimization and characterization of core-shell polyurethane/chitosan nanofibers as a potential platform for bioactive scaffolds.

PubMed

Maleknia, Laleh; Dilamian, Mandana; Pilehrood, Mohammad Kazemi; Sadeghi-Aliabadi, Hojjat; Hekmati, Amir Houshang

2018-06-01

In this paper, polyurethane (PU), chitosan (Cs)/polyethylene oxide (PEO), and core-shell PU/Cs nanofibers were produced at the optimal processing conditions using electrospinning technique. Several methods including SEM, TEM, FTIR, XRD, DSC, TGA and image analysis were utilized to characterize these nanofibrous structures. SEM images exhibited that the core-shell PU/Cs nanofibers were spun without any structural imperfections at the optimized processing conditions. TEM image confirmed the PU/Cs core-shell nanofibers were formed apparently. It that seems the inclusion of Cs/PEO to the shell, did not induce the significant variations in the crystallinity in the core-shell nanofibers. DSC analysis showed that the inclusion of Cs/PEO led to the glass temperature of the composition increased significantly compared to those of neat PU nanofibers. The thermal degradation of core-shell PU/Cs was similar to PU nanofibers degradation due to the higher PU concentration compared to other components. It was hypothesized that the core-shell PU/Cs nanofibers can be used as a potential platform for the bioactive scaffolds in tissue engineering. Further biological tests should be conducted to evaluate this platform as a three dimensional scaffold with the capabilities of releasing the bioactive molecules in a sustained manner.

Effect of coupling agent on durian skin fibre nanocomposite reinforced polypropylene

NASA Astrophysics Data System (ADS)

Siti Nur E'zzati, M. A.; Anuar, H.; Siti Munirah Salimah, A. R.

2018-01-01

This paper reports on the development of a composite-based natural fiber to reduce the reliance on petroleum-based product in order to amplify environmental awareness. The production of Durian Skin Nanofiber (DSNF) was conducted using biological fermentation method via rhizopus oryzae in order to obtain the nano dimension of the particle size. Polypropylene (PP) and DSNF were produced using Haake internal mixer via melt blending technique. The significant effect of maleic anhydride grafted polypropylene (MAPP) on the properties of PP/DSNF nanocomposite was investigated to study its mechanical properties which are tensile strength and thermal stability using thermogravimetric (TGA) and differential scanning analysis (DSC). The tensile property of PP nanocomposites increased from 33 MPa to 38 MPa with the presence of MAPP. The addition of MAPP also increased the thermal stability of PP/DSNF nanocomposite where the char residue increased by 52%. Besides that, the thermal degradation of PP/DSNF and PP/DSNF-MAPP were higher than PP where they exerted higher amount of weight loss at an elevated temperature. The percentage of crystallinity, %Xc, of PP nanocomposites improved with the addition of MAPP by 35% based on the differential scanning calorimetry (DSC) result. The SEM analysis showed that the PP/DSNF-MAPP exerts ductile fracture while PP/DSNF exerts brittle fracture.

Phase transitions in methyl parben doped dipalmitoyl phosphatidylethanolamine vesicles

NASA Astrophysics Data System (ADS)

Panicker, Lata

2013-02-01

Influence of the preservative, methyl paraben (MPB), on the thermal properties of dipalmitoyl phosphatidylethanolamine (DPPE) vesicles was investigated using DSC. DSC measurement of the lipid acyl chain melting transition in DPPE membrane doped with MPB, showed MPB concentration dependant modifications in the membrane thermal properties. The interesting findings are: (1) the presence of parabens increases the membrane fluidity. (2) the MPB molecules seem to be present in the aqueous bilayer interfacial region intercalated between the neighboring lipid polar headgroup (3) high concentration of MPB favored formation of crystalline and glassy phases.

Encapsulation of boswellic acid with β- and hydroxypropyl-β-cyclodextrin: Synthesis, characterization, in vitro drug release and molecular modelling studies

NASA Astrophysics Data System (ADS)

Tambe, Amruta; Pandita, Nancy; Kharkar, Prashant; Sahu, Niteshkumar

2018-02-01

Boswellic acids (BAs) are a group of pentacyclic triterpenes present in gum-resin of Boswellia serrata. They are well known for their anti-inflammatory, hypolipidemic, immunomodulatory and anti-tumor activity, but they have poor aqueous solubility and limited bioavailability. In order to enhance their aqueous solubility, inclusion complexes of BAs with β-cyclodextrin (β-CD) and hydroxypropyl-β-cyclodextrin (HP-β-CD) were synthesized and their drug release profiles were studied. Molecular associations of β-CD and HP-β-CD with BAs were investigated by phase solubility studies. The stability constants were found to be 380.2 and 145.9 M-1 for BA: β-CD and BA: HP-β-CD inclusion complexes, respectively with AN- type curve. BA: β-CD and BA: HP-β-CD inclusion complexes were synthesized using kneading (KN), co-precipitation (CP) and solvent evaporation (SE) methods in 1:1 as well as 1:2 ratios. Further these were characterized by Fourier transform infrared (FTIR) spectrophotometry, Powder X-ray Diffraction (P-XRD) and Differential scanning calorimetric (DSC) analysis. FTIR analysis showed shifting of frequencies in complexes as compared to CDs and BAs. P-XRD data obtained for BA: β-CD complexes synthesized by CP and SE methods showed amorphous pattern. Also, DSC analysis showed a change in thermal behaviour for synthesized complexes. In vitro drug release studies of BA: β-CD complexes showed enhanced release with 1:2 complexes than 1:1 complexes at pH 1.2 and pH 6.8. Similarly, drug release enhancement was observed more with BA: HP-β-CD complexes in 1:2 ratio than 1:1. To understand the interaction of BAs with CD cavity molecular modelling studies were performed which favored 1:2 complex formation over 1:1 complexes. The study thus highlights that CDs can be used for solubility and dissolution enhancement of BAs.

Multiplexed droplet single-cell RNA-sequencing using natural genetic variation.

PubMed

Kang, Hyun Min; Subramaniam, Meena; Targ, Sasha; Nguyen, Michelle; Maliskova, Lenka; McCarthy, Elizabeth; Wan, Eunice; Wong, Simon; Byrnes, Lauren; Lanata, Cristina M; Gate, Rachel E; Mostafavi, Sara; Marson, Alexander; Zaitlen, Noah; Criswell, Lindsey A; Ye, Chun Jimmie

2018-01-01

Droplet single-cell RNA-sequencing (dscRNA-seq) has enabled rapid, massively parallel profiling of transcriptomes. However, assessing differential expression across multiple individuals has been hampered by inefficient sample processing and technical batch effects. Here we describe a computational tool, demuxlet, that harnesses natural genetic variation to determine the sample identity of each droplet containing a single cell (singlet) and detect droplets containing two cells (doublets). These capabilities enable multiplexed dscRNA-seq experiments in which cells from unrelated individuals are pooled and captured at higher throughput than in standard workflows. Using simulated data, we show that 50 single-nucleotide polymorphisms (SNPs) per cell are sufficient to assign 97% of singlets and identify 92% of doublets in pools of up to 64 individuals. Given genotyping data for each of eight pooled samples, demuxlet correctly recovers the sample identity of >99% of singlets and identifies doublets at rates consistent with previous estimates. We apply demuxlet to assess cell-type-specific changes in gene expression in 8 pooled lupus patient samples treated with interferon (IFN)-β and perform eQTL analysis on 23 pooled samples.

Experimental Studies on the Synthesis and Performance of Boron-containing High Temperature Resistant Resin Modified by Hydroxylated Tung Oil

NASA Astrophysics Data System (ADS)

Zhang, J. X.; Y Ren, Z.; Zheng, G.; Wang, H. F.; Jiang, L.; Fu, Y.; Yang, W. Q.; He, H. H.

2017-12-01

In this work, hydroxylated tung oil (HTO) modified high temperature resistant resin containing boron and benzoxazine was synthesized. HTO and ethylenediamine was used to toughen the boron phenolic resin with specific reaction. The structure of product was studied by Fourier-transform infrared spectroscopy(FTIR), and the heat resistance was tested by Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis(TGA). The results indicated that the conjugated triene structure of HTO was involved in the crosslinking of the heating curing progress, and in addition, the open-loop polymerization reaction of benzoxazine resin during heating can effectively reduce the curing temperature of the resin and reduce the release of small molecule volatiles, which is advantageous to follow-up processing. DSC data showed that the initial decomposition temperature of the resin is 350-400 °C, the carbon residue rate under 800 °C was 65%. It indicated that the resin has better heat resistance than normal boron phenolic resin. The resin can be used as an excellent ablative material and anti-friction material and has a huge application market in many fields.

Sparse Feature Selection Identifies H2A.Z as a Novel, Pattern-Specific Biomarker for Asymmetrically Self-Renewing Distributed Stem Cells

PubMed Central

Huh, Yang Hoon; Noh, Minsoo; Burden, Frank R.; Chen, Jennifer C.; Winkler, David A.; Sherley, James L.

2015-01-01

There is a long-standing unmet clinical need for biomarkers with high specificity for distributed stem cells (DSCs) in tissues, or for use in diagnostic and therapeutic cell preparations (e.g., bone marrow). Although DSCs are essential for tissue maintenance and repair, accurate determination of their numbers for medical applications has been problematic. Previous searches for biomarkers expressed specifically in DSCs were hampered by difficulty obtaining pure DSCs and by the challenges in mining complex molecular expression data. To identify DSC such useful and specific biomarkers, we combined a novel sparse feature selection method with combinatorial molecular expression data focused on asymmetric self-renewal, a conspicuous property of DSCs. The analysis identified reduced expression of the histone H2A variant H2A.Z as a superior molecular discriminator for DSC asymmetric self-renewal. Subsequent molecular expression studies showed H2A.Z to be a novel “pattern-specific biomarker” for asymmetrically self-renewing cells with sufficient specificity to count asymmetrically self-renewing DSCs in vitro and potentially in situ. PMID:25636161

Characterization of Antibiotic-Loaded Alginate-Osa Starch Microbeads Produced by Ionotropic Pregelation

PubMed Central

Fontes, Gizele Cardoso; Calado, Verônica Maria Araújo; Rossi, Alexandre Malta; da Rocha-Leão, Maria Helena Miguez

2013-01-01

The aim of this study was to characterize the penicillin-loaded microbeads composed of alginate and octenyl succinic anhydride (OSA) starch prepared by ionotropic pregelation with calcium chloride and to evaluate their in vitro drug delivery profile. The beads were characterized by size, scanning electron microscopy (SEM), zeta potential, swelling behavior, and degree of erosion. Also, the possible interaction between penicillin and biopolymers was investigated by differential scanning calorimetry (DSC), powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) analysis. The SEM micrograph results indicated a homogeneous drug distribution in the matrix. Also, based on thermal analyses (TGA/DSC), interactions were detected between microbead components. Although FTIR spectra of penicillin-loaded microbeads did not reveal the formation of new chemical entities, they confirmed the chemical drug stability. XRD patterns showed that the incorporated crystalline structure of penicillin did not significantly alter the primarily amorphous polymeric network. In addition, the results confirmed a prolonged penicillin delivery system profile. These results imply that alginate and OSA starch beads can be used as a suitable controlled-release carrier for penicillin. PMID:23862146

Research on surface modification of nano-zirconia

NASA Astrophysics Data System (ADS)

Chen, Wen; Zhang, Cun-Lin; Yang, Xiao-Yi

2005-02-01

The mechanisms about the aggregation and dispersibility of nano-zirconia were analyzed in detail. And nano-zirconia powders which were surface-modified with silane coupling reagent WD70 were prepared in order to disperse homogeneously in ethanol in this investigation. The grain size and grain phase of nano-zirconia were obtained by XRD. Research and characterization on the structure and surface characteristic of surface-modified nano-zirconia were achieved by XPS, TG-DSC, TEM and FT-IR. The results given by FT-IR and XPS showed WD70 was jointed on the surface of nano-zirconia through both physical adsorption and chemical binding after the de-methanol reaction between the methoxyl groups of WD70 and the hydroxy groups on the surface of nano-zirconia. And the corresponding model of surface-modified nano-zirconia was given. The images provided by TEM presented intuitionistic effect of surface modification on the dispersibility of nano-zirconia in ethanol. And TG-DSC analysis ascertained the amount of WD70 that was jointed on the surface of nano-zirconia and the amount was about 6.21 percent.

Material selection and evaluation of new encapsulation compounds for electric cables for launch support system

NASA Technical Reports Server (NTRS)

Ray, Asit K.

1992-01-01

Eight urethane compounds were evaluated as possible replacement for the existing encapsulating compoounds for electrical cables for the Launch Support System at Kennedy Space Center (KSC). The existing encapsulating compound, PR-1535, contains the curative MOCA 4-4'-Methylene-BIS (2-chloroaniline), which is a suspect carcinogen and hence may be the subject of further restrictions of its use by the Occupational Safety and Health Administration (OSHA). The samples made in the configuration of cable joints and in the form of disks were evaluated for flammability and hypergolic compatibility. These also underwent accelerated weatherability tests that measured the residual hardness of the exposed samples. Three candidates and the existing compound passed the hardness test. Of these, only one candidate and the existing compound passed the flammability test. The thermal and hydrolytic stability (weatherability) of these samples was studied using thermogravimetric analysis (DSC) techniques. The TMA and DSC data correlated with the residual hardness data; whereas, the TGA data showed no correlation. A hypergolic compatibility test will be conducted on the compound V-356-HE80, which passed both the flammability and accelerated weatherability tests.

Extraction and Physicochemical Characterization of a New Polysaccharide Obtained from the Fresh Fruits of Abelmoschus Esculentus

PubMed Central

Emeje, Martins; Isimi, Christiana; Byrn, Stephen; Fortunak, Joseph; Kunle, Olobayo; Ofoefule, Sabinus

2011-01-01

This paper is the first multi-scale characterization of the fluidize-dried gum extracted from the fresh fruits of the plant Abelmoschus esculentus. It describes the physical, thermal, sorptional and functional properties of this natural gum. Elemental analysis, scanning electron microscopy (SEM), particle size analysis, X-ray powder diffraction (XPRD), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transmittance infra red (FT-IR), and nuclear magnetic resonance (NMR) spectroscopy were used to characterize the gum sample. Abelmoschus Esculentus Gum (AEG) had a glass transition temperature (Tg) of 70°C and no melting peak. It showed a 14.91% loss in weight at 195°C. X-ray diffractogram showed numerous broad halos for AEG. Elemental analysis showed that AEG contains 39.5, 7.3, 51.8, and 1.4% carbon, hydrogen, oxygen and nitrogen respectively. The results obtained in this study established the fundamental characteristics of AEG and suggests its potential application in the food, cosmetic and pharmaceutical sectors. PMID:24250349

A theoretical framework to model DSC-MRI data acquired in the presence of contrast agent extravasation

NASA Astrophysics Data System (ADS)

Quarles, C. C.; Gochberg, D. F.; Gore, J. C.; Yankeelov, T. E.

2009-10-01

Dynamic susceptibility contrast (DSC) MRI methods rely on compartmentalization of the contrast agent such that a susceptibility gradient can be induced between the contrast-containing compartment and adjacent spaces, such as between intravascular and extravascular spaces. When there is a disruption of the blood-brain barrier, as is frequently the case with brain tumors, a contrast agent leaks out of the vasculature, resulting in additional T1, T2 and T*2 relaxation effects in the extravascular space, thereby affecting the signal intensity time course and reducing the reliability of the computed hemodynamic parameters. In this study, a theoretical model describing these dynamic intra- and extravascular T1, T2 and T*2 relaxation interactions is proposed. The applicability of using the proposed model to investigate the influence of relevant MRI pulse sequences (e.g. echo time, flip angle), and physical (e.g. susceptibility calibration factors, pre-contrast relaxation rates) and physiological parameters (e.g. permeability, blood flow, compartmental volume fractions) on DSC-MRI signal time curves is demonstrated. Such a model could yield important insights into the biophysical basis of contrast-agent-extravasastion-induced effects on measured DSC-MRI signals and provide a means to investigate pulse sequence optimization and appropriate data analysis methods for the extraction of physiologically relevant imaging metrics.

Serious game training improves performance in combat life-saving interventions.

PubMed

Planchon, Jerome; Vacher, Anthony; Comblet, Jeremy; Rabatel, Eric; Darses, Françoise; Mignon, Alexandre; Pasquier, Pierre

2018-01-01

In modern warfare, almost 25% of combat-related deaths are considered preventable if life-saving interventions are performed. Therefore, Tactical Combat Casualty Care (TCCC) training for soldiers is a major challenge. In 2014, the French Military Medical Service supported the development of 3D-SC1 ® , a serious game designed for the French TCCC program, entitled Sauvetage au Combat de niveau 1 (SC1). Our study aimed to evaluate the impact on performance of additional training with 3D-SC1 ® . The study assessed the performance of soldiers randomly assigned to one of two groups, before (measure 1) and after (measure 2) receiving additional training. This training involved either 3D-SC1 ® (Intervention group), or a DVD (Control group). The principal measure was the individual performance (on a 16-point scale), assessed by two investigators during a hands-on simulation. First, the mean performance score was compared between the two measures for Intervention and Control groups using a two-tailed paired t-test. Second, a multivariable linear regression was used to determine the difference in the impacts of 3D-SC1 ® and DVD training, and the order of presentation of the two scenarios, on the mean change from baseline in performance scores. A total of 96 subjects were evaluated: seven could not be followed-up, while 50 were randomly allocated to the Intervention group, and 39 to the Control group. Between measure 1 and measure 2, the mean (SD) performance score increased from 9.9 (3.13) to 14.1 (1.23), and from 9.4 (2.97) to 12.5 (1.83), for the Intervention group and Control group, respectively (p<0.0001). The adjusted mean difference in performance scores between 3D-SC1 ® and DVD training was 1.1 (95% confidence interval -0.3, 2.5) (p=0.14). Overall, the study found that supplementing SC1 training with either 3D-SC1 ® or DVD improved performance, assessed by a hands-on simulation. However, our analysis did not find a statistically significant difference between the effects of these two training tools. 3D-SC1 ® could be an efficient and pedagogical tool to train soldiers in life-saving interventions. In the current context of terrorist threat, a specifically-adapted version of 3D-SC1 ® may be a cost-effective and engaging way to train a large civilian public. Copyright © 2017 Elsevier Ltd. All rights reserved.

Identifying Hydrated Salts Using Simultaneous Thermogravimetric Analysis and Differential Scanning Calorimetry

ERIC Educational Resources Information Center

Harris, Jerry D.; Rusch, Aaron W.

2013-01-01

simultaneous thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) to characterize colorless, hydrated salts with anhydrous melting points less than 1100 degrees C. The experiment could be used to supplement the lecture discussing gravimetric techniques. It is…

Structural and thermal properties of silk fibroin - Silver nanoparticles composite films

NASA Astrophysics Data System (ADS)

Shivananda, C. S.; Rao B, B. Lakshmeesha; Shetty, G. Rajesh; Sangappa, Y.

2018-05-01

In this work, silk fibroin-silver nanoparticles (SF-AgNPs) composite films have been prepared by simple solution casting method. The composite films were examined for structural and thermal properties using X-ray diffraction (XRD), thermogravimatric (TGA) and differential scanning calorimetry (DSC) analysis. The XRD results showed that with the introduction of AgNPs in the silk fibroin matrix the amorphous nature of the silk fibroin decreases with increasing nanoparticles concentration. The silk fibroin films possess good thermal stability with the presence of AgNPs.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dan, K.; Roy, M.; Datta, A.

The present manuscript describes the role of entropic and enthalpic forces mediated by organic non-polar (hexane) and polar (methanol) solvents on the bulk and microscopic phase transition of a well known nematic liquid crystalline material MBBA (N-(4-methoxybenzylidene)-4-butylaniline) through Differential Scanning calorimetry (DSC), UV-Visible (UV–Vis), and Fourier Transform Infrared (FTIR) spectroscopy. DSC study indicates continuous linear decreases in both nematic-isotropic (N-I) phase transition temperature and enthalpy of MBBA in presence of hexane while both these parameters show a saturation after an initial decay in methanol. These distinct transitional behaviours were explained in terms of the “depletion force” model for entropic screeningmore » in hexane and “screening-self-screening” model for methanol. Heating rate dependent DSC studies find that non-Arrhenius behaviour, characteristic of pristine MBBA and a manifestation of non-equilibrium nature [Dan et al., J. Chem. Phys. 143, 094501 (2015)], is preserved in presence of entropic screening in the hexane solution, while it changes to Arrhenius behaviour (signifying equilibrium behaviour) in presence of enthalpic screening in methanol solution. FTIR spectra show similar dependence on the solvent induced screening in the intensities of the imine (—C = N) stretch and the out-of-plane distortion vibrations of the benzene rings of MBBA with hexane and methanol as in DSC, further establishing our entropic and enthalpic screening models. UV–Vis spectra of the electronic transitions in MBBA as a function of temperature also exhibit different dependences of intensities on the solvent induced screening, and an exponential decrease is observed in presence of hexane while methanol completely changes the nature of interaction to follow a linear dependence.« less

Status of dye solar cell technology as a guideline for further research.

PubMed

Hinsch, Andreas; Veurman, Welmoed; Brandt, Henning; Jensen, Katrine Flarup; Mastroianni, Simone

2014-04-14

Recently, the first commercial dye solar cell (DSC) products based on the mesoscopic principle were successfully launched. Introduction to the market has been accompanied by a strong increase in patent applications in the field during the last four years, which is a good indication of further commercialization activity. Materials and cell concepts have been developed to such extent that easy uptake by industrial manufacturers is possible. The critical phase for broad market acceptance has therefore been reached, which implies focusing on standardization-related research topics. In parallel the number of scientific publications on DSC is growing further (>3500 since 2012), and the range of new or renewed fundamental topics is broadening. A recent example is the introduction of the perovskite mesoscopic cell, for which an efficiency of 14.1% has been certified. Thus, a growing divergence between market introduction and research could be the consequence. Herein, an attempt is made to show that such an unwanted divergence can be prevented, for example, by developing suitable reference-type cell and module concepts as well as manufacturing routes. An in situ cell manufacturing concept that can be applied to mesoscopic-based solar cells in a broader sense is proposed. As a guideline for future module concepts, recent results for large-area, glass-frit-sealed DSC modules from efficiency studies (6.6% active-area efficiency) and outdoor analysis are discussed. Electroluminescence measurements are introduced as a quality tool. Another important point that is addressed is sustainability, which affects both market introduction and the direction of fundamental research. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of functionalized hydroxyapatite/poly(vinyl alcohol) composites

NASA Astrophysics Data System (ADS)

Stipniece, Liga; Salma-Ancane, Kristine; Rjabovs, Vitalijs; Juhnevica, Inna; Turks, Maris; Narkevica, Inga; Berzina-Cimdina, Liga

2016-06-01

Based on the well-known pharmaceutical excipient potential of poly(vinyl alcohol) (PVA) and clinical success of hydroxyapatite (HAp), the objective of this work was to fabricate functionalized composite microgranules. PVA was modified with succinic anhydride to introduce carboxyl groups (-COOH), respectively, by reaction between the -OH groups of PVA and succinic anhydride, for attachment of drug molecules. For the first time, the functionalized composite microgranules containing HAp/PVA in the ratio of 1:1 were prepared through in situ precipitation of HAp in modified PVA aqueous solutions followed by spray drying of obtained suspensions. The microgranules were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and differential scanning calorimetry (DSC). The presence of -COOH groups was verified by FT-IR, and the amount of functional groups added to PVA molecules (averaging 15 mol%) was determined by nuclear magnetic resonance spectroscopy (NMR). DSC results showed that modification with -COOH groups slightly decreased the thermal stability of PVA. FT-IR and XRD analysis confirmed that the resulting composites contain mainly nanocrystalline HAp and PVA. Moreover, the images taken by FE-SEM revealed that the microgranules consisted of nanosized HAp crystallites homogenously embedded in the PVA matrix. DSC measurements indicated that decomposition mechanism of the HAp/PVA differs from that of pure PVA and occurs at lower temperatures. However, the presence of HAp had minor influence on the thermal decomposition of the PVA modified with succinic anhydride. The investigation of composite microgranules confirmed interaction and integration between the HAp and PVA.

Solid-Solid Phase Transition Kinetics of FOX-7

DOE Office of Scientific and Technical Information (OSTI.GOV)

Burnham, A K; Weese, R K; Wang, R

Since it was developed in the late 1990s, 1,1-diamino-2,2-dinitroethene (FOX-7), with lower sensitivity and comparable performance to RDX, has received increasing interest. This paper will present our results for the phase changes of FOX-7 using DSC and HFC (Heat Flow Calorimetry). DSC thermal curves recorded at linear heating rates of 0.10, 0.35 and 1.0 C min{sup -1} show two endothermic peaks and two exothermic peaks. The two endothermic peaks represent solid-solid phase transitions, which have been observed in the literature at 114 C ({beta}-{gamma}) and 159 C ({gamma}-{delta}) by both DSC and XPD (X-ray powder diffraction) measurements. The first transitionmore » shifts from 114.5 to 115.8 C as the heating rate increases from 0.10 to 1.0 C min{sup -1}, while the second transition shifts from 158.5 to 160.4 C. Cyclical heating experiments show the endotherms and exotherms for a first heating through the {gamma} phase to the {delta} phase, a cooling and reversion to the {alpha} or {beta} phase, and a second heating to the {gamma} and {delta} phases. The data are interpreted using kinetic models with thermodynamic constraints.« less

Determining the critical relative humidity at which the glassy to rubbery transition occurs in polydextrose using an automatic water vapor sorption instrument.

PubMed

Yuan, Xiaoda; Carter, Brady P; Schmidt, Shelly J

2011-01-01

Similar to an increase in temperature at constant moisture content, water vapor sorption by an amorphous glassy material at constant temperature causes the material to transition into the rubbery state. However, comparatively little research has investigated the measurement of the critical relative humidity (RHc) at which the glass transition occurs at constant temperature. Thus, the central objective of this study was to investigate the relationship between the glass transition temperature (Tg), determined using thermal methods, and the RHc obtained using an automatic water vapor sorption instrument. Dynamic dewpoint isotherms were obtained for amorphous polydextrose from 15 to 40 °C. RHc was determined using an optimized 2nd-derivative method; however, 2 simpler RHc determination methods were also tested as a secondary objective. No statistical difference was found between the 3 RHc methods. Differential scanning calorimetry (DSC) Tg values were determined using polydextrose equilibrated from 11.3% to 57.6% RH. Both standard DSC and modulated DSC (MDSC) methods were employed, since some of the polydextrose thermograms exhibited a physical aging peak. Thus, a tertiary objective was to compare Tg values obtained using 3 different methods (DSC first scan, DSC rescan, and MDSC), to determine which method(s) yielded the most accurate Tg values. In general, onset and midpoint DSC first scan and MDSC Tg values were similar, whereas onset and midpoint DSC rescan values were different. State diagrams of RHc and experimental temperature and Tg and %RH were compared. These state diagrams, though obtained via very different methods, showed relatively good agreement, confirming our hypothesis that water vapor sorption isotherms can be used to directly detect the glassy to rubbery transition. Practical Application: The food polymer science (FPS) approach, pioneered by Slade and Levine, is being successfully applied in the food industry for understanding, improving, and developing food processes and products. However, despite its extreme usefulness, the Tg, a key element of the FPS approach, remains a challenging parameter to routinely measure in amorphous food materials, especially complex materials. This research demonstrates that RHc values, obtained at constant temperature using an automatic water vapor sorption instrument, can be used to detect the glassy to rubbery transition and are similar to the Tg values obtained at constant %RH, especially considering the very different approaches of these 2 methods--a transition from surface adsorption to bulk absorption (water vapor sorption) versus a step change in the heat capacity (DSC thermal method).

Deconvolution of complex differential scanning calorimetry profiles for protein transitions under kinetic control.

PubMed

Toledo-Núñez, Citlali; Vera-Robles, L Iraís; Arroyo-Maya, Izlia J; Hernández-Arana, Andrés

2016-09-15

A frequent outcome in differential scanning calorimetry (DSC) experiments carried out with large proteins is the irreversibility of the observed endothermic effects. In these cases, DSC profiles are analyzed according to methods developed for temperature-induced denaturation transitions occurring under kinetic control. In the one-step irreversible model (native → denatured) the characteristics of the observed single-peaked endotherm depend on the denaturation enthalpy and the temperature dependence of the reaction rate constant, k. Several procedures have been devised to obtain the parameters that determine the variation of k with temperature. Here, we have elaborated on one of these procedures in order to analyze more complex DSC profiles. Synthetic data for a heat capacity curve were generated according to a model with two sequential reactions; the temperature dependence of each of the two rate constants involved was determined, according to the Eyring's equation, by two fixed parameters. It was then shown that our deconvolution procedure, by making use of heat capacity data alone, permits to extract the parameter values that were initially used. Finally, experimental DSC traces showing two and three maxima were analyzed and reproduced with relative success according to two- and four-step sequential models. Copyright © 2016 Elsevier Inc. All rights reserved.

Preparation and Evaluation of Montelukast Sodium Loaded Solid Lipid Nanoparticles

PubMed Central

Priyanka, K; Sathali, A Abdul Hasan

2012-01-01

Solid lipid nanoparticles (SLNs) are an alternative carrier system used to load the drug for targeting, to improve the bioavailability by increasing its solubility, and protecting the drug from presystemic metabolism. The avoidance of presystemic metabolism is due to the nano-metric size range, so that the liver cannot uptake the drug from the delivery system and is not metabolized by the liver. Montelukast sodium is an anti-asthmatic drug, because of its poor oral bioavailability, presystemic metabolism, and decreased half-life; it was chosen to formulate as the solid lipid nanoparticle (SLN) system by hot homogenization followed by an ultrasonication method, to overcome the above. Compritol ATO 888, stearic acid, and glyceryl monostearate were used as a lipid matrix and polyvinyl alcohol as a surfactant. The prepared formulations have been evaluated for entrapment efficiency, drug content, in vitro drug release, particle size analysis, scanning electron microscopy, Fourier transform-infrared studies (FT-IR), differential scanning calorimetry (DSC), and stability. Particle size analysis revealed that the SLN prepared from the higher melting point lipid showed a larger particle size and with increased carbon chain length of the fatty acids. Entrapment efficiency (EE) was ranging from 42% to 92%. In vitro release studies showed maximum cumulative drug release was obtained for F 1 (59.1%) containing stearic acid, and the lowest was observed for F 18 (28.1%) containing compritol ATO 888 after 12 h and all the formulations followed first-order release kinetics. FT-IR and DSC studies revealed no interaction between drug and lipids. Studies showed that increase in lipid concentration, increased particle size, EE, and maintained the sustained release of drug. Among all, compritol ATO 888 was chosen as the best lipid for formulating SLN because it had high EE and sustained the drug release. PMID:23112531

Protecting Location Privacy for Outsourced Spatial Data in Cloud Storage

PubMed Central

Gui, Xiaolin; An, Jian; Zhao, Jianqiang; Zhang, Xuejun

2014-01-01

As cloud computing services and location-aware devices are fully developed, a large amount of spatial data needs to be outsourced to the cloud storage provider, so the research on privacy protection for outsourced spatial data gets increasing attention from academia and industry. As a kind of spatial transformation method, Hilbert curve is widely used to protect the location privacy for spatial data. But sufficient security analysis for standard Hilbert curve (SHC) is seldom proceeded. In this paper, we propose an index modification method for SHC (SHC∗) and a density-based space filling curve (DSC) to improve the security of SHC; they can partially violate the distance-preserving property of SHC, so as to achieve better security. We formally define the indistinguishability and attack model for measuring the privacy disclosure risk of spatial transformation methods. The evaluation results indicate that SHC∗ and DSC are more secure than SHC, and DSC achieves the best index generation performance. PMID:25097865

Protecting location privacy for outsourced spatial data in cloud storage.

PubMed

Tian, Feng; Gui, Xiaolin; An, Jian; Yang, Pan; Zhao, Jianqiang; Zhang, Xuejun

2014-01-01

As cloud computing services and location-aware devices are fully developed, a large amount of spatial data needs to be outsourced to the cloud storage provider, so the research on privacy protection for outsourced spatial data gets increasing attention from academia and industry. As a kind of spatial transformation method, Hilbert curve is widely used to protect the location privacy for spatial data. But sufficient security analysis for standard Hilbert curve (SHC) is seldom proceeded. In this paper, we propose an index modification method for SHC (SHC(∗)) and a density-based space filling curve (DSC) to improve the security of SHC; they can partially violate the distance-preserving property of SHC, so as to achieve better security. We formally define the indistinguishability and attack model for measuring the privacy disclosure risk of spatial transformation methods. The evaluation results indicate that SHC(∗) and DSC are more secure than SHC, and DSC achieves the best index generation performance.

Application and interpretation of functional data analysis techniques to differential scanning calorimetry data from lupus patients.

PubMed

Kendrick, Sarah K; Zheng, Qi; Garbett, Nichola C; Brock, Guy N

2017-01-01

DSC is used to determine thermally-induced conformational changes of biomolecules within a blood plasma sample. Recent research has indicated that DSC curves (or thermograms) may have different characteristics based on disease status and, thus, may be useful as a monitoring and diagnostic tool for some diseases. Since thermograms are curves measured over a range of temperature values, they are considered functional data. In this paper we apply functional data analysis techniques to analyze differential scanning calorimetry (DSC) data from individuals from the Lupus Family Registry and Repository (LFRR). The aim was to assess the effect of lupus disease status as well as additional covariates on the thermogram profiles, and use FD analysis methods to create models for classifying lupus vs. control patients on the basis of the thermogram curves. Thermograms were collected for 300 lupus patients and 300 controls without lupus who were matched with diseased individuals based on sex, race, and age. First, functional regression with a functional response (DSC) and categorical predictor (disease status) was used to determine how thermogram curve structure varied according to disease status and other covariates including sex, race, and year of birth. Next, functional logistic regression with disease status as the response and functional principal component analysis (FPCA) scores as the predictors was used to model the effect of thermogram structure on disease status prediction. The prediction accuracy for patients with Osteoarthritis and Rheumatoid Arthritis but without Lupus was also calculated to determine the ability of the classifier to differentiate between Lupus and other diseases. Data were divided 1000 times into separate 2/3 training and 1/3 test data for evaluation of predictions. Finally, derivatives of thermogram curves were included in the models to determine whether they aided in prediction of disease status. Functional regression with thermogram as a functional response and disease status as predictor showed a clear separation in thermogram curve structure between cases and controls. The logistic regression model with FPCA scores as the predictors gave the most accurate results with a mean 79.22% correct classification rate with a mean sensitivity = 79.70%, and specificity = 81.48%. The model correctly classified OA and RA patients without Lupus as controls at a rate of 75.92% on average with a mean sensitivity = 79.70% and specificity = 77.6%. Regression models including FPCA scores for derivative curves did not perform as well, nor did regression models including covariates. Changes in thermograms observed in the disease state likely reflect covalent modifications of plasma proteins or changes in large protein-protein interacting networks resulting in the stabilization of plasma proteins towards thermal denaturation. By relating functional principal components from thermograms to disease status, our Functional Principal Component Analysis model provides results that are more easily interpretable compared to prior studies. Further, the model could also potentially be coupled with other biomarkers to improve diagnostic classification for lupus.

Comparative Study Of Various Grades Of Polyethylene By Differential Scanning Calorimetry (DSC) Correlated With Raman Spectroscopy

NASA Astrophysics Data System (ADS)

Jumeau, Richard; Bourson, Patrice; Ferriol, Michel; Lahure, François; Ducos, Franck; Ligneron, Jérôme

2011-05-01

Polyethylene (PE) is a very important material. In 2008, almost 30% of the world plastics production was dedicated to this polymer (70 million tons) [1]. It is a consumer polymer because of its moderate cost of manufacturing and its physical and mechanical properties compatible with various applications in everyday life. Indeed, PE is generally easily processable. It possesses an excellent electric insulation and shock resistance combined with a very good chemical and biological inertia [2]. For each application, there is a particular grade, i.e. a polyethylene with well defined rheological properties. Therefore, it is essential to know how to differentiate these different grades by suitable methods of characterization. Differential Scanning Calorimetry (DSC) is one of the techniques usually used for this purpose. The knowledge of characteristic temperatures such as melting, cold crystallization or glass transition gives information on the viscosity and thus, on the grade of the polymer. DSC also allows the detection of defects, (for example, presence of unmelted pieces). However DSC is a tedious method for on-line quality control, limiting its scope. The determination of the polymer structure represents a major challenge in the industrial world of polymers. Raman spectroscopy, another technique of polymer analysis, is nowadays growing fast because of the advantages it presents. It is a non-destructive method, capable of also giving useful information about the morphology of the polymer. This technique can be perfectly used in industry by means of adapted sensors and devices with more and more reduced dimensions [3]. That technique is used to obtain the characteristic temperatures of PE and information on the polymer structure. The purpose of this article is to establish the correlation between the viscosity of a polymer and its characteristic temperatures obtained by DSC and subsequent possibilities of quality control in industry. These measurements are correlated with others obtained by Raman spectroscopy, to get additional details concerning the structure and transitions of the material, the final goal being to use these results in on-line analysis.

Delayed Sternal Closure in Infant Heart Surgery-The Importance of Where and When: An Analysis of the STS Congenital Heart Surgery Database.

PubMed

Nelson-McMillan, Kristen; Hornik, Christoph P; He, Xia; Vricella, Luca A; Jacobs, Jeffrey P; Hill, Kevin D; Pasquali, Sara K; Alejo, Diane E; Cameron, Duke E; Jacobs, Marshall L

2016-11-01

Delayed sternal closure (DSC) is commonly used to optimize hemodynamic stability after neonatal and infant heart surgery. We hypothesized that duration of sternum left open (SLO) was associated with rate of infection complications, and that location of sternal closure may mitigate infection risk. Infants (age ≤365 days) undergoing index operations with cardiopulmonary bypass and DSC at STS Congenital Heart Surgery Database centers (from 2007 to 2013) with adequate data quality were included. Primary outcome was occurrence of infection complication, defined as one or more of the following: endocarditis, pneumonia, wound infection, wound dehiscence, sepsis, or mediastinitis. Multivariable regression models were fit to assess association of infection complication with: duration of SLO (days), location of DSC procedure (operating room versus elsewhere), and patient and procedural factors. Of 6,127 index operations with SLO at 100 centers, median age and weight were 8 days (IQR, 5-24) and 3.3 kg (IQR, 2.9-3.8); 66% of operations were STAT morbidity category 4 or 5. At least one infection complication occurred in 18.7%, compared with 6.6% among potentially eligible neonates and infants without SLO. Duration of SLO (median, 3 days; IQR, 2-5) was associated with an increased rate of infection complications (p < 0.001). Location of DSC procedure was operating room (16%), intensive care unit (67%), or other (17%). Location of DSC was not associated with rate of infection complications (p = 0.45). Rate of occurrence of infectious complications is high among infants with sternum left open following cardiac surgery. Longer duration of SLO is associated with increased infection complications. Copyright © 2016 The Society of Thoracic Surgeons. Published by Elsevier Inc. All rights reserved.

Testing the Multispecimen Absolute Paleointensity Method with Archaeological Baked Clays and Bricks: New Data for Central Europe

NASA Astrophysics Data System (ADS)

Schnepp, Elisabeth; Leonhardt, Roman

2014-05-01

The domain-state corrected multiple-specimen paleointensity determination technique (MSP-DSC, Fabian & Leonhardt, EPSL 297, 84, 2010) has been tested for archaeological baked clays and bricks. The following procedure was applied: (1) Exclusion of secondary overprints using alternating field (AF) or thermal demagnetization and assignment of characteristic remanent magnetization (ChRM) direction. (2) Determination of magneto mineralogical alteration using anhysteretic remanent magnetization (ARM) or temperature dependence of susceptibility. (3) Measurement of ARM anisotropy tensor, calculation of the ancient magnetic field direction. (4) Sister specimens were subjected to the MSP-DSC technique aligned (anti-)parallel to the ancient magnetic field direction. (5) Several checks were applied in order to exclude data points from further evaluation: (a) The accuracy of orientation (< 10°), (b) absence of secondary components (< 10°), (c) use of a considerable NRM fraction (20 to 80%), (d) weak alteration (smaller than for domain state change) and finally (e) domain state correction was applied. Bricks and baked clays from archaeological sites with ages between 645 BC and 2003 AD have been subjected to MSP-DSC absolute paleointensity (PI) determination. Aims of study are to check precision and reliability of the method. The obtained PI values are compared with direct field observation, the IGRF, the GUFM1 or Thellier results. The Thellier experiments often show curved lines and pTRM checks fail for higher temperatures. Nevertheless in the low temperature range straight lines have been obtained but they provide scattered paleointensity values. Mean paleointensites have relative errors often exceeding 10%, which are not considered as high quality PI estimates. MSP-DSC experiments for the structures older than 300 years are still under progress. The paleointensities obtained from the MSP-DSC experiments for the young materials (after 1700 AD) have small relative errors of a few or even less than one per cent, although the data points are scattered in some cases. For these sites comparison with the historical field values shows very good agreement. Small deviations could be explained by the higher cooling rates used in the laboratory. These young structures were made of bricks and the unweathered baked clay of the 2003 experimental kiln was like brick, either. The sites provided much material so that tests were done to investigate the MSP-DSC methodology further. For example it was tested, if different NRM deblocking fractions have influence on the paleointensity estimate. It seems that use of fractions lower than 20% of the NRM can lead to an underestimation of PI. Although MSP-DSC experiments carried out on different blocks of the same structure can provide very similar results, the use of several fragments from at least five different units (potshards, bricks, in situ burnt blocks or rocks) of the same structure is recommended in or to obtain a reliable estimate of the experimental errors. Five data points may define already a well constraint straight line, but for a better precision 15 (< 2%) data points may be required. For the young structures the MSP-DSC method provided reliable PI estimates which have been included into the archaeointensity data base

Study of tellurium precipitates in CdTe crystals

NASA Technical Reports Server (NTRS)

Jayatirtha, H. N.; Henderson, D. O.; Burger, A.; Volz, M. P.

1993-01-01

The effect of tellurium precipitates was studied in medium resistivity (10 exp 3-10 exp 6 ohm cm) undoped and Cl-doped CdTe using differential scanning calorimetry (DSC) and mid-infrared spectroscopy and the results were correlated with near-infrared microscopy photographs. When present in a significant quantity (about 0.25 wt pct), we show that Te precipitates are detectable using DSC measurements. In the mid-infrared, the contribution of the absorption by free-carriers is negligible, and therefore, the effect of the Te precipitates in these crystals can be considered uncoupled from the effects of Cd vacancies.

Crystal Growth of Undoped and Doped ZnSe

NASA Technical Reports Server (NTRS)

Davis, Swanson L.; Chen, K.-T.; George, M. A.; Shi, D. T.; Collins, W. E.; Burger, Arnold

1997-01-01

The surface morphology of freshly cleaved ZnSe single crystal grown by the physical vapor transport (PVT) method was investigated by Atomic Force Microscopy (AFM) and the results were correlated with Differential Scanning Calorimetry (DSC) data. Selenium precipitates have been revealed in undoped doped ZnSe crystals having a size of about 50 nm. A transition temperature around 221 C in the DSC measurements is interpreted as the eutectic temperature of Se-saturated ZnSe. The AFM images of doped ZnSe also show that possible Cr clusters are uniformly distributed and they have an estimated size of about 6 nm.

Investigation of Water Absorption and Diffusion in Microparticles Containing Xylitol to Provide a Cooling Effect by Thermal Analysis

NASA Astrophysics Data System (ADS)

Salaün, F.; Bedek, G.; Devaux, E.; Dupont, D.; Deranton, D.

2009-08-01

Polyurethane microparticles containing xylitol as a sweat sensor system were prepared by interfacial polymerization. The structural and thermal properties of the resultant microparticles were studied. The surface morphology and chemical structure of microparticles were investigated using an optical microscope (OM) and a Fourier-transform infrared spectroscope (FTIR), respectively. The thermal properties of samples were investigated by thermogravimetric analysis (TGA) and by differential scanning calorimetry (DSC). Thus, two types of microparticles were synthesized by varying the percentage of monomers introduced. The obtained morphology is directly related to the synthesis conditions. DSC analysis indicated that the mass content of crystalline xylitol was up to 63.8 %, which resulted in a high enthalpy of dilution of 127.7 J · g-1. Furthermore, the water release rate monitored by TGA analysis was found to be faster from the microparticles than from raw xylitol. Thus, the microparticles could be applied for thermal energy storage and moisture sensor enhancement.

Thermal decomposition of ammonium perchlorate in the presence of Al(OH)(3)·Cr(OH)(3) nanoparticles.

PubMed

Zhang, WenJing; Li, Ping; Xu, HongBin; Sun, Randi; Qing, Penghui; Zhang, Yi

2014-03-15

An Al(OH)(3)·Cr(OH)(3) nanoparticle preparation procedure and its catalytic effect and mechanism on thermal decomposition of ammonium perchlorate (AP) were investigated using transmission electron microscopy (TEM), X-ray diffraction (XRD), thermogravimetric analysis and differential scanning calorimetry (TG-DSC), X-ray photoelectron spectroscopy (XPS), and thermogravimetric analysis and mass spectroscopy (TG-MS). In the preparation procedure, TEM, SAED, and FT-IR showed that the Al(OH)(3)·Cr(OH)(3) particles were amorphous particles with dimensions in the nanometer size regime containing a large amount of surface hydroxyl under the controllable preparation conditions. When the Al(OH)(3)·Cr(OH)(3) nanoparticles were used as additives for the thermal decomposition of AP, the TG-DSC results showed that the addition of Al(OH)(3)·Cr(OH)(3) nanoparticles to AP remarkably decreased the onset temperature of AP decomposition from approximately 450°C to 245°C. The FT-IR, RS and XPS results confirmed that the surface hydroxyl content of the Al(OH)(3)·Cr(OH)(3) nanoparticles decreased from 67.94% to 63.65%, and Al(OH)3·Cr(OH)3 nanoparticles were limitedly transformed from amorphous to crystalline after used as additives for the thermal decomposition of AP. Such behavior of Al(OH)(3)·Cr(OH)(3) nanoparticles promoted the oxidation of NH3 of AP to decompose to N2O first, as indicated by the TG-MS results, accelerating the AP thermal decomposition. Copyright © 2014 Elsevier B.V. All rights reserved.

Minimisation of Signal Intensity Differences in Distortion Correction Approaches of Brain Magnetic Resonance Diffusion Tensor Imaging.

PubMed

Lee, Dong-Hoon; Lee, Do-Wan; Henry, David; Park, Hae-Jin; Han, Bong-Soo; Woo, Dong-Cheol

2018-04-12

To evaluate the effects of signal intensity differences between the b0 image and diffusion tensor imaging (DTI) in the image registration process. To correct signal intensity differences between the b0 image and DTI data, a simple image intensity compensation (SIMIC) method, which is a b0 image re-calculation process from DTI data, was applied before the image registration. The re-calculated b0 image (b0 ext ) from each diffusion direction was registered to the b0 image acquired through the MR scanning (b0 nd ) with two types of cost functions and their transformation matrices were acquired. These transformation matrices were then used to register the DTI data. For quantifications, the dice similarity coefficient (DSC) values, diffusion scalar matrix, and quantified fibre numbers and lengths were calculated. The combined SIMIC method with two cost functions showed the highest DSC value (0.802 ± 0.007). Regarding diffusion scalar values and numbers and lengths of fibres from the corpus callosum, superior longitudinal fasciculus, and cortico-spinal tract, only using normalised cross correlation (NCC) showed a specific tendency toward lower values in the brain regions. Image-based distortion correction with SIMIC for DTI data would help in image analysis by accounting for signal intensity differences as one additional option for DTI analysis. • We evaluated the effects of signal intensity differences at DTI registration. • The non-diffusion-weighted image re-calculation process from DTI data was applied. • SIMIC can minimise the signal intensity differences at DTI registration.

Investigation of Thermal and Viscoelastic Properties of Polymers Relevant to Hot Melt Extrusion, IV: Affinisol™ HPMC HME Polymers.

PubMed

Gupta, Simerdeep Singh; Solanki, Nayan; Serajuddin, Abu T M

2016-02-01

Most cellulosic polymers cannot be used as carriers for preparing solid dispersion of drugs by hot melt extrusion (HME) due to their high melt viscosity and thermal degradation at high processing temperatures. Three HME-grade hydroxypropyl methylcelluloses, namely Affinisol™ HPMC HME 15 cP, Affinisol™ HPMC HME 100 cP, and Affinisol™ HPMC HME 4 M, have recently been introduced by The Dow Chemical Co. to enable the preparation of solid dispersion at lower and more acceptable processing temperatures. In the present investigation, physicochemical properties of the new polymers relevant to HME were determined and compared with that of Kollidon(®) VA 64. Powder X-ray diffraction (PXRD), modulated differential scanning calorimetry (mDSC), thermogravimetric analysis (TGA), moisture sorption, rheology, and torque analysis by melt extrusion were applied. PXRD and mDSC showed that the Affinisol™ polymers were amorphous in nature. According to TGA, the onset of degradation for all polymers was >220°C. The Affinisol™ polymers exhibited less hygroscopicity than Kollidon(®) VA 64 and another HPMC polymer, Methocel™ K100LV. The complex viscosity profiles of the Affinisol™ polymers as a function of temperature were similar. The viscosity of the Affinisol™ polymers was highly sensitive to the shear rate applied, and unlike Kollidon(®) VA 64, the viscosity decreased drastically when the angular frequency was increased. Because of the very high shear rate encountered during melt extrusion, Affinisol™ polymers showed capability of being extruded at larger windows of processing temperatures as compared to that of Kollidon(®) VA 64.

Transforming Benzophenoxazine Laser Dyes into Chromophores for Dye-Sensitized Solar Cells: A Molecular Engineering Approach

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schröder, Florian A. Y. N.; Cole, Jacqueline M.; Waddell, Paul G.

2015-02-03

The re-functionalization of a series of four well-known industrial laser dyes, based on benzophenoxazine, is explored with the prospect of molecularly engineering new chromophores for dye-sensitized solar cell (DSC) applications. Such engineering is important since a lack of suitable dyes is stifling the progress of DSC technology. The conceptual idea involves making laser dyes DSC-active by chemical modification, while maintaining their key property attributes that are attractive to DSC applications. This molecular engineering follows a step-wise approach. Firstly, molecular structures and optical absorption properties are determined for the parent laser dyes: Cresyl Violet (1); Oxazine 170 (2); Nile Blue Amore » (3), Oxazine 750 (4). These reveal structure-property relationships which define the prerequisites for computational molecular design of DSC dyes; the nature of their molecular architecture (D-π-A) and intramolecular charge transfer. Secondly, new DSC dyes are computationally designed by the in silico addition of a carboxylic acid anchor at various chemical substitution points in the parent laser dyes. A comparison of the resulting frontier molecular orbital energy levels with the conduction band edge of a TiO2 DSC photoanode and the redox potential of two electrolyte options I-/I3- and Co(II/III)tris(bipyridyl) suggests promise for these computationally designed dyes as co-sensitizers for DSC applications.« less

An evaluation of the thermal and mechanical properties of a salt-modified polyvinyl alcohol hydrogel for a knee meniscus application.

PubMed

Curley, Colin; Hayes, Jennifer C; Rowan, Neil J; Kennedy, James E

2014-12-01

The treatment of irreparable knee meniscus tears remains a major challenge for the orthopaedic community. The main purpose of this research was to analyse the mechanical properties and thermal behaviour of a salt-modified polyvinyl alcohol hydrogel, in order to assess its potential for use as an artificial meniscal implant. Aqueous poly vinyl alcohol was treated with a sodium sulphate solution to precipitate out the polyvinyl alcohol resulting in a pliable hydrogel. The freeze-thaw process, a strictly physical method of crosslinking, was employed to crosslink the hydrogel. Physical crosslinks in the form of crystalline regions were induced within the hydrogel structure which resulted in a large increase in mechanical resistance. Results showed that the optimal sodium sulphate addition of 6.6% (w/v) Na2SO4 in 8.33% (w/v) PVA causes the PVA to precipitate out of its solution. The effect of multiple freeze thaw cycles was also investigated. Investigation comprised of a variety of well-established characterisation techniques such as differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), mechanical analysis, rheometry and swelling studies. DSC analysis showed that samples cross-linked using the freeze thaw process display a thermal shift due to increased crosslink density. FTIR analysis confirmed crystallisation is present at 1142cm(-1) and also showed that no chemical alteration occurs when PVA is treated with sodium sulphate. Swelling studies indicated that that PVA/sodium sulphate hydrogels absorb less water than untreated hydrogels due to increased amounts of PVA present. Compressive strength analysis of PVA/sodium sulphate hydrogels prepared at -80°C displayed average maximum loads of 2472N, 2482.4N and 2476N of over 1, 3 and 5 freeze thaw cycles respectively. Mechanical analysis of the hydrogel indicated that the material is thermally stable and resistant to breakdown by compressive force. These properties are crucial for potential use as a meniscus or cartilage replacement. As such, the results of this study indicate that polyvinyl alcohol modified with sodium sulphate may be a suitable material for the construction of an artificial knee meniscus. Copyright © 2014 Elsevier Ltd. All rights reserved.

Development of a new ferulic acid certified reference material for use in clinical chemistry and pharmaceutical analysis.

PubMed

Yang, Dezhi; Wang, Fengfeng; Zhang, Li; Gong, Ningbo; Lv, Yang

2015-05-01

This study compares the results of three certified methods, namely differential scanning calorimetry (DSC), the mass balance (MB) method and coulometric titrimetry (CT), in the purity assessment of ferulic acid certified reference material (CRM). Purity and expanded uncertainty as determined by the three methods were respectively 99.81%, 0.16%; 99.79%, 0.16%; and 99.81%, 0.26% with, in all cases, a coverage factor (k) of 2 (P=95%). The purity results are consistent indicating that the combination of DSC, the MB method and CT provides a confident assessment of the purity of suitable CRMs like ferulic acid.

Research on choleretic effect of menthol, menthone, pluegone, isomenthone, and limonene in DanShu capsule.

PubMed

Hu, Guanying; Yuan, Xing; Zhang, Sanyin; Wang, Ruru; Yang, Miao; Wu, Chunjie; Wu, Zhigang; Ke, Xiao

2015-02-01

Danshu capsule (DSC) is a medicinal compound in traditional Chinese medicine (TCM). It is commonly used for the treatment of acute & chronic cholecystitis as well as choleithiasis. To study its choleretic effect, healthy rats were randomly divided into DSC high (DSCH, 900mg/kg), medium (DSCM, 450mg/kg), and low (DSCL, 225mg/kg) group, Xiaoyan Lidan tablet (XYLDT, 750mg/kg), and saline group. The bile was collected for 1h after 20-minute stabilization as the base level, and at 1h, 2h, 3h, and 4h after drug administration, respectively. Bile volume, total cholesterol, and total bile acid were measured at each time point. The results revealed that DSC significantly stimulated bile secretion, decreased total cholesterol level and increased total bile acid level. Therefore, it had choleretic effects. To identify the active components contributing to its choleretic effects, five major constituents which are menthol (39.33mg/kg), menthone (18.02mg/kg), isomenthone (8.18mg/kg), pluegone (3.31mg/kg), and limonene (4.39mg/kg) were tested on our rat model. The results showed that menthol and limonene could promote bile secretion when compared to DSC treatment (p > 0.05); Menthol, menthol and limonene could significantly decrease total cholesterol level (p<0.05 or p<0.01) as well as increase total bile acid level (p<0.05 or p<0.01); Isomenthone, as a isomer of menthone, existed slightly choleretic effects; Pluegone had no obvious role in bile acid efflux. These findings indicated that the choleretic effects of DSC may be attributed mainly to its three major constituents: menthol, menthone and limonene. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.

Influence of gamma irradiation on carbon nanotube-reinforced polypropylene.

PubMed

Castell, P; Medel, F J; Martinez, M T; Puértolas, J A

2009-10-01

Single walled carbon nanotubes (SWNT) have been incorporated into a polypropylene (PP) matrix in different concentrations (range: 0.25-2.5 wt%). The nanotubes were blended with PP particles (approximately 500 microm in size) before mixing in an extruder. Finally, rectangular plates were obtained by compression moulding. PP-SWNT composites were gamma irradiated at different doses, 10 and 20 kGy, to promote crosslinking in the matrix and potentially enhance the interaction between nanotubes and PP. Extensive thermal, structural and mechanical characterization was conducted by means of DSC, X-ray diffraction, Raman spectroscopy, uniaxial tensile tests and dynamic mechanical thermal (DMTA) techniques. DSC thermograms reflected higher crystallinity with increasing nanotube concentration. XRD analysis confirmed the only presence of a monoclinic crystals and proved unambiguously that CNTs generated a preferred orientation. Raman spectroscopy confirmed that the intercalation of the polymer between bundles is favored at low CNTs contents. Elastic modulus results confirmed the reinforcement of the polypropylene matrix with increasing SWNT concentration, although stiffness saturation was observed at the highest concentration. Loss tangent DMTA curves showed three transitions for raw polypropylene. While gamma relaxation remained practically unchanged in all the samples, beta relaxation temperatures showed an increase with increasing CNT content due to the reduced mobility of the system. Gamma-irradiated PP exhibited an increase in the beta relaxation temperature, associated with changes in glass transition due to radiation-induced crosslinking. On the contrary, gamma-irradiated nanocomposites did not show this effect probably due to the reaction of radiative free radicals with CNTs.

SU-E-J-107: The Impact of the Tumor Location to Deformable Image Registration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sugawara, Y; Tohoku University School of Medicine, Sendai, Miyagi; Tachibana, H

2015-06-15

Purpose: For four-dimensional planning and adaptive radiotherapy, the accuracy of deformable image registration (DIR) is essential. We evaluated the accuracy of an in-house program with the free-downloadable DIR software library package (NiftyReg) and two commercially available DIR software programs (MIM Maestro and Velocity AI) in lung SBRT cancer patients. In addition to it, the relationship between the tumor location and the accuracy of the DIRs was investigated. Methods: The free-form deformation was implemented in the in-house program and the MIM. The Velocity was based on the B-spline algorithm. The accuracy of the three programs was evaluated in comparison for themore » structures on 4DCT image datasets between at the peak-inhale and at the peak-exhale. The dice similarity coefficient (DSC) and normalized DSC (NDSC) were measured for the gross tumor volumes from 19 lung SBRT patients. Results: The DSC measurement showed the median values of the DSC were 0.885, 0.872 and 0.798 for the In-house program, the MIM and the Velocity, respectively. The Velocity showed significant difference compared to the others. The median NDSC values were 1.027, 1.005 and 0.946 for the In-house, the MIM and the Velocity, respectively. This indicated that the spatial overlap agreement between the reference and the deformed structure for the in-house and MIM was comparable with the accuracy within 1mm uncertainty. There was larger discrepancy within 1–2mm uncertainty for the Velocity. The In-house and the MIM showed the higher NDSC values than the median values when the GTV was not attached to the chest wall and diaphragm(p < 0.05). However, there is no relationship between the accuracy and the tumor location in the Velocity. Conclusion: The difference of the DIR program would affect different accuracy and the accuracy may be reduced when the tumor is located or attached to chest wall or diaphragm.« less

Effects of Processing on Structure and Thermal Properties of Powdered Preterm Infant Formula.

PubMed

Sun, Xiaomeng; Wang, Cuina; Wang, Hao; Guo, Mingruo

2018-06-01

Powdered infant formula is usually manufactured by ingredients mixing, homogenization, pasteurization, evaporation and spray drying. Effects of unit operations on the microstructure, thermal properties and other characteristics of preterm infant formula, fat (F), serum (S), and pellet (P) fractions on centrifugation were investigated using Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Differential Scanning Calorimetry (DSC), and Fourier Transform Infrared (FTIR) spectroscopy. After homogenization, particles which may be casein and denatured whey proteins were observed on the surface of F fraction in microstructure images. DSC results showed that the onset temperature of the second endothermic peak of F fraction shifted to higher temperature, and an endothermic transition appeared at 173.3 °C in P fraction. The -CH 2 group corresponding to F fraction showed less intensity in FTIR spectrum after homogenization. Microstructure images for S and P fractions showed larger aggregates due to the pasteurization processing. Apparent exothermic transition in DSC curve occurred at 101.6 °C indicated whey protein aggregation. Spray drying resulted in some open areas in F fraction and lager aggregates in S fraction revealed by microstructure pictures. A new exothermic transition appeared at 93.6 °C in DSC curve of S fraction. Changes in amide I and amide II regions in FTIR spectra of samples resulted from pasteurization and spray drying indicated the changes in secondary structure of casein and whey proteins. All results indicated that homogenization, pasteurization, and spray drying exhibited pronounced impacts on the microstructure, thermal properties and structural characteristics of samples. Preterm infant formula is an important dairy food for preborn infants. Our results indicate that unit operations especially homogenization, pasteurization, and spray drying during the processing have the most impacts on the microstructure, thermal properties and other characteristics of infant formula. This work provides further understanding of component interactions during the processing of infant formula and theoretical basis for the production of dairy food. © 2018 Institute of Food Technologists®.

Quantification of normal cerebral oxygen extraction and oxygen metabolism by phase-based MRI susceptometry: evaluation of repeatability using two different imaging protocols.

PubMed

Kämpe, Robin; Lind, Emelie; Ståhlberg, Freddy; van Westen, Danielle; Knutsson, Linda; Wirestam, Ronnie

2017-03-01

Global oxygen extraction fraction (OEF) and cerebral metabolic rate of oxygen (CMRO 2 ) were quantified in a test-retest study. Cerebral blood flow (CBF) data, required for CMRO 2 estimation, were obtained using dynamic susceptibility contrast MRI (DSC-MRI). OEF and CMRO 2 were quantified using two separate data sets, that is, conventional high-resolution (HR) gradient echo (GRE) phase maps as well as echo planar imaging (EPI) phase maps taken from the baseline (precontrast) part of the DSC-MRI time series. The EPI phase data were included to elucidate whether an extra HR-GRE scan is needed to obtain information about OEF and CMRO 2 , or if this information can be extracted from the DSC-MRI experiment only. Twenty healthy volunteers were scanned using 3 T MRI on two occasions. Oxygen saturation levels were obtained from phase data measured in the great cerebral vein of Galen, based on HR-GRE as well as EPI phase maps. In combination with DSC-MRI CBF, this allowed for calculation of OEF and CMRO 2 . High-resolution-gradient echo- and EPI-based phase images resulted in similar OEF spread and repeatability, with coefficients of variation/intraclass correlation coefficients of 0·26/0·95 and 0·23/0·81, respectively. Absolute OEF values (HR-GRE: 0·40 ± 0·11, EPI: 0·35 ± 0·08) were consistent with literature data. CMRO 2 showed similar repeatability, somewhat increased spread and reasonable absolute values (HR-GRE: 3·23 ± 1·26 ml O 2 /100 g min -1 , EPI: 2·79 ± 0·89 ml O 2 /100 g min -1 ). In general, the results obtained by HR-GRE and EPI showed comparable characteristics. The EPI methodology could potentially be improved using a slightly modified DSC-MRI protocol (e.g. with regard to spatial resolution and slice gap). © 2015 Scandinavian Society of Clinical Physiology and Nuclear Medicine. Published by John Wiley & Sons Ltd.

Investigation of recrystallization of amorphous trehalose through hot-humidity stage X-ray powder diffraction.

PubMed

Jójárt-Laczkovich, Orsolya; Katona, Gábor; Aigner, Zoltán; Szabó-Révész, Piroska

2016-12-01

The aim of this work was an investigation of the physical changes of the amorphous model material spray-dried trehalose through the use of various analytical techniques and to identify a suitable, rapid method able to quantify the changes. The crystallinity changes and recrystallization process of amorphous samples were investigated by hot-humidity stage X-ray powder diffractometry (HH-XRPD) with fresh samples, conventional X-ray powder diffractometry (XRPD) used stored samples and by differential scanning calorimetry (DSC). The data from the three methods were compared and the various forms of trehalose were analysed. HH-XRPD demonstrated that the recrystallization began at 40 and 60°C up to 45% RH and at 70°C up to 30% RH into dihydrate form. At 70°C up to 60% RH the anhydrous form of trehalose appeared too. Conventional XRPD results showed, that in the 28days stored samples the dihydrate form was detected at 40°C, 50% RH. Storage at 60°C, 40% RH resulted in the appearance of the anhydrous form and at 60°C, 50% RH both polymorphic forms were detected. By carrying out the DSC measurements at different temperatures the fraction of recrystallized trehalose dihydrate was detected. The recrystallization investigated by HH-XRPD and DSC followed Avrami kinetics, the calculated rate constants of isothermal crystallization (K) were same. Both HH-XRPD and conventional XRPD was suitable for the detection of the physical changes of the amorphous model material. DSC measurements showed similar results as HH-XRPD. Primarily HH-XRPD could be suggested for prediction, because the method is fast and every changes could be studied on one sample. Copyright © 2016 Elsevier B.V. All rights reserved.

Drug-polymer interaction between glucosamine sulfate and alginate nanoparticles: FTIR, DSC and dielectric spectroscopy studies

NASA Astrophysics Data System (ADS)

El-Houssiny, A. S.; Ward, A. A.; Mostafa, D. M.; Abd-El-Messieh, S. L.; Abdel-Nour, K. N.; Darwish, M. M.; Khalil, W. A.

2016-06-01

This work involves the preparation and characterization of alginate nanoparticles (Alg NPs) as a new transdermal carrier for site particular transport of glucosamine sulfate (GS). The GS-Alg NPs were examined through transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and dielectric spectroscopy. GS-Alg NPs was efficiently prepared via ionic gelation method which generates favorable conditions for the entrapment of hydrophilic drugs. The TEM studies revealed that GS-Alg NPs are discrete and have spherical shapes. FTIR studies showed a spectral change of the characteristic absorptions bands of Alg NPs after encapsulation with GS because of the amine groups of GS and the carboxylic acid groups of Alg. The DSC data showed changes in the thermal behavior of GS-Alg NPs after the addition of GS indicating signs of main chemical interaction among the drug (GS) and the polymer (Alg). The absence of the drug melting endothermic peak within the DSC thermogram of GS-Alg NPs indicating that GS is molecularly dispersed in the NPs and not crystallize. From the dielectric study, it was found modifications within the dielectric loss (ɛ″) and conductivity (σ) values after the addition of GS. The ɛ″ and σ values of Alg NPs decreased after the addition of GS which indicated the successful encapsulation of GS within Alg NPs. Furthermore, the dielectric study indicated an increase of the activation energy and the relaxation time for the first process in the GS-Alg NPs as compared to Alg NPs. Consequently, the existing observations indicated an initiation of electrostatic interaction among the amine group of GS and carboxyl group of Alg indicating the successful encapsulation of GS inside Alg NPs which could provide favorable circumstance for the encapsulation of GS for topical management.

Physiochemical Characterization and Release Rate Studies of SolidDispersions of Ketoconazole with Pluronic F127 and PVP K-30

PubMed Central

Kumar, Pankaj; Mohan, Chander; KanamSrinivasan Uma Shankar, Mara; Gulati, Monica

2011-01-01

In the present study solid dispersions of the antifungal drug Ketoconazole were prepared with Pluronic F-127 and PVP K-30 with an intention to improve its dissolution properties. Investigations of the properties of the dispersions were performed using release studies, Differential scanning calorimetery (DSC), X-ray powder diffraction (XRD) and Fourier transform infrared (FTIR). The results obtained showed that the rate of dissolution of Ketoconazole was considerably improved when formulated in solid dispersions with PVP K-30 and Pluronic F-127 as compared with pure drug and physical mixtures. The results from DSC and XRD studies showed the transition of crystalline nature of drug to amorphous form, while FTIR studies demonstrated the absence of drug-carriers interaction. PMID:24250403

Ionic conductivity and mixed-ion effect in mixed alkali metaphosphate glasses.

PubMed

Tsuchida, Jefferson Esquina; Ferri, Fabio Aparecido; Pizani, Paulo Sergio; Martins Rodrigues, Ana Candida; Kundu, Swarup; Schneider, José Fabián; Zanotto, Edgar Dutra

2017-03-01

In this work, mixed alkali metaphosphate glasses based on K-Na, Rb-Na, Rb-Li, Cs-Na and Cs-Li combinations were studied by differential scanning calorimetry (DSC), complex impedance spectroscopy, and Raman spectroscopy. DSC analyses show that both the glass transition (T g ) and melting temperatures (T m ) exhibit a clear mixed-ion effect. The ionic conductivity shows a strong mixed-ion effect and decreases by more than six orders of magnitude at room temperature for Rb-Na or Cs-Li alkali pairs. This study confirms that the mixed-ion effect may be explained as a natural consequence of random ion mixing because ion transport is favoured between well-matched energy sites and is impeded due to the structural mismatch between neighbouring sites for dissimilar ions.

Kinetic analysis of overlapping multistep thermal decomposition comprising exothermic and endothermic processes: thermolysis of ammonium dinitramide.

PubMed

Muravyev, Nikita V; Koga, Nobuyoshi; Meerov, Dmitry B; Pivkina, Alla N

2017-01-25

This study focused on kinetic modeling of a specific type of multistep heterogeneous reaction comprising exothermic and endothermic reaction steps, as exemplified by the practical kinetic analysis of the experimental kinetic curves for the thermal decomposition of molten ammonium dinitramide (ADN). It is known that the thermal decomposition of ADN occurs as a consecutive two step mass-loss process comprising the decomposition of ADN and subsequent evaporation/decomposition of in situ generated ammonium nitrate. These reaction steps provide exothermic and endothermic contributions, respectively, to the overall thermal effect. The overall reaction process was deconvoluted into two reaction steps using simultaneously recorded thermogravimetry and differential scanning calorimetry (TG-DSC) curves by considering the different physical meanings of the kinetic data derived from TG and DSC by P value analysis. The kinetic data thus separated into exothermic and endothermic reaction steps were kinetically characterized using kinetic computation methods including isoconversional method, combined kinetic analysis, and master plot method. The overall kinetic behavior was reproduced as the sum of the kinetic equations for each reaction step considering the contributions to the rate data derived from TG and DSC. During reproduction of the kinetic behavior, the kinetic parameters and contributions of each reaction step were optimized using kinetic deconvolution analysis. As a result, the thermal decomposition of ADN was successfully modeled as partially overlapping exothermic and endothermic reaction steps. The logic of the kinetic modeling was critically examined, and the practical usefulness of phenomenological modeling for the thermal decomposition of ADN was illustrated to demonstrate the validity of the methodology and its applicability to similar complex reaction processes.

Study of Hyperbranched Poly(ethyleneimine) Polymers of Different Molecular Weight and Their Interaction with Epoxy Resin

PubMed Central

2018-01-01

Two different commercial hyperbranched poly(ethyleneimine)s (HBPEI), with molecular weights (MW) of 800 and 25,000 g/mol, and denoted as PEI800 and PEI25000, respectively, as well as the mixtures with a Diglycidyl Ether of Bisphenol-A (DGEBA) epoxy resin, have been studied using thermal analysis techniques (DSC, TGA), dielectric relaxation spectroscopy (DRS), and dynamic mechanical analysis (DMA). Only a single glass transition is observed in these mixtures by DSC. DRS of the HBPEIs shows three dipolar relaxations: γ, β, and α. The average activation energy for the γ-relaxation is similar for all HBPEIs and is associated with the motion of the terminal groups. The β-relaxation has the same average activation energy for both PEI800 and PEI25000; this relaxation is attributed to the mobility of the branches. The α-relaxation peak for all the HBPEIs is an asymmetric peak with a shoulder on the high temperature side. This shoulder suggests the existence of ionic charge trapped in the PEI. For the mixtures, the γ- and β-relaxations follow the behaviour of the epoxy resin alone, indicating that the epoxy resin dominates the molecular mobility. The α-relaxation by DRS is observed only as a shoulder, as a consequence of an overlap with conductivity effects, whereas by DMA, it is a clear peak. PMID:29522480

Thermal energy storage behaviour of nanoparticle enhanced PCM during freezing and melting

NASA Astrophysics Data System (ADS)

P, Murugan; P, Ganesh Kumar; V, Kumaresan; M, Meikandan; K, Malar Mohan; R, Velraj

2018-03-01

The present research work aimed to investigate the melting and solidification characteristics of NPCM. The NPCM was prepared using paraffin as the PCM and high conductive MWCNT as the nanomaterial without using any dispersant. The NPCM was prepared by dispersing MWCNTs with volume fractions of 0.3%, 0.6% and 0.9% in PCM as the base PCM. SEM morphology showed the uniform dispersion of MWCNTs in the paraffin wax. The MWCNT nano-additives PCMs showed two peaks in the heating curve by DSC measurement. Lessening in melting and solidification time of 30% and 43% was attained in the case of NPCM with 0.3% and 0.9%, respectively. It is observed from the DSC analysis that the latent heat of pure paraffin during freezing and melting cycle was 139.2 J/g (at 56.61 °C) and 131.8 J/g (at 57.55 °C), respectively. Whereas, the latent heat of NPCM with 0.9% of nanofluid was 150.7 J/g (at 56.36 °C) and 148.3 J/g (58.35 °C). It is construed that a maximum change in latent heat of 7.6% and 11% was observed between pure PCM and NPCM during freezing and melting cycle. For the lesser nanoparticle concentration (0.3% and 0.6%), the percentage change in latent heat was lesser than 0.9%.

Brain perfusion alterations in tick-borne encephalitis-preliminary report.

PubMed

Tyrakowska-Dadełło, Zuzanna; Tarasów, Eugeniusz; Janusek, Dariusz; Moniuszko-Malinowska, Anna; Zajkowska, Joanna; Pancewicz, Sławomir

2018-03-01

Magnetic resonance imaging (MRI) changes in tick-borne encephalitis (TBE) are non-specific and the pathophysiological mechanisms leading to their formation remain unclear. This study investigated brain perfusion in TBE patients using dynamic susceptibility-weighted contrast-enhanced magnetic resonance perfusion imaging (DSC-MRI perfusion). MRI scans were performed for 12 patients in the acute phase, 3-5days after the diagnosis of TBE. Conventional MRI and DSC-MRI perfusion studies were performed. Cerebral blood flow (CBF), cerebral blood volume (CBV), mean transit time (MTT), and time to peak (TTP) parametric maps were created. The bilateral frontal, parietal, and temporal subcortical regions and thalamus were selected as regions of interest. Perfusion parameters of TBE patients were compared to those of a control group. There was a slight increase in CBF and CBV, with significant prolongation of TTP in subcortical areas in the study subjects, while MTT values were comparable to those of the control group. A significant increase in thalamic CBF (p<0.001) and increased CBV (p<0.05) were observed. Increased TTP and a slight reduction in MTT were also observed within this area. The DSC-MRI perfusion study showed that TBE patients had brain perfusion disturbances, expressed mainly in the thalami. These results suggest that DSC-MRI perfusion may provide important information regarding the areas affected in TBE patients. Copyright © 2018 The Authors. Published by Elsevier Ltd.. All rights reserved.

Compatibility of 2, 4, 6, 8, 10,12-Hexanitrohexaazaisowurtzitane with a Selection of Insensitive Explosives

NASA Astrophysics Data System (ADS)

Li, Xi; Lin, Qiu-han; Zhao, Xin-Ying; Han, Zhi-Wei; Wang, Bo-liang

2017-04-01

Thermal techniques (differential scanning calorimetry (DSC) and the vacuum stability test (VST)), according to STANAG 4147, and non-thermal techniques (Fourier transform infrared (FTIR) spectrometry and X-ray diffractometry (XRD)) were used to examine compatibility issues for 2,4,6,8,10,12-hexanitrohexaazaisowurtzitane (CL-20) with a selection of insensitive explosives, including nitroguanidine (NQ), 2,4,6-trinitrotoluene (TNT), 2,6-diamino-3,5-dinitropyridine-1-oxide (ANPyO), 2,4,6-triamino-1,3,5-trinitrobenzene (TATB), 3-nitro-1,2,4-triazol-5-one (NTO) and 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105). DSC measurements showed that ANPyO, TATB, NTO and LLM-105 were compatible with CL-20. The compatibility of CL-20/NQ, CL-20/TNT, CL-20/ANPyO, CL-20/TATB, CL-20/NTO and CL-20/LLM-105 mixtures was further explored using the VST, which revealed that all the selected insensitive explosives were compatible with CL-20. Possible chemical interactions were suspected for CL-20/TATB from the FTIR results and for CL-20/NTO from XRD analysis. In summary, ANPyO and LLM-105 demonstrated the optimal compatibility with CL-20.

Star-shaped azomethines based on tris(2-aminoethyl)amine. Characterization, thermal and optical study.

PubMed

Iwan, Agnieszka; Janeczek, Henryk; Kaczmarczyk, Bozena; Jarzabek, Bozena; Sobota, Michal; Rannou, Patrice

2010-02-01

The synthesis and detailed (physico)-chemical ((1)H/(13)C NMR, FTIR, UV-vis and elemental analysis) characterizations of new star-shaped compounds based on tris(2-aminoethyl)amine, including in their structure an azomethine function (HCN-) and alkoxysemiperfluorinated (-O-(CH(2))(3)-(CF(2))(7)-CF(3)), octadecyloxy aliphatic (-O-(CH(2))(17)-CH(3)) chain or two phenyl rings (-Ph-Ph-) as a terminal group, were reported. The mesomorphic behavior was investigated by means of differential scanning calorimetry (DSC), polarized optical microscopy (POM) and additionally by FTIR(T) and UV-vis(T) spectroscopy. Wide-angle X-ray diffraction (WAXD) technique was used to probe the structural properties of the azomethines. Moreover, the azomethine A1 was electro-spun to prepare fibers with poly(methyl methacrylate) (PMMA) and investigated by DSC and POM. Additionally, a film of the A1 with PMMA was cast from chloroform and the thermal properties of the film were compared with the thermal properties of the fiber and powder. It was showed that terminal groups dramatically influence the thermal and optical properties of the star-shaped azomethines. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Enhanced hydrogen sorption kinetics of Mg 50Ni-LiBH 4 composite by CeCl 3 addition

NASA Astrophysics Data System (ADS)

Gennari, F. C.; Puszkiel, J. A.

Mg 50Ni-LiBH 4 and Mg 50Ni-LiBH 4-CeCl 3 composites have been prepared by short times of ball milling under argon atmosphere. Combination of HP-DSC and volumetric techniques show that Mg 50Ni-LiBH 4-CeCl 3 composite not only uptakes hydrogen faster than Mg 50Ni-LiBH 4, but also releases hydrogen at a lower temperature (225 °C). The presence of CeCl 3 has a catalytic role, but it does not modify the thermodynamic properties of the composite which corresponds to MgH 2. Experimental studies on the hydriding/dehydriding mechanisms demonstrate that LiBH 4 and Ni lead to the formation of MgNi 3B 2 in both composites. In addition, XRD/DSC analysis and thermodynamic calculations demonstrate that the addition of CeCl 3 accounts for the enhancement of the hydrogen absorption/desorption kinetics through the interaction with LiBH 4. The in situ formation and subsequent decomposition of Ce(BH 4) 3 provides a uniform distribution of nanosize CeB 4 compound, which plays an important role in improving the kinetic properties of MgH 2.

Preparation and Characterization of Pyrotechnics Binder-Coated Nano-Aluminum Composite Particles

NASA Astrophysics Data System (ADS)

Ye, Mingquan; Zhang, Shuting; Liu, Songsong; Han, Aijun; Chen, Xin

2017-07-01

The aim of this article is to protect the activity of nano-aluminum (Al) particles in solid rocket propellants and pyrotechnics. The morphology, structure, active aluminum content, and thermal and catalytic properties of the coated samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), thermogravimetry-differential scanning calorimetry (TG-DSC), and oxidation-reduction titration methods. The results indicated that nano-Al particles could be effectively coated with phenolic resin (PF), fluororubber (Viton B), and shellac through a solvent/nonsolvent method. The energetic composite particles have core-shell structures and the thickness of the coating film is about 5-15 nm. Analysis of the active Al content revealed that Viton B coating had a much better protective effect. The TG-DSC results showed that the energy amount and energy release rate of PF-, Viton B-, and shellac-coated Al particles were larger than those of the raw nano-Al particles. The catalytic effects of coated Al particles on the thermal decomposition of ammonium perchlorate (AP) were better than those of raw nano-Al particles, and the effect of shellac-coated Al particles was significantly better than that of Viton B-coated Al particles.

Preparation and Characterization of Nanoparticle β-Cyclodextrin:Geraniol Inclusion Complexes.

PubMed

Hadian, Zahra; Maleki, Majedeh; Abdi, Khosro; Atyabi, Fatemeh; Mohammadi, Abdoreza; Khaksar, Ramin

2018-01-01

The aim of the present study was to formulate β-cyclodextrin (β-CD) nanoparticles loaded with geraniol (GR) essential oil (EO) with appropriate physicochemical properties. Complexation of GR with β-CD was optimized by evaluation of four formulations, using the co-precipitation method, and the encapsulation efficiency (EE), loading, size, particle size distribution (PDI) and zeta potential were investigated. Further characterization was performed with nuclear magnetic resonance spectroscopy ( 1 H NMR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and infra-red (IR) spectroscopy analysis. Results showed that the physicochemical properties of the nanoparticles were affected by GR content in formulations that yielded nanoscale-size particles ranging from 111 to 258 nm. The highest encapsulation efficiency (79.4 ± 5.4%) was obtained when the molar ratio of EO to β-CD was 0.44: 0.13 with negative zeta potential (-21.1 ± 0.5 mV). The 1 H-NMR spectrum confirmed the formation structure of the EO and β-CD nanoparticle complex. Complexation with geraniol resulted in changes of IR profile, NMR chemical shifts, DSC properties, and SEM of β-cyclodextrin. Inclusion complex of essential oil with β-cyclodextrin was considered as promising bioactive materials for designing functional food.

Preparation and Characterization of Nanoparticle β-Cyclodextrin:Geraniol Inclusion Complexes

PubMed Central

Hadian, Zahra; Maleki, Majedeh; Abdi, Khosro; Atyabi, Fatemeh; Mohammadi, Abdoreza; Khaksar, Ramin

2018-01-01

The aim of the present study was to formulate β-cyclodextrin (β-CD) nanoparticles loaded with geraniol (GR) essential oil (EO) with appropriate physicochemical properties. Complexation of GR with β-CD was optimized by evaluation of four formulations, using the co-precipitation method, and the encapsulation efficiency (EE), loading, size, particle size distribution (PDI) and zeta potential were investigated. Further characterization was performed with nuclear magnetic resonance spectroscopy (1H NMR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and infra-red (IR) spectroscopy analysis. Results showed that the physicochemical properties of the nanoparticles were affected by GR content in formulations that yielded nanoscale-size particles ranging from 111 to 258 nm. The highest encapsulation efficiency (79.4 ± 5.4%) was obtained when the molar ratio of EO to β-CD was 0.44: 0.13 with negative zeta potential (-21.1 ± 0.5 mV). The 1H-NMR spectrum confirmed the formation structure of the EO and β-CD nanoparticle complex. Complexation with geraniol resulted in changes of IR profile, NMR chemical shifts, DSC properties, and SEM of β-cyclodextrin. Inclusion complex of essential oil with β-cyclodextrin was considered as promising bioactive materials for designing functional food.

High efficiency and stability of quasi-solid-state dye-sensitized ZnO solar cells using graphene incorporated soluble polystyrene gel electrolytes

NASA Astrophysics Data System (ADS)

Bi, Shi-Qing; Meng, Fan-Li; Zheng, Yan-Zhen; Han, Xue; Tao, Xia; Chen, Jian-Feng

2014-12-01

We report on the preparation of highly effective composite electrolytes by combining the two-dimensional graphene (Gra) and soluble polystyrene (PS) nanobeads on Pt counter electrode for the quasi-solid-state electrolytes of ZnO based dye-sensitized solar cells (DSCs). Under an optimized Gra/electrolyte ratio of 12 mg mL-1, the ionic conductivity (σ) of Gra-PS electrolyte was significantly improved from 32.8 mS cm-1 to 39.8 mS cm-1. And the electrochemical impedance spectroscopy (EIS) analysis proved that the ZnO-DSC with the optimized composite electrolyte possessed the lowest impedance value. As a result, the overall power conversion efficiencies (PCEs) of quasi-solid-state ZnO-DSCs significantly enhanced to 5.08% from initial 4.09%. Moreover, the results of long-term stability assays showed that the gel-state Gra-PS ZnO-DSC could retain over 90% of its initial PCE after radiation of 1000 h under full sunlight outdoors. It is anticipated that this work may provide an effective way to increase the cell efficiency by the introduction of Gra into gel electrolyte as well as a great potential for practical application.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weese, R K; Burnham, A K

Dimensional changes related to temperature cycling of the {beta} and {delta} polymorphs of HMX (octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine) are important for a variety of applications. The coefficient of thermal expansion (CTE) of the {beta} and {delta} phases are measured over a temperature range of -20 C to 215 C by thermo-mechanical analysis (TMA). Dimensional changes associated with the phase transition were also measured, and the time-temperature dependence of the dimensional change is consistent with phase transition kinetics measured earlier by differential scanning calorimetry (DSC). One HMX sample measured by TMA during its initial heating and again three days later during a second heatingmore » showed the {beta}-to-{delta} phase transition a second time, thereby indicating back conversion from {delta}-to-{beta} phase HMX during those three days. DSC was used to measure kinetics of the {delta}-to-{beta} back conversion. The most successful approach was to first heat the material to create the {delta} phase, then after a given period at room temperature, measure the heat absorbed during a second pass through the {beta}-to-{delta} phase transition. Back conversion at room temperature follows nucleation-growth kinetics.« less

The effects of 60Co γ-ray on poly(ethylene-co-vinyl acetate)/carbon black composites

NASA Astrophysics Data System (ADS)

Lee, Kyoung-Yong; Kim, Ki-Yup

2008-04-01

Cables used in a nuclear power plant are irradiation suppressing ones. Until now, researches on the irradiation suppressing cables have mainly been focused on insulation materials. Therefore, in this paper, the non-isothermal crystallization behaviors and degradation characteristics of ethylene vinyl acetate-carbon black (EVA-CB), used as a shielding material, were investigated by means of the Differential scanning calorimetry (DSC) and chemiluminescence analyzer (CL). The specimens were cooled after removing thermal history at 150 °C for 5 min by changing the cooling rates to 5, 7.5, 10, 15 and 20 °C/min with DSC. In addition, after maintaining a thermal equilibrium at each temperature of 25, 50, 75, 100, 125, 150 and 175 °C, their thermoluminescence was measured for 20 min with CL equipment. The 60Co γ-ray was used for irradiation. Tc, T0, T∞ and t1/2 in the DSC experiments are found to decrease gradually as radiation dose increases. Secondly, with the CL experiment, the 0.1, 0.25 and 0.5 MGy EVA-CB composites were found to show a much smaller thermoluminescence than the intact EVA-CB composites, while the 0.75 and 1 MGy EVA-CB composites were found to show a much higher thermoluminescence than ones.

Preparation and drug release behavior of temperature-responsive mesoporous carbons

NASA Astrophysics Data System (ADS)

Wang, Xiufang; Liu, Ping; Tian, Yong

2011-06-01

A temperature-responsive composite based on poly (N-isopropylacrylamide) (PNIPAAm) and ordered mesoporous carbons (OMCs) has been successfully prepared by a simple wetness impregnation technique. The structures and properties of the composite were characterized by infrared spectroscopy (IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), N 2 sorption, thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). The results showed that the inclusion of PNIPAAm had not greatly changed the basic ordered pore structure of the OMCs. Ibuprofen (IBU) was selected as model drug, and in vitro test of IBU release exhibited a temperature-responsive controlled release delivery.

Gelatinisation kinetics of corn and chickpea starches using DSC, RVA, and dynamic rheometry

USDA-ARS?s Scientific Manuscript database

The gelatinisation kinetics (non-isothermal) of corn and chickpea starches at different heating rates were calculated using differential scanning calorimetry (DSC), rapid visco analyser (RVA), and oscillatory dynamic rheometry. The data obtained from the DSC thermogram and the RVA profiles were fitt...

Conjugated Polymer Solar Cells

DTIC Science & Technology

2006-05-01

thermal gravimetry analysis (TGA)............... 12 2.6 Photoluminescence (PL) spectroscopy... gravimetry analysis (TGA) Thermal analysis of polymer films has been accomplished by TGA and DSC methods with the aid of Perkin-Elmer Series 7 Analysers...The MEH-PPV/acceptor films were prepared by spin-casting of the resulting mixture (with or without precipitate ) on glass substrates of diameter 23 mm

47 CFR 80.225 - Requirements for selective calling equipment.

Code of Federal Regulations, 2011 CFR

2011-10-01

... selective calling (DSC) equipment and selective calling equipment installed in ship and coast stations, and...-STD, “RTCM Recommended Minimum Standards for Digital Selective Calling (DSC) Equipment Providing... Class ‘D’ Digital Selective Calling (DSC)—Methods of testing and required test results,” March 2003. ITU...

47 CFR 80.359 - Frequencies for digital selective calling (DSC).

Code of Federal Regulations, 2010 CFR

2010-10-01

... 47 Telecommunication 5 2010-10-01 2010-10-01 false Frequencies for digital selective calling (DSC... for digital selective calling (DSC). (a) General purpose calling. The following table describes the... Digital Selective-Calling Equipment in the Maritime Mobile Service,” with Annexes 1 through 5, 2004, and...

Thermoanalytical Investigation of Some Sulfone-Containing Drugs

PubMed Central

Salama, Nahla N.; El Ries, Mohammed A.; Toubar, Safaa; Abd El Hamid, Maha; Walash, Mohammed I.

2012-01-01

The thermal behavior of some sulfone-containing drugs, namely, dapsone (DDS), dimethylsulfone (MSM), and topiramate (TOP) in drug substances, and products were investigated using different thermal techniques. These include thermogravimetry (TGA), derivative thermogravimetry (DTG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). The thermogravimetric data allowed the determination of the kinetic parameters: activation energy (E a), frequency factor (A), and reaction order (n). The thermal degradation of dapsone and topiramate was followed a first-order kinetic behavior. The calculated data evidenced a zero-order kinetic for dimethylsulfone. The relative thermal stabilities of the studied drugs have been evaluated and follow the order DDS > TOP > MSM. The purity was determined using DSC for the studied compounds, in drug substances and products. The results were in agreement with the recommended pharmacopoeia and manufacturer methods. DSC curves obtained from the tablets suggest compatibility between the drugs, excipients and/or coformulated drugs. The fragmentation pathway of dapsone with mass spectrometry was taken as example, to correlate the thermal decomposition with the resulted MS-EI. The decomposition modes were investigated, and the possible fragmentation pathways were suggested by mass spectrometry. PMID:22792516

Thermoanalytical investigation of some sulfone-containing drugs.

PubMed

Salama, Nahla N; El Ries, Mohammed A; Toubar, Safaa; Abd El Hamid, Maha; Walash, Mohammed I

2012-01-01

The thermal behavior of some sulfone-containing drugs, namely, dapsone (DDS), dimethylsulfone (MSM), and topiramate (TOP) in drug substances, and products were investigated using different thermal techniques. These include thermogravimetry (TGA), derivative thermogravimetry (DTG), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). The thermogravimetric data allowed the determination of the kinetic parameters: activation energy (E(a)), frequency factor (A), and reaction order (n). The thermal degradation of dapsone and topiramate was followed a first-order kinetic behavior. The calculated data evidenced a zero-order kinetic for dimethylsulfone. The relative thermal stabilities of the studied drugs have been evaluated and follow the order DDS > TOP > MSM. The purity was determined using DSC for the studied compounds, in drug substances and products. The results were in agreement with the recommended pharmacopoeia and manufacturer methods. DSC curves obtained from the tablets suggest compatibility between the drugs, excipients and/or coformulated drugs. The fragmentation pathway of dapsone with mass spectrometry was taken as example, to correlate the thermal decomposition with the resulted MS-EI. The decomposition modes were investigated, and the possible fragmentation pathways were suggested by mass spectrometry.

Diclofenac Salts. V. Examples of Polymorphism among Diclofenac Salts with Alkyl-hydroxy Amines Studied by DSC and HSM

PubMed Central

Fini, Adamo; Cavallari, Cristina; Ospitali, Francesca

2010-01-01

Nine diclofenac salts prepared with alkyl-hydroxy amines were analyzed for their properties to form polymorphs by DSC and HSM techniques. Thermograms of the forms prepared from water or acetone are different in most cases, suggesting frequent examples of polymorphism among these salts. Polymorph transition can be better highlighted when analysis is carried out by thermo-microscopy, which in most cases made it possible to observe the processes of melting of the metastable form and re-crystallization of the stable one. Solubility values were qualitatively related to the crystal structure of the salts and the molecular structure of the cation. PMID:27721347

Comparison of the transformation temperatures of heat-activated Nickel-Titanium orthodontic archwires by two different techniques.

PubMed

Obaisi, Noor Aminah; Galang-Boquiren, Maria Therese S; Evans, Carla A; Tsay, Tzong Guang Peter; Viana, Grace; Berzins, David; Megremis, Spiro

2016-07-01

The purpose of this study was to investigate the suitability of the Bend and Free Recovery (BFR) method as a standard test method to determine the transformation temperatures of heat-activated Ni-Ti orthodontic archwires. This was done by determining the transformation temperatures of two brands of heat-activated Ni-Ti orthodontic archwires using the both the BFR method and the standard method of Differential Scanning Calorimetry (DSC). The values obtained from the two methods were compared with each other and to the manufacturer-listed values. Forty heat-activated Ni-Ti archwires from both Rocky Mountain Orthodontics (RMO) and Opal Orthodontics (Opal) were tested using BFR and DSC. Round (0.016 inches) and rectangular (0.019×0.025 inches) archwires from each manufacturer were tested. The austenite start temperatures (As) and austenite finish temperatures (Af) were recorded. For four of the eight test groups, the BFR method resulted in lower standard deviations than the DSC method, and, overall, the average standard deviation for BFR testing was slightly lower than for DSC testing. Statistically significant differences were seen between the transformation temperatures obtained from the BFR and DSC test methods. However, the Af temperatures obtained from the two methods were remarkably similar with the mean differences ranging from 0.0 to 2.1°C: Af Opal round (BFR 26.7°C, DSC 27.6°C) and rectangular (BFR 27.6°C, DSC 28.6°C); Af RMO round (BFR 25.5°C, DSC 25.5°C) and rectangular (BFR 28.0°C, DSC 25.9°C). Significant differences were observed between the manufacturer-listed transformation temperatures and those obtained with BFR and DSC testing for both manufacturers. The results of this study suggest that the Bend and Free Recovery method is suitable as a standard method to evaluate the transformation temperatures of heat-activated Ni-Ti orthodontic archwires. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Revealing the glass transition in shape memory polymers using Brillouin spectroscopy.

PubMed

Steelman, Zachary A; Weems, Andrew C; Traverso, Andrew J; Szafron, Jason M; Maitland, Duncan J; Yakovlev, Vladislav V

2017-12-11

Emerging medical devices which employ shape memory polymers (SMPs) require precise measurements of the glass transition temperature (T g ) to ensure highly controlled shape recovery kinetics. Conventional techniques like differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) have limitations that prevent utilization for certain devices, including limited accuracy and the need for sacrificial samples. In this report, we employ an approach based on Brillouin spectroscopy to probe the glass transition of SMPs rapidly, remotely, and nondestructively. Further, we compare the T g obtained from Brillouin scattering with DMA- and DSC-measured T g to demonstrate the accuracy of Brillouin scattering for this application. We conclude that Brillouin spectroscopy is an accurate technique for obtaining the glass transition temperature of SMPs, aligning closely with the most common laboratory standards while providing a rapid, remote, and nondestructive method for the analysis of unique polymeric medical devices.

Preliminary Analysis of the Social and Scientific Impact of the UAEM-ININ M.Sc. and D.Sc. Graduate Programme in Medical Physics

NASA Astrophysics Data System (ADS)

Mitsoura, Eleni; Isaac-Olive, Keila; Torres-Garcia, Eugenio; Camacho-Lopez, Miguel Angel; Hardy-Perez, Alberto

2010-12-01

Sponsored by the International Atomic Energy Agency (IAEA) in 1994, the Instituto Nacional de Investigaciones Nucleares (ININ) started in Mexico a teaching and training programme (Diplomado) in Radiotherapy Medical Physics. Based on this experience, the Universidad Autónoma del Estado de México (UAEM) and the Instituto Nacional de Investigaciones Nucleares (ININ) launched two years later, the first Graduate Programme in Science (M.Sc. and D.Sc.), specialised in Medical Physics in Mexico. A preliminary analysis of the social and scientific impact of the UAEM-ININ Programme is presented in this work based on the achievements attained, regarding the number of graduated Medical Physicists, their geographic and academic origin, their current professional activities and the number of scientific publications produced as a result of the thesis, as well as their citations.

Revealing the glass transition in shape memory polymers using Brillouin spectroscopy

NASA Astrophysics Data System (ADS)

Steelman, Zachary A.; Weems, Andrew C.; Traverso, Andrew J.; Szafron, Jason M.; Maitland, Duncan J.; Yakovlev, Vladislav V.

2017-12-01

Emerging medical devices which employ shape memory polymers (SMPs) require precise measurements of the glass transition temperature (Tg) to ensure highly controlled shape recovery kinetics. Conventional techniques like differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) have limitations that prevent utilization for certain devices, including limited accuracy and the need for sacrificial samples. In this report, we employ an approach based on Brillouin spectroscopy to probe the glass transition of SMPs rapidly, remotely, and nondestructively. Further, we compare the Tg obtained from Brillouin scattering with DMA- and DSC-measured Tg to demonstrate the accuracy of Brillouin scattering for this application. We conclude that Brillouin spectroscopy is an accurate technique for obtaining the glass transition temperature of SMPs, aligning closely with the most common laboratory standards while providing a rapid, remote, and nondestructive method for the analysis of unique polymeric medical devices.

7 CFR 1710.114 - TIER, DSC, OTIER and ODSC requirements.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 11 2011-01-01 2011-01-01 false TIER, DSC, OTIER and ODSC requirements. 1710.114... AND GUARANTEES Loan Purposes and Basic Policies § 1710.114 TIER, DSC, OTIER and ODSC requirements. (a) General. Requirements for coverage ratios are set forth in the borrower's mortgage, loan contract, or...

High-temperature thermogravimetric analysis and differential scanning calorimetry of nanocomposites (FeCoZr)x(CaF2)100-x

NASA Astrophysics Data System (ADS)

Bondariev, Vitalii

2016-09-01

In this work thermogravimetric-DTG/DSC analysis result for samples of nanocomposite metal-dielectric (FeCoZr)x(CaF2)100-x are presents. Series of samples with, metallic phase content x = 24 - 68 at.% were produced by ionbeam sputtering method in mixed atmosphere of gas argon and oxygen. Study of thermal properties, phase shifts and process of change in mass of nanocomposites were performed using the thermoanalytical system TGA/DSC-1/1600 HF (MettlerToledoInstruments). High-precision weight has a weighing range 1μg - 1g with an accuracy 1μg. The furnace makes it possible to regulate the temperature in range from room temperature to 1600°C and heating rate is 0.01 - 150°C min. After analysis of the results established that initial and final mass of samples of the nanocomposite (FeCoZr)x(CaF2)100-x are different, namely the sample mass is increased by 2 - 20%. It is related to the oxidation of metallic phase particles of nanocomposite. DTG and DSC analysis demonstrated that oxidation of metallic phase is held in two steps, at first oxidized iron atoms, and followed oxidation of the cobalt atoms, what can be seen on the waveform in the form of two humps and whereby oxides Fe2O3, Fe3O4, Co2O3, Co3O4 are formed. Oxide coatings on the surface of atoms represents an additional barrier to electron transfer charges. When a voltage is applied to the layer of the nanocomposite are three possible ways to transfer of charges between atoms and particles of metal, whereby each has its own relaxation time.

Thermal porosity analysis of croscarmellose sodium and sodium starch glycolate by differential scanning calorimetry.

PubMed

Faroongsarng, Damrongsak; Peck, Garnet E

2003-12-30

The aim of the study was to demonstrate the applicability of differential scanning calorimetry (DSC) on porosity analysis for cellulose and starch. Croscarmellose sodium (CCS) and sodium starch glycolate (SSG) were allowed to sorb moisture in 85%, 90%, 95%, and 100% relative humidity (RH) at 40 degrees C for 24 hours. The pretreated samples were then subjected to DSC running temperature ranging from 25 degrees C to -50 degrees C at a cooling rate of 10 degrees C/min. The cooling traces of water crystallization, if present, were transformed to porosity distribution via capillary condensation using Kelvin's equation. The porosity analysis of CCS and SSG was also done using nitrogen adsorption as a reference method. It was found that sorbed water could not be frozen (in cases of 85% and 90% RH) until the moisture content exceeded a cutoff value (in cases of 95% and 100% RH). The nonfreezable moisture content was referred to tightly bound, plasticizing water, whereas the frozen one may be attributed to loosely bound water condensation in pore structure of CCS and SSG surfaces. Not only capillary condensation but also the tightly bound, nonfreezable monolayer water lying along the inner pores of the surface contributed to porosity determination. Good agreement with less than 5% deviation of mean pore size was observed when the results were compared with nitrogen adsorption. The narrower pore size distributions, however, were obtained because of the limitations of the technique. It was concluded that pore analysis by DSC could be successful. Further research needs to be done to account for limitations and to extend the applicability of the technique.

Elimination of Perchlorate Oxidizers from Pyrotechnic Flare Compositions

DTIC Science & Technology

2007-03-09

in candelas ( cd ), where the candela is defined as, 1 cd = 1 lumen /steradian-1. DSC A thermal analysis technique known as Differential...Shorter Wavelength Infrared band routinely monitored in decoy flare performance tests. TGA A thermal analysis technique known as Thermogravimetric ...Scanning Calorimetry DTA A thermal analysis technique known as Differential Thermal Analysis GAP Glycidyl Azide Polymer used as a curable binder in some

Mutual interaction between high and low stereo-regularity components for crystallization and melting behaviors of polypropylene blend fibers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kawai, Kouya; Takarada, Wataru; Kikutani, Takeshi, E-mail: kikutani.t.aa@m.titech.ac.jp

Crystallization and melting behaviors of blend fibers of two types of polypropylene (PP), i.e. high stereo-regularity/high molecular weight PP (HPP) and low stereo-regularity/low molecular weight PP (LPP), was investigated. Blend fibers consisting of various HPP/LPP compositions were prepared through the melt spinning process. Differential scanning calorimetry (DSC), temperature modulated DSC (TMDSC) and wide-angle X-ray diffraction (WAXD) analysis were applied for clarifying the crystallization and melting behaviors of individual components. In the DSC measurement of blend fibers with high LPP composition, continuous endothermic heat was detected between the melting peaks of LPP at around 40 °C and that of HPP atmore » around 160 °C. Such endothermic heat was more distinct for the blend fibers with higher LPP composition indicating that the melting of LPP in the heating process was hindered because of the presence of HPP crystals. On the other hand, heat of crystallization was detected at around 90 °C in the case of blend fibers with LPP content of 30 to 70 wt%, indicating that the crystallization of HPP component was taking place during the heating of as-spun blend fibers in the DSC measurement. Through the TMDSC analysis, re-organization of the crystalline structure through the simultaneous melting and re-crystallization was detected in the cases of HPP and blend fibers, whereas re-crystallization was not detected during the melting of LPP fibers. In the WAXD analysis during the heating of fibers, amount of a-form crystal was almost constant up to the melting in the case of single component HPP fibers, whereas there was a distinct increase of the intensity of crystalline reflections from around 100 °C, right after the melting of LPP in the case of blend fibers. These results suggested that the crystallization of HPP in the spinning process as well as during the conditioning process after spinning was hindered by the presence of LPP.« less

TU-AB-202-06: Quantitative Evaluation of Deformable Image Registration in MRI-Guided Adaptive Radiation Therapy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mooney, K; Zhao, T; Green, O

Purpose: To assess the performance of the deformable image registration algorithm used for MRI-guided adaptive radiation therapy using image feature analysis. Methods: MR images were collected from five patients treated on the MRIdian (ViewRay, Inc., Oakwood Village, OH), a three head Cobalt-60 therapy machine with an 0.35 T MR system. The images were acquired immediately prior to treatment with a uniform 1.5 mm resolution. Treatment sites were as follows: head/neck, lung, breast, stomach, and bladder. Deformable image registration was performed using the ViewRay software between the first fraction MRI and the final fraction MRI, and the DICE similarity coefficient (DSC)more » for the skin contours was reported. The SIFT and Harris feature detection and matching algorithms identified point features in each image separately, then found matching features in the other image. The target registration error (TRE) was defined as the vector distance between matched features on the two image sets. Each deformation was evaluated based on comparison of average TRE and DSC. Results: Image feature analysis produced between 2000–9500 points for evaluation on the patient images. The average (± standard deviation) TRE for all patients was 3.3 mm (±3.1 mm), and the passing rate of TRE<3 mm was 60% on the images. The head/neck patient had the best average TRE (1.9 mm±2.3 mm) and the best passing rate (80%). The lung patient had the worst average TRE (4.8 mm±3.3 mm) and the worst passing rate (37.2%). DSC was not significantly correlated with either TRE (p=0.63) or passing rate (p=0.55). Conclusions: Feature matching provides a quantitative assessment of deformable image registration, with a large number of data points for analysis. The TRE of matched features can be used to evaluate the registration of many objects throughout the volume, whereas DSC mainly provides a measure of gross overlap. We have a research agreement with ViewRay Inc.« less

Fast and robust segmentation of the striatum using deep convolutional neural networks.

PubMed

Choi, Hongyoon; Jin, Kyong Hwan

2016-12-01

Automated segmentation of brain structures is an important task in structural and functional image analysis. We developed a fast and accurate method for the striatum segmentation using deep convolutional neural networks (CNN). T1 magnetic resonance (MR) images were used for our CNN-based segmentation, which require neither image feature extraction nor nonlinear transformation. We employed two serial CNN, Global and Local CNN: The Global CNN determined approximate locations of the striatum. It performed a regression of input MR images fitted to smoothed segmentation maps of the striatum. From the output volume of Global CNN, cropped MR volumes which included the striatum were extracted. The cropped MR volumes and the output volumes of Global CNN were used for inputs of Local CNN. Local CNN predicted the accurate label of all voxels. Segmentation results were compared with a widely used segmentation method, FreeSurfer. Our method showed higher Dice Similarity Coefficient (DSC) (0.893±0.017 vs. 0.786±0.015) and precision score (0.905±0.018 vs. 0.690±0.022) than FreeSurfer-based striatum segmentation (p=0.06). Our approach was also tested using another independent dataset, which showed high DSC (0.826±0.038) comparable with that of FreeSurfer. Comparison with existing method Segmentation performance of our proposed method was comparable with that of FreeSurfer. The running time of our approach was approximately three seconds. We suggested a fast and accurate deep CNN-based segmentation for small brain structures which can be widely applied to brain image analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

The Use of ATR-FTIR in Conjunction with Thermal Analysis Methods for Efficient Identification of Polymer Samples: A Qualitative Multiinstrument Instrumental Analysis Laboratory Experiment

ERIC Educational Resources Information Center

Dickson-Karn, Nicole M.

2017-01-01

A multi-instrument approach has been applied to the efficient identification of polymers in an upper-division undergraduate instrumental analysis laboratory course. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) is used in conjunction with differential scanning calorimetry (DSC) to identify 18 polymer samples and…

77 FR 24539 - Virginia Electric and Power Company; Surry Power Station Units 1 and 2; Independent Spent Fuel...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-04-24

... bounding thermal analysis using ANSYS finite element software to evaluate the misloading events. The ANSYS analysis consists of a half-symmetric, three-dimensional model of a 32PTH DSC with a number of conservative... the maximum fuel cladding temperature presented in the UFSAR analysis dated October 2, 2009, with the...

Coformer screening using thermal analysis based on binary phase diagrams.

PubMed

Yamashita, Hiroyuki; Hirakura, Yutaka; Yuda, Masamichi; Terada, Katsuhide

2014-08-01

The advent of cocrystals has demonstrated a growing need for efficient and comprehensive coformer screening in search of better development forms, including salt forms. Here, we investigated a coformer screening system for salts and cocrystals based on binary phase diagrams using thermal analysis and examined the effectiveness of the method. Indomethacin and tenoxicam were used as models of active pharmaceutical ingredients (APIs). Physical mixtures of an API and 42 kinds of coformers were analyzed using Differential Scanning Calorimetry (DSC) and X-ray DSC. We also conducted coformer screening using a conventional slurry method and compared these results with those from the thermal analysis method and previous studies. Compared with the slurry method, the thermal analysis method was a high-performance screening system, particularly for APIs with low solubility and/or propensity to form solvates. However, this method faced hurdles for screening coformers combined with an API in the presence of kinetic hindrance for salt or cocrystal formation during heating or if there is degradation near the metastable eutectic temperature. The thermal analysis and slurry methods are considered complementary to each other for coformer screening. Feasibility of the thermal analysis method in drug discovery practice is ensured given its small scale and high throughput.

Coordination Polymer: Synthesis, Spectral Characterization and Thermal Behaviour of Starch-Urea Based Biodegradable Polymer and Its Polymer Metal Complexes

PubMed Central

Malik, Ashraf; Parveen, Shadma; Ahamad, Tansir; Alshehri, Saad M.; Singh, Prabal Kumar; Nishat, Nahid

2010-01-01

A starch-urea-based biodegradable coordination polymer modified by transition metal Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) was prepared by polycondensation of starch and urea. All the synthesized polymeric compounds were characterized by Fourier transform-infrared spectroscopy (FT-IR), 1H-NMR spectroscopy, 13C-NMR spectroscopy, UV-visible spectra, magnetic moment measurements, differential scanning calorimeter (DSC), and thermogravimetric analysis (TGA). The results of electronic spectra and magnetic moment measurements indicate that Mn(II), Co(II), and Ni(II) complexes show octahedral geometry, while Cu(II) and Zn(II) complexes show square planar and tetrahedral geometry, respectively. The thermogravimetric analysis revealed that all the polymeric metal complexes are more thermally stable than the parental ligand. In addition, biodegradable studies of all the polymeric compounds were also carried out through ASTM standards of biodegradable polymers by CO2 evolution method. PMID:20414461

Thermal energy storage characteristics of micro-nanoencapsulated heneicosane and octacosane with poly(methylmethacrylate) shell.

PubMed

Sarı, Ahmet; Alkan, Cemil; Biçer, Alper

2016-05-01

In this study, PMMA/heneicosane (C21) and PMMA/octacosane (C28) micro-nano capsules were fabricated via emulsion polymerisation method. The chemical structures of the fabricated capsules were verified with the FT-IR spectroscopy analysis. The results of POM, SEM and PSD analysis indicated that most of the capsules were consisted of micro/nano-sized spheres with compact surface. The DSC measurements showed that the capsules had melting temperature in the range of about 39-60 °C and latent heat energy storage capacity in the range of about 138-152 J/g. The results of TGA showed that sublimit temperature values regarding the first degradation steps of both capsules were quite over the phase change or working temperatures of encapsulated paraffins. The thermal cycling test exhibited that the capsules had good thermal reliability and chemical stability. Additionally, the prepared capsules had reasonably high thermal conductivity.

Characterization of bioactive chitosan and sulfated chitosan from Doryteuthis singhalensis (Ortmann, 1891).

PubMed

Ramasamy, Pasiyappazham; Subhapradha, Namasivayam; Thinesh, Thangadurai; Selvin, Joseph; Selvan, Kanagaraj Muthamizh; Shanmugam, Vairamani; Shanmugam, Annaian

2017-06-01

Chitosan was extracted from the pen of squid Doryteuthis singhalensis and characterized using FT-IR, NMR, CHN, SEM and DSC analysis. Purified chitosan was sulfated with chlorosulfonic acid in N,N-dimethylformamide and the added sulfate group was confirmed with FT-IR analysis. The molecular weight and degree of deacetylation (DDA) of chitosan was found 226.6kDa and 83.76% respectively. Chitosan exhibited potent antioxidant activity evidenced by reducing power, chelating ability on ferrous ions and scavenging activity on DPPH, superoxide and hydroxyl radicals. The anticoagulant assay using activated partial thromboplastin time (APTT) and prothrombin time (PT) showed chitosan as a strong anticoagulant. The results of this study showed possibility of using D. singhalensis pen as a non-conventional source of natural antioxidants and anticoagulant which can be incorporated in functional food formulations. Copyright © 2017 Elsevier B.V. All rights reserved.

Remote Evaluation of Rotational Velocity Using a Quadrant Photo-Detector and a DSC Algorithm

PubMed Central

Zeng, Xiangkai; Zhu, Zhixiong; Chen, Yang

2016-01-01

This paper presents an approach to remotely evaluate the rotational velocity of a measured object by using a quadrant photo-detector and a differential subtraction correlation (DSC) algorithm. The rotational velocity of a rotating object is determined by two temporal-delay numbers at the minima of two DSCs that are derived from the four output signals of the quadrant photo-detector, and the sign of the calculated rotational velocity directly represents the rotational direction. The DSC algorithm does not require any multiplication operations. Experimental calculations were performed to confirm the proposed evaluation method. The calculated rotational velocity, including its amplitude and direction, showed good agreement with the given one, which had an amplitude error of ~0.3%, and had over 1100 times the efficiency of the traditional cross-correlation method in the case of data number N > 4800. The confirmations have shown that the remote evaluation of rotational velocity can be done without any circular division disk, and that it has much fewer error sources, making it simple, accurate and effective for remotely evaluating rotational velocity. PMID:27120607

Moisture-Absorption and Water Dynamics in the Powder of Egg Albumen Peptide, Met-Pro-Asp-Ala-His-Leu.

PubMed

Yang, Shuailing; Liu, Xuye; Zhang, Mingdi; Lin, Songyi; Chen, Feng

2017-01-01

Moisture absorbed into the powder of Met-Pro-Asp-Ala-His-Leu (MPDAHL)-a novel egg albumen antioxidant peptide-profoundly affects its properties. In this study, we elucidated water dynamics in MPDAHL using DVS, DSC, and low-field 1 H NMR. Based on the DVS data, we found that MPDAHL sorption kinetics obey a parallel exponential model. DSC results indicated that both water and heating could change the microstructure of MPDAHL. The T 2 parameters of NMR reflected the different phases of moisture absorption revealed that there were 4 categories of water with different states or mobility in the MPDAHL during the moisture absorption process. The fastest fraction T 2b mainly dominated the hygroscopicity of MPDAHL and the absorbed water significantly changed the proton distribution and structure of MPDAHL. Thus, this study shows that DVS, DSC, and low-field 1 H NMR are effective methods for monitoring water mobility and distribution in synthetic peptides. It can be used to improve the quality assurance of functional peptides. © 2016 Institute of Food Technologists®.

Interactions of tamoxifen with distearoyl phosphatidylcholine multilamellar vesicles: FTIR and DSC studies

NASA Astrophysics Data System (ADS)

Bilge, Duygu; Sahin, Ipek; Kazanci, Nadide; Severcan, Feride

2014-09-01

Interactions of a non-steroidal antiestrogen drug, tamoxifen (TAM), with distearoyl-sn-glycero-3-phosphatidylcholine (DSPC) multilamellar liposomes (MLVs) were investigated as a function of drug concentration (1-15 mol%) by using two noninvasive techniques, namely Fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC). FTIR spectroscopy results show that increasing TAM concentrations (except 1 mol%) increased the wavenumbers of the CH2 stretching modes, implying an disordering effect for DSPC MLVs both in the gel and liquid crystalline phases. The bandwidth values of the CH2 stretchings except for 1 mol% increased when TAM concentrations increased for DSPC liposomes, indicating an increase in the dynamics of liposomes. The Cdbnd O stretching and PO2- antisymmetric double bond stretching bands were analyzed to study interactions of TAM with head groups of lipids. As the concentrations of TAM increased, dehydration occurred around these functional groups in the polar part of the lipids. The DSC studies on thermal properties of DSPC lipids indicate that TAM eliminated the pre transition, shifted the main phase transition to lower temperatures and broadened the phase transition curve of the liposomes.

Fatigue and mechanical properties of nickel-titanium endodontic instruments.

PubMed

Kuhn, Grégoire; Jordan, Laurence

2002-10-01

Shape memory alloys are increasingly used in superelastic conditions under complex cyclic deformation situations. In these applications, it is very difficult to predict the service life based on the theoretical law. In the present work, fatigue properties of NiTi engine-driven rotary files have been characterized by using differential scanning calorimetry (DSC) and mechanical testing (bending). The DSC technique was used to measure precise transformation. The degree of deformation by bending was studied with combined DSC and mechanical property measurements. In these cold-worked files, the high dislocation density influences the reorientation processes and the crack growth. Some thermal treatments are involved in promoting some changes in the mechanical properties and transformation characteristics. Annealing around 400 degrees C shows good results; the recovery allows a compromise between an adequate density for the R-Phase germination and a low density to limit the brittleness of these instruments. In clinical usage, it is important to consider different canal shapes. It could be proposed that only few cycles of use is safe for very curved canals but to follow the manufacturer's advise for straight canals.

Microstructural and thermal study of Al-Si-Mg/melon shell ash particulate composite

NASA Astrophysics Data System (ADS)

Abdulwahab, M.; Umaru, O. B.; Bawa, M. A.; Jibo, H. A.

The microstructural study via scanning electron microscope (SEM) and thermal study via differential scanning calorimetric (DSC) study of Al-7%Si-0.3Mg/melon shell ash particulate composite has been carried out. The melon shell ash was used in the production of MMC ranging from 5% to 20% at interval of 5% addition using stir casting method. The melon shell ash was characterized using X-ray fluorescent (XRF) that reveal the presence of CaO, SiO2, Al2O3, MgO, and TiO2 as major compounds. The composite was machined and subjected to heat treatment. Microstructural analyses of the composite produced were done using scanning electron microscope (SEM). The microstructure obtained reveals a dark ceramic (reinforcer) and white metallic phase. Equally, the 5 wt% DSC result gives better thermal conductivity than other proportions (10 wt%, 15 wt%, and 20 wt%). These results showed that an improved property of Al-Si-Mg alloy was achieved using melon shell ash particles as reinforcement up to a maximum of 20 wt% for microstructural and 5% wt DSC respectively.

Theoretical Aspects of Differential Scanning Calorimetry as a Tool for the Studies of Equilibrium Thermodynamics in Pharmaceutical Solid Phase Transitions.

PubMed

Faroongsarng, Damrongsak

2016-06-01

Although differential scanning calorimetry (DSC) is a non-equilibrium technique, it has been used to gain energetic information that involves phase equilibria. DSC has been widely used to characterize the equilibrium melting parameters of small organic pharmaceutical compounds. An understanding of how DSC measures an equilibrium event could make for a better interpretation of the results. The aim of this mini-review was to provide a theoretical insight into the DSC measurement to obtain the equilibrium thermodynamics of a phase transition especially the melting process. It was demonstrated that the heat quantity obtained from the DSC thermogram (ΔH) was related to the thermodynamic enthalpy of the phase transition (ΔH (P) ) via: ΔH = ΔH (P) /(1 + K (- 1)) where K was the equilibrium constant. In melting, the solid and liquefied phases presumably coexist resulting in a null Gibbs free energy that produces an infinitely larger K. Thus, ΔH could be interpreted as ΔH (P). Issues of DSC investigations on melting behavior of crystalline solids including polymorphism, degradation impurity due to heating in situ, and eutectic melting were discussed. In addition, DSC has been a tool for determination of the impurity based on an ideal solution of the melt that is one of the official methods used to establish the reference standard.

47 CFR 80.1087 - Ship radio equipment-Sea area A1.

Code of Federal Regulations, 2013 CFR

2013-10-01

... an INMARSAT ship earth station capable of two way communication. (b) The VHF radio installation... which the ship is normally navigated, operating either: (1) On VHF using DSC; or (2) Through the polar... voyages within coverage of MF coast stations equipped with DSC; or (4) On HF using DSC; or (5) Through the...

47 CFR 80.1087 - Ship radio equipment-Sea area A1.

Code of Federal Regulations, 2014 CFR

2014-10-01

... an INMARSAT ship earth station capable of two way communication. (b) The VHF radio installation... which the ship is normally navigated, operating either: (1) On VHF using DSC; or (2) Through the polar... voyages within coverage of MF coast stations equipped with DSC; or (4) On HF using DSC; or (5) Through the...

47 CFR 80.1087 - Ship radio equipment-Sea area A1.

Code of Federal Regulations, 2012 CFR

2012-10-01

... an INMARSAT ship earth station capable of two way communication. (b) The VHF radio installation... which the ship is normally navigated, operating either: (1) On VHF using DSC; or (2) Through the polar... voyages within coverage of MF coast stations equipped with DSC; or (4) On HF using DSC; or (5) Through the...

Poloxamer 407/188 binary thermosensitive hydrogels as delivery systems for infiltrative local anesthesia: Physico-chemical characterization and pharmacological evaluation.

PubMed

Akkari, Alessandra C S; Papini, Juliana Z Boava; Garcia, Gabriella K; Franco, Margareth K K Dias; Cavalcanti, Leide P; Gasperini, Antonio; Alkschbirs, Melissa Inger; Yokaichyia, Fabiano; de Paula, Eneida; Tófoli, Giovana R; de Araujo, Daniele R

2016-11-01

In this study, we reported the development and the physico-chemical characterization of poloxamer 407 (PL407) and poloxamer 188 (PL188) binary systems as hydrogels for delivering ropivacaine (RVC), as drug model, and investigate their use in infiltrative local anesthesia for applications on the treatment of post-operative pain. We studied drug-micelle interaction and micellization process by light scattering and differential scanning calorimetry (DSC), the sol-gel transition and hydrogel supramolecular structure by small-angle-X-ray scattering (SAXS) and morphological evaluation by Scanning Electron Microscopy (SEM). In addition, we have presented the investigation of drug release mechanisms, in vitro/in vivo toxic and analgesic effects. Micellar dimensions evaluation showed the formation of PL407-PL188 mixed micelles and the drug incorporation, as well as the DSC studies showed increased enthalpy values for micelles formation after addition of PL 188 and RVC, indicating changes on self-assembly and the mixed micelles formation evoked by drug incorporation. SAXS studies revealed that the phase organization in hexagonal structure was not affected by RVC insertion into the hydrogels, maintaining their supramolecular structure. SEM analysis showed similar patterns after RVC addition. The RVC release followed the Higuchi model, modulated by the PL final concentration and the insertion of PL 188 into the system. Furthermore, the association PL407-PL188 induced lower in vitro cytotoxic effects, increased the duration of analgesia, in a single-dose model study, without evoking in vivo inflammation signs after local injection. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis, Structural, and Adsorption Properties and Thermal Stability of Nanohydroxyapatite/Polysaccharide Composites.

PubMed

Skwarek, Ewa; Goncharuk, Olena; Sternik, Dariusz; Janusz, Wladyslaw; Gdula, Karolina; Gun'ko, Vladimir M

2017-12-01

A series of composites based on nanohydroxyapatite (nHAp) and natural polysaccharides (PS) (nHAp/agar, nHAp/chitosan, nHAp/pectin FB300, nHAp/pectin APA103, nHAp/sodium alginate) was synthesized by liquid-phase two-step method and characterized using nitrogen adsorption-desorption, DSC, TG, FTIR spectroscopy, and SEM. The analysis of nitrogen adsorption-desorption data shows that composites with a nHAp: PS ratio of 4:1 exhibit a sufficiently high specific surface area from 49 to 82 m 2 /g. The incremental pore size distributions indicate mainly mesoporosity. The composites with the component ratio 1:1 preferably form a film-like structure, and the value of S BET varies from 0.3 to 43 m 2 /g depending on the nature of a polysaccharide. Adsorption of Sr(II) on the composites from the aqueous solutions has been studied. The thermal properties of polysaccharides alone and in nHAp/PS show the influence of nHAp, since there is a shift of characteristic DSC and DTG peaks. FTIR spectroscopy data confirm the presence of functional groups typical for nHAp as well as polysaccharides in composites. Structure and morphological characteristics of the composites are strongly dependent on the ratio of components, since nHAp/PS at 4:1 have relatively large S BET values and a good ability to adsorb metal ions. The comparison of the adsorption capacity with respect to Sr(II) of nHAp, polysaccharides, and composites shows that it of the latter is higher than that of nHAp (per 1 m 2 of surface).

Mechanical performance and thermal stability of glass fiber reinforced silica aerogel composites based on co-precursor method by freeze drying

NASA Astrophysics Data System (ADS)

Zhou, Ting; Cheng, Xudong; Pan, Yuelei; Li, Congcong; Gong, Lunlun; Zhang, Heping

2018-04-01

In order to maintain the integrity, glass fiber (GF) reinforced silica aerogel composites were synthesized using methltrimethoxysilane (MTMS) and water glass co-precursor by freeze drying method. The composites were characterized by scanning electron microscopy, Brunauer-Emmett-Teller analysis, uniaxial compressive test, three-point bending test, thermal conductivity analysis, contact angle test, TG-DSC analysis. It was found that the molar ratio of MTMS/water glass could significantly affect the properties of composites. The bulk density and thermal conductivity first decreased and then increased with the increasing molar ratio. The composites showed remarkable mechanical strength and flexibility compared with pure silica aerogel. Moreover, when the molar ratio is 1.8, the composites showed high specific surface area (870.9 m2/g), high contact angle (150°), great thermal stability (560 °C) and low thermal conductivity (0.0248 W/m·K). These outstanding properties indicate that GF/aerogels have broad prospects in the field of thermal insulation.

Synthesis, growth, structure and nonlinear optical properties of a semiorganic 2-carboxy pyridinium dihydrogen phosphate single crystal

NASA Astrophysics Data System (ADS)

Nagapandiselvi, P.; Baby, C.; Gopalakrishnan, R.

2015-09-01

A new semiorganic compound namely, 2-carboxy pyridinium dihydrogen phosphate (2CPDP) was synthesised and grown as single crystals by slow evaporation solution growth technique. Single crystal XRD showed that 2CPDP belongs to monoclinic crystal system with space group P21/n. The molecular structure was further confirmed by modern spectroscopic techniques like FT-NMR (1H, 13C &31P), FT-IR, UV-Vis-NIR and Fluorescence. The UV-Vis-NIR analysis revealed suitability of the crystal for nonlinear optical applications. The photo active nature of the material is established from fluorescence studies. TG-DSC analysis showed that 2CPDP was thermally stable up to 170 °C. The dependence of dielectric properties on frequency and temperature were also studied. Nonlinear optical absorption determined from open aperture Z-Scan analysis by employing picosecond Nd-YAG laser, revealed that 2CPDP can serve as a promising candidate for optical limiting applications.

Dye-sensitized solar cells consisting of dye-bilayer structure stained with two dyes for harvesting light of wide range of wavelength

NASA Astrophysics Data System (ADS)

Inakazu, Fumi; Noma, Yusuke; Ogomi, Yuhei; Hayase, Shuzi

2008-09-01

Dye-sensitized solar cells (DSCs) containing dye-bilayer structure of black dye and NK3705 (3-carboxymethyl-5-[3-(4-sulfobutyl)-2(3H)-bezothiazolylidene]-2-thioxo-4-thiazolidinone, sodium salt) in one TiO2 layer (2-TiO-BD-NK) are reported. The 2-TiO-BD-NK structure was fabricated by staining one TiO2 layer with these two dyes, step by step, under a pressurized CO2 condition. The dye-bilayer structure was observed by using a confocal laser scanning microscope. The short circuit current (Jsc) and the incident photon to current efficiency of the cell (DSC-2-TiO-BD-NK) was almost the sum of those of DSC stained with black dye only (DSC-1-TiO-BD) and DSC stained with NK3705 only (DSC-1-TiO-NK).

DSC and curing kinetics study of epoxy grouting diluted with furfural -acetone slurry

NASA Astrophysics Data System (ADS)

Yin, H.; Sun, D. W.; Li, B.; Liu, Y. T.; Ran, Q. P.; Liu, J. P.

2016-07-01

The use of furfural-acetone slurry as active diluents of Bisphenol-A epoxy resin (DGEBA) groutings has been studied by dynamic and non-isothermal DSC for the first time. Curing kinetics study was investigated by non-isothermal differential scanning calorimetries at different heating rates. Activation enery (Ea) was calculated based on Kissinger and Ozawa Methods, and the results showed that Ea increased from 58.87 to 71.13KJ/mol after the diluents were added. The furfural-acetone epoxy matrix could cure completely at the theoretical curing temperature of 365.8K and the curing time of 139mins, which were determined by the kinetic model parameters.

Uncovering a reconstructive solid-solid phase transition in a metal-organic framework.

PubMed

Longley, L; Li, N; Wei, F; Bennett, T D

2017-11-01

A nanoporous three-dimensional metal-organic framework (MOF), ZnPurBr undergoes a transition to a previously unreported high-temperature phase, ZnPurBr-ht. The transition, which proceeds without mass loss, is uncovered through the use of differential scanning calorimetry (DSC). The new crystal structure was solved using single-crystal X-ray diffraction, and the mechanical properties of both phases investigated by nanoindentation and density functional theory. The anisotropy of the calculated Young's moduli showed good agreement with the crystallographic alignment of the stiff purinate organic linker. The results provide a prototypical example of the importance of the use of DSC in the MOF field, where its use is not currently standard in characterization.

Disturbed State constitutive modeling of two Pleistocene tills

NASA Astrophysics Data System (ADS)

Sane, S. M.; Desai, C. S.; Jenson, J. W.; Contractor, D. N.; Carlson, A. E.; Clark, P. U.

2008-02-01

The Disturbed State Concept (DSC) provides a general approach for constitutive modeling of deforming materials. Here, we briefly explain the DSC and present the results of laboratory tests on two regionally significant North American tills, along with the results of a numerical simulation to predict the behavior of one of the tills in an idealized physical system. Laboratory shear tests showed that plastic strain starts almost from the beginning of loading, and that failure and resulting motion begin at a critical disturbance, when about 85% of the mass has reached the fully adjusted or critical state. Specimens of both tills exhibited distributed strain, deforming into barrel shapes without visible shear planes. DSC parameters obtained from shear and creep tests were validated by comparing model predictions against test data used to find the parameters, as well as against data from independent tests. The DSC parameters from one of the tills were applied in a finite-element simulation to predict gravity-induced motion for a 5000-m long, 100-m thick slab of ice coupled to an underlying 1.5-m thick layer of till set on a 4° incline, with pore-water pressure in the till at 90% of the load. The simulation predicted that in the middle segment of the till layer (i.e., from x=2000 to 3000 m) the induced (computed) shear stress, strain, and disturbance increase gradually with the applied shear stress. Induced shear stress peaks at ˜60 kPa. The critical disturbance, at which failure occurs, is observed after the peak shear stress, at an induced shear stress of ˜23 kPa and shear strain of ˜0.75 in the till. Calculated horizontal displacement over the height of the entire till section at the applied shear stress of 65 kPa is ˜4.5 m. We note that the numerical prediction of critical disturbance, when the displacement shows a sharp change in rate, compares very well with the occurrence of critical disturbance observed in the laboratory triaxial tests, when a sharp change in the rate of strain occurs. This implies that the failure and concomitant initiation of motion occur near the residual state, at large strains. In contrast to the Mohr-Coulomb model, which predicts failure and motion at very small (elastic) strain, the DSC thus predicts failure and initiation of motion after the till has undergone considerable (plastic) strain. These results suggest that subglacial till may be able to sustain stress in the vicinity of 20 kPa even after the motion begins. They also demonstrate the potential of the DSC to model not only local behavior, including potential "sticky spot" mechanisms, but also global behavior for soft-bedded ice.

Thermal and Mechanical Testing of Neoprene Gloves Used in a Space Shuttle Microgravity Glove Box Experiment

NASA Technical Reports Server (NTRS)

Wingard, Charles Doug; Munafo, Paul M. (Technical Monitor)

2001-01-01

Neoprene gloves are used in a Space Shuttle Microgravity Glove Box (MGBX) experiment. In 1999, significant corrosion was observed in the work area and on the outer surface of the left glove ring. Analysis of the corrosion products showed that they contained chlorine. The Neoprene gloves used in this glove box were obtained in 1995, with a recommended shelf life of 3 years. After storage of these gloves in a cabinet drawer until 1999, significant signs of corrosion were also observed in the drawer. Mechanical and thermal properties were determined on samples cut from the finger and sleeve areas of the "good" and "bad" gloves. This data showed significant aging of the left-hand glove, particularly in the sleeve area. Thermal analysis data by DSC and TGA was complimentary to tensile data in showing this aging. However, this test data did not pinpoint the cause of the left-hand glove aging, or of the corrosion products.

Use of DSC and DMA to Study Rubber Crystallization as a Possible Cause for a Tear in a Neoprene Glove Used in a Space Shuttle Pressurized Astronaut Suit

NASA Technical Reports Server (NTRS)

Wingard, Doug

2009-01-01

The Advanced Crew Escape Suit (ACES) is a pressurized suit normally worn by astronauts during launch and landing phases of Space Shuttle operations. In 2008, a large tear (0.5 -1 in. long, between the pinky and ring finger) in the ACES left-hand glove made of neoprene latex rubber was found during training for Shuttle flight STS-124. An investigation to help determine the cause(s) of the glove tear was headed by the NASA Johnson Space Center (JSC) in Houston, Texas. Efforts at JSC to reproduce the actual glove tear pattern by cutting/tearing or rupturing were unsuccessful. Chemical and material property data from JSC such as GC-MS, FTIR, DSC and TGA mostly showed little differences between samples from the torn and control gloves. One possible cause for the glove tear could be a wedding ring/band worn by a male astronaut. Even with a smooth edge, such a ring could scratch the material and initiate the tear observed in the left-hand glove. A decision was later made by JSC to not allow the wearing of such a ring during training or actual flight. Another possible cause for the ACES glove tear is crystallinity induced by strain in the neoprene rubber over a long period of time and use. Neoprene is one several elastomeric materials known to be susceptible to crystallization, and such a process is accelerated with exposure of the material to cold temperatures plus strain. When the temperature is lowered below room temperature, researchers have shown that neoprene crystallization may be maintained at temperatures as high as 45-50 F, with a maximum crystallization rate near 20-25 F (1). A convenient conditioning temperature for inducing neoprene crystallization is a typical freezer that is held near 0 F. For work at the NASA Marshall Space Flight Center (MSFC), samples were cut from several areas/locations (pinky/ring finger crotch, index finger and palm) on each of two pairs of unstrained ACES gloves for DSC and DMA thermal analysis testing. The samples were conditioned in a freezer for various times up to about 14 days. Some rectangular conditioned samples were unstrained, while most were subjected to strains up to 250% with the aid of two slotted aluminum blocks and two aluminum clamps per sample. Trends were observed to correlate DSC data (heat of fusion) and DMA data (linear CTE and stress for iso-strain testing) with: (a) sample location on each glove; and (b) level of strain during conditioning. Control samples cut as is from each glove location were also tested by DSC and DMA.

Use of Several Thermal Analysis Techniques on a Hypalon Paint Coating for the Solid Rocket Booster (SRB) of the Space Shuttle

NASA Technical Reports Server (NTRS)

Wingard, Charles D.; Whitaker, Ann F. (Technical Monitor)

2000-01-01

White Hypalon paint is brush-applied as a moisture barrier coating over cork surfaces on each of the two Space Shuttle SRBs. Fine cracks have been observed in the Hypalon coating three times historically on laboratory witness panels, but never on flight hardware. Samples of the cracked and standard ("good") Hypalon were removed from witness panel cork surfaces, and were tested in 1998 by Thermogravimetric Analysis (TGA), TMA and Differential Scanning Calorimetry (DSC) thermal analysis techniques. The TGA data showed that at 700C, where only paint pigment solids remain, the cracked material had about 9 weight percent more material remaining than the standard material, probably indicating incomplete mixing of the paint before it was brush-applied to produce the cracked material. Use of the TMA film/fiber technique showed that the average modulus (stiffness) vs. temperature was about 3 to 6 times higher for the cracked material than for the standard material. The TMA data also showed that an increase in coating thickness for the cracked Hypalon was not a factor in the anomaly.

Discovery of S···C≡N Intramolecular Bonding in a Thiophenylcyanoacrylate-Based Dye: Realizing Charge Transfer Pathways and Dye···TiO 2 Anchoring Characteristics for Dye-Sensitized Solar Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cole, Jacqueline M.; Blood-Forsythe, Martin A.; Lin, Tze-Chia

Donor-pi-acceptor dyes containing thiophenyl pi-conjugated units and cyanoacrylate acceptor groups are among the best-performing organic chromophores used in dye-sensitized solar cell (DSC) applications. Yet, the molecular origins of their high photovoltaic output have remained unclear until now. This synchrotron-based X-ray diffraction study elucidates these origins for the high-performance thiophenylcyanoacrylate-based dye MK-2 (7.7% DSC device efficiency) and its molecular building block, MK-44. The crystal structures of MK-2 and MK-44 are both determined, while a high-resolution charge-density mapping of the smaller molecule was also possible, enabling the nature of its bonding to be detailed. A strong S center dot center dot centermore » dot C equivalent to N intramolecular interaction is discovered, which bears a bond critical point, thus proving that this interaction should be formally classified as a chemical bond. A topological analysis of the pi-conjugated portion of MK-44 shows that this S center dot center dot center dot C equivalent to N bonding underpins the highly efficient intramolecular charge transfer(ICT) in thiophenylcyanoacrylate dyes. This manifests as two bipartite ICT pathways bearing carboxylate and nitrile end points. In turn, these pathways dictate a preferred COO/CN anchoring mode for the dye as it adsorbs onto TiO2 surfaces, to form the dye TiO2 interface that constitutes the DSC working electrode. These results corroborate a recent proposal that all cyanoacrylate groups anchor onto TiO2 in this COO/CN binding configuration. Conformational analysis of the MK-44 and MK-2 crystal structures reveals that this S center dot center dot center dot C equivalent to N bonding will persist in MK-2. Accordingly, this newly discovered bond affords a rational explanation for the attractive photovoltaic properties of,MK-2. More generally, this study provides the first unequivocal evidence for an S center dot center dot center dot C equivalent to N interaction, confirming previous speculative assignments of such interactions in other compounds.« less

Discovery of S···C≡N Intramolecular Bonding in a Thiophenylcyanoacrylate-Based Dye: Realizing Charge Transfer Pathways and Dye···TiO2 Anchoring Characteristics for Dye-Sensitized Solar Cells.

PubMed

Cole, Jacqueline M; Blood-Forsythe, Martin A; Lin, Tze-Chia; Pattison, Philip; Gong, Yun; Vázquez-Mayagoitia, Álvaro; Waddell, Paul G; Zhang, Lei; Koumura, Nagatoshi; Mori, Shogo

2017-08-09

Donor-π-acceptor dyes containing thiophenyl π-conjugated units and cyanoacrylate acceptor groups are among the best-performing organic chromophores used in dye-sensitized solar cell (DSC) applications. Yet, the molecular origins of their high photovoltaic output have remained unclear until now. This synchrotron-based X-ray diffraction study elucidates these origins for the high-performance thiophenylcyanoacrylate-based dye MK-2 (7.7% DSC device efficiency) and its molecular building block, MK-44. The crystal structures of MK-2 and MK-44 are both determined, while a high-resolution charge-density mapping of the smaller molecule was also possible, enabling the nature of its bonding to be detailed. A strong S···C≡N intramolecular interaction is discovered, which bears a bond critical point, thus proving that this interaction should be formally classified as a chemical bond. A topological analysis of the π-conjugated portion of MK-44 shows that this S···C≡N bonding underpins the highly efficient intramolecular charge transfer (ICT) in thiophenylcyanoacrylate dyes. This manifests as two bipartite ICT pathways bearing carboxylate and nitrile end points. In turn, these pathways dictate a preferred COO/CN anchoring mode for the dye as it adsorbs onto TiO 2 surfaces, to form the dye···TiO 2 interface that constitutes the DSC working electrode. These results corroborate a recent proposal that all cyanoacrylate groups anchor onto TiO 2 in this COO/CN binding configuration. Conformational analysis of the MK-44 and MK-2 crystal structures reveals that this S···C≡N bonding will persist in MK-2. Accordingly, this newly discovered bond affords a rational explanation for the attractive photovoltaic properties of MK-2. More generally, this study provides the first unequivocal evidence for an S···C≡N interaction, confirming previous speculative assignments of such interactions in other compounds.

The Structural Formation and Physical Behaviour of Cross-Linked Epoxy Resins

DTIC Science & Technology

1981-04-01

analysis , at which the heat evolution reaches a maximum, may be used for purposes of characterisation. Aliphatic polyamines react mere quickly than the...DTA, DSC), thermomechanical analysis (TMA), torsional vibration analysis (TVA), deter- mination of the dimensional stability under heat (eq ISO R 75 or...obtained by thermomechanical analysis , taking the temperature of maximum velocity of penetration of a loaded probe (rate of heating - 10°C/min

An elegant access to formation and vaporization enthalpies of ionic liquids by indirect DSC experiment and "in silico" calculations.

PubMed

Verevkin, Sergey P; Zaitsau, Dzmitry H; Emel'yanenko, Vladimir N; Schick, Christoph; Jayaraman, Saivenkataraman; Maginn, Edward J

2012-07-14

We used DSC for determination of the reaction enthalpy of the synthesis of the ionic liquid [C(4)mim][Cl]. A combination of DSC and quantum chemical calculations presents a new, indirect way to study thermodynamics of ionic liquids. The new procedure was validated with two direct experimental measurements and MD simulations.

D-DSC: Decoding Delay-based Distributed Source Coding for Internet of Sensing Things

PubMed Central

Akan, Ozgur B.

2018-01-01

Spatial correlation between densely deployed sensor nodes in a wireless sensor network (WSN) can be exploited to reduce the power consumption through a proper source coding mechanism such as distributed source coding (DSC). In this paper, we propose the Decoding Delay-based Distributed Source Coding (D-DSC) to improve the energy efficiency of the classical DSC by employing the decoding delay concept which enables the use of the maximum correlated portion of sensor samples during the event estimation. In D-DSC, network is partitioned into clusters, where the clusterheads communicate their uncompressed samples carrying the side information, and the cluster members send their compressed samples. Sink performs joint decoding of the compressed and uncompressed samples and then reconstructs the event signal using the decoded sensor readings. Based on the observed degree of the correlation among sensor samples, the sink dynamically updates and broadcasts the varying compression rates back to the sensor nodes. Simulation results for the performance evaluation reveal that D-DSC can achieve reliable and energy-efficient event communication and estimation for practical signal detection/estimation applications having massive number of sensors towards the realization of Internet of Sensing Things (IoST). PMID:29538405

D-DSC: Decoding Delay-based Distributed Source Coding for Internet of Sensing Things.

PubMed

Aktas, Metin; Kuscu, Murat; Dinc, Ergin; Akan, Ozgur B

2018-01-01

Spatial correlation between densely deployed sensor nodes in a wireless sensor network (WSN) can be exploited to reduce the power consumption through a proper source coding mechanism such as distributed source coding (DSC). In this paper, we propose the Decoding Delay-based Distributed Source Coding (D-DSC) to improve the energy efficiency of the classical DSC by employing the decoding delay concept which enables the use of the maximum correlated portion of sensor samples during the event estimation. In D-DSC, network is partitioned into clusters, where the clusterheads communicate their uncompressed samples carrying the side information, and the cluster members send their compressed samples. Sink performs joint decoding of the compressed and uncompressed samples and then reconstructs the event signal using the decoded sensor readings. Based on the observed degree of the correlation among sensor samples, the sink dynamically updates and broadcasts the varying compression rates back to the sensor nodes. Simulation results for the performance evaluation reveal that D-DSC can achieve reliable and energy-efficient event communication and estimation for practical signal detection/estimation applications having massive number of sensors towards the realization of Internet of Sensing Things (IoST).

Analysis of the thermodynamics of binding of an SH3 domain to proline-rich peptides using a chimeric fusion protein.

PubMed

Candel, Adela M; van Nuland, Nico A J; Martin-Sierra, Francisco M; Martinez, Jose C; Conejero-Lara, Francisco

2008-03-14

A complete understanding of the thermodynamic determinants of binding between SH3 domains and proline-rich peptides is crucial to the development of rational strategies for designing ligands for these important domains. Recently we engineered a single-chain chimeric protein by fusing the alpha-spectrin Src homology region 3 (SH3) domain to the decapeptide APSYSPPPPP (p41). This chimera mimics the structural and energetic features of the interaction between SH3 domains and proline-rich peptides. Here we show that analysing the unfolding thermodynamics of single-point mutants of this chimeric fusion protein constitutes a very useful approach to deciphering the thermodynamics of SH3-ligand interactions. To this end, we investigated the contribution of each proline residue of the ligand sequence to the SH3-peptide interaction by producing six single Pro-Ala mutants of the chimeric protein and analysing their unfolding thermodynamics by differential scanning calorimetry (DSC). Structural analyses of the mutant chimeras by circular dichroism, fluorescence and NMR together with NMR-relaxation measurements indicate conformational flexibility at the binding interface, which is strongly affected by the different Pro-Ala mutations. An analysis of the DSC thermograms on the basis of a three-state unfolding model has allowed us to distinguish and separate the thermodynamic magnitudes of the interaction at the binding interface. The model assumes equilibrium between the "unbound" and "bound" states at the SH3-peptide binding interface. The resulting thermodynamic magnitudes classify the different proline residues according to their importance in the interaction as P2 approximately P7 approximately P10>P9 approximately P6>P8, which agrees well with Lim's model for the interaction between SH3 domains and proline-rich peptides. In addition, the thermodynamic signature of the interaction is the same as that usually found for this type of binding, with a strong enthalpy-entropy compensation for all the mutants. This compensation appears to derive from an increase in conformational flexibility concomitant to the weakening of the interactions at the binding interface. We conclude that our approach, based on DSC and site-directed mutagenesis analysis of chimeric fusion proteins, may serve as a suitable tool to analyse the energetics of weak biomolecular interactions such as those involving SH3 domains.

Enhancing Skin Permeation of Biphenylacetic Acid (BPA) Using Salt Formation with Organic and Alkali Metal Bases

PubMed Central

Pawar, Vijay; Naik, Prashant; Giridhar, Rajani; Yadav, Mange Ram

2015-01-01

In the present study, a series of organic and alkali metal salts of biphenylacetic acid (BPA) have been prepared and evaluated in vitro for percutaneous drug delivery. The physicochemical properties of BPA salts were determined using solubility measurements, DSC, and IR. The DSC thermogram and FTIR spectra confirmed the salt formation with organic and alkali metal bases. Among the series, salts with organic amines (ethanolamine, diethanolamine, triethanolamine, and diethylamine) had lowered melting points while the alkali metal salt (sodium) had a higher melting point than BPA. The in vitro study showed that salt formation improves the physicochemical properties of BPA, leading to improved permeability through the skin. Amongst all the prepared salts, ethanolamine salt (1b) showed 7.2- and 5.4-fold higher skin permeation than the parent drug at pH 7.4 and 5.0, respectively, using rat skin. PMID:26839810

Microstructural Characterization of Aluminum-Lithium Alloys 1460 and 2195

NASA Technical Reports Server (NTRS)

Wang, Z. M.; Shenoy, R. N.

1998-01-01

Transmission electron microscopy (TEM) and differential scanning calorimetry (DSC) techniques were employed to characterize the precipitate distributions in lithium-containing aluminum alloys 1460 and 2195 in the T8 condition. TEM examinations revealed delta prime and T1 as the primary strengthening precipitates in alloys 1460 and 2195 respectively. TEM results showed a close similarity of the Russian alloy 1460 to the U.S. alloy 2090, which has a similar composition and heat treatment schedule. DSC analyses also indicate a comparable delta prime volume fraction. TEM study of a fractured tensile sample of alloy 1460 showed that delta prime precipitates are sheared by dislocations during plastic deformation and that intense stress fields arise at grain boundaries due to planar slip. Differences in fracture toughness of alloys 1460 and 2195 are rationalized on the basis of a literature review and observations from the present study.

Epoxy monomers derived from tung oil fatty acids and its regulable thermosets cured in two synergistic ways

USDA-ARS?s Scientific Manuscript database

A new bio-based epoxy monomer with conjugated double bonds, glycidyl ester of eleostearic acid (GEEA), was synthesized from tung oil fatty acids and characterized by 1H-NMR, 13C-NMR and Mass Spectrometry Analysis (MSA). Differential Scanning Calorimetry (DSC) analysis and FT-IR were utilized to inve...

SOM quality and phosphorus fractionation to evaluate degradation organic matter: implications for the restoration of soils after fire

NASA Astrophysics Data System (ADS)

Merino, Agustin; Fonturbel, Maria T.; Omil, Beatriz; Chávez-Vergara, Bruno; Fernandez, Cristina; Garcia-Oliva, Felipe; Vega, Jose A.

2016-04-01

The design of emergency treatment for the rehabilitation of fire-affected soils requires a quick diagnosis to assess the degree of degradation. For its implication in the erosion and subsequent evolution, the quality of soil organic matter (OM) plays a particularly important role. This paper presents a methodology that combines the visual recognition of the severity of soil burning with the use of simple analytical techniques to assess the degree of degradation of OM. The content and quality of the OM was evaluated in litter and mineral soils using thermogravimetry-differential scanning calorimetry (DSC-TG) spectroscopy, and the results were contrasted with 13C CP-MAS NMR. The types of methodologies were texted to assess the thermal analysis: a) the direct calculation of the Q areas related to three degrees of thermal stabilities: Q1 (200-375 °C; labil OM); Q2 (375-475 °C, recalcitrant OM); and Q3 (475-550 °C). b) deconvolution of DSC curves and calculation of each peak was expressed as a fraction of the total DSC curve area. Additionally, a P fractionation was done following the Hedley sequential extraction method. The severity levels visually showed different degrees of SOM degradation. Although the fire caused important SOM losses in moderate severities, changes in the quality of OM only occurred at higher severities. Besides, the labile organic P fraction decreased and the occluded inorganic P fraction increased in the high severity soils. These changes affect the OM processes such as hydrophobicity and erosion largely responsible for soil degradation post-fire. The strong correlations between the thermal parameters and NMR regions and derived measurements such as hydrophobicity and aromaticity show the usefulness of this technique as rapid diagnosis to assess the soil degradation.The marked loss of polysaccharide and transition to highly thermic-resistant compounds, visible in deconvoluted thermograms, which would explain the changes in microbial activity and soil nutrients availability (basal respiration, microbial biomass, qCO2, and enzymatic activity). And also it would have implications in hydrophobicity and stability of soil aggregates, leading to the extreme erosion rates that occur usually are found in soils affected by higher severities.

Better latent heat and specific heat of stearic acid with magnetite/graphene nanocomposite addition for thermal storage application

NASA Astrophysics Data System (ADS)

Andiarto, R.; Nuryadin, M. K.; Taufik, A.; Saleh, R.

2017-04-01

In our previous study, the addition of Magnetite (Fe3O4) into Stearic acid (Sa) as an organic phase change material (PCM) shows an enhancement in the latent heat for thermal energy storage applications. The latent heat of the PCM can also be increased by adding graphene material. Therefore, in this research, the thermal properties of Sa have been studied by the sonication method for several different concentrations of Fe3O4/Graphene nanocomposite additions. The structural properties of all of the samples were observed by X-Ray diffraction (XRD). Melting-solidifying behavior and specific heat value were measured by differential scanning calorimetry (DSC). The thermal degradation process of all samples was investigated by thermogravimetric analysis (TGA). Based on the DSC results, the presence of Fe3O4/Graphene in the Sa enhances the latent heat up to 20%. The specific heat value of the mixture was also found to be increased as the concentration of Fe3O4/Graphene to Sa increased. The TGA results show a lowered thermal degradation process of the Sa by the addition of the Fe3O4/Graphene which indicates a higher thermal stability of the mixture. In conclusion, the results demonstrate that the addition of Fe3O4/Graphene to Sa improves both the sensible heat and the latent heat of the mixture which are very important for thermal energy storage applications

Preparation and characterization of flame retardant n-hexadecane/silicon dioxide composites as thermal energy storage materials.

PubMed

Fang, Guiyin; Li, Hui; Chen, Zhi; Liu, Xu

2010-09-15

Flame retardant n-hexadecane/silicon dioxide (SiO(2)) composites as thermal energy storage materials were prepared using sol-gel methods. In the composites, n-hexadecane was used as the phase change material for thermal energy storage, and SiO(2) acted as the supporting material that is fire resistant. In order to further improve flame retardant property of the composites, the expanded graphite (EG) was added in the composites. Fourier transformation infrared spectroscope (FT-IR), X-ray diffractometer (XRD) and scanning electronic microscope (SEM) were used to determine chemical structure, crystalloid phase and microstructure of flame retardant n-hexadecane/SiO(2) composites, respectively. The thermal properties and thermal stability were investigated by a differential scanning calorimeter (DSC) and a thermogravimetric analysis apparatus (TGA), respectively. The SEM results showed that the n-hexadecane was well dispersed in the porous network of the SiO(2). The DSC results indicated that the melting and solidifying latent heats of the composites are 147.58 and 145.10 kJ/kg when the mass percentage of the n-hexadecane in the composites is 73.3%. The TGA results showed that the loading of the EG increased the charred residue amount of the composites at 700 degrees C, contributing to the improved thermal stability of the composites. It was observed from SEM photographs that the homogeneous and compact charred residue structure after combustion improved the flammability of the composites. Copyright 2010 Elsevier B.V. All rights reserved.

Naproxen Microparticulate Systems Prepared Using In Situ Crystallisation and Freeze-Drying Techniques.

PubMed

Solaiman, Amanda; Tatari, Adam Keenan; Elkordy, Amal Ali

2017-07-01

Poor drug solubility and dissolution rate remain to be one of the major problems facing pharmaceutical scientists, with approximately 40% of drugs in the industry categorised as practically insoluble or poorly water soluble. This in turn can lead to serious delivery challenges and poor bioavailability. The aim of this research was to investigate the effects of the surfactants, poloxamer 407 (P407) and caprol® PGE 860 (CAP), at various concentrations (0.1, 0.5, 1 and 3% w/v) on the enhancement of the dissolution properties of poorly water-soluble drug, naproxen, using in situ micronisation by solvent change method and freeze-drying. The extent at which freeze-drying influences the dissolution rate of naproxen microcrystals is investigated in this study by comparison with desiccant-drying. All formulations were evaluated and characterised using particle size analysis and morphology, in vitro dissolution studies, differential scanning calorimetry (DSC), and Fourier transform infra-red (FT-IR) spectroscopy. An increase in poloxamer 407 concentration in freeze-dried formulations led to enhancement of drug dissolution compared to desiccator-dried formulations, naproxen/caprol® PGE 860 formulations and untreated drug. DSC and FT-IR results show no significant chemical interactions between drug and poloxamer 407, with only very small changes to drug crystallinity. On the other hand, caprol® PGE 860 showed some interactions with drug components, alterations to the crystal lattice of naproxen, and poor dissolution profiles using both drying methods, making it a poor choice of excipient.

Poster — Thur Eve — 59: Atlas Selection for Automated Segmentation of Pelvic CT for Prostate Radiotherapy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mallawi, A; Farrell, T; Diamond, K

2014-08-15

Automated atlas-based segmentation has recently been evaluated for use in planning prostate cancer radiotherapy. In the typical approach, the essential step is the selection of an atlas from a database that best matches the target image. This work proposes an atlas selection strategy and evaluates its impact on the final segmentation accuracy. Prostate length (PL), right femoral head diameter (RFHD), and left femoral head diameter (LFHD) were measured in CT images of 20 patients. Each subject was then taken as the target image to which all remaining 19 images were affinely registered. For each pair of registered images, the overlapmore » between prostate and femoral head contours was quantified using the Dice Similarity Coefficient (DSC). Finally, we designed an atlas selection strategy that computed the ratio of PL (prostate segmentation), RFHD (right femur segmentation), and LFHD (left femur segmentation) between the target subject and each subject in the atlas database. Five atlas subjects yielding ratios nearest to one were then selected for further analysis. RFHD and LFHD were excellent parameters for atlas selection, achieving a mean femoral head DSC of 0.82 ± 0.06. PL had a moderate ability to select the most similar prostate, with a mean DSC of 0.63 ± 0.18. The DSC obtained with the proposed selection method were slightly lower than the maximums established using brute force, but this does not include potential improvements expected with deformable registration. Atlas selection based on PL for prostate and femoral diameter for femoral heads provides reasonable segmentation accuracy.« less

Reticulation of Aqueous Polyurethane Systems Controlled by DSC Method

PubMed Central

Cakic, Suzana; Lacnjevac, Caslav; Rajkovic, Milos B.; Raskovic, Ljiljana; Stamenkovic, Jakov

2006-01-01

The DSC method has been employed to monitor the kinetics of reticulation of aqueous polyurethane systems without catalysts, and with the commercial catalyst of zirconium (CAT®XC-6212) and the highly selective manganese catalyst, the complex Mn(III)-diacetylacetonemaleinate (MAM). Among the polyol components, the acrylic emulsions were used for reticulation in this research, and as suitable reticulation agents the water emulsible aliphatic polyisocyanates based on hexamethylendoisocyanate with the different contents of NCO-groups were employed. On the basis of DSC analysis, applying the methods of Kissinger, Freeman-Carroll and Crane-Ellerstein the pseudo kinetic parameters of the reticulation reaction of aqueous systems were determined. The temperature of the examination ranged from 50°C to 450°C with the heat rate of 0.5°C/min. The reduction of the activation energy and the increase of the standard deviation indicate the catalytic action of the selective catalysts of zirconium and manganese. The impact of the catalysts on the reduction of the activation energy is the strongest when using the catalysts of manganese and applying all the three afore-said methods. The least aberrations among the stated methods in defining the kinetic parameters were obtained by using the manganese catalyst.

DSC studies on gamma irradiated poly(vinylidene fluoride) applied to high gamma dose dosimetry

NASA Astrophysics Data System (ADS)

Batista, Adriana S. M.; Faria, Luiz O.

2017-11-01

Poly(vinylidene fluoride) homopolymer (PVDF) was investigated for use on high gamma dose dosimetry. Samples were irradiated with gamma doses ranging from 100 kGy to 3000 kGy. Differential scanning calorimetry (DSC) was used to construct an unambiguous relationship between the melting transition latent heat (LM) and the absorbed dose (D). DSC thermograms were taken immediately, 1, 2 and 8 months after the irradiation process revealing that the LMx D relationship presented no change for doses ranging from 100 to 2750 kGy. FTIR and UV-Vis spectroscopy data revealed the radio-induction of C˭O and C˭C bonds. These radio-induced bonds were responsible by the chain stiffening and chain oxidation, respectively. SEM microscopy demonstrates that the spherulitic large crystalline structures present in pristine PVDF are destroyed with doses as low as 100 kGy. The DRX analysis revealed that the main effect of high gamma doses in the crystalline structure of PVDF is to provoke a change from the pristine PVDF α-phase to the γ-phase. Both the ability to detect gamma doses in a large dose range and the low fading features make PVDF homopolymers good candidates to be investigated as high gamma dose dosimeters.

"Sticky electrons" transport and interfacial transfer of electrons in the dye-sensitized solar cell.

PubMed

Peter, Laurence

2009-11-17

Dye-sensitized solar cells (DSCs, also known as Gratzel cells) mimic the photosynthetic process by using a sensitizer dye to harvest light energy to generate electrical power. Several functional features of these photochemical devices are unusual, and DSC research offers a rewarding arena in which to test new ideas, new materials, and new methodologies. Indeed, one of the most attractive chemical features of the DSC is that the basic concept can be used to construct a range of devices, replacing individual components with alternative materials. Despite two decades of increasing research activity, however, many aspects of the behavior of electrons in the DSC remain puzzling. In this Account, we highlight current understanding of the processes involved in the functioning of the DSC, with particular emphasis on what happens to the electrons in the mesoporous film following the injection step. The collection of photoinjected electrons appears to involve a random walk process in which electrons move through the network of interconnected titanium dioxide nanoparticles while undergoing frequent trapping and detrapping. During their passage to the cell contact, electrons may be lost by transfer to tri-iodide species in the redox electrolyte that permeates the mesoporous film. Competition between electron collection and back electron transfer determines the performance of a DSC: ideally, all injected electrons should be collected without loss. This Account then goes on to survey recent experimental and theoretical progress in the field, placing particular emphasis on issues that need to be resolved before we can gain a clear picture of how the DSC works. Several important questions about the behavior of "sticky" electrons, those that undergo multiple trapping and detrapping, in the DSC remain unanswered. The most fundamental of these concerns is the nature of the electron traps that appear to dominate the time-dependent photocurrent and photovoltage response of DSCs. The origin of the nonideality factor in the relationship between the intensity and the DSC photovoltage is also unclear, as is the discrepancy in electron diffusion length values determined by steady-state and non-steady-state methods. With these unanswered questions, DSC research is likely to remain an active and fruitful area for some years to come.

Design and Evaluation of Topical Diclofenac Sodium Gel Using Hot Melt Extrusion Technology as a Continuous Manufacturing Process with Kolliphor® P407.

PubMed

Pawar, Jaywant; Narkhede, Rajkiran; Amin, Purnima; Tawde, Vaishali

2017-08-01

The aim of the present context was to develop and evaluate a Kolliphor® P407-based transdermal gel formulation of diclofenac sodium by hot melt extrusion (HME) technology; central composite design was used to optimize the formulation process. In this study, we have explored first time ever HME as an industrially feasible and continuous manufacturing technology for the manufacturing of gel formulation using Kolliphor® P407 and Kollisolv® PEG400 as a gel base. Diclofenac sodium was used as a model drug. The HME parameters such as feeding rate, screw speed, and barrel temperature were crucial for the semisolid product development, and were optimized after preliminary trials. For the processing of the gel formulation by HME, a modified screw design was used to obtain a uniform product. The obtained product was evaluated for physicochemical characterization such as differential scanning calorimetry (DSC), X-ray diffraction (XRD), pH measurement, rheology, surface tension, and texture profile analysis. Moreover, it was analyzed for general appearance, spreadibility, surface morphology, and drug content. The optimized gel formulation showed homogeneity and transparent film when applied on a glass slide under microscope, pH was 7.02 and uniform drug content of 100.04 ± 2.74 (SD = 3). The DSC and XRD analysis of the HME gel formulation showed complete melting of crystalline API into an amorphous form. The Kolliphor® P407 and Kollisolv® PEG400 formed excellent gel formulation using HME with consistent viscoelastic properties of the product. An improved drug release was found for the HME gel, which showed a 100% drug release than that of a marketed product which showed only 88% of drug release at the end of 12 h. The Flux value of the HME gel was 106 than that of a marketed formulation, which showed only about 60 value, inferring a significant difference (P < 0.05) at the end of 1 h. This study demonstrates a novel application of the hot melt extrusion process for manufacturing of topical semisolid products.

Probing Protein Sequences as Sources for Encrypted Antimicrobial Peptides

PubMed Central

Brand, Guilherme D.; Magalhães, Mariana T. Q.; Tinoco, Maria L. P.; Aragão, Francisco J. L.; Nicoli, Jacques; Kelly, Sharon M.; Cooper, Alan; Bloch, Carlos

2012-01-01

Starting from the premise that a wealth of potentially biologically active peptides may lurk within proteins, we describe here a methodology to identify putative antimicrobial peptides encrypted in protein sequences. Candidate peptides were identified using a new screening procedure based on physicochemical criteria to reveal matching peptides within protein databases. Fifteen such peptides, along with a range of natural antimicrobial peptides, were examined using DSC and CD to characterize their interaction with phospholipid membranes. Principal component analysis of DSC data shows that the investigated peptides group according to their effects on the main phase transition of phospholipid vesicles, and that these effects correlate both to antimicrobial activity and to the changes in peptide secondary structure. Consequently, we have been able to identify novel antimicrobial peptides from larger proteins not hitherto associated with such activity, mimicking endogenous and/or exogenous microorganism enzymatic processing of parent proteins to smaller bioactive molecules. A biotechnological application for this methodology is explored. Soybean (Glycine max) plants, transformed to include a putative antimicrobial protein fragment encoded in its own genome were tested for tolerance against Phakopsora pachyrhizi, the causative agent of the Asian soybean rust. This procedure may represent an inventive alternative to the transgenic technology, since the genetic material to be used belongs to the host organism and not to exogenous sources. PMID:23029273

Dielectric, thermal and Raman spectroscopy studies of lead-free (Na0.5Bi0.5)1-xSrxTiO3 (x = 0, 0.04 and 0.06) ceramics

NASA Astrophysics Data System (ADS)

Suchanicz, J.; Bovtun, V.; Dutkiewicz, E. M.; Konieczny, K.; Sitko, D.; Kluczewska, K.; Wajda, A.; Kalvane, A.; Sternberg, A.

2016-08-01

Lead-free (Na0.5Bi0.5)1-xSrxTiO3 (x = 0, 0.04 and 0.06) ceramics with relative densities above 97% were prepared by solid-state synthesis process. Their dielectric, thermal and Raman properties were studied. X-ray diffraction analysis shows perovskite structure with rhombohedral symmetry at room temperature. Sr doping of Na0.5Bi0.5TiO3 (NBT) results in an increase of the dielectric permittivity, diffusing of the permittivity maximum and its shift toward lower temperatures. The temperature of the rhombohedral-tetragonal phase transition indicated by the differential scanning calorimetry (DSC) peak and relaxational dielectric anomaly near the depolarization temperature are also shifted toward lower temperatures. The observed increase and broadening of the permittivity maximum, enhancement of the dielectric relaxation near the depolarization temperature, broadening of the DSC anomaly related to the rhombohedral-tetragonal phase transition and broadening of the Raman bands with increasing Sr content are attributed to the increase of the degree of cationic disorder and evident enhancement of the relaxor-like features in NBT-xST. This enhancement could play a positive role in the improvement of the piezoelectric performance of NBT-based ceramics.

Biosynthesis of silver nanoparticles using Alternanthera sessilis (Linn.) extract and their antimicrobial, antioxidant activities.

PubMed

Niraimathi, K L; Sudha, V; Lavanya, R; Brindha, P

2013-02-01

The present work focuses the use of the aqueous extract of Alternanthera sessilis Linn. (Amaranthaceae) in producing silver nanoparticles (AgNPs) from silver nitrate aqueous. Phytochemical analysis of the extract revealed the presence of alkaloid, tannins, ascorbic acid, carbohydrates and proteins and they serve as effective reducing and capping agents for converting silver nitrate into nanoparticles. The synthesized silver nanoparticles (AgNPs) were also tested for proteins and ascorbic acid. Its pH was also determined (5.63). The AgNPs obtained was characterized by UV-vis spectroscopy, FT-IR spectroscopy, SEM, Zeta sizer and TG-DSC. SEM images which revealed the presence of various shapes and sizes. FT-IR spectrum showed the AgNPs having a coating of proteins indicating a dual role of bio-molecules responsible for capping and efficient stabilization of the silver nanoparticles. Presence of impurities and melting point profile were screened by TG-DSC analyzer. AgNPs were synthesized from the silver nitrate through the reducing power of ascorbic acid present in A. sessilis leaves. In this study, we also investigated antimicrobial and antioxidant activity of green synthesized AgNPs. The antimicrobial activity is investigated by Bauer et al.'s method. Antioxidant activity was done by DPPH method. Copyright © 2012 Elsevier B.V. All rights reserved.

Miscibility of choline-substituted polyphosphazenes with PLGA and osteoblast activity on resulting blends.

PubMed

Weikel, Arlin L; Owens, Steven G; Morozowich, Nicole L; Deng, Meng; Nair, Lakshmi S; Laurencin, Cato T; Allcock, Harry R

2010-11-01

The preparation of phosphazene tissue engineering scaffolds with bioactive side groups has been accomplished using the biological buffer, choline chloride. Mixed-substituent phosphazene cyclic trimers (as model systems) and polymers with choline chloride and glycine ethyl ester, alanine ethyl ester, valine ethyl ester, or phenylalanine ethyl ester were synthesized. Two different synthetic protocols were examined. A sodium hydride mediated route resulted in polyphosphazenes with a low choline content, while a cesium carbonate mediated process produced polyphosphazenes with higher choline content. The phosphazene structures and physical properties were studied using multinuclear NMR, differential scanning calorimetry (DSC), and gel permeation chromatography (GPC) techniques. The resultant polymers were then blended with PLGA (50:50) or PLGA (85:15) and characterized by DSC analysis and scanning electron microscopy (SEM). Polymer products obtained via the sodium hydride route produced miscible blends with both ratios of PLGA, while the cesium carbonate route yielded products with reduced blend miscibility. Heterophase hydrolysis experiments in aqueous media revealed that the polymer blends hydrolyzed to near-neutral pH media (∼5.8 to 6.8). The effect of different molecular structures on cellular adhesion showed osteoblast proliferation with an elevated osteoblast phenotype expression compared to PLGA over a 21-day culture period. Copyright © 2010 Elsevier Ltd. All rights reserved.

Identification of immunohistochemical markers for distinguishing lung adenocarcinoma from squamous cell carcinoma

PubMed Central

Zhan, Cheng; Yan, Li; Wang, Lin; Sun, Yang; Wang, Xingxing; Lin, Zongwu; Zhang, Yongxing; Wang, Qun

2015-01-01

Background Immunohistochemical staining has been widely used in distinguishing lung adenocarcinoma (LUAD) from lung squamous cell carcinoma (LUSC), which is of vital importance for the diagnosis and treatment of lung cancer. Due to the lack of a comprehensive analysis of different lung cancer subtypes, there may still be undiscovered markers with higher diagnostic accuracy. Methods Herein first, we systematically analyzed high-throughput data obtained from The Cancer Genome Atlas (TCGA) database. Combining differently expressed gene screening and receiver operating characteristic (ROC) curve analysis, we attempted to identify the genes which might be suitable as immunohistochemical markers in distinguishing LUAD from LUSC. Then we detected the expression of six of these genes (MLPH, TMC5, SFTA3, DSG3, DSC3 and CALML3) in lung cancer sections using immunohistochemical staining. Results A number of genes were identified as candidate immunohistochemical markers with high sensitivity and specificity in distinguishing LUAD from LUSC. Then the staining results confirmed the potentials of the six genes (MLPH, TMC5, SFTA3, DSG3, DSC3 and CALML3) in distinguishing LUAD from LUSC, and their sensitivity and specificity were not less than many commonly used markers. Conclusions The results revealed that the six genes (MLPH, TMC5, SFTA3, DSG3, DSC3 and CALML3) might be suitable markers in distinguishing LUAD from LUSC, and also validated the feasibility of our methods for identification of candidate markers from high-throughput data. PMID:26380766

Differential Scanning Calorimetry and Evolved Gas Analysis of Hydromagnesite

NASA Technical Reports Server (NTRS)

Lauer, H. V., Jr.; Golden, D. C.; Ming, Douglas W.; Boynton, W. V.

1999-01-01

Volatile-bearing minerals (e.g., Fe-oxyhydroxides, phyllosilicates, carbonates and sulfates) may be important phases on the surface of Mars. In order to characterize these phases the Thermal and Evolved Gas Analyzer (TEGA) flying on the Mars'98 lander will perform analyses on surface samples from Mars. Hydromagnesite [Mg5(CO3)4(OH)2.4H2O] is considered a good standard mineral to examine as a Mars soil analog component because it evolves both H2O and CO2 at temperatures between 0 and 600 C. Our aim here is to interpret the DSC signature of hydromagnesite under ambient pressure and 20 sccm N2 flow in the range 25 to 600 C. The DSC curve for hydromagnesite under the above conditions consists of three endothermic peaks at temperatures 296, 426, and 548 and one sharp exotherm at 511 C. X-ray analysis of the sample at different stop temperatures suggested that the exotherm corresponded with the formation of crystalline magnesite. The first endotherm was due to dehydration of hydromagnesite, and then the second one was due to the decomposition of carbonate, immediately followed by the formation of magnesite (exotherm) and its decomposition to periclase (last endotherm). Evolution of water and CO2 were consistent with the observed enthalpy changes. A library of such DSC-evolved gas curves for putative Martian minerals are currently being acquired in order to facilitate the interpretation of results obtained by a robotic lander.

Kinetics of Cold-Cap Reactions for Vitrification of Nuclear Waste Glass Based on Simultaneous Differential Scanning Calorimetry - Thermogravimetry (DSC-TGA) and Evolved Gas Analysis (EGA)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rodriguez, Carmen P.; Pierce, David A.; Schweiger, Michael J.

2013-12-03

For vitrifying nuclear waste glass, the feed, a mixture of waste with glass-forming and modifying additives, is charged onto the cold cap that covers 90-100% of the melt surface. The cold cap consists of a layer of reacting molten glass floating on the surface of the melt in an all-electric, continuous glass melter. As the feed moves through the cold cap, it undergoes chemical reactions and phase transitions through which it is converted to molten glass that moves from the cold cap into the melt pool. The process involves a series of reactions that generate multiple gases and subsequent massmore » loss and foaming significantly influence the mass and heat transfers. The rate of glass melting, which is greatly influenced by mass and heat transfers, affects the vitrification process and the efficiency of the immobilization of nuclear waste. We studied the cold-cap reactions of a representative waste glass feed using both the simultaneous differential scanning calorimetry thermogravimetry (DSC-TGA) and the thermogravimetry coupled with gas chromatography-mass spectrometer (TGA-GC-MS) as complementary tools to perform evolved gas analysis (EGA). Analyses from DSC-TGA and EGA on the cold-cap reactions provide a key element for the development of an advanced cold-cap model. It also helps to formulate melter feeds for higher production rate.« less

Differential Scanning Calorimetry and Evolved Gas Analysis at Mars Ambient Conditions Using the Thermal Evolved Gas Analyser (TEGA)

NASA Technical Reports Server (NTRS)

Musselwhite, D. S.; Boynton, W. V.; Ming, D. W.; Quadlander, G. A.; Kerry, K. E.; Bode, R. C.; Bailey, S. H.; Ward, M. G.; Pathare, A. V.; Lorenz, R. D.

2000-01-01

We are conducting DSC/EGA experiments at Mars ambient temperature and pressure using the TEGA engineering model. These tests illustrate the outstanding capabilities of a TEGA-like instrument on the surface of Mars.

DSC: software tool for simulation-based design of control strategies applied to wastewater treatment plants.

PubMed

Ruano, M V; Ribes, J; Seco, A; Ferrer, J

2011-01-01

This paper presents a computer tool called DSC (Simulation based Controllers Design) that enables an easy design of control systems and strategies applied to wastewater treatment plants. Although the control systems are developed and evaluated by simulation, this tool aims to facilitate the direct implementation of the designed control system to the PC of the full-scale WWTP (wastewater treatment plants). The designed control system can be programmed in a dedicated control application and can be connected to either the simulation software or the SCADA of the plant. To this end, the developed DSC incorporates an OPC server (OLE for process control) which facilitates an open-standard communication protocol for different industrial process applications. The potential capabilities of the DSC tool are illustrated through the example of a full-scale application. An aeration control system applied to a nutrient removing WWTP was designed, tuned and evaluated with the DSC tool before its implementation in the full scale plant. The control parameters obtained by simulation were suitable for the full scale plant with only few modifications to improve the control performance. With the DSC tool, the control systems performance can be easily evaluated by simulation. Once developed and tuned by simulation, the control systems can be directly applied to the full-scale WWTP.

Thermochemical properties of cellulose acetate blends with acetosolv and sawdust lignin: A comparative study.

PubMed

Peredo, Karol; Escobar, Danilo; Vega-Lara, Johana; Berg, Alex; Pereira, Miguel

2016-02-01

Sawdust (SD) and cotton-lignin blends (CLB) were acetylated and the effect of lignin type and content on thermoplastic properties of the acetate produced was studied. The lignin in samples did not significantly affect the degree of acetylation. An increase in acetyl groups of 1-3% was observed in acetylated SD (ASD) unlike acetylated CLB (ACLB). Thermogravimetric analysis showed two thermal degradation zones; one at 190-200°C and the other at 330-370°C. The early degradation in ASD corresponds to galactoglucomannans while that in ACLB corresponds to the low-molecular-weight lignin. The second degradation is due to decomposition of cellulose acetate and high-molecular-weight lignin. DSC analysis showed homogeneous behaviour in ASD with only one glass transition temperature (Tg) at 170-180°C, unlike ACLB that showed two Tgs at 170-180°C. Sawdust acetylation, taking advantage of its residual lignin, showed higher reactivity and miscibility as compared to the same material produced by adding previously extracted lignin on cotton. Copyright © 2015 Elsevier B.V. All rights reserved.

Reinforced fluropolymer nanocomposites with high-temperature superconducting Bi2Sr2CaCu2Oy

NASA Astrophysics Data System (ADS)

Jayasree, T. K.

2014-10-01

Bismuth Strontium Calcium Copper Oxide (Bi2Sr2CaCu2Oy)/Polyvinylidene fluoride (PVDF) nanocomposite was prepared and their thermal properties were analyzed. The composite consists of the polyvinylidene fluoride (PVDF) as an insulating polymer matrix, and homogenously distributed Bismuth strontium calcium copperoxide (2212) nanoparticles. SEM data shows flaky grains of the superconductor coated and linked by polymer. Differential scanning calorimetry (DSC) results indicated that the melting point was not affected significantly by the addition of BSCCO. However, the addition of superconducting ceramic resulted in an extra melting peak at a lower temperature (145°C). Thermogravimetric analysis of the samples shows that the onset decomposition temperature of the PVDF matrix was decreased by the addition of SC filler.

Evaluation of carbon and nitrogen pools in different soil types amended with different organic inputs by thermogravimetric/calorimetric analysis

NASA Astrophysics Data System (ADS)

Yanardaǧ, Ibrahim H.; Zornoza, Raúl; Büyükkiliç-Yanardaǧ, Asuman; Acosta, Jose A.; Faz, Ángel; Mermut, Ahmet R.

2017-04-01

The objective of this study was to assess the short-term changes in soil organic C (SOC) and N pools after incubation of three different soil types (Regosol, Luvisol and Kastanozem) treated with three amendments differing in organic matter stability (raw pig slurry (PS), manure, and biochar (BC), and to establish relationships between different chemical, spectral and thermal/calorimetric data to assess if thermal/calorimetric analysis could replace conventional analyses to monitor changes in SOC and N poos. Thermogravimetry-Differential Scanning Calorimetry (TG-DSC) analysis showed that amendments had little effect on volatile SOC and inorganic matter, compared to unamended samples in all soils. All amendments significantly increased the labile SOC in Regosol. Manure and BC increased recalcitrant SOC in Regosol and Luvisol. BC significantly increased recalcitrant SOC in all soils. Refractory SOC slightly increased with amendments in the Luvisol compared to the control. These results support the findings obtained with chemical analyses. Selected evolved ions (m/z 30 and 44) detected by quadrupole mass spectrometry (QMS) confirmed findings from TG-DSC. Emissions of C and N containing gases from the Regosol significantly increased with the amendments because this soil contains low SOC content, and the application of these amendments provided additional C. An increase in the CO2 containing gas species (m/z 44) from volatile SOC was observed with PS application only in the Regosol. Carbon dioxide increments (m/z 44) from recalcitrant (380-475°C) and refractory (475-550/600°C) SOC pools were observed with all amendments in all soils especially with BC application. The evolved ions at m/z 44 were higher in the initial soil samples from Kastanozem than after incubation, suggesting a loss of organic compounds, mainly volatile and labile upon incubation. NO peaks (m/z 30) showed similar trends to the C containing gas species in all soils. We carried out linear regressions to estimate soil properties measured by conventional chemical procedures by the use of TG-DSC-QMS. We obtained accurate models to estimate SOC, soil carbonates, recalcitrant C, soluble C and soluble N. These results encourage the use of thermal analyses to study SOM dynamics in soils, since it provides feasible and accurate information about different organic and inorganic C and N fractions. Thermal methods are quite inexpensive, require little sample preparation, are rapid and give reproducible results. However, no relationship between thermal analyses and C and N mineralization and N volatilization was found, suggesting that this technique may be valid to assess the current value of different organic fractions in a soil in a concrete time, but not indicated to predict mineralization or volatilization trends after application of amendments.

Quantitative crystallinity determination for E1010, a novel carbapenem antibiotic, using differential scanning calorimetry.

PubMed

Kushida, Ikuo

2012-03-01

The objective of this study was to develop a quantitative crystallinity analysis method for the bulk drug of E1010 ((+)-(4R,5S,6S)-6-[(R)-1-hydroxyethyl]-3-[(2S,4S)-2-[(R)-1-hydroxy-1-[(R)-pyrrolidin-3 -yl]methyl]pyrrolidin-4-yl]thio-4-methyl-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid monohydrochloride), a novel carbapenem antibiotic. X-ray analyses, thermal analyses and hygroscopicity measurements were used to elucidate the crystal structure and the solid state properties. To develop a quantitative method for the crystallinity of E1010 bulk drug, the relationship between enthalpy change obtained by differential scanning calorimetry (DSC) and crystalline form ratio was investigated. E1010 bulk drug was found to exist in a crystalline trihydrate formed in two layers, i.e. a layer of E1010 free form, and a layer consisting of chloride ions and water molecules. The thermal analysis showed an endothermic peak derived from dehydration with the loss of crystal lattices at around 100°C as an onset. The enthalpy change value for the endothermic peak correlated well with crystalline content in binary physical mixtures of the crystalline trihydrate and the amorphous form. In addition, for nine lots of the bulk drug, a positive correlation between the enthalpy change and chemical stability in the solid state was observed. This quantitative analysis of crystallinity using DSC could be applicable for the quality control of the bulk drug to detect variability among manufacturing batches and to estimate the chemical stability of partially amorphous samples. © 2011 The Author. JPP © 2011 Royal Pharmaceutical Society.

The use of novel biodegradable, optically active and nanostructured poly(amide-ester-imide) as a polymer matrix for preparation of modified ZnO based bionanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abdolmaleki, Amir, E-mail: abdolmaleki@cc.iut.ac.ir; Nanotechnology and Advanced Materials Institute, Isfahan University of Technology, Isfahan 84156-83111, Islamic Republic of Iran; Mallakpour, Shadpour, E-mail: mallak@cc.iut.ac.ir

Highlights: Black-Right-Pointing-Pointer A novel biodegradable and nanostructured PAEI based on two amino acids, was synthesized. Black-Right-Pointing-Pointer ZnO nanoparticles were modified via two different silane coupling agents. Black-Right-Pointing-Pointer PAEI/modified ZnO BNCs were synthesized through ultrasound irradiation. Black-Right-Pointing-Pointer ZnO particles were dispersed homogeneously in PAEI matrix on nanoscale. Black-Right-Pointing-Pointer The effect of ZnO nanoparticles on the properties of synthesized polymer was examined. -- Abstract: A novel biodegradable and nanostructured poly(amide-ester-imide) (PAEI) based on two different amino acids, was synthesized via direct polycondensation of biodegradable N,N Prime -bis[2-(methyl-3-(4-hydroxyphenyl)propanoate)]isophthaldiamide and N,N Prime -(pyromellitoyl)-bis-L-phenylalanine diacid. The resulting polymer was characterized by FT-IR, {sup 1}H NMR,more » specific rotation, elemental analysis, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and field emission scanning electron microscopy (FE-SEM) analysis. The synthesized polymer showed good thermal stability with nano and sphere structure. Then PAEI/ZnO bionanocomposites (BNCs) were fabricated via interaction of pure PAEI and ZnO nanoparticles. The surface of ZnO was modified with two different silane coupling agents. PAEI/ZnO BNCs were studied and characterized by FT-IR, XRD, UV/vis, FE-SEM and TEM. The TEM and FE-SEM results indicated that the nanoparticles were dispersed homogeneously in PAEI matrix on nanoscale. Furthermore the effect of ZnO nanoparticle on the thermal stability of the polymer was investigated with TGA and DSC technique.« less

Characterization of two polymorphs of salmeterol xinafoate crystallized from supercritical fluids.

PubMed

Tong, H H; Shekunov, B Y; York, P; Chow, A H

2001-06-01

To characterize two polymorphs of salmeterol xinafoate (SX-I and SX-II) produced by supercritical fluid crystallization. SX-I and SX-II were crystallized as fine powders using Solution Enhanced Dispersion by Supercritical Fluids (SEDS). The two polymorphs and a reference micronized SX sample (MSX) were characterized using powder X-ray diffractometry (PXRD), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), aqueous solubility (and dissolution) determination at 5-40 degrees C, BET adsorption analysis, and inverse gas chromatography (IGC). Compared with SX-I, SX-II exhibited a lower enthalpy of fusion, a higher equilibrium solubility, a higher intrinsic dissolution rate, a lower enthalpy of solution (based on van't Hoff solubility plots), and a different FTIR spectrum (reflecting differences in intermolecular hydrogen bonding). Solubility ratio plot yielded a transition temperature (-99 degrees C) below the melting points of both polymorphs. MSX showed essentially the same crystal form as SX-I (confirmed by PXRD and FTIR), but a distinctly different thermal behaviour. Mild trituration of SX-I afforded a similar DSC profile to MSX while prolonged grinding of SX-I gave rise to an endotherm at -109 degrees C, corresponding to solid-solid transition of SX-I to SX-II. Surface analysis of MSX, SX-I, and SX-II by IGC revealed significant differences in surface free energy in terms of both dispersive (nonpolar) interactions and specific (polar) acid-base properties. The SEDS-processed SX-I and SX-II display high polymorphic purity and distinctly different physical and surface properties. The polymorphs are related enantiotropically with SX-I being the thermodynamically stable form at room temperature.

Thermal: Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), and Polarized Microscopy Instrumentation for the Analysis of Field-Controlled Anisotropic Nanomaterials

DTIC Science & Technology

2014-11-14

figure 1.2.1, right). The discovery TGA furnace design employs a silicon carbide ( SiC ) inner chamber. Four halogen lamps surrounded by a water...amplification,(13, 17) self-phase modulation (18, 19), and new nonlinear phenomena such as the nonlinear optical mirror ,(20) and the mirrorless optical

Bibliography on Cold Regions Science and Technology. Volume 51, Part 1.

DTIC Science & Technology

1997-12-01

Loess, Plant ecology, Vegetation patterns, Revegeta- tion, Forestry, Soil conservation, Land reclamation, Regional planning, Statistical analysis...printing. Antikainen, M., Griffith, M., Zhang, J., Hon, W.C., Yang, D.S.C., Pihakaski-Maunsbach, K., Plant physi- ology. Mar. 1996, 110(1), p.845-857...65 refs. Plant physiology, Grasses, Plant tissues, Antifreezes, Acclimatization, Chemical analysis, Chemical prop- erties, Temperature effects

Burn Rate Modification with Carborane Polymers

DTIC Science & Technology

2017-11-01

test, ARDEC electrostatic discharge test, and DSC analysis of the small-scale runs were performed to ensure the products were safe to handle. Once...Accessions Division 8725 John J. Kingman Road, Ste 0944 Fort Belvoir, VA 22060-6218 GIDEP Operations Center P.O. Box 8000 Corona , CA

Effect of radiation induced crosslinking and degradation of ETFE films

NASA Astrophysics Data System (ADS)

Zen, H. A.; Ribeiro, G.; Geraldes, A. N.; Souza, C. P.; Parra, D. F.; Lugão, A. B.

2013-03-01

In this study the ETFE film with 125 μm of thickness was placed inside a nylon bag and filled with either acetylene, nitrogen or oxygen. Following the procedure, the samples were irradiated at 5, 10 and 20 kGy. The physical and chemical properties of the modified and pristine films were evaluated by rheological and thermal analyses (TG and DSC), X-ray diffraction (XRD) and infrared spectroscopy (IR-ATR). In rheological analysis the storage modulus (G') indicates opposite profiles when the atmospheres (acetylene and oxygen) are evaluated according to the absorbed dose. For the samples submitted to radiation under oxygen atmosphere it is possible to observe the degradation process with the low levels of the storage modulus. The changes in the degree of crystallinity were verified in all modified samples when compared to the pristine polymer and this behavior was confirmed by DSC analysis. A decrease in the intensity of crystalline peak by X-ray diffraction was observed.

The road to JCAHO disease-specific care certification: a step-by-step process log.

PubMed

Morrison, Kathy

2005-01-01

In 2002, the Joint Commission on Accreditation of Healthcare Organizations (JCAHO) implemented Disease-Specific Care (DSC) certification. This is a voluntary program in which organizations have their disease management program evaluated by this regulatory agency. Some of the DSC categories are stroke, heart failure, acute MI, diabetes, and pneumonia. The criteria for any disease management program certification are: compliance with consensus-based national standards, effective use of established clinical practice guidelines to manage and optimize care, and an organized approach to performance measurement and improvement activities. Successful accomplishment of DSC certification defines organizations as Centers of Excellence in management of that particular disease. This article will review general guidelines for DSC certification with an emphasis on Primary Stroke Center certification.

X-ray structural studies and physicochemical characterization of (E)-6-(3,4-dimethoxyphenyl)-1-ethyl-4-mesitylimino-3-methyl- 3,4-dihydro-2(1H)-pyrimidinone polymorphs.

PubMed

Miyamae, A; Kitamura, S; Tada, T; Koda, S; Yasuda, T

1991-10-01

The polymorphism of (E)-6-(3,4-dimethoxyphenyl)-1-ethyl-4-mesitylimino-3-methyl-3,4-di hydro- 2(1 H)-pyrimidinone (FK664; 1) was characterized by using X-ray powder diffractometry, differential scanning calorimetry (DSC), and IR spectroscopy. Structures of two polymorphs (Forms A and B) were determined by X-ray crystallographic analysis. Form A crystallized in the monoclinic space group P2(1)/c, with a = 13.504(2), b = 6.733(1), c = 24.910(8) A, beta = 96.55(4) degrees, z = 4, and dcal = 1.203 g/cm3, while Form B crystallized in the same space group, with a = 8.067(2), b = 15.128(4), c = 18.657(4) A, beta = 102.34(3) degrees, z = 4, and dcal = 1.216 g/cm3. The conformational features of 1 were very similar between the two polymorphs. Compound 1, in both crystal forms, took an energetically reasonable conformation in three rigid planes, such as 2-pyrimidone, trimethylphenyl, and dimethoxyphenyl rings, but the molecules were packed in different ways between the two polymorphs. In the Form B crystal, a short contact was possible, to form pi-pi interactions between two dimethoxyphenyl groups related with the inversion center in the crystal lattice; this interaction seems to contribute to stabilizing the crystal structure of Form B. Both Forms A and B showed only one endothermic peak due to fusion at 115 and 140 degrees C, respectively, on the DSC thermograms; therefore, it is suggested that there are no transition points between the two polymorphs. The heats of fusion obtained from the DSC thermograms were 33.2(2) kJ/mol for Form A and 36.8(1) kJ/mol for Form B.(ABSTRACT TRUNCATED AT 250 WORDS)

Designing single- and multiple-shell sampling schemes for diffusion MRI using spherical code.

PubMed

Cheng, Jian; Shen, Dinggang; Yap, Pew-Thian

2014-01-01

In diffusion MRI (dMRI), determining an appropriate sampling scheme is crucial for acquiring the maximal amount of information for data reconstruction and analysis using the minimal amount of time. For single-shell acquisition, uniform sampling without directional preference is usually favored. To achieve this, a commonly used approach is the Electrostatic Energy Minimization (EEM) method introduced in dMRI by Jones et al. However, the electrostatic energy formulation in EEM is not directly related to the goal of optimal sampling-scheme design, i.e., achieving large angular separation between sampling points. A mathematically more natural approach is to consider the Spherical Code (SC) formulation, which aims to achieve uniform sampling by maximizing the minimal angular difference between sampling points on the unit sphere. Although SC is well studied in the mathematical literature, its current formulation is limited to a single shell and is not applicable to multiple shells. Moreover, SC, or more precisely continuous SC (CSC), currently can only be applied on the continuous unit sphere and hence cannot be used in situations where one or several subsets of sampling points need to be determined from an existing sampling scheme. In this case, discrete SC (DSC) is required. In this paper, we propose novel DSC and CSC methods for designing uniform single-/multi-shell sampling schemes. The DSC and CSC formulations are solved respectively by Mixed Integer Linear Programming (MILP) and a gradient descent approach. A fast greedy incremental solution is also provided for both DSC and CSC. To our knowledge, this is the first work to use SC formulation for designing sampling schemes in dMRI. Experimental results indicate that our methods obtain larger angular separation and better rotational invariance than the generalized EEM (gEEM) method currently used in the Human Connectome Project (HCP).

Chemokine CCL28 induces apoptosis of decidual stromal cells via binding CCR3/CCR10 in human spontaneous abortion.

PubMed

Sun, Chan; Zhang, Yuan-Yuan; Tang, Chuan-Ling; Wang, Song-Cun; Piao, Hai-Lan; Tao, Yu; Zhu, Rui; Du, Mei-Rong; Li, Da-Jin

2013-10-01

Spontaneous abortion is the most common complication of pregnancy. Immune activation and the subsequent inflammation-induced tissue injury are often observed at the maternal-fetal interface as the final pathological assault in recurrent spontaneous abortion. However, the precise mechanisms responsible for spontaneous abortion involving inflammation are not fully understood. Chemokine CCL28 and its receptors CCR3 and CCR10 are important regulators in inflammatory process. Here, we examined the expression of CCL28 and its receptors in decidual stromal cells (DSCs) by immunochemistry and flow cytometry (FCM), and compared their expression level in DSCs from normal pregnancy versus spontaneous abortion, and their relationship to inflammatory cytokines production by DSCs. We further analyzed regulation of the pro-inflammatory cytokines on CCL28 expression in DSCs by real-time polymerase chain reaction, In-cell Western and FCM. The effects of CCL28-CCR3/CCR10 interaction on DSC apoptosis was investigated by Annexin V staining and FCM analysis or DAPI staining and nuclear morphology. Higher levels of the inflammatory cytokines interleukin (IL)-1β, IL-17A and tumor necrosis factor-α, and increased CCR3/CCR10 expression were observed in DSCs from spontaneous abortion compared with normal pregnancy. Treatment with inflammatory cytokines differently affected CCL28 and CCR3/CCR10 expression in DSCs. Human recombinant CCL28 promoted DSC apoptosis, which was eliminated by pretreatment with neutralizing antibodies against CCR3/CCR10 and CCL28. However, CCL28 did not affect DSC growth. These results suggest that the inflammation-promoted up-regulation of CCL28 and its receptors interaction in DSCs is involved in human spontaneous abortion via inducing DSC apoptosis.

Statistical Validation of Image Segmentation Quality Based on a Spatial Overlap Index1

PubMed Central

Zou, Kelly H.; Warfield, Simon K.; Bharatha, Aditya; Tempany, Clare M.C.; Kaus, Michael R.; Haker, Steven J.; Wells, William M.; Jolesz, Ferenc A.; Kikinis, Ron

2005-01-01

Rationale and Objectives To examine a statistical validation method based on the spatial overlap between two sets of segmentations of the same anatomy. Materials and Methods The Dice similarity coefficient (DSC) was used as a statistical validation metric to evaluate the performance of both the reproducibility of manual segmentations and the spatial overlap accuracy of automated probabilistic fractional segmentation of MR images, illustrated on two clinical examples. Example 1: 10 consecutive cases of prostate brachytherapy patients underwent both preoperative 1.5T and intraoperative 0.5T MR imaging. For each case, 5 repeated manual segmentations of the prostate peripheral zone were performed separately on preoperative and on intraoperative images. Example 2: A semi-automated probabilistic fractional segmentation algorithm was applied to MR imaging of 9 cases with 3 types of brain tumors. DSC values were computed and logit-transformed values were compared in the mean with the analysis of variance (ANOVA). Results Example 1: The mean DSCs of 0.883 (range, 0.876–0.893) with 1.5T preoperative MRI and 0.838 (range, 0.819–0.852) with 0.5T intraoperative MRI (P < .001) were within and at the margin of the range of good reproducibility, respectively. Example 2: Wide ranges of DSC were observed in brain tumor segmentations: Meningiomas (0.519–0.893), astrocytomas (0.487–0.972), and other mixed gliomas (0.490–0.899). Conclusion The DSC value is a simple and useful summary measure of spatial overlap, which can be applied to studies of reproducibility and accuracy in image segmentation. We observed generally satisfactory but variable validation results in two clinical applications. This metric may be adapted for similar validation tasks. PMID:14974593

Pretreatment Dynamic Susceptibility Contrast MRI Perfusion in Glioblastoma: Prediction of EGFR Gene Amplification.

PubMed

Gupta, A; Young, R J; Shah, A D; Schweitzer, A D; Graber, J J; Shi, W; Zhang, Z; Huse, J; Omuro, A M P

2015-06-01

Molecular and genetic testing is becoming increasingly relevant in GBM. We sought to determine whether dynamic susceptibility contrast (DSC) magnetic resonance imaging (MRI) perfusion imaging could predict EGFR-defined subtypes of GBM. We retrospectively identified 106 consecutive glioblastoma (GBM) patients with known EGFR gene amplification, and a subset of 65 patients who also had known EGFRvIII gene mutation status. All patients underwent T2* DSC MRI perfusion. DSC perfusion maps and T2* signal intensity time curves were evaluated, and the following measures of tumor perfusion were recorded: (1) maximum relative cerebral blood volume (rCBV), (2) relative peak height (rPH), and (3) percent signal recovery (PSR). The imaging metrics were correlated to EGFR gene amplification and EGFRvIII mutation status using univariate analyses. EGFR amplification was present in 44 (41.5 %) subjects and absent in 62 (58.5 %). Among the 65 subjects who had undergone EGFRvIII mutation transcript analysis, 18 subjects (27.7 %) tested positive for the EGFRvIII mutation, whereas 47 (72.3 %) did not. Higher median rCBV (3.31 versus 2.62, p = 0.01) and lower PSR (0.70 versus 0.78, p = 0.03) were associated with high levels of EGFR amplification. Higher median rPH (3.68 versus 2.76, p = 0.03) was associated with EGFRvIII mutation. DSC MRI perfusion may have a role in identifying patients with EGFR gene amplification and EGFRvIII gene mutation status, potential targets for individualized treatment protocols. Our results raise the need for further investigation for imaging biomarkers of genetically unique GBM subtypes.

Structure, wettability and thermal degradation of new fluoro-oligomer modified nanoclays.

PubMed

Valsecchi, R; Viganò, M; Levi, M; Turri, S

2008-04-01

Quaternary ammonium salts based on monofunctionalized Perfluoropolyether (PFPE) oligomers were synthesized and used for the cation exchange process of sodium Montmorillonite nanoclays. The new fluoromodified nanoclays were characterized through X-rays diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), termogravimetric analysis (TGA), differential scanning calorimetry (DSC), electronic microscopy (SEM-EDS), and contact angle measurements (CA). In particular XRD showed rather complex patterns (presence of higher order reflections) which allowed the calculation of basal spacings, regularly increasing with the molecular weight of the fluorinated macrocation. Both IR and SEM confirmed the presence of fluorinated segments at clays interface, while TGA showed a limited thermal stability with an onset of degradation temperature which seems not dependent on the molecular weight of the macrocation. CA measurements showed a peculiar behaviour, with evident dynamic hysteresis phenomena and surface tension components quite different from those of commercially available, organomodified clays.

Hydrogen-bonding A(LS)2-type low-molecular-mass gelator and its thermotropic mesomorphic behavior.

PubMed

Hou, Qiufei; Wang, Shichao; Zang, Libin; Wang, Xiaoliang; Jiang, Shimei

2009-10-15

A unique cholesterol-based A(LS)2-type gelator, which is a hydrogen-bonding complex based on an ALS-type non-gelator molecule 3-cholesteryl 4-(trans-2-(4-pyridinyl)vinyl)phenyl succinate and a counterpart 3-cholesteryloxycarbonylpropanoic acid, shows strong gelation ability in alcohol and aromatic solvents. The formed gel has a high Tg at low gelation concentration, and its xerogel shows fibrillar microstructure revealed by scanning electron microscopy (SEM). FTIR confirms the existence of intermolecular hydrogen bond in the gelator, and X-ray diffraction (XRD) analysis reveals that the gelator possesses a folded conformation in gel and self-assembles into the fibrillar structure mainly by van der Waals interaction between cholesteryl moieties of the gelator. Further more, the thermotropic behavior of the xerogel is studied by differential scanning calorimetry (DSC) and polarized optical microscopy (POM), which shows typical optical textures of liquid crystals.

Magnetic resonance imaging in dissociated strabismus complex demonstrates generalized hypertrophy of rectus extraocular muscles.

PubMed

Rajab, Ghada Z; Suh, Soh Youn; Demer, Joseph L

2017-06-01

Dissociated strabismus complex (DSC) is an enigmatic form of strabismus that includes dissociated vertical deviation (DVD) and dissociated horizontal deviation (DHD). We employed magnetic resonance imaging (MRI) to evaluate the extraocular muscles in DSC. We studied 5 patients with DSC and mean age of 25 years (range, 12-42 years), and 15 age-matched, orthotropic control subjects. All patients had DVD; 4 also had DHD. We employed high-resolution, surface coil MRI with thin, 2 mm slices and central target fixation. Volumes of the rectus and superior oblique muscles in the region 12 mm posterior to 4 mm anterior to the globe-optic nerve junction were measured in quasi-coronal planes in central gaze. Patients with DSC had no structural abnormalities of rectus muscles or rectus pulleys or the superior oblique muscle but exhibited modest, statistically significant increased volume of all rectus muscles ranging from 20% for medial rectus to 9% for lateral rectus (P < 0.05). DSC includes various combinations of sursumduction, excycloduction, and abduction not conforming to Hering's law. We have found modest generalized enlargement of all rectus muscles. DSC is associated with generalized rectus extraocular muscle hypertrophy in the absence of other orbital abnormalities. Copyright © 2017 American Association for Pediatric Ophthalmology and Strabismus. Published by Elsevier Inc. All rights reserved.

A Unified Constitutive Model for Subglacial Till, Part II: Laboratory Tests, Disturbed State Modeling, and Validation for Two Subglacial Tills

NASA Astrophysics Data System (ADS)

Desai, C. S.; Sane, S. M.; Jenson, J. W.; Contractor, D. N.; Carlson, A. E.; Clark, P. U.

2006-12-01

This presentation, which is complementary to Part I (Jenson et al.), describes the application of the Disturbed State Concept (DSC) constitutive model to define the behavior of the deforming sediment (till) underlying glaciers and ice sheets. The DSC includes elastic, plastic, and creep strains, and microstructural changes leading to degradation, failure, and sometimes strengthening or healing. Here, we describe comprehensive laboratory experiments conducted on samples of two regionally significant tills deposited by the Laurentide Ice Sheet: the Tiskilwa Till and Sky Pilot Till. The tests are used to determine the parameters to calibrate the DSC model, which is validated with respect to the laboratory tests by comparing the predictions with test data used to find the parameters, and also comparing them with independent tests not used to find the parameters. Discussion of the results also includes comparison of the DSC model with the classical Mohr-Coulomb model, which has been commonly used for glacial tills. A numerical procedure based on finite element implementation of the DSC is used to simulate an idealized field problem, and its predictions are discussed. Based on these analyses, the unified DSC model is proposed to provide an improved model for subglacial tills compared to other models used commonly, and thus to provide the potential for improved predictions of ice sheet movements.

A study of mercuric iodide near melting using differential scanning calorimetry, Raman spectroscopy and X-ray diffraction

NASA Astrophysics Data System (ADS)

Burger, A.; Morgan, S.; Jiang, H.; Silberman, E.; Schieber, M.; Van Den Berg, L.; Keller, L.; Wagner, C. N. J.

1989-11-01

High-temperature studies of mercuric iodide (HgI2) involving differential scanning calorimetry (DSC), Raman spectroscopy and X-ray powder diffraction have failed to confirm the existence of a red-colored tetragonal high-temperature phase called α'-HgI2 reported by S.N. Toubektsis et al. [J. Appl. Phys. 58 (1988) 2070] using DSC measurements. The multiple DSC peaks near melting reported by Toubektsis are found by the present authors only if the sample is heated in a stainless-steel container. Using a Pyrex container or inserting a platinum foil between the HgI2 and the stainless-steel container yields only one sharp, single DSC peak at the melting point. The nonexistence of the α' phase is confirmed by high-temperature X-ray diffraction and Raman spectroscopy performed in the vicinity of the melting point. These methods clearly, indicate the existence of only the yellow orthorhombic β-HgI2 phase. The experimental high-temperature DSC, Raman and X-ray diffraction data are presented and discussed.

Dye-sensitized solar cells employing a SnO2-TiO2 core-shell structure made by atomic layer deposition.

PubMed

Karlsson, Martin; Jõgi, Indrek; Eriksson, Susanna K; Rensmo, Håkan; Boman, Mats; Boschloo, Gerrit; Hagfeldt, Anders

2013-01-01

This paper describes the synthesis and characterization of core-shell structures, based on SnO2 and TiO2, for use in dye-sensitized solar cells (DSC). Atomic layer deposition is employed to control and vary the thickness of the TiO2 shell. Increasing the TiO2 shell thickness to 2 nm improved the device performance of liquid electrolyte-based DSC from 0.7% to 3.5%. The increase in efficiency originates from a higher open-circuit potential and a higher short-circuit current, as well as from an improvement in the electron lifetime. SnO2-TiO2 core-shell DSC devices retain their photovoltage in darkness for longer than 500 seconds, demonstrating that the electrons are contained in the core material. Finally core-shell structures were used for solid-state DSC applications using the hole transporting material 2,2',7,7',-tetrakis(N, N-di-p-methoxyphenyl-amine)-9,9',-spirofluorene. Similar improvements in device performance were obtained for solid-state DSC devices.

Development of stability-enhanced ternary solid dispersions via combinations of HPMCP and Soluplus® processed by hot melt extrusion.

PubMed

Albadarin, Ahmad B; Potter, Catherine B; Davis, Mark T; Iqbal, Javed; Korde, Sachin; Pagire, Sudhir; Paradkar, Anant; Walker, Gavin

2017-10-30

The aim of this study was to evaluate a novel combination of hydroxypropyl methylcellulose phthalate (HPMCP-HP-50) and Soluplus ® polymers for enhanced physicochemical stability and solubility of the produced amorphous solid dispersions (ASDs). This was achieved using hot melt extrusion (HME) to convert the crystalline active pharmaceutical ingredient (API) into a more soluble amorphous form within the ternary systems. Itraconazole (ITZ), a Biopharmaceutics Classification System class II (BCS II) API, was selected as the model drug. The ASDs were characterized by Powder X-Ray diffraction (PXRD), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Fourier Transform Infrared (FTIR) spectroscopy, Solid State Nuclear Magnetic Resonance (ssNMR) and dissolution studies. The data showed that the ASDs were physically and chemically stable at 20°C and 50% RH over 12 months. PXRD results indicated that the ITZ in the ASDs was in the amorphous state and no recrystallization occurred. DSC scans confirmed that each formulation exhibited a single intermediate glass transition (T g ), around 96.4°C, indicating that ITZ was completely miscible in the polymeric blends of HPMCP and Soluplus ® at up to 30% (w/w) drug loading and that the two polymers were miscible with each other in the presence of ITZ. The FTIR analysis indicated the formation of strong hydrogen bonding between ITZ, HPMCP and Soluplus ® . The dissolution end-point of the ASDs was determined to be approximately 10 times greater than that of the crystalline ITZ. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison of bare and amino modified mesoporous silica@poly(ethyleneimine)s xerogel as indomethacin carrier: Superiority of amino modification.

PubMed

Li, Jing; Xu, Lu; Wang, Hongyu; Yang, Baixue; Liu, Hongzhuo; Pan, Weisan; Li, Sanming

2016-02-01

The purpose of this study was to facilely develop amino modified mesoporous silica xerogel synthesized using biomimetic method (B-AMSX) and to investigate its potential ability to be a drug carrier for loading poorly water-soluble drug indomethacin (IMC). For comparison, mesoporous silica xerogel without amino modification (B-MSX) was also synthesized using the same method. The changes of characteristics before and after IMC loading were systemically studied using fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), small angle X-ray scattering (SAXS) and nitrogen adsorption/desorption analysis. The results showed that B-MSX and B-AMSX were spherical nanoparticles with mesoporous structure. Compared with B-MSX, IMC loading capacity of B-AMSX was higher because more drug molecules can be loaded through stronger hydrogen bonding force. DSC and SAXS analysis confirmed the amorphous state of IMC after being loaded into B-MSX and B-AMSX. The in vitro drug release study revealed that B-MSX and B-AMSX improved IMC release significantly, and B-AMSX released IMC a little faster than B-MSX because of larger pore diameter of IMC-AMSX. B-MSX and B-AMSX degraded gradually in dissolution medium evidenced by color reaction and absorbance value, and B-AMSX degraded slower than B-MSX due to amino modification. In conclusion, B-AMSX with superiority of higher loading capacity and enhanced dissolution release can be considered to be a good candidate as drug carrier for IMC. Copyright © 2015 Elsevier B.V. All rights reserved.

Thermal characterization of Titan's tholins by simultaneous TG-MS, DTA, DSC analysis

NASA Astrophysics Data System (ADS)

Nna-Mvondo, Delphine; de la Fuente, José L.; Ruiz-Bermejo, Marta; Khare, Bishun; McKay, Christopher P.

2013-09-01

Three samples of Titan's tholins synthesized in laboratory under simulated Titan's conditions and presenting different degrees of exposure to ambient atmosphere have been used to study in detail their thermal behavior using thermogravimetry coupled with a mass spectrometer (TG-MS), differential thermal analysis (DTA) and differential scanning calorimetry (DSC). The degradation of Titan's tholins under inert atmosphere follows a three-step consecutive decomposition: a drying stage (>150 °C) where moisture is desorbed, this stage indicated the high hydrophilicity of the tholins; a second stage, the main pyrolysis stage (150-575 °C) where endothermic decomposition begins releasing mainly ammonia, HCN, acetonitrile, and methane over a broad temperature range. Few other hydrocarbon fragments such as ethylene and propane are released but no cyclic molecules, aliphatic or aromatic, are observed. The last stage (>575 °C) is the carbonization of the material leading to a non-crystalline graphitic residue. The thermal degradation under oxygen atmosphere shows the same stages as in argon, with a shift of the thermogravimetric peaks toward lower temperatures indicating a lower thermal stability. The last stage in this case is an oxidative combustion of the char residue. This research concludes that even if Titan tholins, subjected to air contamination for few minutes to several years (varying with the storage conditions) transform to produce different C/N and C/O ratios and thermal stabilities, they undergo the same thermal degradation phases and products. This suggests that the studied three tholins have a similar main chemical structure which does not alter by the air exposure. We discuss on the possible nature of this structure.

Diagnostic Values of DCE-MRI and DSC-MRI for Differentiation Between High-grade and Low-grade Gliomas: A Comprehensive Meta-analysis.

PubMed

Liang, Jianye; Liu, Dexiang; Gao, Peng; Zhang, Dong; Chen, Hanwei; Shi, Changzheng; Luo, Liangping

2018-03-01

This study aimed to collect the studies on the role of dynamic contrast-enhanced magnetic resonance imaging (DCE-MRI) and dynamic susceptibility contrast MRI (DSC-MRI) in differentiating the grades of gliomas, and evaluate the diagnostic performances of relevant quantitative parameters in glioma grading. We systematically searched studies on the diagnosis of gliomas with DCE-MRI or DSC-MRI in Medline, PubMed, China National Knowledge Infrastructure database, Cochrane Library, and Embase published between January 2005 and December 2016. Standardized mean differences and 95% confidence intervals were calculated for volume transfer coefficient (K trans ), volume fraction of extravascular extracellular space (V e ), rate constant of backflux (K ep ), relative cerebral blood volume (rCBV), and relative cerebral blood flow (rCBF) using Review Manager 5.2 software. Sensitivity, specificity, area under the curve (AUC), and Begg test were calculated by Stata 12.0. Twenty-two studies with available outcome data were included in the analysis. The standardized mean difference of K trans values between high-grade glioma and low-grade glioma were 1.18 (0.91, 1.45); V e values were 1.43 (1.06, 1.80); K ep values were 0.65 (-0.05, 1.36); rCBV values were 1.44 (1.08, 1.81); and rCBF values were 1.17 (0.68, 1.67), respectively. The results were all significant statistically (P < .05) except K ep values (P = .07), and high-grade glioma had higher K trans , V e , rCBV, and rCBF values than low-grade glioma. AUC values of K trans , V e , rCBV, and rCBF were 0.90, 0.88, 0.93, and 0.73, respectively; rCBV had the largest AUC among the four parameters (P < .05). Both DCE-MRI and DSC-MRI are reliable techniques in differentiating the grades of gliomas, and rCBV was found to be the most sensitive one. Copyright © 2018 The Association of University Radiologists. Published by Elsevier Inc. All rights reserved.

Crystal growth, structural, optical, mechanical and thermal properties of a new nonlinear optical single crystal: L-Ornithine monohydrochloride.

PubMed

Balakrishnan, T; Ramamurthi, K

2009-03-01

Amino acid family crystals exhibit excellent nonlinear optical and electro optical properties. l-Ornithine monohydrochloride single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystals were characterized by single crystal and powder X-ray diffraction analysis, Fourier transform infrared (FTIR) spectroscopy, TGA, DTA and DSC analyses. UV-vis-NIR spectrum shows excellent transmission in the UV, visible and NIR region (300-1600nm). The mechanical properties of grown crystals were studied using Vickers microhardness tester. Its second harmonic generation efficiency was tested using Nd:YAG laser and is 1.25 times that of KDP.

Thermal behaviour and corrosion resistance of nano-ZnO/polyurethane film

NASA Astrophysics Data System (ADS)

Virgawati, E.; Soegijono, B.

2018-03-01

Hybrid materials Nano-ZnO/polyurethane film was prepared with different zinc oxide (ZnO) content in polyurethane as a matrix. The film was deposited on low carbon steel plate using high volume low pressure (HVLP) method. To observe thermal behaviour of the film, the sample was investigated using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Fourier transform infrared spectroscopy (FTIR) was used to see whether any chemical reaction of ZnO in polyurethane occured. TGA and FTIR results showed that the decomposition temperature shifted to a higher point and the chemical reaction of zinc oxide in polyurethane occurred. The surface morphology changed and the corrosion resistance increased with an increase of ZnO content

Determination of Thermal Properties and Morphology of Eucalyptus Wood Residue Filled High Density Polyethylene Composites

PubMed Central

Mengeloglu, Fatih; Kabakci, Ayse

2008-01-01

Thermal behaviors of eucalyptus wood residue (EWR) filled recycled high density polyethylene (HDPE) composites have been measured applying the thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Morphology of the materials was also studied using scanning electron microscope (SEM). Addition of the EWR into the recycled HDPE matrix reduced the starting of degradation temperature. EWR filled recycled HDPE had two main decomposition peaks, one for EWR around 350 °C and one for recycled HDPE around 460 °C. Addition of EWR did not affect the melting temperature of the recycled HDPE. Morphological study showed that addition of coupling agent improved the compatibility between wood residue and recycled HDPE. PMID:19325736

Optical, electrical, thermal properties of cadmium chloride doped PVA – PVP blend

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baraker, Basavarajeshwari M.; Hammannavar, Preeti B.; Lobo, Blaise, E-mail: blaise.lobo@gmail.com

2015-06-24

Films of polyvinylalcohol (PVA) – polyvinylpyrrolidone (PVP) blend doped with Cadmium Chloride (CdCl{sub 2}) in the doping range 1 wt% to 40 wt% were prepared by solution casting technique. These films were characterized using optical/UV-Vis- NIR spectroscopy, Differential Scanning Calorimetry (DSC) and DC electrical measurements. The UV-Visible spectra were quantitatively analyzed to yield the optical parameters. The UV-Visible Spectra show intermediate absorption bands (before the final absorption edge) due to formation of energy bands in the forbidden gap of PVA-PVP. There is a prominent absorption band at 2.9 eV, from 0.5 wt% up to 1.8 wt% doping level (DL) causedmore » by the dopant (CdCl{sub 2}). The DC electrical studies showed an increase in activation energy from 2.8 eV at 0.5 wt% DL up to 3.5 eV at 4.4 wt% DL, reaching a low of 2.4 eV at 11.2 wt% DL. DSC scans show evidence of formation of chain fragments, at doping levels beyond 8 wt%.« less

Detecting phase separation of freeze-dried binary amorphous systems using pair-wise distribution function and multivariate data analysis.

PubMed

Chieng, Norman; Trnka, Hjalte; Boetker, Johan; Pikal, Michael; Rantanen, Jukka; Grohganz, Holger

2013-09-15

The purpose of this study is to investigate the use of multivariate data analysis for powder X-ray diffraction-pair-wise distribution function (PXRD-PDF) data to detect phase separation in freeze-dried binary amorphous systems. Polymer-polymer and polymer-sugar binary systems at various ratios were freeze-dried. All samples were analyzed by PXRD, transformed to PDF and analyzed by principal component analysis (PCA). These results were validated by differential scanning calorimetry (DSC) through characterization of glass transition of the maximally freeze-concentrate solute (Tg'). Analysis of PXRD-PDF data using PCA provides a more clear 'miscible' or 'phase separated' interpretation through the distribution pattern of samples on a score plot presentation compared to residual plot method. In a phase separated system, samples were found to be evenly distributed around the theoretical PDF profile. For systems that were miscible, a clear deviation of samples away from the theoretical PDF profile was observed. Moreover, PCA analysis allows simultaneous analysis of replicate samples. Comparatively, the phase behavior analysis from PXRD-PDF-PCA method was in agreement with the DSC results. Overall, the combined PXRD-PDF-PCA approach improves the clarity of the PXRD-PDF results and can be used as an alternative explorative data analytical tool in detecting phase separation in freeze-dried binary amorphous systems. Copyright © 2013 Elsevier B.V. All rights reserved.

Cu3V2O8 hollow spheres in photocatalysis and primary lithium batteries

NASA Astrophysics Data System (ADS)

Zhang, Shaoyan; Sun, Yan; Li, Chunsheng; Ci, Lijie

2013-11-01

In this paper, Cu3V2O8 hollow spheres have been successfully synthesized via a liquid precipitation method with colloidal carbon spheres as template followed by a subsequent heat treatment process. On the basis of XRD analysis, SEM observation, and TG-DSC analysis of the precursor and products, the formation mechanism of Cu3V2O8 hollow spheres was proposed. UV-vis diffuse reflectance spectra showed that the Cu3V2O8 hollow spheres exhibit strong absorption in a wide wavelength range from UV to visible light. The photocatalytic activity experiment indicated that the as-prepared Cu3V2O8 hollow spheres exhibited good photocatalytic activity in degradation of methyl orange (MO) under 150-W xenon arc lamp light irradiation. Furthermore, electrochemical measurements showed that the Cu3V2O8 hollow spheres exhibited high discharge capacity and excellent high-rate capability, indicating potential cathode candidates for primary lithium batteries used in long-term implantable cardiac defibrillators (ICDs).

In situ immobilization on the silica gel surface and adsorption capacity of polymer-based azobenzene on toxic metal ions

NASA Astrophysics Data System (ADS)

Savchenko, Irina; Yanovska, Elina; Sternik, Dariusz; Kychkyruk, Olga; Ol'khovik, Lidiya; Polonska, Yana

2018-03-01

In situ immobilization of poly[(4-methacryloyloxy-(4'-carboxy)azobenzene] on silica gel surface has been performed by radical polymerization of monomer. The fact of polymer immobilization is confirmed by IR spectroscopy. TG and DSC-MS analysis showed that the mass of the immobilized polymer was 10.61%. The SEM-microphotograph-synthesized composite analysis showed that the immobilized polymer on the silica gel surface is placed in the form of fibers. It has been found that the synthesized composite exhibits the sorption ability in terms of microquantities of Cu(II), Cd(II), Pb(II), Mn(II) and Fe(III) ions in a neutral aqueous medium. The quantitative sorption of microquantities of Pb(II) and Fe(III) ions has been recorded. It has been found that immobilization of the silica gel surface leads to an increase in its sorption capacitance for Fe(III), Cu(II) and Pb(II) ions by half.

Synthesis and characterization of a novel bio-based resin from maleated soybean oil polyols

NASA Astrophysics Data System (ADS)

Li, Y. T.; Yang, L. T.; Zhang, H.

2017-02-01

In this paper, a novel bio-based resin was prepared by the radical copolymerization of maleated soybean oil polyols (MSBOP) and styrene (ST). Structure of the product was studied by Fourier transformation infrared spectrometer (FT-IR), and the result was found to be consistent with that of theoretical structure. Swelling experiments indicated that the crosslinking degree increased with the increase of hydroxyl value. Thermal analysis by differential scanning calorimetry (DSC) and thermo-gravimetric analysis (TG) revealed that glass transition temperature (Tg) of the polymer increased with increasing hydroxyl values, and that its thermal stability showed a good correlation with the hydroxyl value. The tensile strength and impact strength were significantly affected by the hydroxyl value of soybean oil polyols. With increasing hydroxyl value, the tensile strength presented an increasing trend, while the impact strength showed a decreasing one. Moreover, the property of the polymer from elastomer to plastic character also depended on the functionality of the hydroxyl value of soybean oil polyols.

Use of a training program to enhance NICU nurses' cognitive abilities for assessing preterm infant behaviors and offering supportive interventions.

PubMed

Liaw, Jen-Jiuan

2003-06-01

This study tested the use of a developmentally supportive care (DSC) training program in the form of videotaped and personalized instruction to increase nurses' cognitive abilities for assessing preterm infant behavioral signals and offering supportive care. The study used a two-group pre-test post-test quasi-experimental repeated measures design. The participants were 25 NICU nurses, 13 in the intervention group, and 12 in the control group. An instrument developed for the purpose of the study was a video test that measured the effectiveness of the DSC training. The video test questionnaires were administered to the participants twice with an interval of four weeks. ANCOVA controlling the baseline scores was used for data analysis. In general, the results support the hypothesis that nurses' cognitive abilities were enhanced after the DSC training. The increase in nurses' cognitive abilities is the prerequisite for behavioral change, based on the assumptions of Bandura's Social Cognitive Learning Theory (Bandura, 1986). As nurses' cognitive abilities increased, it would be possible that nurse behaviors in taking care of these preterm infants might change. Therefore, the author recommends that in order to improve NICU care quality and the outcomes of preterm infants, the concepts of developmentally supportive care be incorporated into NICU caregiving practice by educating nurses.

Preparation and characterization of metoprolol tartrate containing matrix type transdermal drug delivery system.

PubMed

Malipeddi, Venkata Ramana; Awasthi, Rajendra; Ghisleni, Daniela Dal Molim; de Souza Braga, Marina; Kikuchi, Irene Satiko; de Jesus Andreoli Pinto, Terezinha; Dua, Kamal

2017-02-01

The present study aimed to develop matrix-type transdermal drug delivery system (TDDS) of metoprolol tartrate using polyvinyl pyrrolidone (PVP) and polyvinyl alcohol (PVA). The transdermal films were evaluated for physical parameters, Fourier transform infrared spectroscopy analysis (FTIR), differential scanning calorimetry (DSC), in vitro drug release, in vitro skin permeability, skin irritation test and stability studies. The films were found to be tough, non-sticky, easily moldable and possess good tensile strength. As the concentration of PVA was increased, the tensile strength of the films was also increased. Results of FTIR spectroscopy and DSC revealed the absence of any drug-polymer interactions. In vitro release of metoprolol followed zero-order kinetics and the mechanism of release was found to be diffusion rate controlled. In vitro release studies of metoprolol using Keshary-Chein (vertical diffusion cell) indicated 65.5 % drug was released in 24 h. In vitro skin permeation of metoprolol transdermal films showed 58.13 % of the drug was released after 24 h. In vitro skin permeation of metoprolol followed zero-order kinetics in selected formulations. The mechanism of release was found to be diffusion rate controlled. In a 22-day skin irritation test, tested formulation of transdermal films did not exhibit any allergic reactions, inflammation, or contact dermatitis. The transdermal films showed good stability in the 180-day stability study. It can be concluded that the TDDS of MPT can help in bypassing the first-pass effect and will provide patient improved compliance, without sacrificing the therapeutic advantages of the drugs.

Dendrimer-paclitaxel complexes for efficient treatment in ovarian cancer: study on OVCAR-3 and HEK293T cells.

PubMed

Yao, Hua; Ma, Jinqi

2018-01-01

The present paper investigates the enhancement of the therapeutic effect of Paclitaxel (a potent anticancer drug) by increasing its cellular uptake in the cancerous cells with subsequent reduction in its cytotoxic effects. To fulfill these goals the Paclitaxel (PTX)-Biotinylated PAMAM dendrimer complexes were prepared using biotinylation method. The primary parameter of Biotinylated PAMAM with a terminal HN 2 group - the degree of biotinylation - was evaluated using HABA assay. The basic integrity of the complex was studied using DSC. The Drug Loading (DL) and Drug Release (DR) parameters of Biotinylated PAMAM dendrimer-PTX complexes were also examined. Cellular uptake study was performed in OVCAR-3 and HEK293T cells using fluorescence technique. The statistical analysis was also performed to support the experimental data. The results obtained from HABA assay showed the complete biotinylation of PAMAM dendrimer. DSC study confirmed the integrity of the complex as compared with pure drug, biotinylated complex and their physical mixture. Batch 9 showed the highest DL (12.09%) and DR (70%) for 72 h as compared to different concentrations of drug and biotinylated complex. The OVCAR-3 (cancerous) cells were characterized by more intensive cellular uptake of the complexes than HEK293T (normal) cells. The obtained experimental results were supported by the statistical data. The results obtained from both experimental and statistical evaluation confirmed that the biotinylated PAMAM NH 2 dendrimer-PTX complex not only displays increased cellular uptake but has also enhanced release up to 72 h with the reduction in cytotoxicity.

Thermodynamic Stability Analysis of Tolbutamide Polymorphs and Solubility in Organic Solvents.

PubMed

Svärd, Michael; Valavi, Masood; Khamar, Dikshitkumar; Kuhs, Manuel; Rasmuson, Åke C

2016-06-01

Melting temperatures and enthalpies of fusion have been determined by differential scanning calorimetry (DSC) for 2 polymorphs of the drug tolbutamide: FI(H) and FV. Heat capacities have been determined by temperature-modulated DSC for 4 polymorphs: FI(L), FI(H), FII, FV, and for the supercooled melt. The enthalpy of fusion of FII at its melting point has been estimated from the enthalpy of transition of FII into FI(H) through a thermodynamic cycle. Calorimetric data have been used to derive a quantitative polymorphic stability relationship between these 4 polymorphs, showing that FII is the stable polymorph below approximately 333 K, above which temperature FI(H) is the stable form up to its melting point. The relative stability of FV is well below the other polymorphs. The previously reported kinetic reversibility of the transformation between FI(L) and FI(H) has been verified using in situ Raman spectroscopy. The solid-liquid solubility of FII has been gravimetrically determined in 5 pure organic solvents (methanol, 1-propanol, ethyl acetate, acetonitrile, and toluene) over the temperature range 278 to 323 K. The ideal solubility has been estimated from calorimetric data, and solution activity coefficients at saturation in the 5 solvents determined. All solutions show positive deviation from Raoult's law, and all van't Hoff plots of solubility data are nonlinear. The solubility in toluene is well below that observed in the other investigated solvents. Solubility data have been correlated and extrapolated to the melting point using a semiempirical regression model. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Influences of Soaking Temperature and Storage Conditions on Hardening of Soybeans (Glycine max) and Red Kidney Beans (Phaseolus vulgaris).

PubMed

Koriyama, Takako; Sato, Yoko; Iijima, Kumiko; Kasai, Midori

2017-07-01

The influences of soaking treatment and storage conditions on the softening of cooked beans, namely, soybeans and red kidney beans, were investigated. It was revealed that the softening of fresh soybeans and fresh red kidney beans was suppressed during subsequent boiling after soaking treatment at 50 and 60 °C. Furthermore, in treated aged soybeans and red kidney beans that were subjected to storage at 30 °C/75% relative humidity for 6 mo and soaking treatment at 50 to 60 °C, the hardness during cooking was further amplified. This suggested that the mechanism of softening suppression differs depending on the influences of soaking and storage. Analysis of the pectin fraction in alcohol insoluble solid showed insolubilization of metal ions upon storage at high temperature and high humidity in both soybeans and red kidney beans, which suggests interaction between Ca ions and hemicellulose or cellulose as cell wall polysaccharides. The results of differential scanning calorimetry (DSC) showed that aged soybeans exhibited a shift in the thermal transition temperature of glycinin-based protein to a higher temperature compared with fresh soybeans. From the results of DSC and scanning electron microscopy for aged red kidney beans, damaged starch is not conspicuous in the raw state after storage but is abundant upon soaking treatment. As for the influence of soaking at 60 °C, it can be suggested that its influence on cell wall crosslinking was large in soybeans and red kidney beans in both a fresh state and an aged state. © 2017 Institute of Food Technologists®.

Investigating the effect of an arterial hypertension drug on the structural properties of plasma protein.

PubMed

Hassan, Natalia; Maldonado-Valderrama, Julia; Gunning, A Patrick; Morris, V J; Ruso, Juan M

2011-10-15

Propanolol is a betablocker drug used in the treatment of arterial hypertension related diseases. In order to achieve an optimal performance of this drug it is important to consider the possible interactions of propanolol with plasma proteins. In this work, we have used several experimental techniques to characterise the effect of addition of the betablocker propanolol on the properties of bovine plasma fibrinogen (FB). Differential scanning calorimeter (DSC), circular dichroism (CD), dynamic light scattering (DLS), surface tension techniques and atomic force microscopy (AFM) measurements have been combined to carry out a detailed physicochemical and surface characterization of the mixed system. As a result, DSC measurements show that propranolol can play two opposite roles, either acting as a structure stabilizer at low molar concentrations or as a structure destabilizer at higher concentrations, in different domains of fibrinogen. CD measurements have revealed that the effect of propanolol on the secondary structure of fibrinogen depends on the temperature and the drug concentration and the DLS analysis showed evidence for protein aggregation. Interestingly, surface tension measurements provided further evidence of the conformational change induced by propanolol on the secondary structure of FB by importantly increasing the surface tension of the system. Finally, AFM imaging of the fibrinogen system provided direct visualization of the protein structure in the presence of propanolol. Combination of these techniques has produced complementary information on the behavior of the mixed system, providing new insights into the structural properties of proteins with potential medical interest. Copyright © 2011 Elsevier B.V. All rights reserved.

Characterization of Thermal Behavior of Epoxy Composites Reinforced with Curaua Fibers by Differential Scanning Calorimetry

NASA Astrophysics Data System (ADS)

Barcelos, Mariana A.; Ribeiro, Carolina Gomes D.; Ferreira, Jordana; Vieira, Janaina da S.; Margem, Frederico M.; Monteiro, Sergio N.

Epoxy composites reinforced with natural lignocellulosic fibers have, in recent times, been gaining attention in engineering areas as lighter and cheaper alternatives for traditional composites such as the "fiberglass". The curaua fiber is the one strongest today being considered as reinforcement of composites for automobile interior parts. In fact, several studies are currently being dedicated to curaua fiber composites since physical and mechanical properties are required for practical uses. In this work, the thermal behavior of epoxy composites reinforced with up to 30 % in volume of curaua fibers was investigated by differential scanning calorimetry, DSC. The results showed endothermic and exothermic events associated with water release and possible molecular chain amorphous transformation. Comparison with similar composites permitted to propose mechanism that explains this DSC thermal behavior.

Resveratrol cocrystals with enhanced solubility and tabletability.

PubMed

Zhou, Zhengzheng; Li, Wanying; Sun, Wei-Jhe; Lu, Tongbu; Tong, Henry H Y; Sun, Changquan Calvin; Zheng, Ying

2016-07-25

Two new 1:1 cocrystals of resveratrol (RES) with 4-aminobenzamide (RES-4ABZ) and isoniazid (RES-ISN) were synthesized by liquid assisted grinding (LAG) and rapid solvent removal (RSR) methods using ethanol as solvent. Their physiochemical properties were characterized using PXRD, DSC, solid state and solution NMR, FT-IR, and HPLC. Pharmaceutically relevant properties, including tabletability, solubility, intrinsic dissolution rate, and hygroscopicity, were evaluated. Temperature-composition phase diagram for RES-ISN cocrystal system was constructed from DSC data. Both cocrystals show higher solubility than resveratrol over a broad range of pH. They are phase stable and non-hygroscopic even under high humidity conditions. Importantly, both cocrystals exhibit improved solubility and tabletability compared with RES, which make them more suitable candidates for tablet formulation development. Copyright © 2016 Elsevier B.V. All rights reserved.

Chemical Modification of Kraft Lignin: Effect on Chemical and Thermal Properties

Treesearch

Yao Chen; Nicole M. Stark; Zhiyong Cai; Charles R. Frihart; Linda F. Lorenz; Rebecca E. Ibach

2014-01-01

Esterified kraft lignins (KL) were prepared by reaction with maleic anhydride (MA), succinic anhydride (SA), and phthalic anhydride (PA) in acetone solutions. The esterified lignins were characterized using ATR-FTIR, solid state CP-MAS 13C NMR spectroscopy, thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). PA...

Novel Electroactive Polymers as Environmentally Compliant Coatings for Corrosion Control

DTIC Science & Technology

2006-02-03

Gravametric Analysis (TGA) and Differential Scanning Calorimetry (DSC), respectively. In this work the polymers were characterized by cyclic voltametry ...or less. The Temperature Step / Frequency Sweep method was employed where data were collected from –40 to 100°C and 0.1-100 Hz at a resolution of

Multi-institutional Quantitative Evaluation and Clinical Validation of Smart Probabilistic Image Contouring Engine (SPICE) Autosegmentation of Target Structures and Normal Tissues on Computer Tomography Images in the Head and Neck, Thorax, Liver, and Male Pelvis Areas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Mingyao; Bzdusek, Karl; Brink, Carsten

2013-11-15

Purpose: Clinical validation and quantitative evaluation of computed tomography (CT) image autosegmentation using Smart Probabilistic Image Contouring Engine (SPICE). Methods and Materials: CT images of 125 treated patients (32 head and neck [HN], 40 thorax, 23 liver, and 30 prostate) in 7 independent institutions were autosegmented using SPICE and computational times were recorded. The number of structures autocontoured were 25 for the HN, 7 for the thorax, 3 for the liver, and 6 for the male pelvis regions. Using the clinical contours as reference, autocontours of 22 selected structures were quantitatively evaluated using Dice Similarity Coefficient (DSC) and Mean Slice-wisemore » Hausdorff Distance (MSHD). All 40 autocontours were evaluated by a radiation oncologist from the institution that treated the patients. Results: The mean computational times to autosegment all the structures using SPICE were 3.1 to 11.1 minutes per patient. For the HN region, the mean DSC was >0.70 for all evaluated structures, and the MSHD ranged from 3.2 to 10.0 mm. For the thorax region, the mean DSC was 0.95 for the lungs and 0.90 for the heart, and the MSHD ranged from 2.8 to 12.8 mm. For the liver region, the mean DSC was >0.92 for all structures, and the MSHD ranged from 5.2 to 15.9 mm. For the male pelvis region, the mean DSC was >0.76 for all structures, and the MSHD ranged from 4.8 to 10.5 mm. Out of the 40 autocontoured structures reviews by experts, 25 were scored useful as autocontoured or with minor edits for at least 90% of the patients and 33 were scored useful autocontoured or with minor edits for at least 80% of the patients. Conclusions: Compared with manual contouring, autosegmentation using SPICE for the HN, thorax, liver, and male pelvis regions is efficient and shows significant promise for clinical utility.« less

Vibrational spectroscopic study, structural analysis, photophysical properties and theoretical calculations of cis-(±)-2,4,5-tris(pyridin-2-yl)imidazoline

NASA Astrophysics Data System (ADS)

Baldenebro-López, Jesús; Báez-Castro, Alberto; Glossman-Mitnik, Daniel; Höpfl, Herbert; Cruz-Enríquez, Adriana; Miranda-Soto, Valentín; Parra-Hake, Miguel; Campos-Gaxiola, José J.

2017-02-01

cis-(±)-2,4,5-tris(pyridin-2-yl)imidazoline has been fully characterized by FT-IR, FT-Raman, UV-Vis and fluorescence spectroscopy, one- and two-dimensional NMR spectroscopy (1H, 1H-1H gCOSY, 1H-1H gNOESY,13C{1H} ATP, 1H-13C and 1H-15N gHSQC and 1H-13C gHMBC), high-resolution mass spectrometry (HR-FAB+), TG-DSC analysis and low-temperature single-crystal X-ray diffraction analysis. Additionally, the molecular geometry and the vibrational infrared and Raman frequencies were calculated by density functional theory using the M06/6-31G(d) level of theory, showing good agreement with the experimental results. The title compound showed interesting photophysical properties, which were studied experimentally in solution and in the solid state by UV-Vis and fluorescence spectroscopy and compared to the theoretically obtained parameters using TD-DFT calculations. Natural and Mulliken atomic charges and the molecular electrostatic potential (MEP) have been mapped.

A minitablet formulation made from electrospun nanofibers.

PubMed

Poller, Bettina; Strachan, Clare; Broadbent, Roland; Walker, Greg F

2017-05-01

The purpose of this study was to evaluate electrospun drug loaded nanofibers as a new matrix for minitablets. Prednisone, a poorly water-soluble drug, was loaded into povidone (polyvinylpyrrolidone, PVP) nanofibers using the process of electrospinning. The drug-loaded nanofiber mat was compressed into minitablets with a 2mm diameter and a height of 2.63±0.04mm. SEM analysis of the minitablet identified a nano-web structure with a nanofiber diameter in the range of 400-500nm. The minitablets met the requirements of the US Pharmacopeia with respect to content uniformity and friability. DSC and XRPD analysis of the minitablet indicated that the drug-polymer mixture was a one-phase amorphous system. XRPD analysis of the drug loaded nanofiber mat after 10-months of storage at ambient temperature showed no evidence of recrystallization of the drug. Solubility and dissolution properties of the drug formulated into a nanofiber mat and minitablet were evaluated. These results show that electrospun nanofibers may provide a useful matrix for the further development of minitablets. Copyright © 2017 Elsevier B.V. All rights reserved.

Growth and characterization of benzyl 4-hydroxybenzoate single crystal by vertical Bridgman technique for optical applications

NASA Astrophysics Data System (ADS)

Solanki, S. Siva Bala; Rajesh, N. P.; Suthan, T.

2018-07-01

The benzyl 4-hydroxybenzoate single crystal has been grown by vertical Bridgman technique. The grown crystal was confirmed by single crystal X-ray diffraction studies. The presence of functional groups in the crystal was confirmed by Fourier transform infrared (FTIR) spectral studies. The thermal behaviour of the grown crystal was analyzed by thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetric (DSC) studies. Optical behaviour of the grown benzyl 4-hydroxybenzoate crystal was studied by UV-Vis-NIR spectral analysis. Fluorescence spectrum shows near violet light emission. The second harmonic generation behaviour of benzyl 4-hydroxybenzoate was analyzed. The laser damage threshold value of benzyl 4-hydroxybenzoate was measured as 2.16 GW/cm2. The dielectric measurements of benzyl 4-hydroxybenzoate crystal were carried out with different frequencies 1 kHz to 1 MHz versus different temperatures ranging from 313 to 353 K. Photoconductivity study shows that the grown benzyl 4-hydroxybenzoate crystal belongs to negative photoconductivity property. The mechanical strength of the crystal was calculated by Vickers microhardness study.

Effects of formulation variables and characterization of guaifenesin wax microspheres for controlled release.

PubMed

Mani, Narasimhan; Park, M O; Jun, H W

2005-01-01

Sustained-release wax microspheres of guaifenesin, a highly water-soluble drug, were prepared by the hydrophobic congealable disperse method using a salting-out procedure. The effects of formulation variables on the loading efficiency, particle properties, and in-vitro drug release from the microspheres were determined. The type of dispersant, the amount of wetting agent, and initial stirring time used affected the loading efficiency, while the volume of external phase and emulsification speed affected the particle size of the microspheres to a greater extent. The crystal properties of the drug in the wax matrix and the morphology of the microspheres were studied by differential scanning calorimetry (DSC), powder x-ray diffraction (XRD), and scanning electron microscopy (SEM). The DSC thermograms of the microspheres showed that the drug lost its crystallinity during the microencapsulation process, which was further confirmed by the XRD data. The electron micrographs of the drug-loaded microspheres showed well-formed spherical particles with a rough exterior.

Optical, structural and thermal properties of bismuth nitrate doped polycarbonate composite

NASA Astrophysics Data System (ADS)

Mirji, Rajeshwari; Lobo, Blaise

2018-04-01

Bismuth nitrate (Bi(NO3)3) doped polycarbonate (PC) films were prepared by solution casting method, in the doping range varying from 0.1 wt% to 5 wt %. The prepared samples were characterized using UV-Visible spectroscopy, X-Ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC). Optical band gap was calculated by analyzing the UV-Visible spectra of pure as well as doped PC. Optical band gap is found to decrease from 4.38 eV to 4.33 eV as the Bi(NO3)3 content within PC increases. XRD patterns showed an increase in the degree of crystallinity of Bi(NO3)3 doped PC, especially at 3.5 wt% and 5 wt%. DSC study showed an increase in the degradation temperature, as the doping level is increased from 0 wt% up to 0.3 wt%. A decrease in Tg is observed as the doping level of these samples increases from 0 wt% up to 5 wt%.

Use of Several Thermal Analysis Techniques on a Hypalon Paint Coating for the Solid Rocket Booster (SRB) of the Space Shuttle

NASA Technical Reports Server (NTRS)

Wingard, Charles D.

1999-01-01

White Hypalon paint is brush-applied as a moisture barrier coating over cork surfaces on each of the two Space Shuttle SRBS. Fine cracks have been observed in the Hypalon coating three times historically on laboratory witness panels, but never on flight hardware. Recent samples of the cracked and standard ("good") Hypalon were removed from cork surfaces and were tested by Thermal Gravimetric Analysis (TGA), Thermomechanical (TMA) and Differential Scanning Calorimetry (DSC) thermal analysis techniques. The TGA data showed that at 700 C, where only paint pigment solids remain, the cracked material had about 9 weight percent more material remaining than the standard material, probably indicating incomplete mixing of the paint before it was brush-applied to produce the cracked material. Use of the TMA film tension method showed that the average static modulus vs. temperature was about 3 to 6 times higher for the cracked material than for the standard material, indicating a much higher stiffness for the cracked Hypalon. The TMA data also showed than an increased coating thickness for the cracked Hypalon was not a factor in the anomaly.

Assessment of degree of disorder (amorphicity) of lyophilized formulations of growth hormone using isothermal microcalorimetry.

PubMed

Mosharraf, Mitra

2004-05-01

When determining the degree of disorder of a lyophilized cake of a protein, it is important to use an appropriate analytical technique. Differential scanning calorimetry (DSC) and X-ray powder diffraction (XRPD) are the most commonly used thermoanalytical techniques for characterizing freeze-dried protein formulations. Unfortunately, these methods are unable to detect solid-state disorder at levels < 10%. Also, interpretation of DSC results for freeze-dried protein formulations can be difficult, as a result of the more complex thermal events occurring with this technique. For example, proteins can inhibit the thermally induced recrystallization of the lyophilized cake, resulting in potential misinterpretation of DSC degree of disorder results. The aim of this investigation was to study the use of isothermal microcalorimetry (IMC) in the assessment of degree of solid-state disorder (amorphicity) of lyophilized formulations of proteins. For this purpose, two formulations of growth hormone were prepared by lyophilization. These formulations consisted of the same amounts of protein, mannitol, glycine, and phosphate buffer, but differed in the freeze-drying procedure. After lyophilization, the recrystallization of the samples was studied using IMC at 25 degrees C under different relative humidities (58-75%). The effect of available surface area was studied by determining the heat of recrystallization (Q) of the samples before and after disintegration of the cakes. The results showed that, in contrast to DSC, IMC allowed detection of the recrystallization event in the formulations. Although both formulations were completely disordered and indistinguishable according to XRPD method, IMC revealed that formulation B had a different solid-sate structure than formulation A. This difference was the result of differences in the freeze-drying parameters, demonstrating the importance of choosing appropriate analytical methodology.

Structural, vibrational, thermal and optical studies of organic single crystal: Benzotriazolium p-toluene sulfonate (BTPTS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, R. Ramesh; Sathya, P.; Gopalakrishnan, R., E-mail: krgkrishnan@yahoo.com

Benzotriazolium p-toluene sulfonate (BTPTS) was grown by solution growth technique. The powder X-ray diffraction analysis was carried out to evaluate crystal system of the compound. LeBail Profile fitting analysis was performed to extract the individual peak intensities. FTIR spectrum analysis was recorded to study vibration frequencies of the prepared organic salt. Thermal studies were carried out using TG-DSC analysis. Optical absorption and energy band gap of the title compound was evaluated by UV-Vis spectral study.

Growth and characterization of metal halide perovskite crystals: Benzyltributyl ammonium tetrachloro manganate(II) monohydrate

NASA Astrophysics Data System (ADS)

Dhandapani, M.; Sugandhi, K.; Nithya, S.; Muthuraja, P.; Balachandar, S.; Aranganayagam, K. R.

2018-05-01

The perovskite type organic-inorganic hybrid benzyltributyl ammoniumtetrachloro manganate (II) monohydrates (BTBA-Mn) are synthesized and the single crystals are grown by slow evaporation solution growth technique. The structure of the grown crystals are confirmed by using X-ray diffraction (XRD), unit cell parameter analysis, Fourier transform Infrared (FTIR), elemental analysis and 13C-NMR spectral studies. Thermogravimetry (TG), differential thermal analysis (DTA) and differential scanning colorimetric (DSC) analysis were carried out to understand thermal stability and occurrence of phase transition.

Preparation and Compatibility Evaluation of Polypropylene/High Density Polyethylene Polyblends

PubMed Central

Lin, Jia-Horng; Pan, Yi-Jun; Liu, Chi-Fan; Huang, Chien-Lin; Hsieh, Chien-Teng; Chen, Chih-Kuang; Lin, Zheng-Ian; Lou, Ching-Wen

2015-01-01

This study proposes melt-blending polypropylene (PP) and high density polyethylene (HDPE) that have a similar melt flow index (MFI) to form PP/HDPE polyblends. The influence of the content of HDPE on the properties and compatibility of polyblends is examined by using a tensile test, flexural test, Izod impact test, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), polarized light microscopy (PLM), and X-ray diffraction (XRD). The SEM results show that PP and HDPE are incompatible polymers with PP being a continuous phase and HDPE being a dispersed phase. The FTIR results show that the combination of HDPE does not influence the chemical structure of PP, indicating that the polyblends are made of a physical blending. The DSC and XRD results show that PP and HDPE are not compatible, and the combination of HDPE is not correlated with the crystalline structure and stability of PP. The PLM results show that the combination of HDPE causes stacking and incompatibility between HDPE and PP spherulites, and PP thus has incomplete spherulite morphology and a smaller spherulite size. However, according to mechanical property test results, the combination of HDPE improves the impact strength of PP. PMID:28793750

Preparation and Compatibility Evaluation of Polypropylene/High Density Polyethylene Polyblends.

PubMed

Lin, Jia-Horng; Pan, Yi-Jun; Liu, Chi-Fan; Huang, Chien-Lin; Hsieh, Chien-Teng; Chen, Chih-Kuang; Lin, Zheng-Ian; Lou, Ching-Wen

2015-12-17

This study proposes melt-blending polypropylene (PP) and high density polyethylene (HDPE) that have a similar melt flow index (MFI) to form PP/HDPE polyblends. The influence of the content of HDPE on the properties and compatibility of polyblends is examined by using a tensile test, flexural test, Izod impact test, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), polarized light microscopy (PLM), and X-ray diffraction (XRD). The SEM results show that PP and HDPE are incompatible polymers with PP being a continuous phase and HDPE being a dispersed phase. The FTIR results show that the combination of HDPE does not influence the chemical structure of PP, indicating that the polyblends are made of a physical blending. The DSC and XRD results show that PP and HDPE are not compatible, and the combination of HDPE is not correlated with the crystalline structure and stability of PP. The PLM results show that the combination of HDPE causes stacking and incompatibility between HDPE and PP spherulites, and PP thus has incomplete spherulite morphology and a smaller spherulite size. However, according to mechanical property test results, the combination of HDPE improves the impact strength of PP.

Synthesis and spectroscopic characterization of gallic acid and some of its azo complexes

NASA Astrophysics Data System (ADS)

Masoud, Mamdouh S.; Hagagg, Sawsan S.; Ali, Alaa E.; Nasr, Nessma M.

2012-04-01

A series of gallic acid and azo gallic acid complexes were prepared and characterized by elemental analysis, IR, electronic spectra and magnetic susceptibility. The complexes were of different geometries: Octahedral, Tetrahedral and Square Planar. ESR was studied for copper complexes. All of the prepared complexes were of isotropic nature. The thermal analyses of the complexes were studied by DTA and DSC techniques. The thermodynamic parameters and the thermal transitions, such as glass transitions, crystallization and melting temperatures for some ligands and their complexes were evaluated and discussed. The entropy change values, ΔS#, showed that the transition states are more ordered than the reacting complexes. The biological activities of some ligands and their complexes are tested against Gram positive and Gram negative bacteria. The results showed that some complexes have a well considerable activity against different organisms.

Structural and dynamic characterization of ultrafine fibers based on the poly-3-hydroxybutyrate-dipyridamole system

NASA Astrophysics Data System (ADS)

Olkhov, A. A.; Karpova, S. G.; Staroverova, O. V.; Krutikova, A. A.; Orlov, N. A.; Kucherenko, E. L.; Iordanskii, A. L.

2016-11-01

The fibrous materials (the mats) based on poly-3-hydroxybutyrate (PHB) containing the drug, dipiridomole (DPD) were produced by electrospinning (ES). Thermophysical and dynamical properties of the single filaments and the mats were studied by scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and probe electron paramagnetic resonance spectroscopy (EPR). The effect of annealing temperature on the structure and crystallinity of the fibers was examined. It was shown that the loading of DPD influences on both the melting enthalpy and the morphology of the fibers. Besides the analysis of EPR spectra revealed that there are two populations of spin-probes distributed in the rigid and nonrigid amorphous regions of the PHB fibers respectively. For all fibrous materials with different content of DPD (0-5%) the correlation between thermophysical (DSC) and dynamic data (EPR) was observed.

Controlled release formulations of risperidone antipsychotic drug in novel aliphatic polyester carriers: Data analysis and modelling.

PubMed

Siafaka, Panoraia I; Barmpalexis, Panagiotis; Lazaridou, Maria; Papageorgiou, George Z; Koutris, Efthimios; Karavas, Evangelos; Kostoglou, Margaritis; Bikiaris, Dimitrios N

2015-08-01

In the present study a series of biodegradable and biocompatible poly(ε-caprolactone)/poly(propylene glutarate) (PCL/PPGlu) polymer blends were investigated as controlled release carriers of Risperidone drug (RISP), appropriate for transdermal drug delivery. The PCL/PPGlu carriers were prepared in different weight ratios. Miscibility studies of blends were evaluated through differential scanning calorimetry (DSC) and X-ray diffractometry (XRD). Hydrolysis studies were performed at 37°C using a phosphate buffered saline solution. The prepared blends have been used for the preparation of RISP patches via solvent evaporation method, containing 5, 10 and 15wt% RISP. These formulations were characterized using FT-IR spectroscopy, DSC and WAXD in order to evaluate interactions taking place between polymer matrix and drug, as well as the dispersion and the physical state of the drug inside the polymer matrix. In vitro drug release studies were performed using as dissolution medium phosphate buffered saline simulating body fluids. It was found that in all cases controlled release formulations were obtained, while the RISP release varies due to the properties of the used polymer blend and the different levels of drug loading. Artificial Neural Networks (ANNs) were used for dissolution behaviour modelling showing increased correlation efficacy compared to Multi-Linear-Regression (MLR). Copyright © 2015 Elsevier B.V. All rights reserved.

The thermal properties of beeswaxes: unexpected findings.

PubMed

Buchwald, Robert; Breed, Michael D; Greenberg, Alan R

2008-01-01

Standard melting point analyses only partially describe the thermal properties of eusocial beeswaxes. Differential scanning calorimetry (DSC) revealed that thermal phase changes in wax are initiated at substantially lower temperatures than visually observed melting points. Instead of a sharp, single endothermic peak at the published melting point of 64 degrees C, DSC analysis of Apis mellifera Linnaeus wax yielded a broad melting curve that showed the initiation of melting at approximately 40 degrees C. Although Apis beeswax retained a solid appearance at these temperatures, heat absorption and initiation of melting could affect the structural characteristics of the wax. Additionally, a more complete characterization of the thermal properties indicated that the onset of melting, melting range and heat of fusion of beeswaxes varied significantly among tribes of social bees (Bombini, Meliponini, Apini). Compared with other waxes examined, the relatively malleable wax of bumblebees (Bombini) had the lowest onset of melting and lowest heat of fusion but an intermediate melting temperature range. Stingless bee (Meliponini) wax was intermediate between bumblebee and honeybee wax (Apini) in heat of fusion, but had the highest onset of melting and the narrowest melting temperature range. The broad melting temperature range and high heat of fusion in the Apini may be associated with the use of wax comb as a free-hanging structural material, while the Bombini and Meliponini support their wax structures with exogenous materials.

In vitro and in vivo studies on a novel solid dispersion of repaglinide using polyvinylpyrrolidone as the carrier.

PubMed

Yin, Li-Fang; Huang, Shi-Jing; Zhu, Chun-Li; Zhang, Shu-Hui; Zhang, Qiang; Chen, Xi-Jing; Liu, Qing-Wang

2012-11-01

In order to improve the dissolution and absorption of the water insoluble drug repaglinide, a solid dispersion was developed by solvent method using polyvinylpyrrolidone K30 (PVP K30) as the hydrophilic carrier for the first time. Studies indicated that both solubility and the dissolution rate of repaglinide were significantly increased in the solid dispersion system compared with that of repaglinide raw material or physical mixtures. The repaglinide solid dispersions with PVP K30 solid state was characterized by polarizing microscopy, differential scanning calorimetry (DSC), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). DSC and XRD studies indicated that repaglinide existed in an amorphous form in the solid dispersion. FT-IR analysis demonstrated the presence of intermolecular hydrogen bonding between repaglinide and PVP K30 in the solid dispersion. In the in situ gastrointestinal perfusion experiment, solid dispersion was shown to remarkably enhance the absorption of repaglinide in stomach and all segments of intestine. In vivo pharmacokinetic study in rats showed that immediate and complete release of repaglinide from the solid dispersion resulted in rapid absorption that significantly increased the bioavailability and the maximum plasma concentration over repaglinide raw material. These results demonstrated PVP K30 was an appropriate carrier for solid dispersion of repaglinide, with increased dissolution and oral absorption.

Thermal Analysis of a New Glass Fiber-Reinforced Bismaleimide Composite Material Used for Firefighter Helmets

NASA Astrophysics Data System (ADS)

Ciubotariu–Ana, P.; Micu, C. A.; Lohan, N. M.; Pricop, B.; Bujoreanu, L. G.; Bejinariu, C.

2018-06-01

Safety helmets represent essential Personal Protection Equipment (PPE) used in firefighter protection and emergency situations. They protect firefighter’s face and eyes against flames, heat and flying debris. When temperature levels are high, user’s thermal comfort is affected. A glass fibre-reinforced bismaleimide composite material has a number of improved properties in terms of mechanical and thermal characteristics, as compared to the materials that are currently used. The present paper aims to comparatively analyse the thermal behaviour of an injection moulded polypropylene helmet and the newly developed hot modelling material, under the form of a glass fibre-reinforced bismaleimide composite material. Thermal analysis was performed using Differential Scanning Calorimetry (DSC) and Dynamic-Mechanical Analysis (DMA). DSC and DMA thermograms were corroborated and discussed, from the point of view of the consecutive solid state transitions occurring during heating, mostly in the second heating-cooling cycle. The isothermal behaviour of glass fibre-reinforced bismaleimide composite material, during strain sweeps performed by DMA, enabled the determination of internal friction and storage modulus, under vibratory loads, at different temperatures. The advantages of the newly developed glass fibre-reinforced bismaleimide composite material were highlighted.

Studies on the syntheses, structural Characterization, antimicrobial of the CO-CRYSTAL 1,10-phenanthrolin-1-IUM(1,10-phenH+)-caffeine(caf)-hexafluorophosphate

NASA Astrophysics Data System (ADS)

El Hamdani, H.; El Amane, M.; Duhayon, C.

2018-03-01

Co-crystal of 1,10-phenanthrolin-1-ium-caffeine-hexafluorophosphate was synthesized, studied by FTIR, 1H, 13C NMR, DSC and X-ray structure and crystallized in the monoclinic space group C2/c. The unit cell parameters are a = 19.3761 (3), b = 17.9548 (3), c = 13.8074 (3) with β = 117.8132 (10). The final R value is 0.069 for 29,522 measured reflections. The co-crystal structure analysis indicate the 1,10-phenanthroline is protonated by one nitrogen atom and formed the 1,10-phenanthrolin-1-ium cation, which is stabilized by hydrogen bonds N+-H…Odbnd C interaction with carbonyl and imidazol ring in caffeine molecule. The intermolecular hydrogen bonds: Csbnd H...O, Csbnd H...N, Nsbnd H...O, Csbnd H...F and intramolecular hydrogen bond: C1sbnd H12...O14, together play a vital role in stabilizing the structure of co-crystal. The X-ray structural analysis confirm the assignments of the structure from infrared, 1H, 13C NMR, spectroscopic data DSC and molar conductivity analysis. The antimicrobial activity of the co-crystal was studied.

Predictive Modeling of Fast-Curing Thermosets in Nozzle-Based Extrusion

NASA Technical Reports Server (NTRS)

Xie, Jingjin; Randolph, Robert; Simmons, Gary; Hull, Patrick V.; Mazzeo, Aaron D.

2017-01-01

This work presents an approach to modeling the dynamic spreading and curing behavior of thermosets in nozzle-based extrusions. Thermosets cover a wide range of materials, some of which permit low-temperature processing with subsequent high-temperature and high-strength working properties. Extruding thermosets may overcome the limited working temperatures and strengths of conventional thermoplastic materials used in additive manufacturing. This project aims to produce technology for the fabrication of thermoset-based structures leveraging advances made in nozzle-based extrusion, such as fused deposition modeling (FDM), material jetting, and direct writing. Understanding the synergistic interactions between spreading and fast curing of extruded thermosetting materials will provide essential insights for applications that require accurate dimensional controls, such as additive manufacturing [1], [2] and centrifugal coating/forming [3]. Two types of thermally curing thermosets -- one being a soft silicone (Ecoflex 0050) and the other being a toughened epoxy (G/Flex) -- served as the test materials in this work to obtain models for cure kinetics and viscosity. The developed models align with extensive measurements made with differential scanning calorimetry (DSC) and rheology. DSC monitors the change in the heat of reaction, which reflects the rate and degree of cure at different crosslinking stages. Rheology measures the change in complex viscosity, shear moduli, yield stress, and other properties dictated by chemical composition. By combining DSC and rheological measurements, it is possible to establish a set of models profiling the cure kinetics and chemorheology without prior knowledge of chemical composition, which is usually necessary for sophisticated mechanistic modeling. In this work, we conducted both isothermal and dynamic measurements with both DSC and rheology. With the developed models, numerical simulations yielded predictions of diameter and height of droplets, along with width and height of extruded lines cured at varied temperatures. Experimental results carried out on a goniometric platform and a nozzle-based 3D printer showed agreement with the numerical simulations. Finally, this presentation will show how the models are adaptable to the planning of tool paths and designs in additive manufacturing.

[Investigation on chromatogram-pharmacodynamics relationship of Angelica sinensis on effect of replenishing blood].

PubMed

Yang, Ying-Lai; Cui, Fang; Hu, Fang; Guo, Long; Yang, Tao; Li, Ying-Dong; Feng, Shi-Lan

2013-11-01

Blood deficiency model of mice was copied by subcutaneous injection with 200, 100 and 100 mg x kg(-1) (0.01 mL x g(-1)) acetyl phenylhydrazine (APH) at the frist, fourth, and seventh days. Mice in each group were perfused with different extracted parts of Angelica sinensis (drug dosage was 2.4 g x kg(-1)) at the tenth day, once a day for 10 days. Then compare the influence of different extracted parts of Angelica sinensis to RBC, Hb, PLT and thymus, spleen and weight changes of blood deficiency mice. The peak areas of each common peak from HPLC fingerprint were associated with the date of replenishing blood pharmacodynamics efficacy by using gray relation statistic, which was used to research the chromatogram-pharmacodynamics relationship. The results showed that the part of DSC has the better effect in replenishing blood. The contribution degree of the DSC to replenishing blood of each component were determined by correlation size, and ferulic acid made the largest contribution, but contribution of other components should not be ignored. In this paper, we research the relationship of the HPLC fingerprint and spectrum activity relationship, determine the material basis of the DSC for replenishing blood, and provide effective way to represent the spectral correlation effect.

Exploration of a new method in determining the glass transition temperature of BMGs by electrical resistivity

NASA Astrophysics Data System (ADS)

Guo, Jing; Zu, Fangqiu; Chen, Zhihao; Zheng, Shubin; Yuan, Yuan

2005-07-01

Based on a brief retrospect of the method in establishing Tg of the bulk metallic glasses (BMGs), some perplexities concerning this are pointed out. With the experimental results of Zr-Al-Ni-Cu-X (Nb,Ti) BMGs, a electrical resistivity method is proposed to determine the glass transition temperature of BMGs. With the method, we define two kinds of characteristic temperature related to the glass transition, Tg-dep and Tg-int, respectively. By comparing Tg-dep and Tg-int with Tg determined by the DSC method, we have found that, for the same alloy at the same heating rate, Tg-dep is very close to Tg-onset while Tg-int is approximate to Tg-mid. As a method to determine the glass transition temperature, the electrical resistivity method has proved to be more convenient and practical in comparison with the DSC method, especially when the DSC curve cannot show the glass transition character of BMGs. In addition, we would emphasize that when we refer to Tg, it is necessary to expatiate on the way of denoting the glass transition temperature, such as Tg-dep or Tg-int ( Tg-onset or Tg-mid), and on the heating rate, in order to avoid ambiguity.

Measurements of diagnostic examination performance and correlation analysis using microvascular leakage, cerebral blood volume, and blood flow derived from 3T dynamic susceptibility-weighted contrast-enhanced perfusion MR imaging in glial tumor grading.

PubMed

Server, Andrés; Graff, Bjørn A; Orheim, Tone E Døli; Schellhorn, Till; Josefsen, Roger; Gadmar, Øystein B; Nakstad, Per H

2011-06-01

To assess the diagnostic accuracy of microvascular leakage (MVL), cerebral blood volume (CBV) and blood flow (CBF) values derived from dynamic susceptibility-weighted contrast-enhanced perfusion MR imaging (DSC-MR imaging) for grading of cerebral glial tumors, and to estimate the correlation between vascular permeability/perfusion parameters and tumor grades. A prospective study of 79 patients with cerebral glial tumors underwent DSC-MR imaging. Normalized relative CBV (rCBV) and relative CBF (rCBF) from tumoral (rCBVt and rCBFt), peri-enhancing region (rCBVe and rCBFe), and the value in the tumor divided by the value in the peri-enhancing region (rCBVt/e and rCBFt/e), as well as MVL, expressed as the leakage coefficient K(2) were calculated. Hemodynamic variables and tumor grades were analyzed statistically and with Pearson correlations. Receiver operating characteristic (ROC) curve analyses were also performed for each of the variables. The differences in rCBVt and the maximum MVL (MVL(max)) values were statistically significant among all tumor grades. Correlation analysis using Pearson was as follows: rCBVt and tumor grade, r = 0.774; rCBFt and tumor grade, r = 0.417; MVL(max) and tumor grade, r = 0.559; MVL(max) and rCBVt, r = 0.440; MVL(max) and rCBFt, r = 0.192; and rCBVt and rCBFt, r = 0.605. According to ROC analyses for distinguishing tumor grade, rCBVt showed the largest areas under ROC curve (AUC), except for grade III from IV. Both rCBVt and MVL(max) showed good discriminative power in distinguishing all tumor grades. rCBVt correlated strongly with tumor grade; the correlation between MVL(max) and tumor grade was moderate.

Isolation and characterization of nanocrystalline cellulose from roselle-derived microcrystalline cellulose.

PubMed

Kian, Lau Kia; Jawaid, Mohammad; Ariffin, Hidayah; Karim, Zoheb

2018-07-15

Roselle fiber is a renewable and sustainable agricultural waste enriched with cellulose polysaccharides. The isolation of Nanocrystalline cellulose (NCC) from roselle-derived microcrystalline cellulose (MCC) is an alternative approach to recover the agricultural roselle plant residue. In the present study, acid hydrolysis with different reaction time was carried out to degrade the roselle-derived MCC to form NCC. The characterizations of isolated NCC were conducted through Fourier Transform Infrared Ray (FTIR), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), Energy Dispersive Spectroscopy (EDS), X-ray Diffraction (XRD), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). As evaluated from the performed morphological investigations, the needle-like shape NCC nanostructures were observed under TEM and AFM microscopy studies, while irregular rod-like shape of NCC was observed under FESEM analysis. With 60min hydrolysis time, XRD analysis demonstrated the highest NCC crystallinity degree with 79.5%. In thermal analysis by TGA and DSC, the shorter hydrolysis time tended to produce NCC with higher thermal stability. Thus, the isolated NCC from roselle-derived MCC has high potential to be used in application of pharmaceutical and biomedical fields for nanocomposite fabrication. Copyright © 2018 Elsevier B.V. All rights reserved.

Thermosets of epoxy monomer from Tung oil fatty acids cured in two synergistic ways

USDA-ARS?s Scientific Manuscript database

A new epoxy monomer from tung oil fatty acids, glycidyl ester of eleostearic acid (GEEA), was synthesized and characterized by 1H-NMR and 13C-NMR spectroscopy. Differential scanning calorimetry analysis (DSC) and FT-IR were utilized to investigate the curing process of GEEA cured by both dienophiles...

Diagnostics for the Analysis of Surface Chemistry Effects on Composite Energetic Material Reactions

DTIC Science & Technology

2015-10-30

integration time) and a NETZSCH STA 449 Jupiter that will allow for consistency and efficiency with its automatic 20 sample changer. (2) Together these...Purchase of the NETZSCH STA 449 Jupiter (DSC-TGA) to resolve reaction kinetics under equilibrium conditions. Images of this instrumentation are included in

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shen, Lei; Bai, Yu; Min, Yu-Ting

Three different tetrazole-carboxylate ligands, monotetrazole-carboxylate H{sub 2}tza (H{sub 2}tza=1,5-tetrazole-diacetic acid), Hpztza (Hpztza=5-(2-pyrazinyl)tetrazole-2(1-methyl)acetic acid), ditetrazole-carboxylate H{sub 2}tzpha (H{sub 2}tzpha=1,3-di(tetrazole-5-yl)benzene-N2,N2′-diacetic acid) have been chosen to react with CdCl{sub 2}·6H{sub 2}O, resulting in the formation of three new compounds [Cd{sub 2}(tza){sub 2}] (1), [Cd(pztza){sub 2}] (2) and [Cd(tzpha)(CH{sub 3}OH){sub 2}] (3). The coordinate sites of the three ligands are major influenced by the different substituted group of tetrazole ring. These compounds have been characterized by elemental analysis, IR and single crystal X-ray diffraction. Compound 1 displays a complex 3D structure; compound 2 shows a 3D network and compound 3 features a 2D layermore » network. Furthermore, the luminescence properties investigated at room temperature in the solid state showed excellent ligand-centered luminescence. The obvious enhancement in luminescence makes these compounds potential materials for optical use. The differential scanning calorimetry (DSC) and thermogravimetric-differential thermogravimetric (TG-DTG) analyses were applied to evaluate the thermal decomposition behavior of such compounds, showing that compounds 2 and 3 can be used as potential energetic materials. The relevant thermodynamic parameters ΔH, ΔS and ΔG were calculated as well. - Graphical abstract: H{sub 2}tza, Hpztza and H{sub 2}tzpha have been prepared. Three novel Cd (II)compounds were synthesized by reactions of CdCl{sub 2}·6H{sub 2}O, namely three dimensional [Cd{sub 2}(tza){sub 2}] (1), three dimensional [Cd(pztza){sub 2}] (2), and two dimensional [Cd(tzpha)(CH{sub 3}O){sub 2}] (3). The luminescences were investigated. Furthermore, the DSC show compounds 1 and 3 can be used as potential explosive materials.« less

A study of the homogeneity and deviations from stoichiometry in mercuric iodide

NASA Astrophysics Data System (ADS)

Burger, A.; Morgan, S.; He, C.; Silberman, E.; van den Berg, L.; Ortale, C.; Franks, L.; Schieber, M.

1990-01-01

We have been able to determine the deviations from stoichiometry of mercuric iodide (HgI 2) by using differential scanning calorimetry (DSC). Mercury excess or iodine deficiency in mercuric iodide can be evaluated from the eutectic melting of α-Hgl 2-Hg 2I 2 at 235 °C, which appears as an additional peak in DSC thermograms. I 2 excess can be found from the existence of the I 2-α-HgI 2 eutectic melting at 103°C. An additional DSC peak appears in some samples around 112°C, that could be explained by the presence of iodine inclusions. Using resonance fluorescence spectroscopy (RFS) we have been able to determine the presence of free I 2 that is released by samples during the heating at 120 °C (crystal growth temperature), thus giving additional support to the above DSC results.

A Differential Scanning Calorimetry Method for Construction of Continuous Cooling Transformation Diagram of Blast Furnace Slag

NASA Astrophysics Data System (ADS)

Gan, Lei; Zhang, Chunxia; Shangguan, Fangqin; Li, Xiuping

2012-06-01

The continuous cooling crystallization of a blast furnace slag was studied by the application of the differential scanning calorimetry (DSC) method. A kinetic model describing the correlation between the evolution of the degree of crystallization with time was obtained. Bulk cooling experiments of the molten slag coupled with numerical simulation of heat transfer were conducted to validate the results of the DSC methods. The degrees of crystallization of the samples from the bulk cooling experiments were estimated by means of the X-ray diffraction (XRD) and the DSC method. It was found that the results from the DSC cooling and bulk cooling experiments are in good agreement. The continuous cooling transformation (CCT) diagram of the blast furnace slag was constructed according to crystallization kinetic model and experimental data. The obtained CCT diagram characterizes with two crystallization noses at different temperature ranges.

Channeling of electron transport to improve collection efficiency in mesoporous titanium dioxide dye sensitized solar cell stacks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fakharuddin, Azhar; Ahmed, Irfan; Yusoff, Mashitah M.

2014-02-03

Dye-sensitized solar cell (DSC) modules are generally made by interconnecting large photoelectrode strips with optimized thickness (∼14 μm) and show lower current density (J{sub SC}) compared with their single cells. We found out that the key to achieving higher J{sub SC} in large area devices is optimized photoelectrode volume (V{sub D}), viz., thickness and area which facilitate the electron channeling towards working electrode. By imposing constraints on electronic path in a DSC stack, we achieved >50% increased J{sub SC} and ∼60% increment in photoelectric conversion efficiency in photoelectrodes of similar V{sub D} (∼3.36 × 10{sup −4} cm{sup 3}) without using any metallic gridmore » or a special interconnections.« less

Effects of low molecular sugars on the retrogradation of tapioca starch gels during storage

PubMed Central

Li, Rongfang; Kang, Huaibin; Luo, Denglin; Fan, Jinling; Zhu, Wenxue; Liu, Xinfang; Tong, Qunyi

2017-01-01

The effects of low molecular sugars (sucrose, glucose and trehalose) on the retrogradation of tapioca starch (TS) gels stored at 4°C for different periods were examined with different methods. Decrease in melting enthalpy (ΔHmelt) were obtained through differential scanning calorimetry analysis. Analysis of decrease in crystallization rate constant (k) and increase in semi-crystallization time (τ1/2) results obtained from retrogradation kinetics indicated that low molecular sugars could retard the retrogradation of TS gels and further revealed trehalose as the best inhibitor among the sugars used in this study. Fourier transform infrared (FTIR) analysis indicated that the intensity ratio of 1047 to 1022 cm−1 was increased with the addition of sugars in the order of trehalose > sucrose > glucose. Decrease in hardness parameters and increase in springiness parameters obtained from texture profile analysis (TPA) analysis also indicated that low molecular sugars could retard the retrogradation of TS gels. The results of FTIR and TPA showed a consistent sugar effect on starch retrogradation with those of DSC and retrogradation kinetics analysis. PMID:29284007

Effects of low molecular sugars on the retrogradation of tapioca starch gels during storage.

PubMed

Zhang, Xiaoyu; Li, Rongfang; Kang, Huaibin; Luo, Denglin; Fan, Jinling; Zhu, Wenxue; Liu, Xinfang; Tong, Qunyi

2017-01-01

The effects of low molecular sugars (sucrose, glucose and trehalose) on the retrogradation of tapioca starch (TS) gels stored at 4°C for different periods were examined with different methods. Decrease in melting enthalpy (ΔHmelt) were obtained through differential scanning calorimetry analysis. Analysis of decrease in crystallization rate constant (k) and increase in semi-crystallization time (τ1/2) results obtained from retrogradation kinetics indicated that low molecular sugars could retard the retrogradation of TS gels and further revealed trehalose as the best inhibitor among the sugars used in this study. Fourier transform infrared (FTIR) analysis indicated that the intensity ratio of 1047 to 1022 cm-1 was increased with the addition of sugars in the order of trehalose > sucrose > glucose. Decrease in hardness parameters and increase in springiness parameters obtained from texture profile analysis (TPA) analysis also indicated that low molecular sugars could retard the retrogradation of TS gels. The results of FTIR and TPA showed a consistent sugar effect on starch retrogradation with those of DSC and retrogradation kinetics analysis.

TU-H-CAMPUS-JeP2-05: Can Automatic Delineation of Cardiac Substructures On Noncontrast CT Be Used for Cardiac Toxicity Analysis?

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luo, Y; Liao, Z; Jiang, W

Purpose: To evaluate the feasibility of using an automatic segmentation tool to delineate cardiac substructures from computed tomography (CT) images for cardiac toxicity analysis for non-small cell lung cancer (NSCLC) patients after radiotherapy. Methods: A multi-atlas segmentation tool developed in-house was used to delineate eleven cardiac substructures including the whole heart, four heart chambers, and six greater vessels automatically from the averaged 4DCT planning images for 49 NSCLC patients. The automatic segmented contours were edited appropriately by two experienced radiation oncologists. The modified contours were compared with the auto-segmented contours using Dice similarity coefficient (DSC) and mean surface distance (MSD)more » to evaluate how much modification was needed. In addition, the dose volume histogram (DVH) of the modified contours were compared with that of the auto-segmented contours to evaluate the dosimetric difference between modified and auto-segmented contours. Results: Of the eleven structures, the averaged DSC values ranged from 0.73 ± 0.08 to 0.95 ± 0.04 and the averaged MSD values ranged from 1.3 ± 0.6 mm to 2.9 ± 5.1mm for the 49 patients. Overall, the modification is small. The pulmonary vein (PV) and the inferior vena cava required the most modifications. The V30 (volume receiving 30 Gy or above) for the whole heart and the mean dose to the whole heart and four heart chambers did not show statistically significant difference between modified and auto-segmented contours. The maximum dose to the greater vessels did not show statistically significant difference except for the PV. Conclusion: The automatic segmentation of the cardiac substructures did not require substantial modification. The dosimetric evaluation showed no statistically significant difference between auto-segmented and modified contours except for the PV, which suggests that auto-segmented contours for the cardiac dose response study are feasible in the clinical practice with a minor modification to the PV vessel.« less

Real time neutron diffraction and NMR of the Empress II glass-ceramic system.

PubMed

O'Donnell, M D; Hill, R G; Karpukhina, N; Law, R V

2011-10-01

This study reports real time neutron diffraction on the Empress II glass-ceramic system. The commercial glass-ceramics was characterized by real time neutron diffraction, ³¹P and ²⁹Si solid-state MAS-NMR, DSC and XRD. On heating, the as-received glass ceramic contained lithium disilicate (Li₂Si₂O₅), which melted with increasing temperature. This was revealed by neutron diffraction which showed the Bragg peaks for this phase had disappeared by 958°C in agreement with thermal analysis. On cooling lithium metasilicate (Li₂SiO₃) started to form at around 916°C and a minor phase of cristobalite at around 852°C. The unit cell volume of both Li-silicate phases increased linearly with temperature at a rate of +17×10⁻³ ų.°C⁻¹. Room temperature powder X-ray diffraction (XRD) of the material after cooling confirms presence of the lithium metasilicate and cristobalite as the main phases and shows, in addition, small amount of lithium disilicate and orthophosphate. ³¹P MAS-NMR reveals presence of the lithiorthophosphate (Li₃PO₄) before and after heat treatment. The melting of lithium disilicate on heating and crystallisation of lithium metasilicate on cooling agree with endothermic and exotermic features respectively observed by DSC. ²⁹Si MAS-NMR shows presence of lithium disilicate phase in the as-received glass-ceramic, though not in the major proportion, and lithium metasilicate in the material after heat treatment. Both phases have significantly long T₁ relaxation time, especially the lithium metasilicate, therefore, a quantitative analysis of the ²⁹Si MAS-NMR spectra was not attempted. Significance. The findings of the present work demonstrate importance of the commercially designed processing parameters in order to preserve desired characteristics of the material. Processing the Empress II at a rate slower than recommended 60°C min⁻¹ or long isothermal hold at the maximal processing temperature 920°C can cause crystallization of lithium metasilicate and cristobalite instead of lithium disilicate as major phase. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Religiousness, Spirituality, and Salivary Cortisol in Breast Cancer Survivorship: A Pilot Study.

PubMed

Hulett, Jennifer M; Armer, Jane M; Leary, Emily; Stewart, Bob R; McDaniel, Roxanne; Smith, Kandis; Millspaugh, Rami; Millspaugh, Joshua

Psychoneuroimmunological theory suggests a physiological relationship exists between stress, psychosocial-behavioral factors, and neuroendocrine-immune outcomes; however, evidence has been limited. The primary aim of this pilot study was to determine feasibility and acceptability of a salivary cortisol self-collection protocol with a mail-back option for breast cancer survivors. A secondary aim was to examine relationships between religiousness/spirituality (R/S), perceptions of health, and diurnal salivary cortisol (DSC) as a proxy measure for neuroendocrine activity. This was an observational, cross-sectional study. Participants completed measures of R/S, perceptions of health, demographics, and DSC. The sample was composed of female breast cancer survivors (n = 41). Self-collection of DSC using a mail-back option was feasible; validity of mailed salivary cortisol biospecimens was established. Positive spiritual beliefs were the only R/S variable associated with the peak cortisol awakening response (rs = 0.34, P = .03). Poorer physical health was inversely associated with positive spiritual experiences and private religious practices. Poorer mental health was inversely associated with spiritual coping and negative spiritual experiences. Feasibility, validity, and acceptability of self-collected SDC biospecimens with an optional mail-back protocol (at moderate temperatures) were demonstrated. Positive spiritual beliefs were associated with neuroendocrine-mediated peak cortisol awakening response activity; however, additional research is recommended. Objective measures of DSC sampling that include enough collection time points to assess DSC parameters would increase the rigor of future DSC measurement. Breast cancer survivors may benefit from nursing care that includes spiritual assessment and therapeutic conversations that support positive spiritual beliefs.

Kuipers works with DSC Hardware in the U.S. Laboratory

NASA Image and Video Library

2012-01-16

ISS030-E-155917 (16 Jan. 2012) --- European Space Agency astronaut Andre Kuipers, Expedition 30 flight engineer, prepares to place Diffusion Soret Coefficient (DSC) hardware in stowage containers in the Destiny laboratory of the International Space Station.

Differentiation of brain infection from necrotic glioblastoma using combined analysis of diffusion and perfusion MRI.

PubMed

Chawla, Sanjeev; Wang, Sumei; Mohan, Suyash; Nasrallah, MacLean; Verma, Gaurav; Brem, Steven; O'Rourke, Donald M; Wolf, Ronald L; Poptani, Harish; Nabavizadeh, S Ali

2018-04-20

Accurate differentiation of brain infections from necrotic glioblastomas (GBMs) may not always be possible on morphologic MRI or on diffusion tensor imaging (DTI) and dynamic susceptibility contrast perfusion-weighted imaging (DSC-PWI) if these techniques are used independently. To investigate the combined analysis of DTI and DSC-PWI in distinguishing brain injections from necrotic GBMs. Retrospective. Fourteen patients with brain infections and 21 patients with necrotic GBMs. 3T MRI, DTI, and DSC-PWI. Parametric maps of mean diffusivity (MD), fractional anisotropy (FA), coefficient of linear (CL), and planar anisotropy (CP) and leakage corrected cerebral blood volume (CBV) were computed and coregistered with postcontrast T 1 -weighted and FLAIR images. All lesions were segmented into the central core and enhancing region. For each region, median values of MD, FA, CL, CP, relative CBV (rCBV), and top 90 th percentile of rCBV (rCBV max ) were measured. All parameters from both regions were compared between brain infections and necrotic GBMs using Mann-Whitney tests. Logistic regression analyses were performed to obtain the best model in distinguishing these two conditions. From the central core, significantly lower MD (0.90 × 10 -3  ± 0.44 × 10 -3 mm 2 /s vs. 1.66 × 10 -3  ± 0.62 × 10 -3 mm 2 /s, P = 0.001), significantly higher FA (0.15 ± 0.06 vs. 0.09 ± 0.03, P < 0.001), and CP (0.07 ± 0.03 vs. 0.04 ± 0.02, P = 0.009) were observed in brain infections compared to those in necrotic GBMs. Additionally, from the contrast-enhancing region, significantly lower rCBV (1.91 ± 0.95 vs. 2.76 ± 1.24, P = 0.031) and rCBV max (3.46 ± 1.41 vs. 5.89 ± 2.06, P = 0.001) were observed from infective lesions compared to necrotic GBMs. FA from the central core and rCBV max from enhancing region provided the best classification model in distinguishing brain infections from necrotic GBMs, with a sensitivity of 91% and a specificity of 93%. Combined analysis of DTI and DSC-PWI may provide better performance in differentiating brain infections from necrotic GBMs. 1 Technical Efficacy: Stage 2 J. Magn. Reson. Imaging 2018. © 2018 International Society for Magnetic Resonance in Medicine.

Fire-retardant decorative inks for aircraft interiors

NASA Technical Reports Server (NTRS)

Kourtides, D. A.; Nir, Z.; Mikroyannidis, J. A.

1985-01-01

Commercial and experimental fire retardants were screened as potential fire retardants for acrylic printing inks used on aircraft interior sandwich panels. The fire retardants are selected according to their physical properties and their thermostabilities. A criterion for selecting a more stable fire retardant is established. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) are used to determine thermostabilities. Results show that the fire retardant formulations are more thermally stable than the acrylic ink control. It is determined that an ink formulation containing a brominated phenol and carboxy-terminated butadiene acrylonitrile which has been modified with a brominated polymeric additive (BPA), yields the highest limiting oxygen index (LOI) of all the compounds tested. All of the fire-retardant formulations have a higher oxygen index than the baseline acrylic ink.

Morphological and thermal studies of chitin-curcumin blends derived polyurethanes.

PubMed

Mahmood, Kashif; Zia, Khalid Mahmood; Zuber, Mohammad; Tabasum, Shazia; Rehman, Saima; Zia, Fatima; Noreen, Aqdas

2017-12-01

The present study describes a novel ecofriendly series of chitin/curcumin/1,4-butane diol (BDO) blend derived polyurethanes (PUs), using hydroxy terminated polybutadiene (HTPB) and hexamethylene diisocyanate (HDI) along with different mole ratio of chitin, curcumin and BDO. The structural and morphological elucidation of the prepared films was done by FTIR and SEM techniques. The swelling behavior of the films was analyzed in both water and DMSO, which showed that incorporation of chitin increases the hydrophobicity and decreases the rate of swelling. Thermal analysis of synthesized PU blends revealed better thermal stability with following mole ratio 1:0.5:0.5 of chitin: curcumin: BDO as determined by TGA and DSC techniques. Copyright © 2017 Elsevier B.V. All rights reserved.

Investigation on Thermal Properties of Kenaf Fibre Reinforced Polyurethane Bio-Composites

NASA Astrophysics Data System (ADS)

Athmalingam, Mathan; Vicki, W. V.

2018-01-01

This research focuses on the effect of Kenaf fibre on thermal properties of Polyurethane (PU) reinforced kenaf bio-composites. The samples were prepared using the polymer casting method with different percentages of kenaf fibre content (5 wt%, 10 wt%, 15 wt%). The thermal properties of Kenaf/PU bio-composite are determined through the Thermogravimetric Analysis and Differential Scanning Calorimeter test. The TGA results revealed that 10 wt% Kenaf/PU bio-composite appeared to be more stable. DSC results show that the glass transition temperature (Tg) value of 10 wt% Kenaf/PU composite is significant to pure polyurethane. It can be said that the thermal stability of 10 wt% Kenaf/PU bio-composite exhibits higher thermal stability compared to other samples.

Thermally Switchable Thin Films of an ABC Triblock Copolymer of Poly(n-butyl methacrylate)-poly(methyl methacrylate)-poly(2-fluoroethyl methacrylate)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Shanju; Liu, Zhan; Bucknall, David G.

2011-01-01

The thermo-responsive behavior of polymer films consisting of novel linear triblock copolymers of poly(n-butyl methacrylate)-poly(methyl methacrylate)-poly(2-fluoroethyl methacrylate) (PnBuMA-PMMA-P2FEMA) are reported using differential scanning calorimetry (DSC), atomic forcing microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and contacting angle (CA) measurements. The surface morphology, wettability and chemical structure of thin films of these triblock copolymers on silicon wafers as a function of temperature have been investigated. It has been shown that the wettability of the films is thermally switchable. Detailed structural analysis shows that thermo-responsive surface composition changes are produced. The underlying mechanism of the thermoresponsive behavior is discussed.

Effects of the annealing temperature and time on the microstructural evolution and corresponding the mechanical properties of cold-drawn steel wires

NASA Astrophysics Data System (ADS)

Park, D. B.; Lee, J. W.; Lee, Y. S.; Park, K. T.; Nam, W. J.

2008-02-01

The effects of the annealing temperature and annealing time on the microstructural evolution and corresponding mechanical properties of cold-drawn high carbon steel wires were investigated. During the annealing of cold-drawn steel wires, the increment of the tensile strength at low temperatures found to be due to age hardening, while the decrease in the tensile strength at high temperatures was attributed to age softening, involving the spheroidization of lamellar cementite and recovery of lamellar ferrite. To investigate the mechanisms of strain ageing, a thermal analysis using DSC was performed. The mechanisms for the first and second stages were found to be the diffusion of carbon atoms to dislocations in the lamellar ferrite and the decomposition of lamellar cementite. The third peak of the DSC curves was controlled by the re-precipitation of cementite or by the spheroidization of lamellar cementite.

Adaptive dynamic surface control of flexible-joint robots using self-recurrent wavelet neural networks.

PubMed

Yoo, Sung Jin; Park, Jin Bae; Choi, Yoon Ho

2006-12-01

A new method for the robust control of flexible-joint (FJ) robots with model uncertainties in both robot dynamics and actuator dynamics is proposed. The proposed control system is a combination of the adaptive dynamic surface control (DSC) technique and the self-recurrent wavelet neural network (SRWNN). The adaptive DSC technique provides the ability to overcome the "explosion of complexity" problem in backstepping controllers. The SRWNNs are used to observe the arbitrary model uncertainties of FJ robots, and all their weights are trained online. From the Lyapunov stability analysis, their adaptation laws are induced, and the uniformly ultimately boundedness of all signals in a closed-loop adaptive system is proved. Finally, simulation results for a three-link FJ robot are utilized to validate the good position tracking performance and robustness against payload uncertainties and external disturbances of the proposed control system.

Tunable Thermosetting Epoxies Based on Fractionated and Well-Characterized Lignins.

PubMed

Gioia, Claudio; Lo Re, Giada; Lawoko, Martin; Berglund, Lars

2018-03-21

Here we report the synthesis of thermosetting resins from low molar mass Kraft lignin fractions of high functionality, refined by solvent extraction. Such fractions were fully characterized by 31 P NMR, 2D-HSQC NMR, SEC, and DSC in order to obtain a detailed description of the structures. Reactive oxirane moieties were introduced on the lignin backbone under mild reaction conditions and quantified by simple 1 H NMR analysis. The modified fractions were chemically cross-linked with a flexible polyether diamine ( M n ≈ 2000), in order to obtain epoxy thermosets. Epoxies from different lignin fractions, studied by DSC, DMA, tensile tests, and SEM, demonstrated substantial differences in terms of thermo-mechanical properties. For the first time, strong relationships between lignin structures and epoxy properties could be demonstrated. The suggested approach provides unprecedented possibilities to tune network structure and properties of thermosets based on real lignin fractions, rather than model compounds.

Kinetics of thermolysis of lanthanum nitrate with hexamethylenetetramine: Crystal structure, TG-DSC, impact and friction sensitivity studies, Part-96

NASA Astrophysics Data System (ADS)

Nibha; Baranwal, B. P.; Singh, Gurdip; Singh, C. P.; Daniliuc, Constantin G.; Soni, P. K.; Nath, Yogeshwar

2014-11-01

The development of high energetic materials includes process ability and the ability to attain insensitive munitions (IM). This paper investigates the preparation of lanthanum metal nitrate complex of hexamethylenetetramine in water at room temperature. This complex of molecular formulae [La (NO3)2(H2O)6] (2HMTA) (NO3-) (H2O) was characterized by X-ray crystallography. Thermal decomposition was investigated using TG, TG-DSC and ignition delay measurements. Kinetic analysis of isothermal TG data has been investigated using model fitting methods as well as model free isoconversional methods. The sensitivity measurements towards mechanical destructive stimuli such as impact and friction were carried out and the complex was found to be insensitive. In order to identify the end product of thermolysis, X-ray diffraction patterns of end product was carried out which proves the formation of La2O3.

Effect of Injection Molding Melt Temperatures on PLGA Craniofacial Plate Properties during In Vitro Degradation.

PubMed

de Melo, Liliane Pimenta; Salmoria, Gean Vitor; Fancello, Eduardo Alberto; Roesler, Carlos Rodrigo de Mello

2017-01-01

The purpose of this article is to present mechanical and physicochemical properties during in vitro degradation of PLGA material as craniofacial plates based on different values of injection molded temperatures. Injection molded plates were submitted to in vitro degradation in a thermostat bath at 37 ± 1°C by 16 weeks. The material was removed after 15, 30, 60, and 120 days; then bending stiffness, crystallinity, molecular weights, and viscoelasticity were studied. A significant decrease of molecular weight and mechanical properties over time and a difference in FT-IR after 60 days showed faster degradation of the material in the geometry studied. DSC analysis confirmed that the crystallization occurred, especially in higher melt temperature condition. DMA analysis suggests a greater contribution of the viscous component of higher temperature than lower temperature in thermomechanical behavior. The results suggest that physical-mechanical properties of PLGA plates among degradation differ per injection molding temperatures.

Gamma (γ) irradiated and non-irradiated poly (L-lactide) carboxymethyl starch composite film

NASA Astrophysics Data System (ADS)

Yusof, Mohd Reusmaazran; Shamsudin, Roslinda; Abdullah, Yusof; Yaacob, Norzita

2018-04-01

A film of poly (L-lactide)(PLLA) and carboxymethyl starch (CMS) is prepared by casting evaporation method. The use of CMS blended with PLLA induces the porous film that is potentially used in tissue engineering applications. PLLA is blended with CMS in solution form and rolled on glass to produce a film. The film is then irradiated with gamma-ray (γ) at 10 and 80 kGy. FTIR analysis indicates weak interaction between PLLA and CMS at 10 kGy. Degradation and crosslinking are predicted to have occurred simultaneously at 10 kGy and massive degradation at 80 kGy as indicated in differential scanning calorimetry (DSC) curves. Mechanical analysis shows a higher strength at 10 kGy indicating that crosslinking has occured whereas degradation takes place at higher doses as shown in the reduction of mechanical strength for both PLLA and PLLA/CMS.

Crystal structure and vibrational spectra of melaminium arsenate

NASA Astrophysics Data System (ADS)

Anbalagan, G.; Marchewka, M. K.; Pawlus, K.; Kanagathara, N.

2015-01-01

The crystals of the new melaminium arsenate (MAS) [C3H7N6+ṡH2AsO4-] were obtained by the slow evaporation of an aqueous solution at room temperature. Single crystal X-ray diffraction analysis reveals that the crystal belongs to triclinic system with centro symmetric space group P-1. The crystals are built up from single protonated melaminium residues and single dissociated arsenate H2AsO4- anions. The protonated melaminium ring is almost planar. A combination of ionic and donor-acceptor hydrogen-bond interactions linking together the melaminium and arsenate residues forms a three-dimensional network. Vibrational spectroscopic analysis is reported on the basis of FT-IR and FT-Raman spectra recorded at room temperature. Hydrogen bonded network present in the crystal gives notable vibrational effect. DSC has also been performed for the crystal shows no phase transition in the studied temperature range (113-293 K).

[Effect of crystallization temperature of palm oil on its crystallization. IV. The influence of tripalmitoylglycerol (PPP) on the crystallization of 1,3-dipalmitoyl-2-oleoyl-glycerol (POP) and 1,2-dioleoyl-3-palmitoyl-glycerol (POO)].

PubMed

Mihara, Hiroaki; Ishiguro, Takashi; Fukano, Hidenori; Taniuchi, Shigeyuki; Ogino, Keizo

2007-01-01

Triacylglycerin in Palm Oil contains POP (1,3-dipalmitoyl-2-oleoyl-glycerol) at 30%, POO (1,2-dioleoyl-3-palmitoyl-glycerol) at 20% and PPP (tripalmitoylglycerol) at 5%. The crystallization temperature of PPP is high and the rates of crystal nuclear formation and growth are fast. It is thus considered that PPP may have some effect on the manner or mode of Palm Oil. Examination was thus made to clarify how PPP may affect the crystallization of POP and POO by differential scanning calorimetry (DSC) and X ray diffractometry (XRD) conducted on PPP/POP and PPP/POO mixtures. High and low temperature peaks were noted to appear on the DSC crystallization curve for either of these mixtures. The high temperature peak was considered possibly due to PPP, and the low temperature peak, to POP or POO. DSC isothermal analysis indicated the rate of crystal growth of either mixture to exceed that of pure of POP or POO. Crystal mixture structure was also seen to be complicated than either compound in pure form. The present findings thus clearly indicate that clarification should be made of the effects of high melting point triacylglycerin, such as PPP, on the crystallization of Palm Oil.

Reversing and nonreversing heat capacity of poly(lactic acid) in the glass transition region by TMDSC

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pyda, Marek; Wunderlich, Bernhard

2005-11-01

A study of the glass transition of an amorphous and a semicrystalline poly(lactic acid) (PLA) is performed with adiabatic calorimetry, differential scanning calorimetry (DSC), and temperature-modulated DSC (TMDSC). The reversing, total, and nonreversing apparent heat capacities of samples with different contents of L- and D-lactic acid and with various thermal histories were evaluated. Different modes of TMDSC analyses of amorphous and semicrystalline PLA were compared to the total heat capacity from standard DSC. The enthalpy relaxation and the cold crystallization in the glass transition region are largely irreversible. The melting is largely irreversible, but a 100% reversing fraction is observedmore » at low temperatures from 375 to 420 K, which becomes small inside the major melting peak at about 440 K. From the TMDSC of amorphous PLA, the combined information on endothermic and exothermic enthalpy relaxation and glass transition were deconvoluted into the reversing and nonreversing components. The glass transition temperature from the reversing heat capacity and the enthalpy relaxation peaks from the nonreversing component shift to higher temperature for increasingly annealed PLA. The relaxation times for aging decrease on cooling until the glass transition is reached and then increase. This behavior is linked to cooperativity. All quantitative thermal analyses are based on the heat capacity of the solid and liquid, evaluated earlier with the advanced thermal analysis system (ATHAS).« less

Segregation of Visual Response Properties in the Mouse Superior Colliculus and Their Modulation during Locomotion

PubMed Central

2017-01-01

The superior colliculus (SC) receives direct input from the retina and integrates it with information about sound, touch, and state of the animal that is relayed from other parts of the brain to initiate specific behavioral outcomes. The superficial SC layers (sSC) contain cells that respond to visual stimuli, whereas the deep SC layers (dSC) contain cells that also respond to auditory and somatosensory stimuli. Here, we used a large-scale silicon probe recording system to examine the visual response properties of SC cells of head-fixed and alert male mice. We found cells with diverse response properties including: (1) orientation/direction-selective (OS/DS) cells with a firing rate that is suppressed by drifting sinusoidal gratings (negative OS/DS cells); (2) suppressed-by-contrast cells; (3) cells with complex-like spatial summation nonlinearity; and (4) cells with Y-like spatial summation nonlinearity. We also found specific response properties that are enriched in different depths of the SC. The sSC is enriched with cells with small RFs, high evoked firing rates (FRs), and sustained temporal responses, whereas the dSC is enriched with the negative OS/DS cells and with cells with large RFs, low evoked FRs, and transient temporal responses. Locomotion modulates the activity of the SC cells both additively and multiplicatively and changes the preferred spatial frequency of some SC cells. These results provide the first description of the negative OS/DS cells and demonstrate that the SC segregates cells with different response properties and that the behavioral state of a mouse affects SC activity. SIGNIFICANCE STATEMENT The superior colliculus (SC) receives visual input from the retina in its superficial layers (sSC) and induces eye/head-orientating movements and innate defensive responses in its deeper layers (dSC). Despite their importance, very little is known about the visual response properties of dSC neurons. Using high-density electrode recordings and novel model-based analysis, we found several novel visual response properties of the SC cells, including encoding of a cell's preferred orientation or direction by suppression of the firing rate. The sSC and the dSC are enriched with cells with different visual response properties. Locomotion modulates the cells in the SC. These findings contribute to our understanding of how the SC processes visual inputs, a critical step in comprehending visually guided behaviors. PMID:28760858

Physicochemical characterization and water vapor sorption of organic solution advanced spray-dried inhalable trehalose microparticles and nanoparticles for targeted dry powder pulmonary inhalation delivery.

PubMed

Li, Xiaojian; Mansour, Heidi M

2011-12-01

Novel advanced spray-dried inhalable trehalose microparticulate/nanoparticulate powders with low water content were successfully produced by organic solution advanced spray drying from dilute solution under various spray-drying conditions. Laser diffraction was used to determine the volumetric particle size and size distribution. Particle morphology and surface morphology was imaged and examined by scanning electron microscopy. Hot-stage microscopy was used to visualize the presence/absence of birefringency before and following particle engineering design pharmaceutical processing, as well as phase transition behavior upon heating. Water content in the solid state was quantified by Karl Fisher (KF) coulometric titration. Solid-state phase transitions and degree of molecular order were examined by differential scanning calorimetry (DSC) and powder X-ray diffraction, respectively. Scanning electron microscopy showed a correlation between particle morphology, surface morphology, and spray drying pump rate. All advanced spray-dried microparticulate/nanoparticulate trehalose powders were in the respirable size range and exhibited a unimodal distribution. All spray-dried powders had very low water content, as quantified by KF. The absence of crystallinity in spray-dried particles was reflected in the powder X-ray diffractograms and confirmed by thermal analysis. DSC thermal analysis indicated that the novel advanced spray-dried inhalable trehalose microparticles and nanoparticles exhibited a clear glass transition (T(g)). This is consistent with the formation of the amorphous glassy state. Spray-dried amorphous glassy trehalose inhalable microparticles and nanoparticles exhibited vapor-induced (lyotropic) phase transitions with varying levels of relative humidity as measured by gravimetric vapor sorption at 25°C and 37°C.

Electron-Beam Irradiation Effect on Thermal and Mechanical Properties of Nylon-6 Nanocomposite Fibers Infused with Diamond and Diamond Coated Carbon Nanotubes

NASA Astrophysics Data System (ADS)

Imam, Muhammad A.; Jeelani, Shaik; Rangari, Vijaya K.; Gome, Michelle G.; Moura, Esperidiana. A. B.

2016-02-01

Nylon-6 is an engineering plastic with excellent properties and processability, which are essential in several industrial applications. The addition of filler such as diamond (DN) and diamond coated carbon nanotubes (CNTs) to form molded composites may increase the range of Nylon-6 applications due to the resulting increase in strength. The effects of electron-beam irradiation on these thermoplastic nanocomposites are either increase in the cross-linking or causes chain scission. In this study, DN-coated CNTs were synthesized using the sonochemical technique in the presence of cationic surfactant cetyltrimethyl ammonium bromide (CTAB). The DN-coated CNTs nanoparticles and diamond nanoparticles were then introduced into Nylon-6 polymer through a melt extrusion process to form nanocomposite fibers. They were further tested for their mechanical (Tensile) and thermal properties (thermogravimetric analysis (TGA), differential scanning calorimetry (DSC)). These composites were further exposed to the electron-beam (160kGy, 132kGy and 99kGy) irradiation using a 1.5MeV electron-beam accelerator, at room temperature, in the presence of air and tested for their thermal and mechanical properties. The best ultimate tensile strength was found to be 690MPa and 864MPa irradiated at 132 for DN/CNTs/Nylon-6 and Diamond/Nylon-6 nanocomposite fiber as compared to 346MPa and 321MPa for DN/CNTs/Nylon-6 and Diamond/Nylon-6 nanocomposite fiber without irradiation. The neat Nylon-6 tensile strength was 240MPa. These results are consistent with the activation energy calculated from TGA graphs. DSC analysis result shows that the slight increase in glass transition temperature (Tg) and decrease in melting temperature (Tm) which was expected from high electron-beam radiation dose.

Influence of Network Structure on Glass Transition Temperature of Elastomers

PubMed Central

Bandzierz, Katarzyna; Reuvekamp, Louis; Dryzek, Jerzy; Dierkes, Wilma; Blume, Anke; Bielinski, Dariusz

2016-01-01

It is generally believed that only intermolecular, elastically-effective crosslinks influence elastomer properties. The role of the intramolecular modifications of the polymer chains is marginalized. The aim of our study was the characterization of the structural parameters of cured elastomers, and determination of their influence on the behavior of the polymer network. For this purpose, styrene-butadiene rubbers (SBR), cured with various curatives, such as DCP, TMTD, TBzTD, Vulcuren®, DPG/S8, CBS/S8, MBTS/S8 and ZDT/S8, were investigated. In every series of samples a broad range of crosslink density was obtained, in addition to diverse crosslink structures, as determined by equilibrium swelling and thiol-amine analysis. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) were used to study the glass transition process, and positron annihilation lifetime spectroscopy (PALS) to investigate the size of the free volumes. For all samples, the values of the glass transition temperature (Tg) increased with a rise in crosslink density. At the same time, the free volume size proportionally decreased. The changes in Tg and free volume size show significant differences between the series crosslinked with various curatives. These variations are explained on the basis of the curatives’ structure effect. Furthermore, basic structure-property relationships are provided. They enable the prediction of the effect of curatives on the structural parameters of the network, and some of the resulting properties. It is proved that the applied techniques—DSC, DMA, and PALS—can serve to provide information about the modifications to the polymer chains. Moreover, on the basis of the obtained results and considering the diversified curatives available nowadays, the usability of “part per hundred rubber” (phr) unit is questioned. PMID:28773731

Selected Physical Properties of 2-Chloroethyl-3-Chloropropyl Sulfide (CECPRS)

DTIC Science & Technology

2010-10-01

Analysis * For this work, a TA Instruments 910 Differential Scanning Calorimeter and 2200 Controller were used. Prior to sample measurements, the DSC...controlled mass flow rate over a known time, concentrated, and the mass quantified by GC-FID analysis . This step enables vapor pressure measurements for low...Bellefonte, PA), with a 1.0 (im RTx-1 ( polydimethylsiloxane ) stationary phase, was maintained at 40 °C for 2 min following sample introduction, then heated

An investigation of indomethacin-nicotinamide cocrystal formation induced by thermal stress in the solid or liquid state.

PubMed

Lin, Hong-Liang; Zhang, Gang-Chun; Huang, Yu-Ting; Lin, Shan-Yang

2014-08-01

The impact of thermal stress on indomethacin (IMC)-nicotinamide (NIC) cocrystal formation with or without neat cogrinding was investigated using differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) microspectroscopy, and simultaneous DSC-FTIR microspectroscopy in the solid or liquid state. Different evaporation methods for preparing IMC-NIC cocrystals were also compared. The results indicated that even after cogrinding for 40 min, the FTIR spectra for all IMC-NIC ground mixtures were superimposable on the FTIR spectra of IMC and NIC components, suggesting there was no cocrystal formation between IMC and NIC after cogrinding. However, these IMC-NIC ground mixtures appear to easily undergo cocrystal formation after the application of DSC determination. Under thermal stress induced by DSC, the amount of cocrystal formation increased with increasing cogrinding time. Moreover, simultaneous DSC-FTIR microspectroscopy was a useful one-step technique to induce and clarify the thermal-induced stepwise mechanism of IMC-NIC cocrystal formation from the ground mixture in real time. Different solvent evaporation rates induced by thermal stress significantly influenced IMC-NIC cocrystal formation in the liquid state. In particular, microwave heating may promote IMC-NIC cocrystal formation in a short time. © 2014 Wiley Periodicals, Inc. and the American Pharmacists Association.

Preparation of UV-protective kefiran/nano-ZnO nanocomposites: physical and mechanical properties.

PubMed

Shahabi-Ghahfarrokhi, Iman; Khodaiyan, Faramarz; Mousavi, Mohammad; Yousefi, Hossein

2015-01-01

In this study, we investigated the effect of ZnO nanoparticles (ZN) as a UV-protective agent of kefiran biopolymers. Our results showed that with increasing ZN content, the tensile strength, elongation at break, and tensile energy to break the kefiran film and nanocomposites also increased. Kefiran nanocomposites with a ZN content higher than 2% produced a UV-protective film with good visual properties, low sensibility to water, and low water-vapor permeability. The thermal properties of all specimens, analyzed by DSC, showed that the ZN content had a negative effect on Tg and a positive effect on nanocomposites' melting point. TEM, SEM micrography and XRD spectrum analysis confirmed the hypothesis that ZNs act like a ball bearing, making movement of kefiran chains easier and increasing elongation at break, while simultaneously decreasing the Tg of kefiran nanocomposites. Copyright © 2014 Elsevier B.V. All rights reserved.

Physicochemical and mechanical properties of paracetamol cocrystal with 5-nitroisophthalic acid.

PubMed

Hiendrawan, Stevanus; Veriansyah, Bambang; Widjojokusumo, Edward; Soewandhi, Sundani Nurono; Wikarsa, Saleh; Tjandrawinata, Raymond R

2016-01-30

We report novel pharmaceutical cocrystal of a popular antipyretic drug paracetamol (PCA) with coformer 5-nitroisophhthalic acid (5NIP) to improve its tabletability. The cocrystal (PCA-5NIP at molar ratio of 1:1) was synthesized by solvent evaporation technique using methanol as solvent. The physicochemical properties of cocrystal were characterized by powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), thermogravimetry analysis (TGA), fourier transform infrared spectroscopy (FTIR), hot stage polarized microscopy (HSPM) and scanning electron microscopy (SEM). Stability of the cocrystal was assessed by storing them at 40°C/75% RH for one month. Compared to PCA, the cocrystal displayed superior tableting performance. PCA-5NIP cocrystal showed a similar dissolution profile as compared to PCA and exhibited good stability. This study showed the utility of PCA-5NIP cocrystal for improving mechanical properties of PCA. Copyright © 2015 Elsevier B.V. All rights reserved.

The intracellular region of ClC-3 chloride channel is in a partially folded state and a monomer.

PubMed

Li, Shu Jie; Kawazaki, Masanobu; Ogasahara, Kyoko; Nakagawa, Atsushi

2006-05-01

In contrast to bacterial ClC chloride channels, all eukaryotic ClC chloride channels have a conserved long intracellular region that makes up of the carboxyl terminus of the protein and is necessary for channel functions as a channel gate. Little is known, however, about the molecular structure of the intracellular region of ClC chloride channels so far. Here, for the first time, we have expressed and purified the intracellular region of the rat ClC-3 chloride channel (C-ClC-3) as a water-soluble protein under physiological conditions, and investigated its structural characteristics and assembly behavior by means of circular dichroism (CD) spectroscopy, differential scanning calorimetry (DSC), size exclusion chromatography and analytical ultracentrifugation. The far-UV CD spectra of C-ClC-3 in the native state and in the presence of urea clearly show that the protein has a significantly folded secondary structure consisting of alpha-helices and beta-sheets, while the near-UV CD spectra and DSC experiments indicate the protein is deficient in well-defined tertiary packing. Its Stokes radius is larger than its expected size as a folded globular protein, as determined on size exclusion chromatography. Furthermore, the DisEMBL program, a useful computational tool for the prediction of disordered/unstructured regions within a protein sequence, predicts that the protein is in a partially folded state. Based on these results, we conclude that C-ClC-3 is partially folded. On the other hand, both size exclusion chromatography and sedimentation equilibrium analysis show that C-ClC-3 exists as a monomer in solution, not a dimer like the whole ClC-3 molecule.

Physicochemical, morphological and rheological properties of canned bean pastes "negro Queretaro" variety (Phaseolus vulgaris L.).

PubMed

Martínez-Preciado, A H; Estrada-Girón, Y; González-Álvarez, A; Fernández, V V A; Macías, E R; Soltero, J F A

2014-09-01

Proximate, thermal, morphological and rheological properties of canned "negro Querétaro" bean pastes, as a function of fat content (0, 2 and 3 %) and temperature (60, 70 and 85 °C), were evaluated. Raw and precooked bean pastes were characterized by scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). Well-defined starch granules in the raw bean pastes were observed, whereas a gelatinized starch paste was observed for the canned bean pastes. The DSC analysis showed that the raw bean pastes had lower onset peak temperatures (79 °C, 79.1 °C) and gelatinization enthalpy (1.940 J/g), compared to that precooked bean pastes (70.4 °C, 75.7 °C and 1.314 J/g, respectively) thermal characteristics. Moreover, the dynamic rheological results showed a gel-like behavior for the canned bean pastes, where the storage modulus (G') was frequency independent and was higher than the loss modulus (G″). The non-linear rheological results exhibited a shear-thinning flow behavior, where the steady shear-viscosity was temperature and fat content dependent. For canned bean pastes, the shear-viscosity data followed a power law equation, where the power law index (n) decreased when the temperature and the fat content increased. The temperature effect on the shear-viscosity was described by an Arrhenius equation, where the activation energy (Ea) was in the range from 19.04 to 36.81 KJ/mol. This rheological behavior was caused by gelatinization of the starch during the cooking and sterilization processes, where starch-lipids and starch-proteins complex were formed.

An attempt to stabilize tanshinone IIA solid dispersion by the use of ternary systems with nano-CaCO3 and poloxamer 188.

PubMed

Yan, Hong-Mei; Zhang, Zhen-Hai; Jiang, Yan-Rong; Ding, Dong-Mei; Sun, E; Jia, Xiao-Bin

2014-04-01

Tanshinone IIA (TSIIA) on solid dispersions (SDs) has thermodynamical instability of amorphous drug. Ternary solid dispersions (tSDs) can extend the stability of the amorphous form of drug. Poloxamer 188 was used as a SD carrier. Nano-CaCO3 played an important role in adsorption of biomolecules and is being developed for a host of biotechnological applications. The aim of the present study was to investigate the dissolution behavior and accelerated stability of TSIIA on solid dispersions (SDs) by the use of ternary systems with nano-CaCO3 and poloxamer 188. The TSIIA tSDs were prepared by a spray-drying method. First, the effect of combination of poloxamer 188 and nano-CaCO3 on TSIIA dissolution was studied. Subsequently, a set of complementary techniques (DSC, XRPD, SEM and FTIR) was used to monitor the physical changes of TSIIA in the SDs. Finally, stability test was carried out under the conditions 40°C/75% RH for 6 months. The characterization of tSDs by differential scanning calorimetry analysis (DSC) and X-ray powder diffraction (XRPD) showed that TSIIA was present in its amorphous form. Fourier transforms infrared spectroscopy (FTIR) suggested the presence of interactions between TSIIA and carriers in tSDs. Improvement in the dissolution rate was observed for all SDs. The stability study conducted on SDs with nano-CaCO3 showed stable drug content and dissolution behavior, over the period of 6 months as compared with freshly prepared SDs. SDs preparation with nano-CaCO3 and poloxamer 188 may be a promising approach to enhance the dissolution and stability of TSIIA.

Improvement of the dissolution rate of artemisinin by means of supercritical fluid technology and solid dispersions.

PubMed

Van Nijlen, T; Brennan, K; Van den Mooter, G; Blaton, N; Kinget, R; Augustijns, P

2003-03-26

The purpose of this study was to enhance the dissolution rate of artemisinin in order to improve the intestinal absorption characteristics. The effect of: (1) micronisation and (2) formation of solid dispersions with PVPK25 was assessed in an in vitro dissolution system [dissolution medium: water (90%), ethanol (10%) and sodium lauryl sulphate (0.1%)]. Coulter counter analysis was used to measure particle size. X-ray diffraction and DSC were used to analyse the physical state of the powders. Micronisation by means of a jet mill and supercritical fluid technology resulted in a significant decrease in particle size as compared to untreated artemisinin. All powders appeared to be crystalline. The dissolution rate of the micronised forms improved in comparison to the untreated form, but showed no difference in comparison to mechanically ground artemisinin. Solid dispersions of artemisinin with PVPK25 as a carrier were prepared by the solvent method. Both X-ray diffraction and DSC showed that the amorphous state was reached when the amount of PVPK25 was increased to 67%. The dissolution rate of solid dispersions with at least 67% of PVPK25 was significantly improved in comparison to untreated and mechanically ground artemisinin. Modulation of the dissolution rate of artemisinin was obtained by both particle size reduction and formation of solid dispersions. The effect of particle size reduction on the dissolution rate was limited. Solid dispersions could be prepared by using a relatively small amount of PVPK25. The formation of solid dispersions with PVPK25 as a carrier appears to be a promising method to improve the intestinal absorption characteristics of artemisinin. Copyright 2003 Elsevier Science B.V.

Valorization of titanium metal wastes as tanning agent used in leather industry.

PubMed

Crudu, Marian; Deselnicu, Viorica; Deselnicu, Dana Corina; Albu, Luminita

2014-10-01

The development of new tanning agents and new technologies in the leather sector is required to cope with the increasingly higher environmental pressure on the current tanning materials and processes such as tanning with chromium salts. In this paper, the use of titanium wastes (cuttings) resulting from the process of obtaining highly pure titanium (ingots), for the synthesis of new tanning agent and tanning bovine hides with new tanning agent, as alternative to tanning with chromium salts are investigated. For this purpose, Ti waste and Ti-based tanning agent were characterized for metal content by inductively coupled plasma mass spectrometry (ICP-MS) and chemical analysis; the tanned leather (wet white leather) was characterized by Scanning Electron Microscope/Energy Dispersive Using X-ray (Analysis). SEM/EDX analysis for metal content; Differential scanning calorimetric (DSC), Micro-Hot-Table and standard shrinkage temperature showing a hydrothermal stability (ranged from 75.3 to 77°C) and chemical analysis showing the leather is tanned and can be processed through the subsequent mechanical operations (splitting, shaving). On the other hand, an analysis of major minor trace substances from Ti-end waste (especially vanadium content) in new tanning agent and wet white leather (not detected) and residue stream was performed and showed that leachability of vanadium is acceptable. The results obtained show that new tanning agent obtained from Ti end waste can be used for tanning bovine hides, as eco-friendly alternative for chrome tanning. Copyright © 2014 Elsevier Ltd. All rights reserved.

SHI induced modification in structural, optical, dielectric and thermal properties of poly ethylene oxide films

NASA Astrophysics Data System (ADS)

Patel, Gnansagar B.; Bhavsar, Shilpa; Singh, N. L.; Singh, F.; Kulriya, P. K.

2016-07-01

Poly ethylene oxide (PEO) films were synthesized by solution cast method. These self-standing films were exposed with 60 MeV C+5 ion and 100 MeV Ni+7 ion at different fluences. SHI induced effect was investigated by employing various techniques. The crystalline size decreased upon irradiation as observed from XRD analysis. FTIR analysis reveals the decrement in the peak intensity upon irradiation. Tauc's method was used to determine the optical band gap (Eg), which shows decreasing trends with increase of fluence. The dielectric properties were investigated in the frequency range 10 Hz to 10 MHz for unirradiated and irradiated films. The dielectric constant remains same for the broad-spectrum of frequency and increases at lower frequency. The dielectric loss also moderately influence as a function of frequency due to irradiation. DSC analysis validated the results of XRD. Scanning electron microscopy (SEM) reveals that there is significant change in the surface morphology due to irradiation.

Microwave irradiation induced modifications on the interfaces in SAN/EVA/PVC and PVAc/BPA/PVP ternary polymer blends: Positron lifetime study

NASA Astrophysics Data System (ADS)

Dinesh, Meghala; Chikkakuntappa, Ranganathaiah

2013-09-01

Ternary polymer blends of poly(styrene-co-acrylonitrile)/poly(ethylene-co-vinylacetate)/poly(vinyl chloride) (SAN/EVA/PVC) and poly(vinyl acetate)/bisphenol A/polyvinylpyrrolidone (PVAc/BPA/PVP) with different compositions have been prepared by solvent casting method and characterized by positron lifetime spectroscopy and differential scanning calorimetry DSC. Phase modifications have been induced by irradiating the blends with microwave radiation. These changes have been monitored by measuring the free-volume content in the blends. The results clearly show improved interactions between the constituent polymers of the blends upon microwave irradiation. However, the free-volume data and DSC measurements are found to be inadequate to reveal the changes at the interfaces and the interfaces determine the final properties of the blend. For this we have used hydrodynamic interaction (αij) approach developed by us to measure strength of hydrodynamic interaction at the interfaces. These results show that microwave irradiation stabilizes the interfaces if the blend contains strong polar groups. SAN/EVA/PVC blend shows an increased effective hydrodynamic interaction from -3.18 to -4.85 at composition 50/35/15 upon microwave irradiation and PVAc/BPA/PVP blend shows an increased effective hydrodynamic interaction from -3.81 to -7.57 at composition 20/50/30 after irradiation.

7 CFR 1717.850 - General.

Code of Federal Regulations, 2011 CFR

2011-01-01

... Earned Ratio (TIER), Debt Service Coverage (DSC), and other case-specific economic and financial factors; (ii) The variability and uncertainty of future revenues, costs, margins, TIER, DSC, and other case... construction work orders and other records, all moneys disbursed from the separate subaccount during the period...

An epoxy monomer derived from Tung oil fatty acids and its products cured by two synergistic reactions

USDA-ARS?s Scientific Manuscript database

A new bio-based epoxy monomer containing conjugated double bonds, the glycidyl ester of eleostearic acid (GEEA), was synthesized from tung oil fatty acids. It was characterized using 1H-NMR, 13C-NMR and mass spectrometric analysis. Differential scanning calorimetry (DSC) and FT-IR spectroscopy were ...

Physiochemical/Rheological Control of Nonmetallic Materials.

DTIC Science & Technology

1982-08-01

CONCLUSIONS ... .. .. . .oo.. .. .. .. .. .. .. .... 23 APPENDIX A - Infrared Spectra of Nonmetallic Consumables .. ......... 24 77’. 1SN 7.. Tiii LIST OF...Spectrometer IR Infrared Spectroscopy GC Gas Chromatrography MS Mass Spectrometry * DSC Differenitial Scanning Calorimetry RT Room Temperature ET Elevated...Linear Heating Rate *FTIR Fourier Transform Infrared TGA Thermogravimetric Analysis Vi 1.0 INTRODUCTION AND SUOARY Over the past 10 years

Characterization of plasticized PEO-PAM blend polymer electrolyte system

NASA Astrophysics Data System (ADS)

Dave, Gargi; Kanchan, Dinesh

2017-05-01

Present study reports characterization studies of NaCF3SO3 based PEO-PAM Blend Polymer Electrolyte (BPE) system with varying amount of EC+PC as plasticizer prepared by solution cast technique. Structural analysis and surface topography have been performed using FTIR and SEM studies. To understand, thermal properties, DSC studies have been undertaken in the present paper

Neonatal Desensitization Supports Long-Term Survival and Functional Integration of Human Embryonic Stem Cell-Derived Mesenchymal Stem Cells in Rat Joint Cartilage Without Immunosuppression

PubMed Central

Zhang, Shufang; Jiang, Yang Zi; Zhang, Wei; Chen, Longkun; Tong, Tong; Liu, Wanlu; Mu, Qin; Liu, Hua; Ji, Junfeng; Ouyang, Hong Wei

2013-01-01

Immunological response hampers the investigation of human embryonic stem cells (hESCs) or their derivates for tissue regeneration in vivo. Immunosuppression is often used after surgery, but exhibits side effects of significant weight loss and allows only short-term observation. The purpose of this study was to investigate whether neonatal desensitization supports relative long-term survival of hESC-derived mesenchymal stem cells (hESC-MSCs) and promotes cartilage regeneration. hESC-MSCs were injected on the day of birth in rats. Six weeks after neonatal injection, a full-thickness cylindrical cartilage defect was created and transplanted with a hESC-MSC-seeded collagen bilayer scaffold (group d+s+c) or a collagen bilayer scaffold (group d+s). Rats without neonatal injection were transplanted with the hESC-MSC-seeded collagen bilayer scaffold to serve as controls (group s+c). Cartilage regeneration was evaluated by histological analysis, immunohistochemical staining, and biomechanical test. The role of hESC-MSCs in cartilage regeneration was analyzed by CD4 immunostaining, cell death detection, and visualization of human cells in regenerated tissues. hESC-MSCs expressed CD105, CD73, CD90, CD29, and CD44, but not CD45 and CD34, and possessed trilineage differentiation potential. Group d+s+c exhibited greater International Cartilage Repair Society (ICRS) scores than group d+s or group s+c. Abundant collagen type II and improved mechanical properties were detected in group d+s+c. There were less CD4+ inflammatory cell infiltration and cell death at week 1, and hESC-MSCs were found to survive as long as 8 weeks after transplantation in group d+s+c. Our study suggests that neonatal desensitization before transplantation may be an efficient way to develop a powerful tool for preclinical study of human cell-based therapies in animal models. PMID:22788986

Neonatal desensitization supports long-term survival and functional integration of human embryonic stem cell-derived mesenchymal stem cells in rat joint cartilage without immunosuppression.

PubMed

Zhang, Shufang; Jiang, Yang Zi; Zhang, Wei; Chen, Longkun; Tong, Tong; Liu, Wanlu; Mu, Qin; Liu, Hua; Ji, Junfeng; Ouyang, Hong Wei; Zou, Xiaohui

2013-01-01

Immunological response hampers the investigation of human embryonic stem cells (hESCs) or their derivates for tissue regeneration in vivo. Immunosuppression is often used after surgery, but exhibits side effects of significant weight loss and allows only short-term observation. The purpose of this study was to investigate whether neonatal desensitization supports relative long-term survival of hESC-derived mesenchymal stem cells (hESC-MSCs) and promotes cartilage regeneration. hESC-MSCs were injected on the day of birth in rats. Six weeks after neonatal injection, a full-thickness cylindrical cartilage defect was created and transplanted with a hESC-MSC-seeded collagen bilayer scaffold (group d+s+c) or a collagen bilayer scaffold (group d+s). Rats without neonatal injection were transplanted with the hESC-MSC-seeded collagen bilayer scaffold to serve as controls (group s+c). Cartilage regeneration was evaluated by histological analysis, immunohistochemical staining, and biomechanical test. The role of hESC-MSCs in cartilage regeneration was analyzed by CD4 immunostaining, cell death detection, and visualization of human cells in regenerated tissues. hESC-MSCs expressed CD105, CD73, CD90, CD29, and CD44, but not CD45 and CD34, and possessed trilineage differentiation potential. Group d+s+c exhibited greater International Cartilage Repair Society (ICRS) scores than group d+s or group s+c. Abundant collagen type II and improved mechanical properties were detected in group d+s+c. There were less CD4+ inflammatory cell infiltration and cell death at week 1, and hESC-MSCs were found to survive as long as 8 weeks after transplantation in group d+s+c. Our study suggests that neonatal desensitization before transplantation may be an efficient way to develop a powerful tool for preclinical study of human cell-based therapies in animal models.

Linking collection of stormwater runoff to managed aquifer recharge using a geographic information system and hydrologic modeling

NASA Astrophysics Data System (ADS)

Teo, E. K.; Young, K. S.; Beganskas, S.; Fisher, A. T.; Lozano, S.; Weir, W. B.; Harmon, R. E.

2016-12-01

We are completing a regional analysis of Santa Cruz and northern Monterey Counties, CA to assess conditions for using distributed stormwater collection to support managed aquifer recharge (DSC-MAR). DSC-MAR constitutes an important component in a portfolio of innovative techniques being developed in order to improve groundwater management and to adapt to prolonged drought and changes in climate and anthropogenic water demands by increasing recharge during and soon after winter precipitation events, the season when excess water is most abundant. Our analyses focus specifically on the distributed collection of stormwater runoff, a source that has historically been treated as a nuisance, with the goal of infiltrating ≥100 ac-ft/yr within individual projects. The first part of this project is a spatial analysis, using a geographic information system to combine surface and subsurface data. There is complete spatial coverage for most surface data (elevation, soil and bedrock properties, land use) for the full study region ( 1,400 km2), but subsurface data (aquifer distribution, properties, and storage space) are available for only 43% of the region. Sites that are most suitable for DSC-MAR have high soil infiltration capacity, are well-connected to an underlying aquifer with good transmissive and storage properties, and have space to receive water. Based on surface data, 35% of the region is suitable for MAR (480 km2). In contrast, 14% of the area for which both surface and subsurface datasets are available is suitable for MAR (84 km2). We have assessed the availability of hillslope runoff for collection in support of MAR using a distributed hydrologic model (PRMS) and a catalog of historical, high-resolution climate data. In the simulations, enclosed topographic basins are divided into hydrologic response units (HRUs) having an area of 25 to 250 acres (0.1 to 1 km2). Simulations of the San Lorenzo River Basin (SLRB), northern Santa Cruz County, suggest that during years of normal precipitation, 12% of the region is composed of HRUs that are both suitable for MAR and generate at least 100 acre-feet of runoff per year. These criteria are met by 5% of the SLRB in dry years and 19% in wet years. Collectively, these results suggest that the DSC-MAR approach can help to sustain groundwater resources over the long term.

Electrical, thermal and structural properties of plasticized waste cooking oil-based polyurethane solid polymer electrolyte

NASA Astrophysics Data System (ADS)

Huzaizi, Rahmatina Mohd; Tahir, Syuhada Mohd; Mahbor, Kamisah Mohamad

2017-12-01

Waste cooking oil-based polyol was synthesized using epoxidation and hydroxylation methods. The polyol was combined with 4,4-diphenylmethane diisocyanate to produce polyurethane (PU) to be used as polymer host in solid polymer electrolyte. 30 wt% LiClO4 was added as doping salt and two types of plasticizers were used; ethylene carbonate (PU-EC) and polyethylene glycol (PU-PEG). The SPE films were characterized using Fourier transform infrared spectroscopy, electrochemical impedance spectroscopy, differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The highest conductivity achieved was 8.4 x 10-8 S cm-1 upon addition of 10 wt% EC. The XRD results showed a decrease of crystalline peaks in PU-EC and the increase in PU-PEG. DSC results revealed that the films; PU, PU-EC and PU-PEG had glass transition temperatures of 159.7, 106.0 and 179.7 °C, respectively. The results showed that the addition of EC increased the amorphous region and the free volume in the SPE structure, thus resulted in higher ionic conductivity.

Preparation, characterization and in vitro evaluation of solid dispersions containing docetaxel.

PubMed

Chen, Jie; Qiu, Liyan; Hu, Minxin; Jin, Yi; Han, Jieru

2008-06-01

Solid dispersions using water-soluble carriers were studied for improving the dissolution of docetaxel, a poorly soluble compound. In order to obtain the most optimized formulation, we prepared many solid dispersions with different carriers, different solvents, or at a series of drug-to-carrier ratios, and compared their dissolution. The accumulative dissolution of docetaxel from poloxamer 188 was more excellent than that from PVP(k30) and glyceryl monostearate, and the dissolution of docetaxel from solid dispersion was markedly higher than that of pure docetaxel; meanwhile the increased dissolution was partly dependent on the ratios of docetaxel and poloxamer 188. The ethanol used to prepare solid dispersion is of more significant effect on the dissolution of docetaxel than that of acetone. The docetaxel/poloxamer 188 system was characterized by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), and environmental scanning electron microscope (ESEM). The results of DSC, XRD, and ESEM analyses of docetaxel/poloxamer 188 system showed that there are intermolecular interactions between docetaxel and poloxamer, and the crystallinity of docetaxel disappeared. These results show that solid dispersion is a promising approach of developing docetaxel drug formulates.

Compatibilizing Bulk Polymer Blends by Using Organoclays

NASA Astrophysics Data System (ADS)

Si, Mayu; Gersappe, Dilip; Zhang, Wenhua; Ade, Harald; Rafailovich, Miriam; Sokolov, Jonathan; Rudomen, Gregory; Schwartz, Bradley; Fisher, Robert

2004-03-01

We investigated the compatiblizing performance of organoclays on melt mixed binary and tertiary polymer blends, such as, PS/PMMA, PC/SAN, PS/PMMA/PVC and PS/PMMA/PE. These polymer blends were characterized by TEM, STXM, DSC and DMA. TEM and STXM photographs show that the addition of organoclays into polymer blends drastically reduces the average domain size of the component phases. And the organoclay goes to the interfacial region between the different polymers and effectively slows down the domain size increasing during high temperature annealing. DMA and DSC results show the effect of organoclays on the mechanical properties and glass transitions temperature, which indicates the compatibilization on the molecular level. The generalized compatibilization induced by the nanoscale fillers for blends can be explained in terms of mean field models where the reduction of interfacial tension induced by in-situ grafting is counterbalanced by the increased bending energy due to the rigidity of the filler. This in turn can be shown to be a function of the degree of exfoliation, aspect ratio, and polymer filler interactions. Supported by NSF funded MRSEC at Stony Brook

Learning from adaptive neural dynamic surface control of strict-feedback systems.

PubMed

Wang, Min; Wang, Cong

2015-06-01

Learning plays an essential role in autonomous control systems. However, how to achieve learning in the nonstationary environment for nonlinear systems is a challenging problem. In this paper, we present learning method for a class of n th-order strict-feedback systems by adaptive dynamic surface control (DSC) technology, which achieves the human-like ability of learning by doing and doing with learned knowledge. To achieve the learning, this paper first proposes stable adaptive DSC with auxiliary first-order filters, which ensures the boundedness of all the signals in the closed-loop system and the convergence of tracking errors in a finite time. With the help of DSC, the derivative of the filter output variable is used as the neural network (NN) input instead of traditional intermediate variables. As a result, the proposed adaptive DSC method reduces greatly the dimension of NN inputs, especially for high-order systems. After the stable DSC design, we decompose the stable closed-loop system into a series of linear time-varying perturbed subsystems. Using a recursive design, the recurrent property of NN input variables is easily verified since the complexity is overcome using DSC. Subsequently, the partial persistent excitation condition of the radial basis function NN is satisfied. By combining a state transformation, accurate approximations of the closed-loop system dynamics are recursively achieved in a local region along recurrent orbits. Then, the learning control method using the learned knowledge is proposed to achieve the closed-loop stability and the improved control performance. Simulation studies are performed to demonstrate the proposed scheme can not only reuse the learned knowledge to achieve the better control performance with the faster tracking convergence rate and the smaller tracking error but also greatly alleviate the computational burden because of reducing the number and complexity of NN input variables.

Electrical conductivity, differential scanning calorimetry, X-ray diffraction, and 7Li nuclear magnetic resonance studies of n-C x H(2 x+1)OSO3Li ( x = 12, 14, 16, 18, and 20)

NASA Astrophysics Data System (ADS)

Hirakawa, Satoru; Morimoto, Yoshiaki; Honda, Hisashi

2015-04-01

Electrical conductivity ( σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C x H (2 x+1) OSO 3Li ( x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C x H (2 x+1) OSO 3Na and n-C x H (2 x+1) OSO 3K ( x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (Δ S). For n-C 18 H 37 OSO 3Li and n-C 20 H 41 OSO 3Li salts, each melting point produced a small Δ S mp value compared with the total entropy change in the solid phases (Δ S tr1+Δ S tr2). Additionally, Li + ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. 7Li NMR spectra of n-C 18 H 37 OSO 3Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals.

Kinetics of Glass Transition and Crystallization of a Zr40Hf10Ti4Y1Al10Cu25Ni7Co2Fe1 Bulk Metallic Glass with High Mixing Entropy

NASA Astrophysics Data System (ADS)

Gong, Pan; Wang, Sibo; Li, Fangwei; Wang, Xinyun

2018-04-01

The kinetics of glass transition and crystallization of a novel Zr40Hf10Ti4Y1Al10Cu25Ni7Co2Fe1 bulk metallic glass (BMG) with high mixing entropy have been studied by differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The continuous DSC curves show five stages of crystallization at lower heating rates (≤ 20 K/min). The activation energies of glass transition were determined by Moynihan and Kissinger methods, while the activation energies of crystallization were calculated utilizing Kissinger, Ozawa, and Boswell models. The crystalline phases corresponding to each crystallization step have been found out. The kinetic fragility of Zr40Hf10Ti4Y1Al10Cu25Ni7Co2Fe1 BMG has also been evaluated. Based on the isothermal DSC curves, the Avrami exponent, evaluated from the Johnson-Mehl-Avrami equation, has been analyzed in detail. The current study reveals that the crystallization behavior of Zr40Hf10Ti4Y1Al10Cu25Ni7Co2Fe1 BMG exhibits characteristics of both the high entropy BMGs and traditional BMGs with a single principal element, leading to its high glass-forming ability.

Interfacial behaviour of sodium stearoyllactylate (SSL) as an oil-in-water pickering emulsion stabiliser.

PubMed

Kurukji, D; Pichot, R; Spyropoulos, F; Norton, I T

2013-11-01

The ability of a food ingredient, sodium stearoyllactylate (SSL), to stabilise oil-in-water (O/W) emulsions against coalescence was investigated, and closely linked to its capacity to act as a Pickering stabiliser. Results showed that emulsion stability could be achieved with a relatively low SSL concentration (≥0.1 wt%), and cryogenic-scanning electron microscopy (cryo-SEM) visualisation of emulsion structure revealed the presence of colloidal SSL aggregates adsorbed at the oil-water interface. Surface properties of SSL could be modified by altering the size of these aggregates in water; a faster decrease in surface tension was observed when SSL dispersions were subjected to high pressure homogenisation (HPH). The rate of SSL adsorption at the sunflower oil-water interface also increased after HPH, and a higher interfacial tension (IFT) was observed with increasing SSL concentration. Differential scanning calorimetry (DSC) enabled a comparison of the thermal behaviour of SSL in aqueous dispersions with SSL-stabilised O/W emulsions. SSL melting enthalpy depended on emulsion interfacial area and the corresponding DSC data was used to determine the amount of SSL adsorbed at the oil-water interface. An idealised theoretical interfacial coverage calculation based on Pickering emulsion theory was in general agreement with the mass of SSL adsorbed as predicted by DSC. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

In-situ synchrotron wide-angle X-ray diffraction as a rapid method for cocrystal/salt screening.

PubMed

Dong, Pin; Lin, Ling; Li, Yongcheng; Huang, Zhengwei; Lang, Tianqun; Wu, Chuanbin; Lu, Ming

2015-12-30

The purpose of this work was to explore in-situ synchrotron wide-angle X-ray diffraction (WAXD) as a rapid and accurate tool to screen and monitor the formation of cocrystal/salts during heating. The active pharmaceutical ingredients (caffeine, carbamazepine and lamotrigine) were respectively mixed with the coformer (saccharin), and then heated by the hot stage. Real-time process monitoring was performed using synchrotron WAXD to assess cocrystal formation and subsequently compared to differential scanning calorimetry (DSC) measurements. The effect of heating rates and cocrystal growth behavior were investigated. Synchrotron WAXD was fast and sensitive to detect cocrystal formation with the appearance of characteristic diffraction rings, even at the heating rate of 30°C/min, while DSC curves showed overlapped peaks. Unlike the indirect characterization of DSC on endo/exothermic peaks, synchrotron WAXD can directly and qualitatively determine cocrystal by diffraction peaks. The diffraction intensity-temperature curves and the corresponding first-derivative curves clearly exhibited the growth behavior of cocrystal upon heating, providing useful information to optimize the process temperature of hot melt extrusion to continuously manufacture cocrystal. The study suggests that in-situ synchrotron WAXD could provide a one-step process to screen cocrystal at high efficiency and reveal the details of cocrystal/salts growth behavior. Copyright © 2015 Elsevier B.V. All rights reserved.

Diffusion of liquid polystyrene into glassy poly(phenylene oxide) characterized by DSC

NASA Astrophysics Data System (ADS)

Li, Linling; Wang, Xiaoliang; Zhou, Dongshan; Xue, Gi

2013-03-01

We report a diffusion study on the polystyrene/poly(phenylene oxide) (PS/PPO) mixture consisted by the PS and PPO nanoparticles. Diffusion of liquid PS into glassy PPO (l-PS/g-PPO) is promoted by annealing the PS/PPO mixture at several temperatures below Tg of the PPO. By tracing the Tgs of the PS-rich domain behind the diffusion front using DSC, we get the relationships of PS weight fractions and diffusion front advances with the elapsed diffusion times at different diffusion temperatures using the Gordon-Taylor equation and core-shell model. We find that the plots of weight fraction of PS vs. elapsed diffusion times at different temperatures can be converted to a master curve by Time-Temperature superposition, and the shift factors obey the Arrhenius equation. Besides, the diffusion front advances of l-PS into g-PPO show an excellent agreement with the t1/2 scaling law at the beginning of the diffusion process, and the diffusion coefficients of different diffusion temperatures also obey the Arrhenius equation. We believe the diffusion mechanism for l-PS/g-PPO should be the Fickean law rather than the Case II, though there are departures of original linearity at longer diffusion times due to the limited liquid supply system. Diffusion of liquid polystyrene into glassy poly(phenylene oxide) characterized by DSC

On the Structure of Some Pentaerythritol-Related Molecular Crystals with Pseudotetrahedral Molecular Structure. Ordered Structure of 2,2-Bis(bromomethyl)-1,3-propanediol and Orientationally Disordered Structure of 2-Chloromethyl-2-methyl-1,3-dichloropropane; 35Cl NQR

NASA Astrophysics Data System (ADS)

Dou, Shi-qi; Fuess, Hartmut; Strauß, Roman; Weiss, Alarich

1996-06-01

C(CH2Cl)3(CH3), melting point Tm = 291.3 K, shows in the DTA/DSC experiment a phase tran-sition from an orientationally disordered plastic phase I into an ordered phase II at TI ⃗ II = 235.9 K. From 77 K up to TII ⃗ I the 35Cl NQR spectrum is a triplet with (ν in MHz, T=77 K) ν1 = 34.213, ν2 = 34.183, ν3 = 33.786. The 35Cl NQR fade-out temperature Tf = 247 K coincides with TII ⃗ I found from the DSC experiment. The plastic phase of 2-chloromethyl-2-methyl-l,3-propanediol is cubic bcc, Im3m, Z = 2 and the lattice constant increases linearly 755 pm at 235 K to 768 pm at 283 K. In the heating cycle we found (ΔH in kJ/mol): ΔHII ⃗ I = 12.0, ΔSm/R = 1.0. The compound belongs to the group of plastic molecules formed by ellipsoid like distorted tetrahedra and is derived by substitution from methane. The crystal structure of 2,2-bis(bromomethyl)-1,3-propanediol was determined. DTA-DSC show that an orientationally disordered plastic phase does not exist. At room temperature C(CH2Br)2(CH2OH)2 crystallizes monoclinic, space group Cc, Z = 4, a = 628.2 pm, 6 = 2015.5 pm, c = 659.6 pm, β = 94.27°. The molecules interact by intermolecular hydrogen bonds between the OH-groups and by van der Waals forces Br…Br.

Maternal Vaccination with a Fimbrial Tip Adhesin and Passive Protection of Neonatal Mice against Lethal Human Enterotoxigenic Escherichia coli Challenge

PubMed Central

Luiz, Wilson B.; Rodrigues, Juliana F.; Crabb, Joseph H.

2015-01-01

Globally, enterotoxigenic Escherichia coli (ETEC) is a leading cause of childhood and travelers' diarrhea, for which an effective vaccine is needed. Prevalent intestinal colonization factors (CFs) such as CFA/I fimbriae and heat-labile enterotoxin (LT) are important virulence factors and protective antigens. We tested the hypothesis that donor strand-complemented CfaE (dscCfaE), a stabilized form of the CFA/I fimbrial tip adhesin, is a protective antigen, using a lethal neonatal mouse ETEC challenge model and passive dam vaccination. For CFA/I-ETEC strain H10407, which has been extensively studied in volunteers, an inoculum of 2 × 107 bacteria resulted in 50% lethal doses (LD50) in neonatal DBA/2 mice. Vaccination of female DBA/2 mice with CFA/I fimbriae or dscCfaE, each given with a genetically attenuated LT adjuvant (LTK63) by intranasal or orogastric delivery, induced high antigen-specific serum IgG and fecal IgA titers and detectable milk IgA responses. Neonates born to and suckled by dams antenatally vaccinated with each of these four regimens showed 78 to 93% survival after a 20× LD50 challenge with H10407, compared to 100% mortality in pups from dams vaccinated with sham vaccine or LTK63 only. Crossover experiments showed that high pup survival rates after ETEC challenge were associated with suckling but not birthing from vaccinated dams, suggesting that vaccine-specific milk antibodies are protective. In corroboration, preincubation of the ETEC inoculum with antiadhesin and antifimbrial bovine colostral antibodies conferred a dose-dependent increase in pup survival after challenge. These findings indicate that the dscCfaE fimbrial tip adhesin serves as a protective passive vaccine antigen in this small animal model and merits further evaluation. PMID:26371126

Assessment of a Novel Ternary Eutectic Chloride Salt for Next Generation High-Temperature Sensible Heat Storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vidal, Judith C; Mohan, Gowtham; Venkataraman, Mahesh

A novel ternary eutectic salt mixture for high-temperature sensible heat storage, composed of sodium chloride, potassium chloride and magnesium chloride (NaKMg-Cl) was developed based on a phase diagram generated with FactSage(R). The differential scanning calorimetry (DSC) technique was used to experimentally validate the predicted melting point of the ternary eutectic composition, which was measured as 387 degrees C, in good agreement with the prediction. The ternary eutectic was compared to two binary salts formulated based on prediction of the eutectic composition by FactSage, but unfortunately DSC measurements showed that neither binary salt composition was eutectic. Nonetheless, the measured thermo-physical propertiesmore » of the ternary and the two binary mixtures are compared. Liquid heat capacities of both the ternary and binary salts were determined by using DSC with sapphire as the standard reference. The average heat capacity of the ternary mixture was recorded as 1.18 J g-1 K-1. The mass loss of the molten eutectic salts was studied up to 1000 degrees C using a thermogravimetric analyser in nitrogen, argon and air. The results showed a significant mass loss due to vaporisation in an open system, particularly above 700 degrees C. However, simulation of mass loss in a closed system with an inert cover gas indicates storage temperatures above 700 degrees C may be feasible, and highlights the importance of the design of the storage tank system. In terms of storage material cost, the NaKMg-Cl mixture is approximately 4.5 USD/kWh, which is 60% cheaper than current state-of-the-art nitrate salt mixtures.« less

Kinetics of the subtransition in dipalmitoylphosphatidylcholine.

PubMed

Tristram-Nagle, S; Wiener, M C; Yang, C P; Nagle, J F

1987-07-14

The kinetics of the interconversions of the subgel and gel phases in dipalmitoylphosphatidylcholine have been studied by using differential dilatometry, differential scanning calorimetry (DSC), and neutral buoyancy centrifugation as a function of incubation temperature and deuteriation of the solvent. As seen by others, DSC scans show two peaks in the subgel transition region for incubation temperatures below 1 degree C. After incubation at 0.1 degree C, the DSC peak that occurs at the lower scanning temperature appears with an incubation half-time of 0.5 day and eventually converts into a peak at higher scanning temperature with an incubation half-time of 18 days. By varying the scanning rate, we show that these two peaks merge into one at slow scanning rates with a common equilibrium transition temperature of 13.8 degrees C, in agreement with equilibrium calorimetry and dilatometry (delta V = 0.017 +/- 0.001 mL/g). For incubation temperatures above 4.6 degrees C, only one peak appears in both scanning dilatometry and calorimetry. While the initial rate of subgel conversion is smaller at the higher incubation temperatures, after 300 h a higher percentage of the sample has converted to subgel than at the lower incubation temperatures. We suggest that higher incubation temperatures (near 5 degrees C) are preferable for forming the stable subgel phase, and we present a colliding domain picture that indicates why this may be so. Our results in D2O and the similarity of the kinetics of volume decrease with the kinetics of wide-angle diffraction lines also support the suggestion that the partial loss of interlamellar water plays a kinetic role in subgel formation.

Microstructural, mechanical and electrochemical behaviour of a 7017 Al–Zn–Mg alloy of different tempers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rout, Prasanta Kumar, E-mail: prasantonnet55@yahoo.com; Ghosh, M.M.; Ghosh, K.S., E-mail: ksghosh2001@yahoo.co.uk

2015-06-15

The aim of the investigation is to assess the microstructural features and associated physical, mechanical and electrochemical properties of a 7017 Al–Zn–Mg alloy of various tempers. A 7017 Al–Zn–Mg alloy was subjected to different ageing schedules to produce under-(T4), peak-(T6), over-(T7) and highly over-aged tempers. Optical microscopy, hardness measurement, electrical conductivity measurement, tensile testing and SEM fractographs, differential scanning calorimetry (DSC), transmission electron microscopy (TEM), and electrochemical polarization studies have been used to characterize the alloy tempers. Hardness measurement and tensile testing showed the characteristic age hardening phenomenon of aluminium alloys. Optical and TEM micrographs have revealed the variation inmore » size of matrix strengthening η′ (MgZn{sub 2}) and also the size and distribution of grain boundary η (MgZn{sub 2}) precipitate with ageing time. DSC thermograms exhibiting exothermic and endothermic peaks indicated the characteristic solid state reaction sequence of the 7017 alloy. Potentiodynamic polarization study of the 7017 alloy of various tempers in 3.5 wt.% NaCl solution at near neutral pH showed typical active metal dissolution behaviour, but at pH 12 an active–passive–transpassive transition behaviour has been observed. - Graphical abstract: TEM micrograph of the 7017 aluminium alloy of various tempers (a, b) under aged (T4), (c, d) peak aged (T6), (e, f) over aged (T7) and (g, h) highly over-aged. Display Omitted - Highlights: • 7017 Al-Zn-Mg alloy was subjected to different artificial ageing treatments. • Characterization of 7017 alloy tempers by hardness, tensile, DSC, TEM and electrochemical behaviour. • Structure-properties relationship of the 7017 Al-Zn-Mg alloy of various tempers.« less

Effects of some polymeric additives on the cocrystallization of caffeine

NASA Astrophysics Data System (ADS)

Chung, Jihae; Kim, Il Won

2011-11-01

Effects of polymeric additives on the model cocrystallization were examined. The model cocrystal was made from caffeine and oxalic acid, and poly(ethylene glycol) (PEG), poly( L-lactide) (PLLA), poly(ɛ-caprolactone) (PCL), and poly(acrylic acid) (PAA) were the additives. The cocrystals were formed as millimeter-sized crystals without additives, and they became microcrystals with PLLA and PCL, and nanocrystals with PAA. XRD and IR revealed that the cocrystal structure was unchanged despite the strong effects of the additives on the crystal morphology, although some decrease in crystallinity was observed with PAA as confirmed by DSC. The DSC study also showed that the cocrystal melted and recrystallized to form α-caffeine upon heating. The present study verified that the polymeric additives can be utilized to modulate the size and morphology of the cocrystals without interfering the intermolecular interactions essential to the integrity of the cocrystal structures.

Azide derivatized anticancer agents of Vitamin K 3: X-ray structural, DSC, resonance spectral and API studies

NASA Astrophysics Data System (ADS)

Badave, Kirti; Patil, Yogesh; Gonnade, Rajesh; Srinivas, Darbha; Dasgupta, Rajan; Khan, Ayesha; Rane, Sandhya

2011-12-01

Compound 1 [1-imino (acetyl hydrazino)-Vitamin K 3], displays valence tautomerically related electronic isomers as Form I and Form II. Form I exhibits 2D packing fragment with 1D ribbon chains of N-H⋯O hydrogen bonds and shows EPR silent features. While Form II is EPR active and exhibits biradical nature with double quantum transitions at g = 2.0040. 1H NMR of compound 2, [1-imino (hydrazino carboxylate)-Vitamin K 3] and Form II exhibit π delocalization via resonance assisted H-bonding [RAHB] effect compared to Form I. Molecular interactions in Form I and II are visualized by DSC. The electronic structures of compounds 1 and 2 have been correlated to their API values by measuring anticancer activities, mitochondrial potentials and DNA shearing patterns. Form II and compound 2 indicate mitochondria mediated apoptosis (˜75% cell death) while Form I causes 35% cell death.

Properties of alginate fiber spun-dyed with fluorescent pigment dispersion.

PubMed

Wang, Ping; Tawiah, Benjamin; Tian, Anli; Wang, Chunxia; Zhang, Liping; Fu, Shaohai

2015-03-15

Spun-dyed alginate fiber was prepared by the spun-dyeing method with the mixture of fluorescent pigment dispersion and sodium alginate fiber spinning solution, and its properties were characterized by SEM, TGA, DSC, and XRD. The results indicate that fluorescent pigment dispersion prepared with esterified poly (styrene-alt maleic acid) had excellent compatibility with sodium alginate fiber spinning solution, and small amount of fluorescent pigment could reduce the viscosity of spun-dyed spinning solutions. SEM photo of spun-dyed alginate fiber indicated that fewer pigment particles deposited on its surface. TGA, DSC, and XRD results suggested that thermal properties and crystal phase of spun-dyed alginate fibers had slight changes compared to the original alginate fibers. The fluorescence intensity of spun-dyed alginate fiber reached its maximum when the content of fluorescent pigment was 4%. The spun-dyed alginate fiber showed excellent rubbing and washing fastness. Copyright © 2014 Elsevier Ltd. All rights reserved.

Mechanical and thermal behavior of ionic polymer metal composites: effects of electroded metals

NASA Astrophysics Data System (ADS)

Park, Il-Seok; Kim, Sang-Mun; Kim, Kwang J.

2007-08-01

In this study, we investigated the mechanical properties of various types of ionic polymer-metal composites (IPMCs) and Pt, Au, Pd, and Pt electroded ionic liquid (IL-Pt) IPMCs, by testing tensile modulus and dynamic mechanical behavior. The SEM was utilized to investigate the characteristics of the doped electroding layer, and the DSC was probed in order to look into the thermal behavior of various types of IPMCs. Au IPMCs, having a 5-7 µm-doped layer and nanosized Au particles (ca. 10 nm), showed the highest tensile strength (56 MPa) and modulus (602 MPa) in dried conditions. With regards to thermal behavior, Au IPMC had the highest Tg (153 °C) and Tm (263 °C) in both the DMA and DSC results. The fracture behavior of various types of IPMCs followed the behavior of the base material, Nafion™, which is represented as the semicrystalline polymer characteristic.

The mechanical properties of ionic polymer-metal composites

NASA Astrophysics Data System (ADS)

Park, Il-Seok; Kim, Sang-Mun; Kim, Doyeon; Kim, Kwang J.

2007-04-01

In this study, we investigated the mechanical properties of various type ionic polymer-metal composites (IPMCs) and Pt, Au, Pd, and Pt electroded ionic liquid (IL-Pt) IPMCs, by testing tensile modulus and dynamic mechanical behavior. The SEM was utilized to investigate the characteristics of the doped electroding layer, and the DSC was probed in order to look into the thermal behavior of various types of IPMCs. Au IPMCs, having a 5~7 μm doped layer and nano-sized Au particles (ca. 10 nm), showed the highest tensile strength (56 MPa) and modulus (602 MPa) in a dried condition. In a thermal behavior, Au IPMC has the highest T g (153°C) and T m (263°C) in both the DMA and DSC results. The fracture behavior of various types IPMCs followed base material's behavior, Nafion TM, which is represented as the semicrystalline polymer characteristic.

Crystallization kinetics of Fe based amorphous alloy

NASA Astrophysics Data System (ADS)

Shanker Rao, T.; Lilly Shanker Rao, T.

2015-02-01

Differential Scanning Calorimetry(DSC) experimental data under non-isothermal conditions for Fe based Metglas 2605SA1 (wt% Fe=85-95, Si=5-10, B=1-5) metallic glass ribbons are reported and discussed. The DSC Scans performed at different heating rates showed two step crystallization processes and are interpreted in terms of different models like Kissinger, Ozawa, Boswell, Augis & Bennett and Gao & Wang. From the heating rate dependence of the onset temperature (To) and the crystallization peak temperature (Tp), the kinetic triplet, activation energy of crystallization (E), Avrami exponent (n) and the frequency factor (A) are determined. The determined E for peak I is 354.5 ± 2.5 kJ/mol and for the peak II is 348.2 ± 2.2 kJ/mol, respectively. The frequency factor for peak I is 1.1 × 1023sec-1 and for peak II is 6.1 × 1020sec-1.

Effect of electron beam irradiation on the structural properties of poly(vinyl alcohol) formulations with triphenyl tetrazolium chloride dye (TTC)

NASA Astrophysics Data System (ADS)

Ali, Z. I.; Said, Hossam M.; Ali, H. E.

2006-01-01

Films of poly(vinyl alcohol) (PVA) composites with triphenyl tetrazolium chloride (TTC) dye were prepared and exposed to various radiation doses delivered by accelerated electrons. The results showed that at a low dose of 50 kGy, the colour difference (Δ E*) of PVA/TTC films was increased by ˜10 times of the initial value. However, the change in colour differences did not go systematically with increasing the TTC content, in which the composite with 1.5 wt% displayed higher value than that with 3.5 wt%. The differential scanning calorimetry (DSC) showed that the presence of the TTC dye caused a depression in the melting point ( Tm) and heat of fusion (Δ Hf) of the PVA bulk polymer. However, the thermogravimetric analysis (TGA) showed that the presence of the TTC dye improved the thermal stability of PVA. Also, the tensile strength at break of PVA/TTC composites was improved after electron beam irradiation.

Sorting of a multi-subunit ubiquitin ligase complex in the endolysosome system

PubMed Central

Yang, Xi; Arines, Felichi Mae; Zhang, Weichao

2018-01-01

The yeast Dsc E3 ligase complex has long been recognized as a Golgi-specific protein ubquitination system. It shares a striking sequence similarity to the Hrd1 complex that plays critical roles in the ER-associated degradation pathway. Using biochemical purification and mass spectrometry, we identified two novel Dsc subunits, which we named as Gld1 and Vld1. Surprisingly, Gld1 and Vld1 do not coexist in the same complex. Instead, they compete with each other to form two functionally independent Dsc subcomplexes. The Vld1 subcomplex takes the AP3 pathway to reach the vacuole membrane, whereas the Gld1 subcomplex travels through the VPS pathway and is cycled between Golgi and endosomes by the retromer. Thus, instead of being Golgi-specific, the Dsc complex can regulate protein levels at three distinct organelles, namely Golgi, endosome, and vacuole. Our study provides a novel model of achieving multi-tasking for transmembrane ubiquitin ligases with interchangeable trafficking adaptors. PMID:29355480

Determination of the heat of hydride formation/decomposition by high-pressure differential scanning calorimetry (HP-DSC).

PubMed

Rongeat, Carine; Llamas-Jansa, Isabel; Doppiu, Stefania; Deledda, Stefano; Borgschulte, Andreas; Schultz, Ludwig; Gutfleisch, Oliver

2007-11-22

Among the thermodynamic properties of novel materials for solid-state hydrogen storage, the heat of formation/decomposition of hydrides is the most important parameter to evaluate the stability of the compound and its temperature and pressure of operation. In this work, the desorption and absorption behaviors of three different classes of hydrides are investigated under different hydrogen pressures using high-pressure differential scanning calorimetry (HP-DSC). The HP-DSC technique is used to estimate the equilibrium pressures as a function of temperature, from which the heat of formation is derived. The relevance of this procedure is demonstrated for (i) magnesium-based compounds (Ni-doped MgH2), (ii) Mg-Co-based ternary hydrides (Mg-CoHx) and (iii) Alanate complex hydrides (Ti-doped NaAlH4). From these results, it can be concluded that HP-DSC is a powerful tool to obtain a good approximation of the thermodynamic properties of hydride compounds by a simple and fast study of desorption and absorption properties under different pressures.

Psychological stress during exercise: cardiorespiratory and hormonal responses.

PubMed

Webb, Heather E; Weldy, Michael L; Fabianke-Kadue, Emily C; Orndorff, G R; Kamimori, Gary H; Acevedo, Edmund O

2008-12-01

The purpose of this study was to examine the cardiorespiratory (CR) and stress hormone responses to a combined physical and mental stress. Eight participants (VO2(max) = 41.24 +/- 6.20 ml kg(-1) min(-1)) completed two experimental conditions, a treatment condition including a 37 min ride at 60% of VO2(max) with participants responding to a computerized mental challenge dual stress condition (DSC) and a control condition of the same duration and intensity without the mental challenge exercise alone condition (EAC). Significant interactions across time were found for CR responses, with heart rate, ventilation, and respiration rate demonstrating higher increases in the DSC. Additionally, norepinephrine was significantly greater in the DSC at the end of the combined challenge. Furthermore, cortisol area-under-the-curve (AUC) was also significantly elevated during the DSC. These results demonstrate that a mental challenge during exercise can exacerbate the stress response, including the release of hormones that have been linked to negative health consequences (cardiovascular, metabolic, autoimmune illnesses).

Ionic liquids: differential scanning calorimetry as a new indirect method for determination of vaporization enthalpies.

PubMed

Verevkin, Sergey P; Emel'yanenko, Vladimir N; Zaitsau, Dzmitry H; Ralys, Ricardas V; Schick, Christoph

2012-04-12

Differential scanning calorimetry (DSC) has been used to measure enthalpies of synthesis reactions of the 1-alkyl-3-methylimidazolium bromide [C(n)mim][Br] ionic liquids from 1-methylimidazole and n-alkyl bromides (with n = 4, 5, 6, 7, and 8). The optimal experimental conditions have been elaborated. Enthalpies of formation of these ionic liquids in the liquid state have been determined using the DSC results according to the Hess Law. The ideal-gas enthalpies of formation of [C(n)mim][Br] were calculated using the methods of quantum chemistry. They were used together with the DSC results to derive indirectly the enthalpies of vaporization of the ionic liquids under study. In order to validate the indirect determination, the experimental vaporization enthalpy of [C(4)mim][Br] was measured by using a quartz crystal microbalance (QCM). The combination of reaction enthalpy measurements by DSC with modern high-level first-principles calculations opens valuable indirect thermochemical options to obtain values of vaporization enthalpies of ionic liquids.

Intelligent processing for thick composites

NASA Astrophysics Data System (ADS)

Shin, Daniel Dong-Ok

2000-10-01

Manufacturing thick composite parts are associated with adverse curing conditions such as large in-plane temperature gradient and exotherms. The condition is further aggravated because the manufacturer's cycle and the existing cure control systems do not adequately counter such affects. In response, the forecast-based thermal control system is developed to have better cure control for thick composites. Accurate cure kinetic model is crucial for correctly identifying the amount of heat generated for composite process simulation. A new technique for identifying cure parameters for Hercules AS4/3502 prepreg is presented by normalizing the DSC data. The cure kinetics is based on an autocatalytic model for the proposed method, which uses dynamic and isothermal DSC data to determine its parameters. Existing models are also used to determine kinetic parameters but rendered inadequate because of the material's temperature dependent final degree of cure. The model predictions determined from the new technique showed good agreement to both isothermal and dynamic DSC data. The final degree of cure was also in good agreement with experimental data. A realistic cure simulation model including bleeder ply analysis and compaction is validated with Hercules AS4/3501-6 based laminates. The nonsymmetrical temperature distribution resulting from the presence of bleeder plies agreed well to the model prediction. Some of the discrepancies in the predicted compaction behavior were attributed to inaccurate viscosity and permeability models. The temperature prediction was quite good for the 3cm laminate. The validated process simulation model along with cure kinetics model for AS4/3502 prepreg were integrated into the thermal control system. The 3cm Hercules AS4/3501-6 and AS4/3502 laminate were fabricated. The resulting cure cycles satisfied all imposed requirements by minimizing exotherms and temperature gradient. Although the duration of the cure cycles increased, such phenomena was inevitable since longer time was required to maintain acceptable temperature gradient. The derived cure cycles were slightly different than what was anticipated by the offline simulation. Nevertheless, the system adapted to unanticipated events to satisfy the cure requirements.

ZnO nanoparticles via Moringa oleifera green synthesis: Physical properties & mechanism of formation

NASA Astrophysics Data System (ADS)

Matinise, N.; Fuku, X. G.; Kaviyarasu, K.; Mayedwa, N.; Maaza, M.

2017-06-01

The research work involves the development of better and reliable method for the bio-fabrication of Zinc oxide nanoparticles through green method using Moringa Oleifera extract as an effective chelating agent. The electrochemical activity, crystalline structure, morphology, isothermal behavior, chemical composition and optical properties of ZnO nanoparticles were studied using various characterization techniques i.e. Cyclic voltammetry (CV), X-ray powder diffraction (XRD), High resolution transmission electron microscopy (HRTEM), Selected area electron diffraction (SEAD), Differential scanning calorimetry/thermogravimetric analysis (DSC/TGA), Fourier Transform Infrared analysis (FTIR) and Ultraviolet spectroscopy studies (UV-vis). The electrochemical analysis proved that the ZnO nano has high electrochemical activity without any modifications and therefore are considered as a potential candidate in electrochemical applications. The XRD pattern confirmed the crystallinity and pure phase of the sample. DSC/TGA analysis of ZnO sample (before anneal) revealed three endothermic peaks around 140.8 °C, 223.7 °C and 389.5 °C. These endothermic peaks are attributed to the loss of volatile surfactant, conversion of zinc hydroxide to zinc oxide nanoparticles and transformation of zinc oxide into zinc nanoparticles. Mechanisms of formation of the ZnO nanoparticles via the chemical reaction of the Zinc nitrate precursor with the bioactive compounds of the Moringa oleifera are proposed for each of the major family compounds: Vitamins, Flavonoids, and Phenolic acids.

Preparation of oridonin-loaded solid lipid nanoparticles and studies on them in vitro and in vivo

NASA Astrophysics Data System (ADS)

Zhang, Dianrui; Tan, Tianwei; Gao, Lei

2006-12-01

Oridonin, a lipophilic Chinese medicine, has very low oral bioavailability due to its poor solubility. Solid lipid nanoparticle (SLN) delivery systems of oridonin have been formed using stearic acid, soybean lecithin and pluronic F68 in our studies to overcome this problem. Emulsion evaporation-solidification at low temperature was used to prepare SLN dispersions. The particle size and morphology were examined by transmission electron microscopy (TEM), and the zeta potential was measured by a television micro-electrophoresis apparatus. Process and formulation variables have been studied and optimized on the basis of entrapment efficiency. Differential scanning calorimetry (DSC) and powder x-ray diffraction (PXRD) studies were performed to characterize the state of the drug. In vitro release studies were performed in phosphate-buffer solution (PBS) (pH 7.4). The tissue distribution in mice and the pharmacokinetics in rabbits were studied to evaluate the tissue targeted property of SLNs. Stable SLN formulations of oridonin having a mean size range of 15-35 nm and mean zeta potential -45.07 mV were developed. More than 40% oridonin was entrapped in SLNs. DSC and PXRD analysis showed that oridonin is dispersed in SLNs in an amorphous state. The release pattern of the drug was analysed and found to follow the Higuchi equations. In vivo studies demonstrated that oridonin-loaded SLNs obviously increased the concentration of oridonin in liver, lung and spleen, while its distribution in heart and kidney decreased.

Novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum hydrogel film: Mechanical, thermal and water barrier properties.

PubMed

Balasubramanian, R; Kim, Sam Soo; Lee, Jaewoong

2018-06-24

The aim is to develop novel synergistic transparent k-Carrageenan/Xanthan gum/Gellan gum (k-C/X/G) hydrogel films with different weight ratio composition and to study the effect of these compositions on the physical properties of the films. The structure and morphological properties of the films were investigated by Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD) and differential scanning calorimeter (DSC). Results for FT-IR, DSC and SEM analysis showed a clear interaction between k-C, X, and G to form a new material. The mechanical, thermal and water barrier properties such as water vapor permeability (WVP), water contact angle (WCA) and moisture content were determined. The temperature at 5% weight loss (T 5% ) are in the range of 64.2-121.9 °C. The WVP exhibits are in the range of 1.8-2.4, contact angle are in the range of 32-65.8° and moisture content 16.5-21.51. The hydrogel film had good tensile strength of 19.1-31.0 MPa and elongation at break of 13-19% and tensile modulus of 1.6-2.4 GPa. The UV results indicate that the films were very transparent. The range of properties of the ternary k-C/X/G hydrogel films suggest that the presence molecular interaction and cross linking within the blends. Copyright © 2018. Published by Elsevier B.V.

Formulation and optimization of mouth dissolve tablets containing rofecoxib solid dispersion.

PubMed

Sammour, Omaima A; Hammad, Mohammed A; Megrab, Nagia A; Zidan, Ahmed S

2006-06-16

The purpose of the present investigation was to increase the solubility and dissolution rate of rofecoxib by the preparation of its solid dispersion with polyvinyl pyrrolidone K30 (PVP K30) using solvent evaporation method. Drug-polymer interactions were investigated using differential scanning calorimetry (DSC), x-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). For the preparation of rofecoxib mouth dissolve tablets, its 1:9 solid dispersion with PVP K30 was used with various disintegrants and sublimable materials. In an attempt to construct a statistical model for the prediction of disintegration time and percentage friability, a 3(2) randomized full and reduced factorial design was used to optimize the influence of the amounts of superdisintegrant and subliming agent. The obtained results showed that dispersion of the drug in the polymer considerably enhanced the dissolution rate. The drug-to-carrier ratio was the controlling factor for dissolution improvement. FTIR spectra revealed no chemical incompatibility between the drug and PVP K30. As indicated from XRD and DSC data, rofecoxib was in the amorphous form, which explains the better dissolution rate of the drug from its solid dispersions. Concerning the optimization study, the multiple regression analysis revealed that an optimum concentration of camphor and a higher percentage of crospovidone are required for obtaining rapidly disintegrating tablets. In conclusion, this investigation demonstrated the potential of experimental design in understanding the effect of the formulation variables on the quality of mouth dissolve tablets containing solid dispersion of a hydrophobic drug.

Development of solid self-emulsifying drug delivery system (SEDDS) I: use of poloxamer 188 as both solidifying and emulsifying agent for lipids.

PubMed

Shah, Ankita V; Serajuddin, Abu T M

2012-10-01

To develop solid self-emulsifying drug delivery systems (SEDDS) for lipids using poloxamer 188 as both solidifying and emulsifying agents. Mixtures of various lipids with poloxamer 188 and PEG 8000 were prepared at ~75°C. The molten mixtures, with and without dissolved drugs (fenofibrate and probucol), were then cooled to room temperature. When solids formed, they were characterized by powder XRD, DSC, microscopy using cross-polarization and confocal fluorescence techniques, dispersion test in water and particle size analysis of dispersions. When mixed with poloxamer 188 or PEG 8000, lipids consisting of monoesters of fatty acids with glycerol or propylene glycol formed solid systems, but not di- and tri-esters, which showed phase separation. Added to water, the solid systems containing poloxamer 188 started to disperse in water forming oil globules of 200-600 nm. No emulsification of lipids was observed from solids containing PEG 8000, indicating that the surfactant property of poloxamer 188 was responsible for emulsification. Powder XRD, DSC and microscopic examination revealed that poloxamer 188 and PEG 8000 maintained their crystallinity in solid systems, while the lipids were interspersed in between crystalline regions. The drug remained solubilized in the lipid phase. A novel solid SEDDS is developed where the drug can be solubilized in liquid lipids and then the lipidic solution can be converted to solid mass by dispersing into the microstructure of poloxamer 188.

The preparation and investigation into properties of ionomer fiber

NASA Astrophysics Data System (ADS)

Ejigiri, Everest Emmanuel

The purpose of this study was to demonstrate the preparation and characterization of ionomer fiber. Two outstanding features of oriented-fiber composites are their high strength-to- weight ratio and controlled anisotropy which is because fibers are formed when polymer chains (in case of polymeric materials) are all lined up in the same direction. And the chains can pack together tightly. Materials can be made into fiber for the purpose of getting better properties and to make the application flexible. In this study, ionomer fiber was prepared. The physical and mechanical properties were examined through a variety of tests- including tensile test, dynamic mechanical analysis (DMA), differential scanning calorimetry (DSC), free shape recovery test, and constrained stress recovery test. The ionomer fibers were made into muscles fiber, and the tensile actuation behavior of the muscle was studied. From the DMA, Storage modulus, loss modulus, tan delta and glass transition temperature were obtained. DSC was also used to obtain the glass transition temperature which also closely aligned with glass transition obtained from DMA. Also according to the test results, ionomer fiber (filament) demonstrated considerable stress recovery, high ductility and however, the filament did not produce high recovery ratio. The fiber was made into artificial muscle and actuation test was also carried out, which indicated that because the fiber being too much elastic - the fiber was not able to expand and contract when heat was applied to it. Instead it showed continuous expansion.

Thermal stability of active/inactive nanocomposite anodes based on Cu2Sb in lithium-ion batteries

NASA Astrophysics Data System (ADS)

Allcorn, Eric; Kim, Sang-Ok; Manthiram, Arumugam

2015-12-01

Various active/inactive nanocomposites of Cu2Sb-Al2O3@C, Cu2Sb-TiC, and Cu2Sb-TiC@C have been synthesized by high energy mechanical milling and investigated by differential scanning calorimetry (DSC) to determine the lithiated phase stability and heat generation arising from these electrodes. The milling process reduces the Li3Sb phase stability, relative to the un-milled samples, to below ∼200 °C. However, the incorporation of the reinforcing, inactive phases Al2O3, TiC, and carbon black offer a slight improvement. DSC curves also show that the low-temperature heat generation in the SEI-layer reaction range is not noticeably altered by either the milling process or the addition of the inactive phases. A strong exothermic peak is observed at ∼200 °C for the 0% state of charge electrodes of Cu2Sb-Al2O3@C and Cu2Sb-TiC@C that was caused by the incorporation of carbon black into the composite. This peak was not present in the electrodes of milled Cu2Sb or Cu2Sb-TiC, suggesting that efforts to extend the cycle life of alloy anodes should avoid carbon black due to its destabilizing effects on delithiated electrodes. Fourier Transform infrared spectroscopy analysis indicates that the reaction arising from the incorporation of carbon black is tied to a low-temperature breakdown of the lithium salt LiPF6.

Differential scanning calorimetry: An invaluable tool for a detailed thermodynamic characterization of macromolecules and their interactions

PubMed Central

Chiu, Michael H.; Prenner, Elmar J.

2011-01-01

Differential Scanning Calorimetry (DSC) is a highly sensitive technique to study the thermotropic properties of many different biological macromolecules and extracts. Since its early development, DSC has been applied to the pharmaceutical field with excipient studies and DNA drugs. In recent times, more attention has been applied to lipid-based drug delivery systems and drug interactions with biomimetic membranes. Highly reproducible phase transitions have been used to determine values, such as, the type of binding interaction, purity, stability, and release from a drug delivery mechanism. This review focuses on the use of DSC for biochemical and pharmaceutical applications. PMID:21430954

Improving Thermo-Oxidative Stability of Nitrile Rubber Composites by Functional Graphene Oxide.

PubMed

Zhong, Rui; Zhang, Zhao; Zhao, Hongguo; He, Xianru; Wang, Xin; Zhang, Rui

2018-05-30

Graphene oxide (GO), modified with anti-aging agent p -phenylenediamine (PPD), was added into nitrile rubber (NBR) in order to improve the thermo-oxidative stability of NBR. The modification of GO and the transformation of functional groups were characterized by Fourier transform infrared spectroscopy (FTIR), Raman, and X-ray diffraction (XRD). Mechanical performances of NBR composites before and after the thermo-oxidative aging were recorded. The results of dynamic mechanical analysis (DMA) show an increased storage modulus (G') and a decreased value of area of tan δ peak after introducing modified GO into NBR. It indicates that filler particles show positive interaction with molecular chains. The thermo-oxidative stability of composites was investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Then, the thermo-oxidative aging kinetic parameters were obtained by the Flynn⁻Wall⁻Ozawa (FWO) equation. The results of aging tests show that the thermo-oxidative stability of rubber matrix increases obviously after introducing GO⁻PPD. In addition, mechanical properties (tensile strength and elongation at break) of both before and after aged NBR/GO⁻PPD composites were superior to that of NBR. This work provides meaningful guidance for achieving multifunction thermo-oxidative aging resistance rubber composites.

Supramolecular interactions between triphenylphosphine oxide and benzamide evaluated by positron annihilation lifetime spectroscopy

NASA Astrophysics Data System (ADS)

Oliveira, F. C.; Denadai, A. M. L.; Fulgêncio, F.; Oliveira, A. M.; Andrade, A. C. A.; Melo, A. C. A.; Yoshida, M. I.; Windmöller, D.; Magalhães, W. F.

2017-04-01

In the present work, intermolecular interactions between triphenylphosphine oxide (TPPO) and benzamide (BZM) has been studied in solid state by Positron Annihilation Lifetime Spectroscopy (PALS) and supported by several analytical techniques (in solid state and in solution) and by computational modeling (in gaseous phase). Isothermal Titration Calorimetry (ITC) in ethyl acetate solvent showed that complexation is a stepwise process, with 2:1 and 1:1 TPPO/BZM stoichiometries, both driven by entropy. HPLC analysis of isolated single crystal confirmed the existence of a 2:1 TPPO/BZM crystalline complex in solid state. The results of thermal analysis (TGA, DTA and DSC) and FTIR spectroscopy showed that the interactions in the complexes are relatively weaker than those found in pure precursors. Finally, PALS showed higher positronium formation probability (I3) at [TPPO0.62·BZM0.38] and [TPPO0.25·BZM0.75] molar fractions, corroborating the existence of two stoichiometries for the TPPO/BZM system and suggesting greater electronic availability of n- and π-electrons in heterosynton complexes, as resulting of interactions, bring forward new evidences of the participation of electronic excited states on the positronium formation mechanism.

Development of Antimicrobial Packaging Film Made from Poly(Lactic Acid) Incorporating Titanium Dioxide and Silver Nanoparticles.

PubMed

Li, Wenhui; Zhang, Cheng; Chi, Hai; Li, Lin; Lan, Tianqing; Han, Peng; Chen, Haiyan; Qin, Yuyue

2017-07-13

Polylactide (PLA)/nano-TiO₂ and PLA/nano-TiO₂/nano-Ag blends films were prepared by a solvent volatilization method. Compared to pure PLA film, the nano-blend films have low water vapor permeability (WVP) and a poor transparency. With the increase of the NPs in the PLA, the tensile strength (TS) and elastic modulus (EM) decreased, while the elongation at break (ε) increased. SEM analysis indicated a rougher cross-section of the nano-blend films. According to the FTIR analysis, no new chemical bonds were formed in the nano-blend films. By using DSC to examine the crystallization and melting behavior, the result shows that the NPs have no effect on the glass transition (T g ) and melting temperature (T m ), but they caused an increase on the cold crystallization (T c) and crystallinity ( X c ). TGA results show that the addition of nanoparticles significantly improved the thermal stability. The PLA nano-blend films show a good antimicrobial activity against. E. coli and Listeria monocytogenes . Most important, we carried out migration tests, and verified that the release of NPs from the nano-blend films was within the standard limits.

A Comparative Study on the Mechanical, Thermal and Morphological Characterization of Poly(lactic acid)/Epoxidized Palm Oil Blend

PubMed Central

Giita Silverajah, V. S.; Ibrahim, Nor Azowa; Yunus, Wan Md Zin Wan; Hassan, Hazimah Abu; Woei, Chieng Buong

2012-01-01

In this work, poly(lactic acid) (PLA) a fully biodegradable thermoplastic polymer matrix was melt blended with three different epoxidized palm oil (EPO). The aim of this research was to enhance the flexibility, mechanical and thermal properties of PLA. The blends were prepared at various EPO contents of 1, 2, 3, 4 and 5 wt% and characterized. The SEM analysis evidenced successful modification on the neat PLA brittle morphology. Tensile tests indicate that the addition of 1 wt% EPO is sufficient to improve the strength and flexibility compared to neat PLA. Additionally, the flexural and impact properties were also enhanced. Further, DSC analysis showed that the addition of EPO results in a decrease in Tg, which implies an increase in the PLA chain mobility. In the presence of 1 wt% EPO, TGA results revealed significant increase in the thermal stability by 27%. Among the three EPOs used, EPO(3) showed the best mechanical and thermal properties compared to the other EPO’s, with an optimum loading of 1 wt%. Conclusively, EPO showed a promising outcome to overcome the brittleness and improve the overall properties of neat PLA, thus can be considered as a potential plasticizer. PMID:22754338

A comparative study on the mechanical, thermal and morphological characterization of poly(lactic acid)/epoxidized Palm Oil blend.

PubMed

Giita Silverajah, V S; Ibrahim, Nor Azowa; Yunus, Wan Md Zin Wan; Hassan, Hazimah Abu; Woei, Chieng Buong

2012-01-01

In this work, poly(lactic acid) (PLA) a fully biodegradable thermoplastic polymer matrix was melt blended with three different epoxidized palm oil (EPO). The aim of this research was to enhance the flexibility, mechanical and thermal properties of PLA. The blends were prepared at various EPO contents of 1, 2, 3, 4 and 5 wt% and characterized. The SEM analysis evidenced successful modification on the neat PLA brittle morphology. Tensile tests indicate that the addition of 1 wt% EPO is sufficient to improve the strength and flexibility compared to neat PLA. Additionally, the flexural and impact properties were also enhanced. Further, DSC analysis showed that the addition of EPO results in a decrease in T(g), which implies an increase in the PLA chain mobility. In the presence of 1 wt% EPO, TGA results revealed significant increase in the thermal stability by 27%. Among the three EPOs used, EPO(3) showed the best mechanical and thermal properties compared to the other EPO's, with an optimum loading of 1 wt%. Conclusively, EPO showed a promising outcome to overcome the brittleness and improve the overall properties of neat PLA, thus can be considered as a potential plasticizer.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, J; Balter, P; Court, L

Purpose: To evaluate the performance of commercially available automatic segmentation tools built into treatment planning systems (TPS) in terms of their segmentation accuracy and flexibility in customization. Methods: Twelve head-and-neck cancer patients and twelve thoracic cancer patients were retrospectively selected to benchmark the model-based segmentation (MBS) and atlas-based segmentation (ABS) in RayStation TPS and the Smart Probabilistic Image Contouring Engine (SPICE) in Pinnacle TPS. Multi-atlas contouring service (MACS) that was developed in-house as a plug-in of Pinnacle TPS was evaluated as well. Manual contours used in clinic were reviewed and modified for consistency and served as ground truth for themore » evaluation. Head-and-neck evaluation included six regions of interest (ROIs): left and right parotid glands, brainstem, spinal cord, mandible, and submandibular glands. Thoracic evaluation includes seven ROIs: left and right lungs, spinal cord, heart, esophagus, and left and right brachial plexus. Auto-segmented contours were compared with the manual contours using the Dice similarity coefficient (DSC) and the mean surface distance (MSD). Results: In head- and-neck evaluation, only mandible has a high accuracy in all segmentations (DSC>85%); SPICE achieved DSC>70% for parotid glands; MACS achieved this for both parotid glands and submandibular glands; and RayStation ABS achieved this for spinal cord. In thoracic evaluation, SPICE achieved the best in lung and heart segmentation, while MACS achieved the best for all other structures. The less distinguishable structures on CT images, such as brainstem, spinal cord, parotid glands, submandibular glands, esophagus, and brachial plexus, showed great variability in different segmentation tools (mostly DSC<70% and MSD>3mm). The template for RayStation ABS can be easily customized by users, while RayStation MBS and SPICE rely on the vendors to provide the templates/models. Conclusion: Great variability was observed in different segmentation tools applied to different structures. These commercially-available segmentation tools should be carefully evaluated before clinical use.« less

Dynamic susceptibility contrast (DSC) perfusion MRI in differential diagnosis between radionecrosis and neoangiogenesis in cerebral metastases using rCBV, rCBF and K2.

PubMed

Muto, Mario; Frauenfelder, Giulia; Senese, Rossana; Zeccolini, Fabio; Schena, Emiliano; Giurazza, Francesco; Jäger, Hans Rolf

2018-07-01

Distinction between treatment-related changes and tumour recurrence in patients who have received radiation treatment for brain metastases can be difficult on conventional MRI. In this study, we investigated the ability of dynamic susceptibility contrast (DSC) perfusion in differentiating necrotic changes from pathological angiogenesis and compared measurements of relative cerebral blood volume (rCBV), relative cerebral blood flow (rCBF) and K2, using a dedicated software. Twenty-nine patients with secondary brain tumors were included in this retrospective study and underwent DSC perfusion MRI with a 3-month follow-up imaging after chemo- or radiation-therapy. Region-of-interests were drawn around the contrast enhancing lesions and measurements of rCBV, rCBF and K2 were performed in all patients. Based on subsequent histological examination or clinico-radiological follow-up, the cohort was divided in two groups: recurrent disease and stable disease. Differences between the two groups were analyzed using the Student's t test. Sensitivity, specificity and diagnostic accuracy of rCBV measurements were analyzed considering three different cut-off values. Between patients with and without disease, only rCBV and rCBF values were significant (p < 0.05). The only cut-off value giving the best diagnostic accuracy of 100% was rCBV = 2.1 (sensitivity = 100%; specificity = 100%). Patients with tumor recurrence showed a higher mean value of rCBV (mean = 4.28, standard deviation = 2.09) than patients with necrotic-related changes (mean = 0.77, standard deviation = 0.44). DSC-MRI appears a clinically useful method to differentiate between tumor recurrence, tumor necrosis and pseudoprogression in patients treated for cerebral metastases. Relative CBV using a cut-off value of 2.1 proved to be the most accurate and reliable parameter.

Ceramide-1-Phosphate, in Contrast to Ceramide, Is Not Segregated into Lateral Lipid Domains in Phosphatidylcholine Bilayers

PubMed Central

Morrow, Michael R.; Helle, Anne; Perry, Joshua; Vattulainen, Ilpo; Wiedmer, Susanne K.; Holopainen, Juha M.

2009-01-01

Sphingolipids are key lipid regulators of cell viability: ceramide is one of the key molecules in inducing programmed cell death (apoptosis), whereas other sphingolipids, such as ceramide 1-phosphate, are mitogenic. The thermotropic and structural behavior of binary systems of N-hexadecanoyl-D-erythro-ceramide (C16-ceramide) or N-hexadecanoyl-D-erythro-ceramide-1-phosphate (C16-ceramide-1-phosphate; C16-C1P) with 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) was studied with DSC and deuterium nuclear magnetic resonance (2H-NMR). Partial-phase diagrams (up to a mole fraction of sphingolipids X = 0.40) for both mixtures were constructed based on DSC and 2H-NMR observations. For C16-ceramide-containing bilayers DSC heating scans showed already at Xcer = 0.025 a complex structure of the main-phase transition peak suggestive of lateral-phase separation. The transition width increased significantly upon increasing Xcer, and the upper-phase boundary temperature of the mixture shifted to ∼65°C at Xcer = 0.40. The temperature range over which 2H-NMR spectra of C16-ceramide/DPPC-d62 mixtures displayed coexistence of gel and liquid crystalline domains increased from ∼10° for Xcer = 0.1 to ∼21° for Xcer = 0.4. For C16-C1P/DPPC mixtures, DSC and 2H-NMR observations indicated that two-phase coexistence was limited to significantly narrower temperature ranges for corresponding C1P concentrations. To complement these findings, C16-ceramide/1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine (POPC) and C16-C1P/POPC mixtures were also studied by 2H-NMR and fluorescence techniques. These observations indicate that DPPC and POPC bilayers are significantly less perturbed by C16-C1P than by C16-ceramide and that C16-C1P is miscible within DPPC bilayers at least up to XC1P = 0.30. PMID:19289048

SU-E-J-226: Propagation of Pancreas Target Contours On Respiratory Correlated CT Images Using Deformable Image Registration

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, F; Yorke, E; Mageras, G

2014-06-01

Purpose: Respiratory Correlated CT (RCCT) scans to assess intra-fraction motion among pancreatic cancer patients undergoing radiotherapy allow for dose sparing of normal tissues, in particular for the duodenum. Contour propagation of the gross tumor volume (GTV) from one reference respiratory phase to 9 other phases is time consuming. Deformable image registration (DIR) has been successfully used for high contrast disease sites but lower contrast for pancreatic tumors may compromise accuracy. This study evaluates the accuracy of Fast Free Form (FFF) registration-based contour propagation of the GTV on RCCT scans of pancreas cancer patients. Methods: Twenty-four pancreatic cancer patients were retrospectivelymore » studied; 20 had tumors in the pancreatic head/neck, 4 in the body/tail. Patients were simulated with RCCT and images were sorted into 10 respiratory phases. A radiation oncologist manually delineated the GTV for 5 phases (0%, 30%, 50%, 70% and 90%). The FFF algorithm was used to map deformations between the EE (50%) phase and each of the other 4 phases. The resultant deformation fields served to propagate GTV contours from EE to the other phases. The Dice Similarity Coefficient (DSC), which measures agreement between the DIR-propagated and manually-delineated GTVs, was used to quantitatively examine DIR accuracy. Results: Average DSC over all scans and patients is 0.82 and standard deviation is 0.09 (DSC range 0.97–0.57). For GTV volumes above and below the median volume of 20.2 cc, a Wilcoxon rank-sum test shows significantly different DSC (p=0.0000002). For the GTVs above the median volume, average +/− SD is 0.85 +/− 0.07; and for the GTVs below, the average +/− SD is 0.75 +/−0.08. Conclusion: For pancreatic tumors, the FFF DIR algorithm accurately propagated the GTV between the images in different phases of RCCT, with improved performance for larger tumors.« less

Determining the main thermodynamic parameters of caffeine melting by means of DSC

NASA Astrophysics Data System (ADS)

Agafonova, E. V.; Moshchenskii, Yu. V.; Tkachenko, M. L.

2012-06-01

The temperature and enthalpy of the melting of caffeine, which are 235.5 ± 0.1°C and 19.6 ± 0.2 kJ/mol, respectively, are determined by DSC. The melting entropy and the cryoscopic constant of caffeine are calculated.

47 CFR 80.225 - Requirements for selective calling equipment.

Code of Federal Regulations, 2010 CFR

2010-10-01

... manufacture, importation, sale or installation of non-portable DSC equipment that does not comply with either..., 2011. (5) The manufacture, importation, or sale of handheld, portable DSC equipment that does not... to establish or maintain communications provided that: (i) These signalling techniques are not used...

Physico-chemical characteristics of papaya (Carica papaya L.) seed oil of the Hong Kong/Sekaki variety.

PubMed

Yanty, Noorzianna Abdul Manaf; Marikkar, Jalaldeen Mohammed Nazrim; Nusantoro, Bangun Prajanto; Long, Kamariah; Ghazali, Hasanah Mohd

2014-01-01

A study was carried out to determine the physicochemical characteristics of the oil derived from papaya seeds of the Hong Kong/Sekaki variety. Proximate analysis showed that seeds of the Hong Kong/Sekaki variety contained considerable amount of oil (27.0%). The iodine value, saponification value, unsaponifiable matter and free fatty acid contents of freshly extracted papaya seed oil were 76.9 g I2/100g oil, 193.5 mg KOH/g oil, 1.52% and 0.91%, respectively. The oil had a Lovibond color index of 15.2Y + 5.2B. Papaya seed oil contained ten detectable fatty acids, of which 78.33% were unsaturated. Oleic (73.5%) acid was the dominant fatty acids followed by palmitic acid (15.8%). Based on the high performance liquid chromatography (HPLC) analysis, seven species of triacylglycerols (TAGs) were detected. The predominant TAGs of papaya seed oil were OOO (40.4%), POO (29.1%) and SOO (9.9%) where O, P, and S denote oleic, palmitic and stearic acids, respectively. Thermal analysis by differential scanning calorimetry (DSC) showed that papaya seed oil had its major melting and crystallization transitions at 12.4°C and -48.2°C, respectively. Analysis of the sample by Z-nose (electronic nose) instrument showed that the sample had a high level of volatile compounds.

The Multidimensional Influence of Acculturation on Digit Symbol-Coding and Wisconsin Card Sorting Test in Hispanics.

PubMed

Krch, Denise; Lequerica, Anthony; Arango-Lasprilla, Juan Carlos; Rogers, Heather L; DeLuca, John; Chiaravalloti, Nancy D

2015-01-01

The purpose of the current study was to evaluate the relative contribution of acculturation to two tests of nonverbal test performance in Hispanics. This study compared 40 Hispanic and 20 non-Hispanic whites on Digit Symbol-Coding (DSC) and the Wisconsin Card Sorting Test (WCST) and evaluated the relative contribution of the various acculturation components to cognitive test performance in the Hispanic group. Hispanics performed significantly worse on DSC and WCST relative to non-Hispanic whites. Multiple regressions conducted within the Hispanic group revealed that language use uniquely accounted for 11.0% of the variance on the DSC, 18.8% of the variance on WCST categories completed, and 13.0% of the variance in perseverative errors on the WCST. Additionally, years of education in the United States uniquely accounted for 14.9% of the variance in DSC. The significant impact of acculturation on DSC and WCST lends support that nonverbal cognitive tests are not necessarily culture free. The differential contribution of acculturation proxies highlights the importance of considering these separate components when interpreting performance on neuropsychological tests in clinical and research settings. Factors, such as the country where education was received, may in fact be more meaningful information than the years of education of education attained. Thus, acculturation should be considered an important factor in any cognitive evaluation of culturally diverse individuals.

Thermophysical, interfacial and decomposition analyses of polyhydroxyalkanoates introduced against organic and inorganic surfaces

NASA Astrophysics Data System (ADS)

Dagnon, Koffi Leonard

The development of a "cradle-to-cradle" mindset with both material performance during utilization and end of life disposal is a critical need for both ecological and economic considerations. The main limitation to the use of the biopolymers is their mechanical properties. Reinforcements are therefore a good alternative but disposal concerns then arise. Thus the objective of this dissertation is to investigate a biopolymer nanocomposite where the filler is a synthetically prepared layer double hydroxide (inorganic interface); and a biopolymer paper (organic interface) based coating or laminate. The underlying issues driving performance are the packing density of the biopolymer and the interaction with the reinforcement. Since the polyhydroxyalkanoates or PHAs (the biopolymers used for the manufacture of the nanocomposites and coatings) are semicrystalline materials, the glass transition was investigated using dynamic mechanical analysis (DMA) and dielectric spectroscopy (DES), whereas the melt crystallization, cold crystallization and melting points were investigated using differential scanning calorimetry (DSC). Fourier transform infrared (FTIR) spectroscopy was used to estimate crystallinity in the coated material given the low thermal mass of the PHA in the PHA coating. The significant enhancement of the crystallization rate in the PHA nanocomposite was probed using DSC and polarized optical microscopy (POM) and analyzed using Avrami and Lauritzen-Hoffman models. Both composites showed a significant improvement in the mechanical performance obtained by DMA, tensile and impact testing. The degradation and decomposition of the two composites were investigated in low microbial activity soil for the cellulose paper (to slow down the degradation rate that occurs in compost) and in compost. An in-house system according to the American Society for Testing and Materials ASTM D-98 (2003) was engineered. Soil decomposition showed that PHA coating into and onto the cellulose paper can be considered to be a useful method for the assessment of the degradability of the biopolymer. PHA nanocomposite showed enhanced compostability.

The effect of specific proline residues on the kinetic stability of the triosephosphate isomerases of two trypanosomes.

PubMed

Guzmán-Luna, Valeria; Quezada, Andrea G; Díaz-Salazar, A Jessica; Cabrera, Nallely; Pérez-Montfort, Ruy; Costas, Miguel

2017-04-01

The effect of specific residues on the kinetic stability of two closely related triosephosphate isomerases (from Trypanosoma cruzi, TcTIM and Trypanosoma brucei, TbTIM) has been studied. Based on a comparison of their β-turn occurrence, we engineered two chimerical enzymes where their super secondary β-loop-α motifs 2 ((βα) 2 ) were swapped. Differential scanning calorimetry (DSC) experiments showed that the (βα) 2 motif of TcTIM inserted into TbTIM (2Tc) increases the kinetic stability. On the other hand, the presence of the (βα) 2 motif of TbTIM inserted into TcTIM (2Tb) gave a chimerical protein difficult to purify in soluble form and with a significantly reduced kinetic stability. The comparison of the contact maps of the (βα) 2 of TbTIM and TcTIM showed differences in the contact pattern of residues 43 and 49. In TcTIM these residues are prolines, located at the N-terminal of loop-2 and the C-terminal of α-helix-2. Twelve mutants were engineered involving residues 43 and 49 to study the effect over the unfolding activation energy barrier (E A ). A systematic analysis of DSC data showed a large decrease on the E A of TcTIM (ΔE A ranging from 468 to 678 kJ/mol) when the single and double proline mutations are present. The relevance of Pro43 to the kinetic stability is also revealed by mutation S43P, which increased the free energy of the transition state of TbTIM by 17.7 kJ/mol. Overall, the results indicate that protein kinetic stability can be severely affected by punctual mutations, disturbing the complex network of interactions that, in concerted action, determine protein stability. Proteins 2017; 85:571-579. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Novel Energetic Materials for Space Propulsion

DTIC Science & Technology

2011-04-30

Thermogravimetric analysis (TGA) experiments with percent weight loss versus temperature for a range of heating rates. Labels and TGA traces have...conditions  for  a  specified  period  of  time.  Thermogravimetric   analysis   (TGA)  and  differential  scanning  calorimetry  (DSC)  analyses  were...Experiments  The  thermal  decomposition  of  ammonia  borane was  first  studied  by  Hu  et al.  [97]  using  thermogravimetric   analysis   (TGA), where

47 CFR 80.179 - Unattended operation.

Code of Federal Regulations, 2011 CFR

2011-10-01

... DSC in accordance with ITU-R Recommendation M.493-11, “Digital Selective-calling System for Use in the...., Washington, DC (Reference Information Center) or at the National Archives and Records Administration (NARA... condition related to ship safety. (3) The “ROUTINE” DSC category must be used. (4) Communications must be...

47 CFR 80.359 - Frequencies for digital selective calling (DSC).

Code of Federal Regulations, 2013 CFR

2013-10-01

... calling frequencies for use by authorized ship and coast stations for general purpose DSC. There are three.... The “Series A” designation includes coast stations along, and ship stations in, the Atlantic Ocean... location of the called station and propagation conditions. Acknowledgement is made on the paired frequency...

47 CFR 80.359 - Frequencies for digital selective calling (DSC).

Code of Federal Regulations, 2012 CFR

2012-10-01

... calling frequencies for use by authorized ship and coast stations for general purpose DSC. There are three.... The “Series A” designation includes coast stations along, and ship stations in, the Atlantic Ocean... location of the called station and propagation conditions. Acknowledgement is made on the paired frequency...

47 CFR 80.359 - Frequencies for digital selective calling (DSC).

Code of Federal Regulations, 2014 CFR

2014-10-01

... calling frequencies for use by authorized ship and coast stations for general purpose DSC. There are three.... The “Series A” designation includes coast stations along, and ship stations in, the Atlantic Ocean... location of the called station and propagation conditions. Acknowledgement is made on the paired frequency...

Structure and Phase Transitions of Poly (Hexamethylene p,p'-Bibenzoate) as Studied by DSC and Real-Time SAXS/WAXS Employing Synchrotron Radiation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Katerska, B.; Krasteva, M.; Perez, E.

2007-04-23

Real-time small and wide angle X-ray scattering as well as DSC studies were carried out in order to analyzes the structure and phase transitions of liquid crystalline thermotropic poly(methylene p,p' bibenzoat)

77 FR 42498 - Information Collection(s) Being Submitted for Review and Approval to the Office of Management and...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-19

...: Section 80.103, Digital Selective Calling (DSC) Operating Procedures--Maritime Mobile Identity (MMSI...: Individuals or households; business or other for- profit entities and Federal Government. Number of... Marine VHF radios with Digital Selective Calling (DSC) capability in this collection. The licensee...

Vapor Pressure Data and Analysis for Selected Organophosphorus Compounds: DIBMP, DCMP, IMMP, IMPA, EMPA, and MPFA

DTIC Science & Technology

2017-04-01

Methodology, Statistics, and Applications; CRDEC-TR-386; U.S. Army Chemical Research, Development and Engineering Center: Aberdeen Proving Ground...Approved for public release; distribution unlimited. 13. SUPPLEMENTARY NOTES 14. ABSTRACT: Recent work from our laboratory has focused on chemical ...vaporization Volatility Differential scanning calorimetry (DSC) Vapor saturation Boiling point Diisobutyl methylphosphonate (DIBMP), Chemical Abstracts

Evaluation of the cure kinetics of the wood/pMDI bondline

Treesearch

David P. Harper; Michael P. Wolcott; Timothy G. Rials

2001-01-01

Micro-dielectric analysis (µDEA) and differentia1 scanning calorimetry (DSC) were used to monitor cure of polymeric diphenyl-methane diisocyanate (pMDI) resin with wood strands in a saturated steam environment. A first-order autocatalyzed kinetic model was employed to determine kinetic parameters. The kinetics were found to follow an Arrhenius relation. A single ramp...

Influence of adding Sea Spaghetti seaweed and replacing the animal fat with olive oil or a konjac gel on pork meat batter gelation. Potential protein/alginate association.

PubMed

Fernández-Martín, F; López-López, I; Cofrades, S; Colmenero, F Jiménez

2009-10-01

Standard and modulated differential scanning calorimetry (DSC, MDSC) and dynamic rheological thermal analysis (DRTA) were used to in situ simulate the batter gelation process. Texture profile analysis (TPA) and conventional quality evaluations were applied to processed products. Sea Spaghetti seaweed addition was highly effective at reinforcing water/oil retention capacity, hardness and elastic modulus in all formulations. Olive oil substituting half pork fat yielded a presumably healthier product with slightly better characteristics than control. A konjac-starch mixed gel replacing 70% of pork fat produced a similar product to control but with nearly 10% more water. DSC revealed the currently unknown phenomenon that Sea Spaghetti alginates apparently prevented thermal denaturation of a considerable protein fraction. MDSC confirmed that this mainly concerned non-reversing effects, and displayed glass transition temperatures in the range of 55-65°C. DRTA and TPA indicated however much stronger alginate-type gels. It is tentatively postulated that salt-soluble proteins associate athermally with seaweed alginates on heating to constitute a separate phase in a thermal composite-gelling process.

Selective removal of monoterpenes from bergamot oil by inclusion in deoxycholic acid.

PubMed

Fantin, Giancarlo; Fogagnolo, Marco; Maietti, Silvia; Rossetti, Stefano

2010-05-12

A new approach for removing monoterpenes (MTs) from bergamot oil by selective inclusion in deoxycholic acid (DCA) is proposed. The inclusion process is very efficient, the included fraction being composed mainly of limonene (71.7%) and gamma-terpinene (19.8%). On the other hand, the deterpenated bergamot oil fraction showed for the linalool and linalyl acetate derivatives significant increases from 16.6 and 21.4% to 18.3 and 42.2%, respectively. The major advantages of this methodology are its simplicity, the mild conditions employed, and the quantitative recovery of both host (DCA) and guest (monoterpenes) compounds. Differential scanning calorimetry (DSC), thermal gravimetry (TG), powder X-ray diffractometry (XRPD), infrared spectroscopy (IR), and proton magnetic resonance ((1)H NMR) analysis were used to investigate and characterize the inclusion compounds.

Mechanisms of fibrinogen-acebutolol interactions: Insights from DSC, CD and LS.

PubMed

Hassan, Natalia; Ruso, Juan M; Somasundaran, P

2011-02-01

The complex formed due to the interaction of the amphiphilic betablocker acebutolol with fibrinogen in a buffer solution (50mN glycine, pH of 8.5) has been investigated using a multipronged physicochemical approach. Differential scanning calorimetry measurements of the complexes have shown no reversibility of thermal denaturation as indicated by the three observed peaks and the opposite role that acebutolol plays in the folding different domains of the fibrinogen molecule and the stability of such domains. While circular dichroism measurements have revealed that interaction of acebutolol with fibrinogen affects the protein secondary structure to a different extent depending on the temperature and drug concentration, dynamic light scattering analysis showed evidence for protein aggregation mainly to tetramers and dimers. Copyright © 2010 Elsevier B.V. All rights reserved.

Host-guest inclusion system of ferulic acid with p-Sulfonatocalix[n]arenes: Preparation, characterization and antioxidant activity

NASA Astrophysics Data System (ADS)

Chao, Jianbin; Wang, Huijuan; Song, Kailun; Wang, Yongzhao; Zuo, Ying; Zhang, Liwei; Zhang, Bingtai

2017-02-01

The inclusion complexes of ferulic acid (FA) with p-Sulfonatocalix[n]arenes (SCXn, n = 4, 6, 8) were prepared and characterized both in the solid state and in solution using fluorescence spectroscopy, 1H nuclear magnetic resonance (1H NMR), attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR), atomic force microscopy (AFM) and differential scanning calorimetry (DSC). The results show that FA is able to form inclusion complexes with SCXn in a molar ratio of 1:1, causing a significant decrease in the fluorescence intensity of FA. The association constant of the inclusion complexes was calculated from the fluorescence titration data. 1H NMR spectroscopy analysis demonstrates that the aromatic ring and methoxy group of FA are partially covered by SCXn.

[Effect of glyceryl triacetate on properties of PLA/PBAT blends].

PubMed

Yang, Nan; Wang, Xiyuan; Weng, Yunxuan; Jin, Yujuan; Zhang, Min

2016-06-25

Poly lactic acid (PLA)/Poly (butyleneadipate-co-terephthalate)(PBAT) and glyceryl triacetate (GTA) blend were prepared by torque rheometer, and the effect of GTA on thermodynamical performance, mechanical properties and microstructure of PLA/PBAT composites were studied using differential scanning calorimeter(DSC), dynamic mechanical analysis(DMA), universal testing machine, impact testing machine and scanning electron microscope(SEM). After adding GTA, Tg values of the two phases gradually became closer, blends cold crystallization temperature and melting temperature decreased. When with 3 phr GTA, the dispersed phase particle size of PLA/PBAT blend decreased. Mechanics performance test showed that the elongation at break and impact strength of the PLA/PBAT blend was greatly increased with 3 phr GTA, and the elongation at break increased 2.6 times, improved from 17.7% to 64.1%.

Self-Assembly, Supramolecular Organization, and Phase Behavior of L-Alanine Alkyl Esters (n = 9-18) and Characterization of Equimolar L-Alanine Lauryl Ester/Lauryl Sulfate Catanionic Complex.

PubMed

Sivaramakrishna, D; Swamy, Musti J

2015-09-08

A homologous series of l-alanine alkyl ester hydrochlorides (AEs) bearing 9-18 C atoms in the alkyl chain have been synthesized and characterized with respect to self-assembly, supramolecular structure, and phase transitions. The CMCs of AEs bearing 11-18 C atoms were found to range between 0.1 and 10 mM. Differential scanning calorimetric (DSC) studies showed that the transition temperatures (Tt), enthalpies (ΔHt) and entropies (ΔSt) of AEs in the dry state exhibit odd-even alternation, with the odd-chain-length compounds having higher Tt values, but the even-chain-length homologues showing higher values of ΔHt and ΔSt. In DSC measurements on hydrated samples, carried out at pH 5.0 and pH 10.0 (where they exist in cationic and neutral forms, respectively), compounds with 13-18 C atoms in the alkyl chain showed sharp gel-to-liquid crystalline phase transitions, and odd-even alternation was not seen in the thermodynamic parameters. The molecular structure, packing properties, and intermolecular interactions of AEs with 9 and 10 C atoms in the alkyl chain were determined by single crystal X-ray diffraction, which showed that the alkyl chains are packed in a tilted interdigitated bilayer format. d-Spacings obtained from powder X-ray diffraction studies exhibited a linear dependence on the alkyl chain length, suggesting that the other AEs also adopt an interdigitated bilayer structure. Turbidimetric, fluorescence spectroscopic, and isothermal titration calorimetric (ITC) studies established that in aqueous dispersions l-alanine lauryl ester hydrochloride (ALE·HCl) and sodium dodecyl sulfate (SDS) form an equimolar complex. Transmission electron microscopic and DSC studies indicate that the complex exists as unilamellar liposomes, which exhibit a sharp phase transition at ∼39 °C. The aggregates were disrupted at high pH, suggesting that the catanionic complex would be useful to develop a base-labile drug delivery system. ITC studies indicated that ALE·HCl forms a strong complex with DNA, suggesting that the AEs may find use in DNA therapeutics as well.

Bio-Inspired Metallo-Supramolecular Polymers for Combined Mechanical Properties

DTIC Science & Technology

2010-01-01

3 4 5 6 0 50 100 150 200 Temp (°C) H ea t F lo w (m W ) Figure 8. DSC trace of polymer 7. 1H NMR analysis indicated complete reaction of the...static and dynamic mechanical analysis methods. 11 5. References 1. Guan, Z. Polymer International 2007, 56, 467. 2. Oberhauser, A. F ...Hansma, P. K.; Carrion-Vazques, M.; Fernandez, J. M. Proc. Natl. Acad. Sci. USA 2001, 98, 468. 3. Reif, M. Gautel, M.; Oesterhelt, F .; Fernandez, J

Analytical solutions by squeezing to the anisotropic Rabi model in the nonperturbative deep-strong-coupling regime

NASA Astrophysics Data System (ADS)

Zhang, Yu-Yu; Chen, Xiang-You

2017-12-01

An unexplored nonperturbative deep strong coupling (npDSC) achieved in superconducting circuits has been studied in the anisotropic Rabi model by the generalized squeezing rotating-wave approximation. Energy levels are evaluated analytically from the reformulated Hamiltonian and agree well with numerical ones in a wide range of coupling strength. Such improvement ascribes to deformation effects in the displaced-squeezed state presented by the squeezed momentum variance, which are omitted in previous displaced states. The atom population dynamics confirms the validity of our approach for the npDSC strength. Our approach offers the possibility to explore interesting phenomena analytically in the npDSC regime in qubit-oscillator experiments.

Summary of Results from the Mars Phoenix Lander's Thermal Evolved Gas Analyzer

NASA Technical Reports Server (NTRS)

Sutter, B.; Ming, D. W.; Boynton, W. V.; Niles, P. B.; Hoffman, J.; Lauer, H. V.; Golden, D. C.

2009-01-01

The Mars Phoenix Scout Mission with its diverse instrument suite successfully examined several soils on the Northern plains of Mars. The Thermal and Evolved Gas Analyzer (TEGA) was employed to detect evolved volatiles and organic and inorganic materials by coupling a differential scanning calorimeter (DSC) with a magnetic-sector mass spectrometer (MS) that can detect masses in the 2 to 140 dalton range [1]. Five Martian soils were individually heated to 1000 C in the DSC ovens where evolved gases from mineral decompostion products were examined with the MS. TEGA s DSC has the capability to detect endothermic and exothermic reactions during heating that are characteristic of minerals present in the Martian soil.

Mechanical performance of hybrid polyester composites reinforced Cloisite 30B and kenaf fibre

NASA Astrophysics Data System (ADS)

Bonnia, N. N.; Surip, S. N.; Ratim, S.; Mahat, M. M.

2012-06-01

Hybridization of rubber toughened polyester-kenaf nanocomposite was prepared by adding various percentage of kenaf fiber with 4% Cloisite 30B in unsaturated polyester resin. Composite were prepared by adding filler to modified polyester resin subsequently cross-linked using methyl ethyl ketone peroxide and the accelerator cobalt octanoate 1%. Three per hundred rubbers (phr) of liquid natural rubber (LNR) were added in producing this composite. This composite expected to be applied in the interior of passenger cars and truck cabins. This is a quality local product from a combination of good properties polyester and high performance natural fiber, kenaf that is suitable for many applications such as in automotive sector and construction sector. The mechanical and thermal properties of composite were characterized using Durometer Shore-D hardness test, Izod impact test, Scanning electron microscopy, thermogravimetry (TGA) and differential scanning calorimetry (DSC). Result shows that addition of LNR give good properties on impact, flexural and hardness compare to without LNR composite. DSC curve shows that all composition of composites is fully cured and good in thermal properties. Addition of higher percentage of kenaf will lead the composite to elastic behavior and decrease the toughened properties of the composite. Hybrid system composite showed the flexural properties within the flexural properties of kenaf - polyester and Cloisite 30B.

Radiation-induced grafting of acrylic acid onto polypropylene film and its biodegradability

NASA Astrophysics Data System (ADS)

Mandal, Dev K.; Bhunia, Haripada; Bajpai, Pramod K.; Chaudhari, C. V.; Dubey, K. A.; Varshney, L.

2016-06-01

Polypropylene based commodity polyolefins are widely used in packaging, manufacturing, electrical, pharmaceutical and other applications. The aim of the present work is to study the effect of grafting of acrylic acid on the biodegradability of acrylic acid grafted polypropylene. The effect of different conditions showed that grafting percentage increased with increase in monomer concentration, radiation dose and inhibitor concentration but decreased with increase in radiation dose rate. The maximum grafting of 159.4% could be achieved at optimum conditions. The structure of grafted polypropylene films at different degree of grafting was characterized by EDS, FTIR, TGA, DSC, SEM and XRD. EDS studies showed that the increase in acrylic acid grafting percentage increased the hydrophilicity of the grafted films. FTIR studies indicated the presence of acrylic acid on the surface of polypropylene film. TGA studies revealed that thermal stability decreased with increase in grafting percentage. DSC studies showed that melting temperature and crystallinity of the grafted polypropylene films lower than polypropylene film. SEM studies indicated that increase in acrylic acid grafting percentage increased the wrinkles in the grafted films. The maximum biodegradability could be achieved to 6.85% for 90.5% grafting. This suggested that microorganisms present in the compost could biodegrade acrylic acid grafted polypropylene.

Variable-focus microscopy and UV surface dissolution imaging as complementary techniques in intrinsic dissolution rate determination.

PubMed

Ward, Adam; Walton, Karl; Box, Karl; Østergaard, Jesper; Gillie, Lisa J; Conway, Barbara R; Asare-Addo, Kofi

2017-09-15

This work reports a novel approach to the assessment of the surface properties of compacts used in Surface Dissolution Imaging (SDI). SDI is useful for determining intrinsic dissolution rate (IDR), an important parameter in early stage drug development. Surface topography, post-compaction and post-SDI run, have been measured using a non-contact, optical, three-dimensional microscope based on focus variation, the Alicona Infinite Focus Microscope, with the aim of correlating the IDRs to the surface properties. Ibuprofen (IBU) was used as a model poorly-soluble drug. DSC and XRD were used to monitor possible polymorphic changes that may have occurred post-compaction and post-SDI run. IBUs IDR decreased from 0.033mg/min/cm 2 to 0.022mg/min/cm 2 from 10 to 20min, respectively, during the experiment. XRD and DSC showed no form changes during the SDI run. The surface topography images showed that a distinct imprint was embossed on the surfaces of some compacts which could affect IDRs. Surface parameter values were associated with the SDI experiments which showed strong correlations with the IDR values. The variable-focus microscope can be used as a complimentary tool in the determination of IDR values from the SDI. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Implications of Thermal Annealing on the Benzene Vapor Sensing Behavior of PEVA-Graphene Nanocomposite Threads.

PubMed

Patel, Sanjay V; Cemalovic, Sabina; Tolley, William K; Hobson, Stephen T; Anderson, Ryan; Fruhberger, Bernd

2018-03-23

The effect of thermal treatments, on the benzene vapor sensitivity of polyethylene (co-)vinylacetate (PEVA)/graphene nanocomposite threads, used as chemiresistive sensors, was investigated using DC resistance measurements, differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). These flexible threads are being developed as low-cost, easy-to-measure chemical sensors that can be incorporated into smart clothing or disposable sensing patches. Chemiresistive threads were solution-cast or extruded from PEVA and <10% graphene nanoplatelets (by mass) in toluene. Threads were annealed at various temperatures and showed up to 2 orders of magnitude decrease in resistance with successive anneals. Threads heated to ≥80 °C showed improved limits of detection, resulting from improved signal-noise, when exposed to benzene vapor in dry air. In addition, annealing increased the speed of response and recovery upon exposure to and removal of benzene vapor. DSC results showed that the presence of graphene raises the freezing point, and may allow greater crystallinity, in the nanocomposite after annealing. SEM images confirm increased surface roughness/area, which may account for the increase response speed after annealing. Benzene vapor detection at 5 ppm is demonstrated with limits of detection estimated to be as low as 1.5 ppm, reflecting an order of magnitude improvement over unannealed threads.

Effect of Chemical Washing Pre-treatment of Empty Fruit Bunch (EFB) biochar on Characterization of Hydrogel Biochar composite as Bioadsorbent

NASA Astrophysics Data System (ADS)

Meri, N. H.; Alias, A. B.; Talib, N.; Rashid, Z. A.; Wan, W. A.; Ghani, Ab Karim

2018-05-01

Hydrogel biochar composite (HBC) is a recent interest among researchers because of the hydrophilic characteristic which can adsorb chemical fluid and showed a versatile potential as adsorbent in removing hazardous material in wastewater and gas stream. In this study, the effect of chemical washing pre-treatment by using two different type of chemical agent Hydrochloric Acid (HCL) and Hydrogen Peroxide (H2O2) was analysed and investigated. The raw EFB biochar was prepared using microwave assisted pyrolysis under 1000W for 30 min under N2 flow with 150 mL/min. To improve the adsoprtion ability, the EFB biochar has been chemical washed pre-treatment with Hydrochloric Acid (HCl) and Hydrogen Peroxide (H2O2) before polymerization process with acrylamide (AAm) as monomer, N,N’-methylenebisacrylamide (MBA) as crosslinker and ammonium persulfate (APS) as initiator. The characterization has studied by using Fourier transform infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). FTIR result shows that, the formation of Raw EFB to Hydrogel Biochar Composite (Raw EFB > EFB Biochar > Treated Biochars (HCl & H2O2) > Hydrogel Biochar Composite) have changed in functional group. For DSC result it shows that the thermal behaviour of all samples is endothermic process and have high thermal resistance.

Improved Cytotoxic Effect of Doxorubicin by Its Combination with Sclareol in Solid Lipid Nanoparticle Suspension.

PubMed

Oliveira, Mariana Silva; Lima, Bruno Henrique Santiago; Goulart, Gisele Assis Castro; Mussi, Samuel Vidal; Borges, Gabriel Silva Marques; Oréfice, Rodrigo Lambert; Ferreira, Lucas Antônio Miranda

2018-08-01

This work aims to develop, characterize, and evaluate the anticancer activity of solid lipid nanoparticles (SLN) containing doxorubicin (DOX), an antitumoral from the antracycline class, and sclareol (SC), a lipophilic labdene diterpene (SLN-DOX-SC). The SLN were characterized by Differential Scanning Calorimetry (DSC), X-ray Diffraction (XRD), Small Angle X-ray Diffraction (SAXS), in vitro release, transmission electron microscopy, and polarized light microscopy. Evaluation of cell viability was performed in two cell cultures: MCF-7 (human breast cancer) and 4T1 (murine breast cancer). The SLN showed a size in the range of 128 nm, negative zeta potential, DOX encapsulation efficiency (EE) of 99%, and drug loading (DL) of 66 mg/g. Characterization of the formulation by DSC, XRD, and SAXS revealed the presence of DOX inside the nanoparticles of SLN and suggested increased expulsion/release of this drug when associated with SC. The release profiles revealed that the SLN-DOX-SC showed controlled release of DOX at pH 7.4 with enhanced drug release at low pH, useful for cancer treatment. The SLN-DOX-SC demonstrated to be more effective than the free DOX against 4T1 cells. So, the developed SLN efficiently encapsulate DOX and SC and show good potential as an alternative for cancer treatment.

Physicochemical characteristics and antioxidant activity of Prunus cerasoides D. Don gum exudates.

PubMed

Malsawmtluangi, C; Thanzami, K; Lalhlenmawia, H; Selvan, Veenus; Palanisamy, Selvamani; Kandasamy, Ruckmani; Pachuau, Lalduhsanga

2014-08-01

The physicochemical properties and antioxidant activity of Prunus cerasoides D. Don gum exudates was investigated in this study. The total carbohydrate and protein content were found to be 73.72±2.44% and 2.33±1.25%, respectively. Analysis of monosaccharide composition by HPLC-RI system after acid hydrolysis of the gum showed the presence of arabinose, galactose, glucose, rhamnose and xylose. The molecular weight of the gum was also found to be 5.55×10(5)Da. FTIR and DSC studies showed characteristics typical of a natural polysaccharide. The viscosity of 2% aqueous solution of the gum exhibited non-Newtonian type of flow and the gum was also found to show pH dependent swelling. Determination of the angle of repose, Carr's index and Hausner ratio indicate the gum possess fairly good powder flow property. The antioxidant properties of the gum were evaluated by determining DPPH and hydroxyl scavenging activities, reducing power and total phenolic contents which showed the gum possess antioxidant property. Copyright © 2014 Elsevier B.V. All rights reserved.

Drill Sergeant Candidate Transformation

DTIC Science & Technology

2009-02-01

leadership styles of NCOs entering Drill Sergeant School (DSS). ARI also developed and administered a prototype DS Assessment Battery to assess...preferred leadership styles . DSS training increases both the degree to which the DSC feels obligated to and identifies with the Army. DSS training...4 TABLE 3. PREFERRED LEADERSHIP STYLES DEFINITIONS .............................................6 TABLE 4. DSC CHANGE IN

TU-CD-BRA-04: Evaluation of An Atlas-Based Segmentation Method for Prostate and Peripheral Zone Regions On MRI

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nelson, AS; Piper, J; Curry, K

2015-06-15

Purpose: Prostate MRI plays an important role in diagnosis, biopsy guidance, and therapy planning for prostate cancer. Prostate MRI contours can be used to aid in image fusion for ultrasound biopsy guidance and delivery of radiation. Our goal in this study is to evaluate an automatic atlas-based segmentation method for generating prostate and peripheral zone (PZ) contours on MRI. Methods: T2-weighted MRIs were acquired on 3T-Discovery MR750 System (GE, Milwaukee). The Volumes of Interest (VOIs): prostate and PZ were outlined by an expert radiation oncologist and used to create an atlas library for atlas-based segmentation. The atlas-segmentation accuracy was evaluatedmore » using a leave-one-out analysis. The method involved automatically finding the atlas subject that best matched the test subject followed by a normalized intensity-based free-form deformable registration of the atlas subject to the test subject. The prostate and PZ contours were transformed to the test subject using the same deformation. For each test subject the three best matches were used and the final contour was combined using Majority Vote. The atlas-segmentation process was fully automatic. Dice similarity coefficients (DSC) and mean Hausdorff values were used for comparison. Results: VOIs contours were available for 28 subjects. For the prostate, the atlas-based segmentation method resulted in an average DSC of 0.88+/−0.08 and a mean Hausdorff distance of 1.1+/−0.9mm. The number of patients (#) in DSC ranges are as follows: 0.60–0.69(1), 0.70–0.79(2), 0.80–0.89(13), >0.89(11). For the PZ, the average DSC was 0.72+/−0.17 and average Hausdorff of 0.9+/−0.9mm. The number of patients (#) in DSC ranges are as follows: <0.60(4), 0.60–0.69(6), 0.70–0.79(7), 0.80–0.89(9), >0.89(1). Conclusion: The MRI atlas-based segmentation method achieved good results for both the whole prostate and PZ compared to expert defined VOIs. The technique is fast, fully automatic, and has the potential to provide significant time savings for prostate VOI definition. AS Nelson and J Piper are partial owners of MIM Software, Inc. AS Nelson, J Piper, K Curry, and A Swallen are current employees at MIM Software, Inc.« less