Aqueous solutions of proline and NaCl studied by differential scanning calorimetry at subzero temperatures

DEFF Research Database (Denmark)

Rasmussen, Peter Have; Jørgensen, Bo; Nielsen, Jette

1997-01-01

The hydration properties of proline are studied by differential scanning calorimetry (DSC) in aqueous solutions during freezing to -60 degrees C and subsequent heating to +20 degrees C. The concentration of proline in the freeze concentrated solution was estimated to approximately 50 wt% (w/w) in...... plants and insects living under water stress conditions is discussed. (C) 1997 Elsevier Science B.V....

Recent advances and potential applications of modulated differential scanning calorimetry (mDSC) in drug development

DEFF Research Database (Denmark)

Knopp, Matthias Manne; Löbmann, Korbinian; Elder, David P.

2016-01-01

Differential scanning calorimetry (DSC) is frequently the thermal analysis technique of choice within preformulation and formulation sciences because of its ability to provide detailed information about both the physical and energetic properties of a substance and/or formulation. However, convent......-dried formulations. However, as discussed in the present review, a number of other potential applications could also be relevant for the pharmaceutical scientist....

Modulated Temperature Differential Scanning Calorimetry Theoretical and Practical Applications in Polymer Characterisation

CERN Document Server

Reading, Mike

2006-01-01

MTDSC provides a step-change increase in the power of calorimetry to characterize virtually all polymer systems including curing systems, blends and semicrystalline polymers. It enables hidden transitions to be revealed, miscibility to be accurately assessed, and phases and interfaces in complex blends to be quantified. It also enables crystallinity in complex systems to be measured and provides new insights into melting behaviour. All of this is achieved by a simple modification of conventional DSC. In 1992 a new calorimetric technique was introduced that superimposed a small modulation on top of the conventional linear temperature program typically used in differential scanning calorimetry. This was combined with a method of data analysis that enabled the sample’s response to the linear component of the temperature program to be separated from its response to the periodic component. In this way, for the first time, a signal equivalent to that of conventional DSC was obtained simultaneously with a measure ...

On the Frequency Correction in Temperature-Modulated Differential Scanning Calorimetry of Glass Transition

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, J.C.; Allan, D.C.

2012-01-01

Temperature-modulated differential scanning calorimetry (TMDSC) is based on conventional DSC but with a sinusoidally modulated temperature path. Simulations of TMDSC signals were performed for Corning EAGLE XG® glass over a wide range of modulation frequencies. Our results reveal that the frequency...... correction commonly used in the interpretation of TMDSC signals leads to a master nonreversing heat flow curve independent of modulation frequency, provided that sufficiently high frequencies are employed in the TMDSC measurement. A master reversing heat flow curve can also be generated through the frequency...

Insights into glass transition and relaxation behavior using temperature-modulated differential scanning calorimetry

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, J.C.; Allan, D.C.

Temperature-modulated differential scanning calorimetry (TMDSC) is based on conventional DSC but with a sinusoidally modulated temperature path. Our simulations of TMDSC signals prove that the frequency correction of non-reversing heat flow can give a master curve within a certain range...... of frequencies. This frequency range is dependent not only on the measurement parameters such as linear heating/cooling rate and frequency and amplitude of the modulation, but also on the previous thermal history before the TMDSC measurement. The frequency correction for the reversing heat flow gives more...

Physico-chemical changes in heavy ions irradiated polymer foils by differential scanning calorimetry

International Nuclear Information System (INIS)

Ciesla, K.; Trautmann, Ch.; Vansant, E.F.

1994-01-01

The sample of commercial PETP (Hostaphan) and very heavy ions irradiated products were investigated by differential scanning calorimetry in nitrogen flow. Irradiation were performed with Dy ions of 13 MeV/u with fluences 5 x 10 10 ions/cm 2 . Differences were observed in melting behaviour of unirradiated and irradiated foils. The influence of irradiation conditions on the results was noticed. Moreover the samples of polyimide (Kapton) and polycarbonate (Macrofol) irradiated in similar conditions were examined by DSC. The DSC traces have been compared with those of unirradiated reference samples. (author). 8 refs, 5 figs

Hydrogen concentration determination in pressure tube samples using differential scanning calorimetry (dsc)

International Nuclear Information System (INIS)

Marinescu, R.; Mincu, M.

2015-01-01

Zirconium alloys are widely used as a structural material in nuclear reactors. It is known that zirconium based cladding alloys absorb hydrogen as a result of service in a pressurized water reactor. Hydrogen absorbed (during operation of the reactor) in the zirconium alloy, out of which the pressure tube is made, is one of the major factors determining the life time of the pressure tube. For monitoring the hydrides, samples of the pressure tube are periodically taken and analyzed. At normal reactor operating temperature, hydrogen has limited solubility in the zirconium lattice and precipitates out of solid solution as zirconium hydride when the solid solubility is exceeded. As a consequences material characterization of Zr-2.5Nb CANDU pressure tubes is required after manufacturing but also during the operation to assess its structural integrity and to predict its behavior until the next in-service inspection. Hydrogen and deuterium concentration determination is one of the most important parameters to be evaluated during the experimental tests. Hydrogen present in zirconium alloys has a strong effect of weakening. Following the zirconium-hydrogen reaction, the resulting zirconium hydride precipitates in the mass of material. Weakening of the material, due to the presence of 10 ppm of precipitated hydrogen significantly affects some of its properties. The concentration of hydrogen in a sample can be determined by several methods, one of them being the differential scanning calorimetry (DSC). The principle of the method consists in measuring the difference between the amount of heat required to raise the temperature of a sample and a reference to a certain value. The experiments were made using a TA Instruments DSC Q2000 calorimeter. This paper contains experimental work for hydrogen concentration determination by Differential Scanning Calorimetry (DSC) method. Also, the reproducibility and accuracy of the method used at INR Pitesti are presented. (authors)

Irreversible denaturation of maltodextrin glucosidase studied by differential scanning calorimetry, circular dichroism, and turbidity measurements.

Science.gov (United States)

Goyal, Megha; Chaudhuri, Tapan K; Kuwajima, Kunihiro

2014-01-01

Thermal denaturation of Escherichia coli maltodextrin glucosidase was studied by differential scanning calorimetry, circular dichroism (230 nm), and UV-absorption measurements (340 nm), which were respectively used to monitor heat absorption, conformational unfolding, and the production of solution turbidity. The denaturation was irreversible, and the thermal transition recorded at scan rates of 0.5-1.5 K/min was significantly scan-rate dependent, indicating that the thermal denaturation was kinetically controlled. The absence of a protein-concentration effect on the thermal transition indicated that the denaturation was rate-limited by a mono-molecular process. From the analysis of the calorimetric thermograms, a one-step irreversible model well represented the thermal denaturation of the protein. The calorimetrically observed thermal transitions showed excellent coincidence with the turbidity transitions monitored by UV-absorption as well as with the unfolding transitions monitored by circular dichroism. The thermal denaturation of the protein was thus rate-limited by conformational unfolding, which was followed by a rapid irreversible formation of aggregates that produced the solution turbidity. It is thus important to note that the absence of the protein-concentration effect on the irreversible thermal denaturation does not necessarily means the absence of protein aggregation itself. The turbidity measurements together with differential scanning calorimetry in the irreversible thermal denaturation of the protein provided a very effective approach for understanding the mechanisms of the irreversible denaturation. The Arrhenius-equation parameters obtained from analysis of the thermal denaturation were compared with those of other proteins that have been reported to show the one-step irreversible thermal denaturation. Maltodextrin glucosidase had sufficiently high kinetic stability with a half-life of 68 days at a physiological temperature (37°C).

Evaluation of errors in determination of DNA melting curve registered with differential scanning calorimetry

International Nuclear Information System (INIS)

Lando, D.Y.; Fridman, A.S.; Galyuk, E.N.; Dalyan, Y.B.; Grigoryan, I.E.; Haroutiunian, S.G.

2013-01-01

The differential scanning calorimetry (DSC) is more sensitive than UV absorption spectrophotometry as a tool for the measurement of DNA melting curves. The advantage of DSC is a direct determination of differential melting curves (DMC) obtained without numerical differentiation. However, the difference between the helix-coil transition enthalpies of AT and GC base pairs can cause distortions in the shape of melting curve. Up to date, the errors caused by those distortions were not evaluated. In this study, a simple procedure of recalculation of a calorimetric DMC into a real DMC is developed. It demonstrates that the 'real' melting curve and differential melting curve deviate very slightly from the same two curves calculated from DSC data. The melting temperature and the temperature melting range are usually the same even if the difference in the enthalpies is several times higher than a real one

Application of the modulated temperature differential scanning calorimetry technique for the determination of the specific heat of copper nanofluids

International Nuclear Information System (INIS)

De Robertis, E.; Cosme, E.H.H.; Neves, R.S.; Kuznetsov, A.Yu.; Campos, A.P.C.; Landi, S.M.; Achete, C.A.

2012-01-01

The purpose of this work is to investigate the applicability of the modulated temperature differential scanning calorimetry technique to measure specific heat of copper nanofluids by using the ASTM E2719 standard procedure, which is generally applied to thermally stable solids and liquids. The one-step method of preparation of copper nanofluid samples is described. The synthesized nanoparticles were separated from the base fluid and examined by X-ray diffraction and transmission electron microscopy in order to evaluate their structure, morphology and chemical nature. The presence of copper nanoparticles in the base fluid alters the characteristics of crystallization and melting processes and reduces the specific heat values of nanofluids in the whole studied temperature range. - Highlights: ► Copper nanofluids prepared by one-step method. ► Methodology of synthesis improved nanofluid stability. ► Specific heat determinations using modulated temperature differential scanning calorimetry. ► Good agreement between theoretical and experimental values.

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

Science.gov (United States)

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.

Glass transition of anhydrous starch by fast scanning calorimetry.

Science.gov (United States)

Monnier, Xavier; Maigret, Jean-Eudes; Lourdin, Denis; Saiter, Allisson

2017-10-01

By means of fast scanning calorimetry, the glass transition of anhydrous amorphous starch has been measured. With a scanning rate of 2000Ks -1 , thermal degradation of starch prior to the glass transition has been inhibited. To certify the glass transition measurement, structural relaxation of the glassy state has been investigated through physical aging as well as the concept of limiting fictive temperature. In both cases, characteristic enthalpy recovery peaks related to the structural relaxation of the glass have been observed. Thermal lag corrections based on the comparison of glass transition temperatures measured by means of differential and fast scanning calorimetry have been proposed. The complementary investigations give an anhydrous amorphous starch glass transition temperature of 312±7°C. This estimation correlates with previous extrapolation performed on hydrated starches. Copyright © 2017 Elsevier Ltd. All rights reserved.

Reversible amorphous-crystalline phase changes in a wide range of Se1-xTex alloys studied using ultrafast differential scanning calorimetry

NARCIS (Netherlands)

Vermeulen, Paul. A.; Momand, Jamo; Kooi, Bart J.

The reversible amorphous-crystalline phase change in a chalcogenide material, specifically the Se1-xTex alloy, has been investigated for the first time using ultrafast differential scanning calorimetry. Heating rates and cooling rates up to 5000 K/s were used. Repeated reversible

Low-temperature transitions in cod and tuna determined by differential scanning calorimetry

DEFF Research Database (Denmark)

Jensen, Kristina Nedenskov; Jørgensen, Bo; Nielsen, Jette

2003-01-01

Differential scanning calorimetry measurements have revealed different thermal transitions in cod and tuna samples. Transition temperatures detected Lit -11degreesC, -15degreesC and -21degreesC were highly dependent on the annealing temperature. In tuna muscle an additional transition was observed...... at -72degreesC. This transition appeared differently than the thermal events observed at higher temperatures, as it spanned a broad temperature interval of 25degreesC. The transition was comparable to low-temperature glass transitions reported in protein-rich systems. No transition at this low...... temperature was detected in cod samples. The transitions observed at higher temperatures (-11degreesC to -21degreesC) may possibly stein from a glassy matrix containing muscle proteins. However, the presence of a glass transition at - 11degreesC was in disagreement with the low storage stability at -18degrees...

Resolving glass transition in Te-based phase-change materials by modulated differential scanning calorimetry

Science.gov (United States)

Chen, Yimin; Mu, Sen; Wang, Guoxiang; Shen, Xiang; Wang, Junqiang; Dai, Shixun; Xu, Tiefeng; Nie, Qiuhua; Wang, Rongping

2017-10-01

Glass transitions of Te-based phase-change materials (PCMs) were studied by modulated differential scanning calorimetry. It was found that both Ge2Sb2Te5 and GeTe are marginal glass formers with ΔT (= T x - T g) less than 2.1 °C when the heating rate is below 3 °C min-1. The fragilities of Ge2Sb2Te5 and GeTe can be estimated as 46.0 and 39.7, respectively, around the glass transition temperature, implying that a fragile-to-strong transition would be presented in such Te-based PCMs. The above results provide direct experimental evidence to support the investigation of crystallization kinetics in supercooled liquid PCMs.

Phase-separation phenomena in solutions of poly(2,6-dimethyl-1,4 phenylene oxide). II. Differential scanning calorimetry of solutions in toluene

NARCIS (Netherlands)

Koenhen, D.M.; Smolders, C.A.

1977-01-01

The phase-separation phenomena observed in solutions of poly(2,6 dimethyl-1,4 phenylene oxide) in toluene have been investigated by differential scanning calorimetry. These measurements supplement the experimental evidence in favor of the concept that the phase transitions observed are

Effect of temperature on studtite stability: Thermogravimetry and differential scanning calorimetry investigations

International Nuclear Information System (INIS)

Rey, A.; Casas, I.; Gimenez, J.; Quinones, J.; Pablo, J. de

2009-01-01

The main objective of this work is the study of the influence of temperature on the stability of the uranyl peroxide tetrahydrate (UO 2 O 2 . 4H 2 O) studtite, which may form on the spent nuclear fuel surface as a secondary solid phase. Preliminary results on the synthesis of studtite in the laboratory at different temperatures have shown that the solid phases formed when mixing hydrogen peroxide and uranyl nitrate depends on temperature. Studtite is obtained at 298 K, meta-studtite (UO 2 O 2 . 2H 2 O) at 373 K, and meta-schoepite (UO 3 . nH 2 O, with n 3 O 8 . By means of the differential scanning calorimetry the molar enthalpies of the transformations occurring at 403 and 504 K have been determined to be -42 ± 10 and -46 ± 2 kJ mol -1 , respectively

Pressure-modulated differential scanning calorimetry. An approach to the continuous, simultaneous determination of heat capacities and expansion coefficients.

Science.gov (United States)

Boehm, K; Rösgen, J; Hinz, H-J

2006-02-15

A new method is described that permits the continuous and synchronous determination of heat capacity and expansibility data. We refer to it as pressure-modulated differential scanning calorimetry (PMDSC), as it involves a standard DSC temperature scan and superimposes on it a pressure modulation of preselected format. The power of the method is demonstrated using salt solutions for which the most accurate heat capacity and expansibility data exist in the literature. As the PMDSC measurements could reproduce the parameters with high accuracy and precision, we applied the method also to an aqueous suspension of multilamellar DSPC vesicles for which no expansibility data had been reported previously for the transition region. Excellent agreement was obtained between data from PMDSC and values from independent direct differential scanning densimetry measurements. The basic theoretical background of the method when using sawtooth-like pressure ramps is given under Supporting Information, and a complete statistical thermodynamic derivation of the general equations is presented in the accompanying paper.

Study of phase changing characteristics of granular composites using differential scanning calorimetry

International Nuclear Information System (INIS)

Rady, Mohamed

2009-01-01

Characterization of the phase changing behavior of granular materials is an important issue for design and optimization of latent heat thermal energy storage (LHTES) systems. In the present work, differential scanning calorimetry (DSC) has been used to study the phase changing behavior of granular composites consisting of ceramic encapsulated phase change material (EPCM) with particle diameters of 1-3 mm. The obtained DSC curves characterizing melting and solidification of the composite material are shown to be dependent upon the values of heating and cooling rates. Direct utilization of the measured DSC curves could result in an inexact representation of the sample enthalpy change. A simple procedure has been advised to obtain accurate quantitative results from the DSC measurements based on the estimation of the thermal resistance between the sample and its enclosure. Analysis of the evolution of latent heat of EPCM with temperature at different values of cooling/heating rates is presented.

Using differential scanning calorimetry, laser refractometry, electrical conductivity and spectrophotometry for discrimination of different types of Bulgarian honey

International Nuclear Information System (INIS)

Vlaeva, I; Nikolova, K; Tsankova, D; Bodurov, I; Marudova, M; Viraneva, A; Yovcheva, T; Lekova, S

2017-01-01

The potential of several physical methods for investigation of the botanical origin of honey has been discussed. Samples from the three most prevalent types of honey in Bulgaria (acacia, linden and honeydew) have been used. They have been examined by laser refractometry, UV, VIS and FTIR spectroscopy, electric conductivity measurement and differential scanning calorimetry. The purpose of this study was to reveal the physical characterizations of honeys from different flora produced in Bulgaria and to identify honeys with a high apitherapy potential for future studies. (paper)

Study and characterization of ammonium diuranate and uranium trioxide by thermogravimetry and differential scanning calorimetry

International Nuclear Information System (INIS)

Dantas, J.M.

1983-01-01

Thermogravimetry (TG), Differential Thermogravimetry (DTG) and Differential Scanning Calorimetry (DSC) were used to characterize the thermal behavior of ammonium diuranate (ADU) and uranium trioxide (UO 3 ) produced at IPEN'S Chemical Enginnering Department. Compounds characterization was done using the molar ratios among the compounds and the oxides resulting from thermal decomposition. The TG and DTG curves registered for each sample were used for the determination of the following temperatures: - temperature of water evolution (free and crystallized water); - ammonia evolution and oxidation temperature; - ocluded ammonium nitrate decomposition temperature and - oxygen release temperature. The intermediate phases and their thermal stabilities were also identified by TG and DTG and confirmed by DSC curves, DSC curves showed also the exothermic and endothermic behavior of the processes involved. Finally, the great amount of data collected in this study can be handed as a guide by the professionals responsible for the operation of ADU,UO 3 and UF 4 pilot plants. (Author) [pt

Stability of some Cactaceae proteins based on fluorescence, circular dichroism, and differential scanning calorimetry measurements.

Science.gov (United States)

Gorinstein, S; Zemser, M; Vargas-Albores, F; Ochoa, J L; Paredes-Lopez, O; Scheler, C; Aksu, S; Salnikow, J

1999-02-01

Characterization of three cactus proteins (native and denatured) from Machaerocereus gummosus (Pitahaya agria), Lophocereu schottii (Garambullo), and Cholla opuntia (Cholla), was based on electrophoretic, fluorescence, CD (circular dichroism), DSC (differential scanning calorimetry), and FT-IR (Fourier transform infrared) measurements. The obtained results of intrinsic fluorescence, DSC, and CD were dissimilar for the three species of cactus, providing evidence of differences in secondary and tertiary structures. Cactus proteins may be situated in the following order corresponding to their relative stability: Machaerocereus gummosus (Pitahaya agria) > Cholla opuntia (Cholla) > Lophocereu schottii (Garambullo). Thermodynamic properties of proteins and their changes upon denaturation (temperature of denaturation, enthalphy, and the number of ruptured hydrogen bonds) were correlated with the secondary structure of proteins and disappearance of alpha-helix.

Morphological Investigation into Starch Bio-Nanocomposites via Synchrotron Radiation and Differential Scanning Calorimetry

Directory of Open Access Journals (Sweden)

Huihua Liu

2011-01-01

Full Text Available We studied a hydrophilic, plasticized bionanocomposite system involving sorbitol plasticizer, amylose biopolymer, and montmorillonite (MMT for the presence of competitive interactions among them at different moisture content. Synchrotron analysis via small angle X-ray scattering (SAXS and thermal analysis using differential scanning calorimetry (DSC were performed to understand crystalline growth and the distribution of crystalline domains within the samples. The SAXS diffraction patterns showed reduced interhelix spacing in the amylose network indicating strong amylose-sorbitol interactions. Depending on the sorbitol and MMT concentration, these interactions also affected the free moisture content and crystalline domains. Domains of around 95 Å and 312 Å were found in the low-moisture-content samples as compared to a single domain of 95 Å in the high-moisture-content samples. DSC measurements confirmed that the MMT increased the onset and the melting temperature of nanocomposites. Moreover, the results showed that the ternary interactions among sorbitol-amylose-MMT supported the crystalline heterogeneity through secondary nucleation.

Measurement and Model Validation of Nanofluid Specific Heat Capacity with Differential Scanning Calorimetry

Directory of Open Access Journals (Sweden)

Harry O'Hanley

2012-01-01

Full Text Available Nanofluids are being considered for heat transfer applications; therefore it is important to know their thermophysical properties accurately. In this paper we focused on nanofluid specific heat capacity. Currently, there exist two models to predict a nanofluid specific heat capacity as a function of nanoparticle concentration and material. Model I is a straight volume-weighted average; Model II is based on the assumption of thermal equilibrium between the particles and the surrounding fluid. These two models give significantly different predictions for a given system. Using differential scanning calorimetry (DSC, a robust experimental methodology for measuring the heat capacity of fluids, the specific heat capacities of water-based silica, alumina, and copper oxide nanofluids were measured. Nanoparticle concentrations were varied between 5 wt% and 50 wt%. Test results were found to be in excellent agreement with Model II, while the predictions of Model I deviated very significantly from the data. Therefore, Model II is recommended for nanofluids.

Measurement of the enthalpies of vaporization and sublimation of solids aromatic hydrocarbons by differential scanning calorimetry

International Nuclear Information System (INIS)

Rojas, Aaron; Orozco, Eulogio

2003-01-01

An experimental procedure is proposed for direct measurement of the heat involved in the vaporization of a solid organic compound above its normal melting temperature. This technique consists on the fusion of a solid aromatic hydrocarbon, which is then vaporized by a sudden decrease of the pressure. The direct register of heat flow as function of time by differential scanning calorimetry allows the quantifying of the enthalpy of vaporization of compounds such as phenanthrene, β-naphthol, pyrene, and anthracene. Enthalpies of vaporization were measured in an isothermal mode over a range of temperatures from 10 to 20 K above the melting temperatures of each compound, while enthalpies of fusion were determined from separate experiments performed in a scanning mode. Enthalpies of sublimation are computed from results of fusion and vaporization, and then compared with results from the literature, which currently are obtained by calorimetric or indirect techniques

Characterization of the molecular distribution of drugs in glassy solid dispersions at the nano-meter scale, using differential scanning calorimetry and gravimetric water vapour sorption techniques

NARCIS (Netherlands)

van Drooge, D J; Hinrichs, W L J; Visser, M R; Frijlink, H W

2006-01-01

The molecular distribution in fully amorphous solid dispersions consisting of poly(vinylpyrrolidone) (PVP)-diazepam and inulin-diazepam was studied. One glass transition temperature (T-g), as determined by temperature modulated differential scanning calorimetry (TMDSC), was observed in PVP-diazepam

Detection of a new 'nematic-like' phase in liquid crystal-amphiphile mixture by differential scanning calorimetry

Energy Technology Data Exchange (ETDEWEB)

Dan, Kaustabh, E-mail: kaustabhdan@gmail.com; Roy, Madhusudan, E-mail: kaustabhdan@gmail.com; Datta, Alokmay, E-mail: kaustabhdan@gmail.com [Surface Physics and Materials Science Division, Saha Institute of Nuclear Physics, 1/AF Bidhannagar Block, Sector 1, Kolkata-700064 (India)

2014-04-24

Differential Scanning Calorimetry (DSC) studies on phase transitions of the pure liquid crystalline material N-4-methoxybenzylidene-4-butylaniline (MBBA) and mixtures of MBBA and the amphiphile Stearic Acid (StA) show significant changes in the behavior of mixture from pure MBBA, as regards the nematic-isotropic (N-I) transition temperature (T{sub c}) and other thermodynamic parameters like enthalpy, specific heat and activation energy with concentration of StA. In particular, the convexity of the Arrhenius plot in pure MBBA vanishes with StA concentration pointing to the formation of a new, perhaps 'nematic-like', phase in the mixtures.

Investigation of phase transformations in ductile cast iron of differential scanning calorimetry

International Nuclear Information System (INIS)

Przeliorz, R; Piatkowski, J

2011-01-01

The effect of heating rate on phase transformations to austenite range in ductile cast iron of the EN-GJS-450-10 grade was investigated. For studies of phase transformations, the technique of differential scanning calorimetry (DSC) was used. Micro structure was examined by optical microscopy. The calorimetric examinations have proved that on heating three transformations occur in this grade of ductile iron, viz. magnetic transformation at the Curie temperature, pearlite→austenite transformation and ferrite→austenite transformation. An increase in the heating rate shifts the pearlite→austenite and ferrite→austenite transformations to higher temperature range. At the heating rate of 5 and 15 deg. C min -1 , local extrema have been observed to occur: for pearlite→austenite transformation at 784 deg. C and 795 deg. C, respectively, and for ferrite+ graphite →austenite transformation at 805 deg. C and 821 deg. C, respectively. The Curie temperature of magnetic transformation was extrapolated to a value of 740 deg. C. Each transformation is related with a specific thermal effect. The highest value of enthalpy is accompanying the ferrite→austenite transformation, the lowest occurs in the case of pearlite→austenite transformation.

A Differential Scanning Calorimetry Method for Construction of Continuous Cooling Transformation Diagram of Blast Furnace Slag

Science.gov (United States)

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.

PHARMACEUTICAL AMORPHOUS ORGANIC MATERIALS CHARACTERIZATION BY USING THE DIFFERENTIAL SCANNING CALORIMETRY AND DYNAMIC MECHANICAL ANALYSIS

Directory of Open Access Journals (Sweden)

Ion Dranca

2011-12-01

Full Text Available This research has been carried out in order to demonstrate the use of differential scanning calorimetry (DSC in detecting and measuring α- and β-relaxation processes in amorphous pharmaceutical systems. DSC has been employed to study amorphous samples of poly (vinylpyrrolidone (PVP, indomethacin (InM, and ursodeoxycholic acid (UDA that are annealed at temperature (Ta around 0.8 of their glass transition temperature (Tg. Dynamic mechanical analysis (DMA is used to measure β- relaxation in PVP. Yet, the DSC has been used to study the glassy indomethacin aged at 0 and -10 oC for periods of time up to 109 and 210 days respectively. The results demonstrate the emergence of a small melting peak of the α-polymorph after aging for 69 days at 0°C and for 147 days at -10°C (i.e., ~55°C below the glass transition temperature that provides evidence of nucleation occurring in the temperature region of the β-relaxation.

Ionic liquids: differential scanning calorimetry as a new indirect method for determination of vaporization enthalpies.

Science.gov (United States)

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.

New methodology developed for the differential scanning calorimetry analysis of polymeric matrixes incorporating phase change materials

International Nuclear Information System (INIS)

Barreneche, Camila; Solé, Aran; Miró, Laia; Martorell, Ingrid; Cabeza, Luisa F; Fernández, A Inés

2012-01-01

Nowadays, thermal comfort needs in buildings have led to an increase in energy consumption of the residential and service sectors. For this reason, thermal energy storage is shown as an alternative to achieve reduction of this high consumption. Phase change materials (PCM) have been studied to store energy due to their high storage capacity. A polymeric material capable of macroencapsulating PCM was developed by the authors of this paper. However, difficulties were found while measuring the thermal properties of these materials by differential scanning calorimetry (DSC). The polymeric matrix interferes in the detection of PCM properties by DSC. To remove this interfering effect, a new methodology which replaces the conventional empty crucible used as a reference in the DSC analysis by crucibles composed of the polymeric matrix was developed. Thus, a clear signal from the PCM is obtained by subtracting the new full crucible signal from the sample signal. (paper)

Characterization of phase change materials for thermal control of photovoltaics using Differential Scanning Calorimetry and Temperature History Method

International Nuclear Information System (INIS)

Hasan, A.; McCormack, S.J.; Huang, M.J.; Norton, B.

2014-01-01

Highlights: • Five PCM are characterized using tow techniques for PV temperature regulation. • Thermophysical properties of interest are determined and compared with literature. • Determined PCM properties are discussed as criteria for PV temperature regulation. • One PCM identified as potential candidate for PV temperature regulation. - Abstract: Five solid–liquid phase change materials comprising three basic classes, paraffin waxes, salt hydrates and mixtures of fatty acids were thermophysically characterized for thermal regulation applications in photovoltaics. The PCM were investigated using Differential Scanning Calorimetry and Temperature History Method to find their thermophysical properties of interest. The relationship between thermophysical properties of the PCM and their choice as temperature regulators in photovoltaics is discussed in relation to the ambient conditions under which PV systems operate

Application of Differential Scanning Calorimetry (DSC in study of phase transformations in ductile iron

Directory of Open Access Journals (Sweden)

R. Przeliorz

2010-04-01

Full Text Available The effect of heating rate on phase transformations to austenite range in ductile iron of the EN-GJS-450-10 grade was investigated. For studies of phase transformations, the technique of differential scanning calorimetry (DSC was used. Microstructure was examined by optical microscopy. The calorimetric examinations have proved that on heating three transformations occur in this grade of ductile iron, viz. magnetic transformation at the Curie temperature, pearlite→austenite transformation and ferrite→austenite transformation. An increase in the heating rate shifts the pearlite→austenite and ferrite→austenite transformations to higher temperature range. At the heating rate of 5 and 15°C/min, local extrema have been observed to occur: for pearlite→austenite transformation at 784°C and 795°C, respectively, and for ferrite→austenite transformation at 805°C and 821°C, respectively. The Curie temperature of magnetic transformation was extrapolated to a value of 740°C. Each transformation is related with a specific thermal effect. The highest value of enthalpy is accompanying the ferrite→austenite transformation, the lowest occurs in the case of pearlite→austenite transformation.

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

Science.gov (United States)

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.

Recent advances and potential applications of modulated differential scanning calorimetry (mDSC) in drug development.

Science.gov (United States)

Knopp, Matthias Manne; Löbmann, Korbinian; Elder, David P; Rades, Thomas; Holm, René

2016-05-25

Differential scanning calorimetry (DSC) is frequently the thermal analysis technique of choice within preformulation and formulation sciences because of its ability to provide detailed information about both the physical and energetic properties of a substance and/or formulation. However, conventional DSC has shortcomings with respect to weak transitions and overlapping events, which could be solved by the use of the more sophisticated modulated DSC (mDSC). mDSC has multiple potential applications within the pharmaceutical field and the present review provides an up-to-date overview of these applications. It is aimed to serve as a broad introduction to newcomers, and also as a valuable reference for those already practising in the field. Complex mDSC was introduced more than two decades ago and has been an important tool for the quantification of amorphous materials and development of freeze-dried formulations. However, as discussed in the present review, a number of other potential applications could also be relevant for the pharmaceutical scientist. Copyright © 2015 Elsevier B.V. All rights reserved.

Study of phase transformations of Fe-Cr-C system using the technique of differential scanning calorimetry

International Nuclear Information System (INIS)

Facal, L.S.; Noreña, H. C.; Bruzzoni, P.

2013-01-01

The family of 9% Cr-1% Mo steels has been considered by The Generation IV International Forum as candidate materials for the construction of these prospective advanced nuclear reactors. A simple system related with these steels is the Fe-Cr-C system. In this work, a laboratory made Fe-10% Cr-0,1% C alloy has been studied. Particularly, the effect of the cooling rate on the transformations that take place when the alloy is cooled from the austenitic field was analyzed. To perform this analysis two techniques have been used: The differential scanning calorimetry (DSC) and the scanning electron microscopy (SEM). Different cooling rates of 4, 10, 50 and 90 °C/min were tested in the DSC and the resulting microstructures were observed by SEM. At the rates of 50 and 90 °C/min the cooling treatment produced a martensitic structure. Contrarily, cooling at a rate of 4 °C/min produced a microstructure consisting mainly of ferrite-pearlite with a low fraction of martensite. In the heating step which followed the cooling step, the magnetic transformation is well resolved as a broad peak which presents a maximum at 753 ± 1 °C for all the cooling rates. (author) [es

A modulated differential scanning calorimetry and small-angle x-ray scattering study of the interfacial region in structured latices

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Hourston Douglas J.

2001-01-01

Full Text Available The interfacial structure of poly(styrene (PS-poly(methyl acrylate (PMA structured latices has been investigated by means of modulated-temperature differential scanning calorimetry (M-TDSC and small-angle x-ray scattering (SAXS. The differential of heat capacity, dCp/dT, signal from M-TDSC was used to quantify the weight fraction of interface in these latices. For PS-PMA (50:50 by weight structured latices in which the PS component had different crosslink densities (0, 1, 3, 5 and 10 mol% of crosslinking agent, the weight fraction of interface was about 13%. With increasing crosslink density, the fraction of interface increased only slightly. A core-shell model has been used to analyse SAXS data for these PS-PMA latices. M-TDSC can only provide information about the weight fraction of interface, but the combination of M-TDSC and SAXS can provide much more information on the morphology of such structured latices.

Dimyristoylphosphatidylcholine/C16 : 0-ceramide binary liposomes studied by differential scanning calorimetry and wide- and small-angle X-ray scattering

DEFF Research Database (Denmark)

Holopainen, J. M.; Lemmich, Jesper; Richter, F.

2000-01-01

hydrated binary membranes composed of dimyristoylphosphatidylcholine (DMPC) and N-palmitoyl-ceramide (C16:0-ceramide, up to a mole fraction X-cer = 0.35) were resolved in further detail by high-sensitivity differential scanning calorimetry (DSC) and x-ray diffraction. Both methods reveal very strong...... hysteresis in the thermal phase behavior of ceramide-containing membranes. A partial phase diagram was constructed based on results from a combination of these two methods. DSC heating scans show that with increased X-cer the pretransition temperature T-P first increases, whereafter at X-cer > 0.06 it can...... no longer be resolved. The main transition enthalpy Delta H remains practically unaltered while its width increases significantly, and the upper phase boundary temperature of the mixture shifts to similar to 63 degrees C at X-cer = 0.30. Upon cooling, profound phase separation is evident, and for all...

Quantitative determination of the specific heat and the glass transition of moist samples by temperature modulated differential scanning calorimetry.

Science.gov (United States)

Schubnell, M; Schawe, J E

2001-04-17

In differential scanning calorimetry (DSC), remnant moisture loss in samples often overlaps and distorts other thermal events, e.g. glass transitions. To separate such overlapping processes, temperature modulated DSC (TMDSC) has been widely used. In this contribution we discuss the quantitative determination of the heat capacity of a moist sample from TMDSC measurements. The sample was a spray-dried pharmaceutical compound run in different pans (hermetically-sealed pan, pierced lid pan [50 microm] and open pan). The apparent heat capacity was corrected for the remaining amount of moisture. Using this procedure we could clearly identify the glass transition of the dry and the moist sample. We found that a moisture content of about 6.2% shifts the glass transition by about 50 degrees C.

Evaluation of thermal stability of paraffin wax by differential scanning calorimetry; Avaliacao da estabilidade termica de parafina por calorimetria diferencial de varredura

Energy Technology Data Exchange (ETDEWEB)

Godinho, K.O.; Silva, A.G.P.; Holanda, J.N.F. [Universidade Estadual do Norte Fluminense (LAMAV/UENF), Campos dos Goytacazes, RJ (Brazil). Grupo de Materiais Ceramicos], Email: holanda@uenf.br

2010-07-01

Phase change materials for heat storage are used as passive solar energy storage materials, which can be impregnated into construction materials. In this work the thermal stability (heating/cooling cycle) of the paraffin wax was investigated using differential scanning calorimetry. The latent heat and fusion temperature were determined for the following thermal cycles: 0, 30, 180 and 360. The thermal stability for paraffin wax infiltrated in support of gypsum was also determined. The experimental results showed that the paraffin wax showed good thermal stability in the states pure and infiltrated for up to 360 thermal cycles. (author)

Application of TZERO calibrated modulated temperature differential scanning calorimetry to characterize model protein formulations.

Science.gov (United States)

Badkar, Aniket; Yohannes, Paulos; Banga, Ajay

2006-02-17

The objective of this study was to evaluate the feasibility of using T(ZERO) modulated temperature differential scanning calorimetry (MDSC) as a novel technique to characterize protein solutions using lysozyme as a model protein and IgG as a model monoclonal antibody. MDSC involves the application of modulated heating program, along with the standard heating program that enables the separation of overlapping thermal transitions. Although characterization of unfolding transitions for protein solutions requires the application of high sensitive DSC, separation of overlapping transitions like aggregation and other exothermic events may be possible only by use of MDSC. A newer T(ZERO) calibrated MDSC model from TA instruments that has improved sensitivity than previous models was used. MDSC analysis showed total, reversing and non-reversing heat flow signals. Total heat flow signals showed a combination of melting endotherms and overlapping exothermic events. Under the operating conditions used, the melting endotherms were seen in reversing heat flow signal while the exothermic events were seen in non-reversing heat flow signal. This enabled the separation of overlapping thermal transitions, improved data analysis and decreased baseline noise. MDSC was used here for characterization of lysozyme solutions, but its feasibility for characterizing therapeutic protein solutions needs further assessment.

Differential Scanning Calorimetry and Thermodynamic Predictions—A Comparative Study of Al-Zn-Mg-Cu Alloys

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Gernot K.-H. Kolb

2016-08-01

Full Text Available Al-Zn-Mg-Cu alloys are widely used in aircraft applications because of their superior mechanical properties and strength/weight ratios. Commercial Al-Zn-Mg-Cu alloys have been intensively studied over the last few decades. However, well-considered thermodynamic calculations, via the CALPHAD approach, on a variation of alloying elements can guide the fine-tuning of known alloy systems and the development of optimized heat treatments. In this study, a comparison was made of the solidus temperatures of different Al-Zn-Mg-Cu alloys determined from thermodynamic predictions and differential scanning calorimetry (DSC measurements. A variation of the main alloying elements Zn, Mg, and Cu generated 38 experimentally produced alloys. An experimental determination of the solidus temperature via DSC was carried out according to a user-defined method, because the broad melting interval present in Al-Zn-Mg-Cu alloys does not allow the use of the classical onset method for pure substances. The software algorithms implemented in FactSage®, Pandat™, and MatCalc with corresponding commercially available databases were deployed for thermodynamic predictions. Based on these investigations, the predictive power of the commercially available CALPHAD databases and software packages was critically reviewed.

Scan-rate dependence in protein calorimetry: the reversible transitions of Bacillus circulans xylanase and a disulfide-bridge mutant.

OpenAIRE

Davoodi, J.; Wakarchuk, W. W.; Surewicz, W. K.; Carey, P. R.

1998-01-01

The stabilities of Bacillus circulans xylanase and a disulfide-bridge-containing mutant (S100C/N148C) were investigated by differential scanning calorimetry (DSC) and thermal inactivation kinetics. The thermal denaturation of both proteins was found to be irreversible, and the apparent transition temperatures showed a considerable dependence upon scanning rate. In the presence of low (nondenaturing) concentrations of urea, calorimetric transitions were observed for both proteins in the second...

Differential scanning microcalorimetry of intrinsically disordered proteins.

Science.gov (United States)

Permyakov, Sergei E

2012-01-01

Ultrasensitive differential scanning calorimetry (DSC) is an indispensable thermophysical technique enabling to get direct information on enthalpies accompanying heating/cooling of dilute biopolymer solutions. The thermal dependence of protein heat capacity extracted from DSC data is a valuable source of information on intrinsic disorder level of a protein. Application details and limitations of DSC technique in exploration of protein intrinsic disorder are described.

Microstructure characterization of a food-grade U-type microemulsion system by differential scanning calorimetry and electrical conductivity techniques.

Science.gov (United States)

Zhang, Hui; Taxipalati, Maierhaba; Que, Fei; Feng, Fengqin

2013-12-01

The microstructure transitions of a food-grade U-type microemulsion system containing glycerol monolaurate and propionic acid at a 1:1 mass ratio as oil phase and Tween 80 as surfactant were investigated along a water dilution line at a ratio of 80:20 mass% surfactant/oil phase, based on a previously studied phase diagram. From the water thermal behaviours detected by differential scanning calorimetry, three structural regions are identified along the dilution line. In the first region, all water molecules are confined to the water core of the reverse micelles, leading to the formation of w/o microemulsion. As the water content increases, the water gains mobility, transforms into bicontinuous in the second region, and finally the microemulsion become o/w in the third region. The thermal transition points coincide with the structural phase transitions by electrical conductivity measurements, indicating that the structural transitions occur at 35 and 65 mass% of water along the dilution line. Copyright © 2013 Elsevier Ltd. All rights reserved.

Changes in chromatin structure during the aging of cell cultures as revealed by differential scanning calorimetry

International Nuclear Information System (INIS)

Almagor, M.; Cole, R.D.

1989-01-01

Nuclei from cultured human cells were examined by differential scanning calorimetry. Their melting profiles revealed four structural transitions at 60, 76, 88, and 105 degrees C (transitions I-IV, respectively). In immortalized (i.e., tumor) cell cultures and in normal cell cultures of low passage number, melting profiles were dominated by the 105 degrees C transition (transition IV), but in vitro aging of normal and Werner syndrome cells was associated with a marked decrease in transition IV followed by an increase in transition III at the expense of transition IV. At intermediate times in the aging process, much DNA melted at a temperature range (95-102 degrees C) intermediate between transitions III and IV, and this is consistent with the notion that aging of cell cultures is accompanied by an increase in single-strand character of the DNA. Calorimetric changes were observed in the melting profile of nuclei from UV-irradiated tumor cells that resembled the age-induced intermediate melting of chromatin. It is suggested that aging is accompanied by an increase in single-stranded character of the DNA in chromatin, which lowers its melting temperature, followed by strand breaks in the DNA that destroy its supercoiling potential

Solid-state characterization of triamcinolone acetonide nanosuspensiones by X-ray spectroscopy, ATR Fourier transforms infrared spectroscopy and differential scanning calorimetry analysis

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Eva García-Millán

2017-12-01

Full Text Available The data presented in this article describe the physical state of the triamcinolone acetonide (TA in nanosuspension stabilized with polyvinyl alcohol (PVA and poloxamer 407 (PL. The data were assessed by X-ray spectroscopy, ATR Fourier transforms infrared spectroscopy measurements (FTIR, and Differential scanning calorimetry (DSC analysis. PVA, PL and polymeric mixture (PVA and PL were compared with nanosuspension and the interactions between drug triamcinolone acetonide and polymers were studied. The data are related and are complementary to the research article entitle “Improved release of triamcinolone acetonide from medicated soft contact lenses loaded with drug nanosuspensions” (García-Millán et al., 2017 [1]. Keywords: Triamcinolona acetonide nanosuspensiones, X-ray spectroscopy, FTIR spectroscopy, DSC

Influência de alguns parâmetros experimentais nos resultados de análises calorimétricas diferenciais - DSC Influence of some experimental parameters on the results of differential scanning calorimetry - DSC.

OpenAIRE

Cláudia Bernal; Andréa Boldarini Couto; Susete Trazzi Breviglieri; Éder Tadeu Gomes Cavalheiro

2002-01-01

A series of experiments were performed in order to demonstrate to undergraduate students or users of the differential scanning calorimetry (DSC), that several factors can influence the qualitative and quantitative aspects of DSC results. Saccharin, an artificial sweetner, was used as a probe and its thermal behavior is also discussed on the basis of thermogravimetric (TG) and DSC curves.

One-step simultaneous differential scanning calorimetry-FTIR microspectroscopy to quickly detect continuous pathways in the solid-state glucose/asparagine Maillard reaction.

Science.gov (United States)

Hwang, Deng-Fwu; Hsieh, Tzu-Feng; Lin, Shan-Yang

2013-01-01

The stepwise reaction pathway of the solid-state Maillard reaction between glucose (Glc) and asparagine (Asn) was investigated using simultaneous differential scanning calorimetry (DSC)-FTIR microspectroscopy. The color change and FTIR spectra of Glc-Asn physical mixtures (molar ratio = 1:1) preheated to different temperatures followed by cooling were also examined. The successive reaction products such as Schiff base intermediate, Amadori product, and decarboxylated Amadori product in the solid-state Glc-Asn Maillard reaction were first simultaneously evidenced by this unique DSC-FTIR microspectroscopy. The color changed from white to yellow-brown to dark brown, and appearance of new IR peaks confirmed the formation of Maillard reaction products. The present study clearly indicates that this unique DSC-FTIR technique not only accelerates but also detects precursors and products of the Maillard reaction in real time.

Differential scanning calorimetry (DSC) and temperature-modulated DSC study of three mouthguard materials.

Science.gov (United States)

Meng, Frank H; Schricker, Scott R; Brantley, William A; Mendel, Deborah A; Rashid, Robert G; Fields, Henry W; Vig, Katherine W L; Alapati, Satish B

2007-12-01

Employ differential scanning calorimetry (DSC) and temperature-modulated DSC (TMDSC) to investigate thermal transformations in three mouthguard materials and provide insight into their previously investigated energy absorption. Samples (13-21mg) were obtained from (a) conventional ethylene vinyl acetate (EVA), (b) Pro-form, another EVA polymer, and (c) PolyShok, an EVA polymer containing polyurethane. Conventional DSC (n=5) was first performed from -80 to 150 degrees C at a heating rate of 10 degrees C/min to determine the temperature range for structural transformations. Subsequently, TMDSC (n=5) was performed from -20 to 150 degrees C at a heating rate of 1 degrees C/min. Onset and peak temperatures were compared using ANOVA and the Tukey-Kramer HSD test. Other samples were coated with a gold-palladium film and examined with an SEM. DSC and TMDSC curves were similar for both conventional EVA and Pro-form, showing two endothermic peaks suggestive of melting processes, with crystallization after the higher-temperature peak. Evidence for crystallization and the second endothermic peak were much less prominent for PolyShok, which had no peaks associated with the polyurethane constituent. The onset of the lower-temperature endothermic transformation is near body temperature. No glass transitions were observed in the materials. SEM examination revealed different surface morphology and possible cushioning effect for PolyShok, compared to Pro-form and EVA. The difference in thermal behavior for PolyShok is tentatively attributed to disruption of EVA crystal formation, which may contribute to its superior impact resistance. The lower-temperature endothermic peak suggests that impact testing of these materials should be performed at 37 degrees C.

Optimization of glibenclamide tablet composition through the combined use of differential scanning calorimetry and D-optimal mixture experimental design.

Science.gov (United States)

Mura, P; Furlanetto, S; Cirri, M; Maestrelli, F; Marras, A M; Pinzauti, S

2005-02-07

A systematic analysis of the influence of different proportions of excipients on the stability of a solid dosage form was carried out. In particular, a d-optimal mixture experimental design was applied for the evaluation of glibenclamide compatibility in tablet formulations, consisting of four classic excipients (natrosol as binding agent, stearic acid as lubricant, sorbitol as diluent and cross-linked polyvinylpyrrolidone as disintegrant). The goal was to find the mixture component proportions which correspond to the optimal drug melting parameters, i.e. its maximum stability, using differential scanning calorimetry (DSC) to quickly obtain information about possible interactions among the formulation components. The absolute value of the difference between the melting peak temperature of pure drug endotherm and that in each analysed mixture and the absolute value of the difference between the enthalpy of the pure glibenclamide melting peak and that of its melting peak in the different analyzed mixtures, were chosen as indexes of the drug-excipient interaction degree.

Rheological Behavior, Granule Size Distribution and Differential Scanning Calorimetry of Cross-Linked Banana (Musa paradisiaca) Starch.

Science.gov (United States)

Núñez-Santiago, María C.; Maristany-Cáceres, Amira J.; Suárez, Francisco J. García; Bello-Pérez, Arturo

2008-07-01

Rheological behavior at 60 °C, granule size distribution and Differential Scanning Calorimetry (DSC) tests were employed to study the effect of diverse reaction conditions: adipic acid concentration, pH and temperature during cross-linking of banana (Musa paradisiaca) starch. These properties were determined in native banana starch pastes for the purpose of comparison. Rheological behavior from pastes of cross-linked starch at 60 °C did not show hysteresis, probably due the cross-linkage of starch that avoided disruption of granules, elsewhere, native starch showed hysteresis in a thixotropic loop. All pastes exhibited non-Newtonian shear thinning behavior. In all cases, size distribution showed a decrease in the median diameter in cross-linked starches. This condition produces a decrease in swelling capacity of cross-linked starch. The median diameter decreased with an increase of acid adipic concentration; however, an increase of pH and Temperature produced an increase in this variable. Finally, an increase in gelatinization temperature and entalphy (ΔH) were observed as an effect of cross-linkage. An increase in acid adipic concentration produced an increase in Tonset and a decrease in ΔH. pH and temperature. The cross-linked of banana starch produced granules more resistant during the pasting procedure.

Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

Directory of Open Access Journals (Sweden)

Nichola C Garbett

Full Text Available Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN and extent of spread of invasive carcinomas of the cervix (IC are needed. Differential scanning calorimetry (DSC has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate

Detection of cervical cancer biomarker patterns in blood plasma and urine by differential scanning calorimetry and mass spectrometry.

Science.gov (United States)

Garbett, Nichola C; Merchant, Michael L; Helm, C William; Jenson, Alfred B; Klein, Jon B; Chaires, Jonathan B

2014-01-01

Improved methods for the accurate identification of both the presence and severity of cervical intraepithelial neoplasia (CIN) and extent of spread of invasive carcinomas of the cervix (IC) are needed. Differential scanning calorimetry (DSC) has recently been shown to detect specific changes in the thermal behavior of blood plasma proteins in several diseases. This methodology is being explored to provide a complementary approach for screening of cervical disease. The present study evaluated the utility of DSC in differentiating between healthy controls, increasing severity of CIN and early and advanced IC. Significant discrimination was apparent relative to the extent of disease with no clear effect of demographic factors such as age, ethnicity, smoking status and parity. Of most clinical relevance, there was strong differentiation of CIN from healthy controls and IC, and amongst patients with IC between FIGO Stage I and advanced cancer. The observed disease-specific changes in DSC profiles (thermograms) were hypothesized to reflect differential expression of disease biomarkers that subsequently bound to and affected the thermal behavior of the most abundant plasma proteins. The effect of interacting biomarkers can be inferred from the modulation of thermograms but cannot be directly identified by DSC. To investigate the nature of the proposed interactions, mass spectrometry (MS) analyses were employed. Quantitative assessment of the low molecular weight protein fragments of plasma and urine samples revealed a small list of peptides whose abundance was correlated with the extent of cervical disease, with the most striking plasma peptidome data supporting the interactome theory of peptide portioning to abundant plasma proteins. The combined DSC and MS approach in this study was successful in identifying unique biomarker signatures for cervical cancer and demonstrated the utility of DSC plasma profiles as a complementary diagnostic tool to evaluate cervical cancer

Challenges of the Usual Graphical Methods Used to Characterize Phase Change Materials by Differential Scanning Calorimetry

Directory of Open Access Journals (Sweden)

Stéphane Gibout

2018-01-01

Full Text Available Modeling the thermal behavior of a plant or devices using Phase Change Materials (PCM requires to know their thermophysical properties. The Differential Scanning Calorimetry (DSC is a technic largely used to investigate them. However, under the pretext to experiment with small samples, some authors consider the DSC curves as directly representing the properties of the materials without realizing that this interpretation is very often incompatible with the thermodynamics laws: as an example, although a pure substance melts at a fixed temperature T F , it is proposed a melting through a temperature range higher than T F and depending on the experiments (heating rates, sample masses..., for solutions the suggested characteristic temperatures are incompatible with the phase diagram, and also a hysteresis phenomenon is invented... In this paper, we demonstrate by a model coupling thermodynamics and conduction heat transfers, that the DSC curves are exactly compatible with the thermodynamics of phase changes (melting at fixed temperature for pure substances, in conformity with phase diagrams for solutions.... The cases of pure substances, saline solutions, substances with impurities or solid solutions are detailed. We indicate which information can, however, be given by the curves. We also propose a more sophisticated method by inverse calculations to determine the specific enthalpy whose all the thermodynamical properties can be deduced. Finally, we give some indications to understand and use the results indicating supercooling.

Weak interactions in clobazam–lactose mixtures examined by differential scanning calorimetry: Comparison with the captopril–lactose system

International Nuclear Information System (INIS)

Toscani, S.; Cornevin, L.; Burgot, G.

2012-01-01

Highlights: ► Thermodynamic and kinetic parameters of weak interactions in binary systems by DSC. ► Energy-barrier decrease for lactose dehydration induced by clobazam. ► Recrystallisation of metastable liquid clobazam induced by anhydrous alpha lactose. ► Decrease of lactose dehydration temperature in binary mixtures with captopril. ► Increase of lactose dehydration enthalpy in binary mixtures with captopril. - Abstract: The thermal behaviour of binary mixtures of two drugs (clobazam and captopril, respectively) and a pharmaceutical excipient (lactose monohydrate) was measured with differential scanning calorimetry to determine thermodynamic and kinetic parameters (dehydration and melting enthalpies and dehydration and glass-transition activation energies) which might be affected by intermolecular interactions. A kinetic study showed that lactose dehydration is not a single-step conversion and that clobazam contributed to reduce the energy barrier for the bulk dehydration of the excipient. On the other hand, the physical interactions between metastable liquid clobazam and crystalline anhydrous α-lactose obtained from monohydrate dehydration gave rise to the recrystallisation of clobazam. In the captopril–lactose system, the liquid captopril influenced the lactose dehydration: a sharp increase of the dehydration enthalpy and a concurrent reduction of the dehydration temperature were observed. Finally, it turned out that solid-phase transitions were enhanced by the contact with a liquid phase.

Shape Memory Alloys for Monitoring Minor Over-Heating/Cooling Based on the Temperature Memory Effect via Differential Scanning Calorimetry: A Review of Recent Progress

Science.gov (United States)

Wang, T. X.; Huang, W. M.

2017-12-01

The recent development in the temperature memory effect (TME) via differential scanning calorimetry in shape memory alloys is briefly discussed. This phenomenon was also called the thermal arrest memory effect in the literature. However, these names do not explicitly reveal the potential application of this phenomenon in temperature monitoring. On the other hand, the standard testing process of the TME has great limitation. Hence, it cannot be directly applied for temperature monitoring in most of the real engineering applications in which temperature fluctuation occurs mostly in a random manner within a certain range. However, as shown here, after proper modification, we are able to monitor the maximum or minimum temperature in either over-heating or over-cooling with reasonable accuracy.

Estimating heat transfer bias of kinetic measurement for polymers by differential scanning calorimetry with isothermal mode; Evaluation de l'erreur due au transfert de chaleur lors des mesures cinetiques dans les polymeres par calorimetrie differentielle a balayage en mode isotherme

Energy Technology Data Exchange (ETDEWEB)

Danes, Florin; Garnier, Bertrand [Laboratoire de Thermocinetique, UMR CNRS 6607, Ecole Polytechnique de l' Universite de Nantes, rue C. Pauc, BP50609, 44306 cedex 3, Nantes (France)

2003-06-01

The non-uniformity of temperatures in the DSC sample, and the subsequent difference between mean sample temperature and measured one (in the support of the crucible) are identified as the main source of bias for the isothermal mode determination of kinetic characteristics by differential scanning calorimetry. Chemical reactions under consideration are these with important heat effects into thermal insulators, as for example the reticulation of polymeric materials.By introducing an analytical model of heat transfer in DSC reactive samples, we have performed an estimation for the upper limit of the maximal size of samples which corresponds to a given relative error of the reaction rate, as measured by isothermal DSC calorimetry. For example, with a 5% error and flat samples, we have found admissible sample thicknesses which decrease with temperature and are between 1.9 and 3.1 mm for the sulphur vulcanization of a natural rubber and between 0.6 and 1.1 mm for the reticulation of a pre-polymerized epoxy resin. (authors)

Characteristics of rose hip (Rosa canina L.) cold-pressed oil and its oxidative stability studied by the differential scanning calorimetry method.

Science.gov (United States)

Grajzer, Magdalena; Prescha, Anna; Korzonek, Katarzyna; Wojakowska, Anna; Dziadas, Mariusz; Kulma, Anna; Grajeta, Halina

2015-12-01

Two new commercially available high linolenic oils, pressed at low temperature from rose hip seeds, were characterised for their composition, quality and DPPH radical scavenging activity. The oxidative stability of oils was assessed using differential scanning calorimetry (DSC). Phytosterols, tocopherols and carotenoids contents were up to 6485.4; 1124.7; and 107.7 mg/kg, respectively. Phenolic compounds determined for the first time in rose hip oil totalled up to 783.55 μg/kg, with a predominant presence of p-coumaric acid methyl ester. Antiradical activity of the oils reached up to 3.00 mM/kg TEAC. The acid, peroxide and p-anisidine values as well as iron and copper contents indicated good quality of the oils. Relatively high protection against oxidative stress in the oils seemed to be a result of their high antioxidant capacity and the level of unsaturation of fatty acids. Copyright © 2015 Elsevier Ltd. All rights reserved.

Evaluation of shrinkage temperature of bovine pericardium tissue for bioprosthetic heart valve application by differential scanning calorimetry and freeze-drying microscopy

Directory of Open Access Journals (Sweden)

Virgilio Tattini Jr

2007-03-01

Full Text Available Bovine pericardium bioprosthesis has become a commonly accepted device for heart valve replacement. Present practice relies on the measurement of shrinkage temperature, observed as a dramatic shortening of tissue length. Several reports in the last decade have utilized differential scanning calorimetry (DSC as an alternative method to determine the shrinkage temperature, which is accompanied by the absorption of heat, giving rise to an endothermic peak over the shrinkage temperature range of biological tissues. Usually, freeze-drying microscope is used to determine collapse temperature during the lyophilization of solutions. On this experiment we used this technique to study the shrinkage event. The aim of this work was to compare the results of shrinkage temperature obtained by DSC with the results obtained by freeze-drying microscopy. The results showed that both techniques provided excellent sensitivity and reproducibility, and gave information on the thermal shrinkage transition via the thermodynamical parameters inherent of each method.

High Pressure Differential Scanning Calorimetry of poly(4-methyl-pentene-1)

NARCIS (Netherlands)

Hoehne, G.W.H.; Rastogi, S.; Wunderlich, B.

2000-01-01

The polymer poly(4-methyl pentene-1), P4MP1, displays an unusual pressure–temperature phase diagram. The previous exploration of this phase behavior through X-ray diffraction has been extended through high-pressure calorimetry. The resulting phase diagram displays a melt area, the common tetragonal

Differential Binding Models for Direct and Reverse Isothermal Titration Calorimetry.

Science.gov (United States)

Herrera, Isaac; Winnik, Mitchell A

2016-03-10

Isothermal titration calorimetry (ITC) is a technique to measure the stoichiometry and thermodynamics from binding experiments. Identifying an appropriate mathematical model to evaluate titration curves of receptors with multiple sites is challenging, particularly when the stoichiometry or binding mechanism is not available. In a recent theoretical study, we presented a differential binding model (DBM) to study calorimetry titrations independently of the interaction among the binding sites (Herrera, I.; Winnik, M. A. J. Phys. Chem. B 2013, 117, 8659-8672). Here, we build upon our DBM and show its practical application to evaluate calorimetry titrations of receptors with multiple sites independently of the titration direction. Specifically, we present a set of ordinary differential equations (ODEs) with the general form d[S]/dV that can be integrated numerically to calculate the equilibrium concentrations of free and bound species S at every injection step and, subsequently, to evaluate the volume-normalized heat signal (δQ(V) = δq/dV) of direct and reverse calorimetry titrations. Additionally, we identify factors that influence the shape of the titration curve and can be used to optimize the initial concentrations of titrant and analyte. We demonstrate the flexibility of our updated DBM by applying these differentials and a global regression analysis to direct and reverse calorimetric titrations of gadolinium ions with multidentate ligands of increasing denticity, namely, diglycolic acid (DGA), citric acid (CIT), and nitrilotriacetic acid (NTA), and use statistical tests to validate the stoichiometries for the metal-ligand pairs studied.

Differential scanning calorimetry method for purity determination: A case study on polycyclic aromatic hydrocarbons and chloramphenicol

International Nuclear Information System (INIS)

Kestens, V.; Zeleny, R.; Auclair, G.; Held, A.; Roebben, G.; Linsinger, T.P.J.

2011-01-01

Highlights: → Purity assessment of polycyclic aromatic hydrocarbons and chloramphenicol by DSC. → DSC results compared with traditional purity methods. → Different methods give different results, multiple method approach recommended. → DSC sensitive to impurities that have similar structures as main component. - Abstract: In this study the validity and suitability of differential scanning calorimetry (DSC) to determine the purity of selected polycyclic aromatic hydrocarbons and chloramphenicol has been investigated. The study materials were two candidate certified reference materials (CRMs), 6-methylchrysene and benzo[a]pyrene, and two different batches of commercially available highly pure chloramphenicol. The DSC results were compared with those obtained by other methods, namely gas and liquid chromatography with mass spectrometric detection, liquid chromatography with diode array detection, and quantitative nuclear magnetic resonance. The purity results obtained by these different analytical methods confirm the well-known challenges of comparing results of different method-defined measurands. In comparison with other methods, DSC has a much narrower working range. This limits the applicability of DSC as purity determination method, for instance during the assignment of the purity value of a CRM. Nevertheless, this study showed that DSC can be a powerful technique to detect impurities that are structurally very similar to the main purity component. From this point of view, and because of its good repeatability, DSC can be considered as a valuable technique to investigate the homogeneity and stability of candidate purity CRMs.

Weak interactions in clobazam-lactose mixtures examined by differential scanning calorimetry: Comparison with the captopril-lactose system

Energy Technology Data Exchange (ETDEWEB)

Toscani, S. [Departement de Chimie - UMR 6226, Faculte des Sciences, Universite de Rennes 1, Batiment 10B, 263 avenue du General Leclerc, F-35042 Rennes Cedex (France); Cornevin, L. [Universite de Rennes 1, Faculte de Pharmacie, 2 Avenue Leon Bernard, F-35043 Rennes Cedex (France); Burgot, G., E-mail: Gwenola.burgot@univ-rennes1.fr [Universite de Rennes 1, Faculte de Pharmacie, Laboratoire de Chimie Analytique, EA 1274 ' Mouvement, sports, sante' , 2 Avenue Leon Bernard, F-35043 Rennes Cedex (France); CHGR Rennes, Pole Medico-Technique Pharmacie, F-35703 Rennes Cedex (France)

2012-09-10

Highlights: Black-Right-Pointing-Pointer Thermodynamic and kinetic parameters of weak interactions in binary systems by DSC. Black-Right-Pointing-Pointer Energy-barrier decrease for lactose dehydration induced by clobazam. Black-Right-Pointing-Pointer Recrystallisation of metastable liquid clobazam induced by anhydrous alpha lactose. Black-Right-Pointing-Pointer Decrease of lactose dehydration temperature in binary mixtures with captopril. Black-Right-Pointing-Pointer Increase of lactose dehydration enthalpy in binary mixtures with captopril. - Abstract: The thermal behaviour of binary mixtures of two drugs (clobazam and captopril, respectively) and a pharmaceutical excipient (lactose monohydrate) was measured with differential scanning calorimetry to determine thermodynamic and kinetic parameters (dehydration and melting enthalpies and dehydration and glass-transition activation energies) which might be affected by intermolecular interactions. A kinetic study showed that lactose dehydration is not a single-step conversion and that clobazam contributed to reduce the energy barrier for the bulk dehydration of the excipient. On the other hand, the physical interactions between metastable liquid clobazam and crystalline anhydrous {alpha}-lactose obtained from monohydrate dehydration gave rise to the recrystallisation of clobazam. In the captopril-lactose system, the liquid captopril influenced the lactose dehydration: a sharp increase of the dehydration enthalpy and a concurrent reduction of the dehydration temperature were observed. Finally, it turned out that solid-phase transitions were enhanced by the contact with a liquid phase.

Study on the characterization and thermal decomposition of uranium compounds by thermogravimetry (TG) and differential scanning calorimetry (DSC)

International Nuclear Information System (INIS)

Dantas, J.M.; Abrao, A.

1981-04-01

A contribution to the characterization of several uranium compounds obtained at the IPEN' Uranium Pilot Plant is given. Particularly, samples of ammonium diuranate (ADU) and uranium oxides were studied. The main objective was to know the stoichiometry of the ADU and the oxides resulting from its thermal transformation. ADU samples were prepared by batchwise precipitation, stationary dewatering into stove and batchwise thermal decomposition, or, alternatively, continuous precipitation, continuous filtration, continuous drying and continuous thermal decomposition inside a temperature gradient electrical furnace. All ADU were precipitated using NH 3 gas from uranul sulfate or uranyl nitrate solutions. The thermal decomposition of ADU and uranium oxides were studied in an air atmosphere by thermogravimetry (TG) and differential scanning calorimetry (DSC). Any correlation between the parameters of precipitation, drying, calcination and the hystory of the obtaintion of the several uraniumm compounds and their initial and final composition was looked for. Heating program was established to have the U 3 O 8 oxide as the final product. Intermediary phases were tentatively identified. Temperatures at which occurred the absorption water elimination, crystallization water elimination, evolution or oxidation of NH 3 , decomposition of NO -3 ion and oxygen evolution and the exo- and endothermic process for each sample were identified. (Author) [pt

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

Science.gov (United States)

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.

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

International Nuclear Information System (INIS)

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

2010-01-01

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.

Structural domains and conformational changes in nuclear chromatin: a quantitative thermodynamic approach by differential scanning calorimetry.

Science.gov (United States)

Balbi, C; Abelmoschi, M L; Gogioso, L; Parodi, S; Barboro, P; Cavazza, B; Patrone, E

1989-04-18

A good deal of information on the thermodynamic properties of chromatin was derived in the last few years from optical melting experiments. The structural domains of the polynucleosomal chain, the linker, and the core particle denature as independent units. The differential scanning calorimetry profile of isolated chromatin is made up of three endotherms, at approximately 74, 90, and 107 degrees C, having an almost Gaussian shape. Previous work on this matter, however, was mainly concerned with the dependence of the transition enthalpy on external parameters, such as the ionic strength, or with the melting of nuclei from different sources. In this paper we report the structural assignment of the transitions of rat liver nuclei, observed at 58, 66, 75, 92, and 107 degrees C. They are representative of the quiescent state of the cell. The strategy adopted in this work builds on the method developed for the investigation of complex biological macromolecules. The heat absorption profile of the nucleus was related to the denaturation of isolated nuclear components; electron microscopy and electrophoretic techniques were used for their morphological and molecular characterization. The digestion of chromatin by endogenous nuclease mimics perfectly the decondensation of the higher order structure and represented the source of several misinterpretations. This point was carefully examined in order to define unambiguously the thermal profile of native nuclei. The low-temperature transitions, centered around 58 and 66 degrees C, arise from the melting of scaffolding structures and of the proteins associated with heterogeneous nuclear RNA.(ABSTRACT TRUNCATED AT 250 WORDS)

Thermal dehydration of cobalt and zinc formate dihydrates by controlled-rate thermogravimetry (CRTG) and simultaneous X-ray diffractometry-differential scanning calorimetry (XRD-DSC)

International Nuclear Information System (INIS)

Arii, T.; Kishi, A.

1999-01-01

The thermal dehydration study of the similar hydrated salts, cobalt and zinc formate dihydrates, have been carried out successfully by means of X-ray diffractometry-differential scanning calorimetry (XRD-DSC) and controlled-rate thermogravimetry (CRTG). X-ray diffraction analysis recorded simultaneously indicates that the resulting anhydrous product, Zn(HCO 2 ) 2 , was crystalline, while Co(HCO 2 ) 2 was amorphous.The XRD-DSC data are proven to be invaluable in verifying the interpretation of overlapping processes in thermal events. In addition, these differences in the resulting anhydrous products can be explained from kinetic analysis results based on the CRTG data. The kinetic mechanism governing the dehydration of zinc formate dihydrate is a nucleation and growth process, while in the case of cobalt formate dihydrate a phase boundary controlled reaction is the governing mechanism. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

Effect of heating and cooling rate on the kinetics of allotropic phase changes in uranium: A differential scanning calorimetry study

International Nuclear Information System (INIS)

Rai, Arun Kumar; Raju, S.; Jeyaganesh, B.; Mohandas, E.; Sudha, R.; Ganesan, V.

2009-01-01

The kinetic aspects of allotropic phase changes in uranium are studied as a function of heating/cooling rate in the range 10 0 -10 2 K min -1 by isochronal differential scanning calorimetry. The transformation arrest temperatures revealed a remarkable degree of sensitivity to variations of heating and cooling rate, and this is especially more so for the transformation finish (T f ) temperatures. The results obtained for the α → β and β → γ transformations during heating confirm to the standard Kolmogorov-Johnson-Mehl-Avrami (KJMA) model for a nucleation and growth mediated process. The apparent activation energy Q eff for the overall transformation showed a mild increase with increasing heating rate. In fact, the heating rate normalised Arrhenius rate constant, k/β reveals a smooth power law decay with increasing heating rate (β). For the α → β phase change, the observed DSC peak profile for slower heating rates contained a distinct shoulder like feature, which however is absent in the corresponding profiles found for higher heating rates. The kinetics of γ → β phase change on the other hand, is best described by the two-parameter Koistinen-Marburger empirical relation for the martensitic transformation

Comments on the interpretation of differential scanning calorimetry results for thermoelastic martensitic transformations: Athermal versus thermally activated kinetics

International Nuclear Information System (INIS)

Morris, A.; Lipe, T.

1996-01-01

In a previous article Van Humbeeck and Planes have made a number of criticisms of the authors' recent paper concerning the interpretation of the results obtained by Differential Scanning Calorimetry (DSC) from the Martensitic Transformation of Cu-Al-Ni-Mn-B alloys. Although the martensitic transformation of these shape memory alloys is generally classified as athermal, it has been confirmed that the capacity of the alloys to undergo a more complete thermoelastic transformation (i.e. better reversibility of the transformation) increased with the Mn content. This behavior has been explained by interpreting the DSC results obtained during thermal cycling in terms of a thermally activated mechanism controlling the direct and reverse transformations. When the heating rate increases during the reverse transformation the DSC curves shift towards higher temperatures while they shift towards the lower temperatures when the cooling rate was increased during the direct transformation. Since the starting transformation temperatures (As, Ms) do not shift, Van Humbeeck and Planes state that there is no real peak shift and assume that the DCS experiments were carried out without taking into account the thermal lag effect between sample and cell. On the following line they deduce a time constant, τ, of 60 seconds because the peak maximum shifts. In fact the assumption made by Van Humbeeck and Planes is false

Differential scanning calorimetry study on the binding of nucleic acids to dimyristoylphosphatidylcholine-sphingosine liposomes.

Science.gov (United States)

Kõiv, A; Mustonen, P; Kinnunen, P K

1994-03-31

Binding of DNA and RNA to sphingosine-containing dimyristoylphosphatidylcholine (DMPC) liposomes was characterized by differential scanning calorimetry. The thermal phase behaviour of neat DMPC liposomes was unaffected by the presence of the nucleic acids. However, significant alterations in the melting profiles of the DMPC/sphingosine composite membranes were produced by DNA and RNA, thus revealing their binding to the liposomes. For example, for 79:21 (molar ratio) DMPC/sphingosine liposomes a single endotherm at 29.1 degrees C with an enthalpy of 6.3 kcal/mol lipid was observed. In the presence of DNA at the nucleotide/sphingosine ratio of 0.6 this endotherm separated into three distinct peaks at 28.0, 31.4 and 35.1 degrees C, together with an approximately 22% reduction in the total enthalpy. Further increase in DNA concentration up to 1.5 nucleotides per sphingosine led to complete loss of the original heat absorption peak of the DMPC/sphingosine liposomes, while an endotherm at 34.3 degrees C with delta H of 2.7 kcal/mol developed. By visual inspection, rapid and extensive aggregation of the liposomes due to DNA was evident. Evidence for DNA-induced phase separation was also provided by compression isotherms of sphingosine containing DMPC monolayers recorded over an aqueous buffer both in the presence and absence of DNA. The effects of RNA on the thermal phase behaviour of the composite liposomes were qualitatively similar to those described above for DNA. Notably, the presence of eggPA abolished the nucleic acid induced heat capacity changes for DMPC/sphingosine liposomes probably because of neutralization of the positive charge of sphingosine. The binding of DNA to DMPC/sphingosine liposomes occurred both below and above the lipid phase transition temperature, as shown by fluorescence resonance energy transfer utilizing adriamycin-labelled DNA as a quencher and membrane incorporated pyrene-labelled phospholipid as a donor. However, the apparent binding to

Compatibilidad química por calorimetría diferencial de barrido y termogravimetría del auranofin tabletas 3 mg Chemical compatibility of 3 mg Auranofin tablets demonstrated by differential scanning calorimetry and thermogravimetry

Directory of Open Access Journals (Sweden)

Luis Octavio Martínez Álvarez

2011-03-01

Full Text Available Como parte de la pre-estabilidad de la preformulación de auranofin tabletas, se realizó un estudio de compatibilidad química, para lo cual se emplearon técnicas de análisis térmico como la calorimetría diferencial de barrido y la termogravimetría. Previo a dichos estudios se caracterizó térmicamente por calorimetría diferencial de barrido el principio activo y cada uno de los excipientes. Posteriormente se procedió a la realización del estudio de compatibilidad química, mediante la preparación de mezclas físicas binarias entre el principio activo y cada uno de los excipientes. Se detectó por ambos métodos que el principio activo tuvo una transición física de fusión, no reportada en la literatura, lo que permitió poder calcular su pureza por calorimetría diferencial de barrido. Mediante la técnica calorimétrica fue posible inferir la ausencia de incompatibilidad química entre el principio activo y los excipientes estudiados. Además, mediante el cálculo de la energía de activación se estableció el siguiente orden de estabilidad térmica: auranofin:PVP> auranofin:lactosa> auranofin:explotab> auranofin:estearato> auranofin:aerosil> auranofin:celulosa, por lo que se recomienda el uso de estos excipientes en la elaboración de la formulación farmacéutica.As part of the pre-stability study of the Auranofin tablet pre-formulation, a chemical compatibility study was conducted using thermal analysis techniques such as the differential scanning calorimetry and the thermogravimetry. Prior to these studies, the active principle and each of the excipients were thermally characterized with the aid of the differential scanning calorimetry. Then, there proceeded to carry out the chemical compatibility study by preparing binary physical mixtures between the active principle and each of the excipients. Both methods showed that the active principle had a melting physical transition, not reported in the literature, which allowed

Specific heat capacities of different clayey samples obtained by differential scanning calorimetry

International Nuclear Information System (INIS)

Fernandez, A.M.

2012-01-01

Document available in extended abstract form only. The thermo-physical properties allow to calculate heat flows and to determine the thermal behaviour of the materials. Temperature influences the rates of the physical, chemical and biological reactions and processes in the soil or a material. Variations in temperature and water content in thermal, hydraulic, mechanical and geochemical processes affect the thermal properties such as density, specific heat, thermal conductivity and thermal diffusivity. Therefore, mathematical models that describe the dependence of the thermal properties on temperature and concentration are of interest to be used in computational programs applied to the modelling of coupled thermo-mechanical-hydraulic and chemical (THMC) processes. In this work, the specific heat capacity of different clayey international reference materials was determined. Differential Scanning Calorimetry (DSC) was used for such purpose. DSC is the main tool for determining the specific heat capacities of materials as a function of temperature. The specific heat capacity, c p (J/Kg.K), is a measurement of the amount of heat required to raise the temperature of a unit mass of a substance by one unit of temperature. A change in temperature, caused by a gain or a loss of heat from a material, depends on the specific heat capacity of the material. Thus, the specific heat capacity is a key and characteristic property of a material and/or substance, which should be determine accurately. The specific heat capacity is an intensive property and, unlike the thermal conductivity and thermal diffusivity, is independent of the dry density of the material. C p of the solid samples was determined by using a SETSYS Evolution 16 thermal analyser coupled to a differential scanning calorimeter (TG-DSC-DTA) from SETARAM Instrumentation. The thermal analyser system can use a heating rate from 0.01 to 100 C/min under a dynamic argon atmosphere and temperatures ranging from ambient to

Characterization of crystallization kinetics of a Ni- (Cr, Fe, Si, B, C, P) based amorphous brazing alloy by non-isothermal differential scanning calorimetry

International Nuclear Information System (INIS)

Raju, S.; Kumar, N.S. Arun; Jeyaganesh, B.; Mohandas, E.; Mudali, U. Kamachi

2007-01-01

The thermal stability and crystallization kinetics of a Ni- (Cr, Si, Fe, B, C, P) based amorphous brazing foil have been investigated by non-isothermal differential scanning calorimetry. The glass transition temperature T g , is found to be 720 ± 2 K. The amorphous alloy showed three distinct, yet considerably overlapping crystallization transformations with peak crystallization temperatures centered around 739, 778 and 853 ± 2 K, respectively. The solidus and liquidus temperatures are estimated to be 1250 and 1300 ± 2 K, respectively. The apparent activation energies for the three crystallization reactions have been determined using model free isoconversional methods. The typical values for the three crystallization reactions are: 334, 433 and 468 kJ mol -1 , respectively. The X-ray diffraction of the crystallized foil revealed the presence of following compounds Ni 3 B (Ni 4 B 3 ), CrB, B 2 Fe 15 Si 3 , CrSi 2 , and Ni 4.5 Si 2 B

Stoichiometrical trends in differential scanning calorimetry measurements on phase-change materials

Energy Technology Data Exchange (ETDEWEB)

Klein, Michael; Linn, Malte; Wuttig, Matthias [I. Physikalisches Institut, RWTH Aachen University, Aachen (Germany)

2009-07-01

Phase-change materials are alloys which can be rapidly switched between two metastable states, the amorphous and the crystalline phase. At the same time they show pronounced contrast in their electrical and optical properties. They are widely used as the functional layer in rewritable optical discs. Prototypes of electrical devices employing phase change materials as non-volatile memory are already entering the market. Here we present calorimetric measurements, mainly on ternary Ge-Sb-Te alloys. Scratched-off thin film samples were heated in a differential scanning calorimeter to measure the transition from as-deposited amorphous to metastable crystalline phase and finally to the stable crystalline phase. The different transition temperatures will be analysed as a function of stoichiometry in order to improve the understanding of their interconnection.

Differential scanning calorimetry of whole Escherichia coli treated with the antimicrobial peptide MSI-78 indicate a multi-hit mechanism with ribosomes as a novel target

Directory of Open Access Journals (Sweden)

Alexander M. Brannan

2015-12-01

Full Text Available Differential Scanning Calorimetry (DSC of intact Escherichia coli (E. coli was used to identify non-lipidic targets of the antimicrobial peptide (AMP MSI-78. The DSC thermograms revealed that, in addition to its known lytic properties, MSI-78 also has a striking effect on ribosomes. MSI-78’s effect on DSC scans of bacteria was similar to that of kanamycin, an antibiotic drug known to target the 30S small ribosomal subunit. An in vitro transcription/translation assay helped confirm MSI-78’s targeting of ribosomes. The scrambled version of MSI-78 also affected the ribosome peak of the DSC scans, but required greater amounts of peptide to cause a similar effect to the unscrambled peptide. Furthermore, the effect of the scrambled peptide was not specific to the ribosomes; other regions of the DSC thermogram were also affected. These results suggest that MSI-78’s effects on E. coli are at least somewhat dependent on its particular structural features, rather than a sole function of its overall charge and hydrophobicity. When considered along with earlier work detailing MSI-78’s membrane lytic properties, it appears that MSI-78 operates via a multi-hit mechanism with multiple targets.

On the interpretation of differential scanning calorimetry results for thermoelastic martensitic transformations: Athermal versus thermally activated kinetics

International Nuclear Information System (INIS)

Van Humbeeck, J.; Planes, A.

1996-01-01

Experimentally, two distinct classes of martensitic transformations are considered: athermal and isothermal. In the former class, on cooling, at some well-defined start temperature (M s ), isolated small regions of the martensitic product begin to appear in the parent phase. The transformation at any temperature appears to be instantaneous in practical time scales, and the amount of transformed material (x) does not depend on time, i.e., it increases at each step of lowering temperature. The transition is not completed until the temperature is lowered below M f (martensite finish temperature). The transformation temperatures are only determined by chemical (composition and degree of order) and microstructural factors. The external controlling parameter (T or applied stress) determines the free energy difference between the high and the low temperature phases, which provides the driving force for the transition. In the development of athermal martensite activation kinetics is secondary. Athermal martensite, as observed in the well known shape memory alloys Cu-Zn-Al, Cu-Al-Ni and Ni-Ti, cannot be attributed to a thermally activated mechanism for which kinetics are generally described by the Arrhenius rate equation. However, the latter has been applied by Lipe and Morris to results for the Martensitic Transformation of Cu-Al-Ni-B-Mn obtained by conventional Differential Scanning Calorimetry (DSC). It is the concern of the authors of this letter to point out the incongruences arising from the analysis of calorimetric results, corresponding to forward and reverse thermoelastic martensitic transformations, in terms of standard kinetic analysis based on the Arrhenius rate equation

Cure Kinetics of Benzoxazine/Cycloaliphatic Epoxy Resin by Differential Scanning Calorimetry

Science.gov (United States)

Gouni, Sreeja Reddy

Understanding the curing kinetics of a thermoset resin has a significant importance in developing and optimizing curing cycles in various industrial manufacturing processes. This can assist in improving the quality of final product and minimizing the manufacturing-associated costs. One approach towards developing such an understanding is to formulate kinetic models that can be used to optimize curing time and temperature to reach a full cure state or to determine time to apply pressure in an autoclave process. Various phenomenological reaction models have been used in the literature to successfully predict the kinetic behavior of a thermoset system. The current research work was designed to investigate the cure kinetics of Bisphenol-A based Benzoxazine (BZ-a) and Cycloaliphatic epoxy resin (CER) system under isothermal and nonisothermal conditions by Differential Scanning Calorimetry (DSC). The cure characteristics of BZ-a/CER copolymer systems with 75/25 wt% and 50/50 wt% have been studied and compared to that of pure benzoxazine under nonisothermal conditions. The DSC thermograms exhibited by these BZ-a/CER copolymer systems showed a single exothermic peak, indicating that the reactions between benzoxazine-benzoxazine monomers and benzoxazine-cycloaliphatic epoxy resin were interactive and occurred simultaneously. The Kissinger method and isoconversional methods including Ozawa-Flynn-Wall and Freidman were employed to obtain the activation energy values and determine the nature of the reaction. The cure behavior and the kinetic parameters were determined by adopting a single step autocatalytic model based on Kamal and Sourour phenomenological reaction model. The model was found to suitably describe the cure kinetics of copolymer system prior to the diffusion-control reaction. Analyzing and understanding the thermoset resin system under isothermal conditions is also important since it is the most common practice in the industry. The BZ-a/CER copolymer system with

Experimental determination of the (vapor + liquid) equilibrium data of binary mixtures of fatty acids by differential scanning calorimetry

International Nuclear Information System (INIS)

Matricarde Falleiro, Rafael M.; Meirelles, Antonio J.A.; Kraehenbuehl, Maria A.

2010-01-01

(Vapor + liquid) equilibrium (VLE) data for three binary mixtures of saturated fatty acids were obtained by differential scanning calorimetry (DSC). However, changes in the calorimeter pressure cell and the use of hermetic pans with holes (φ = 250 mm) in the lids were necessary to make it possible to apply this analytical technique, obtaining accurate results with smaller samples and shorter operational times. The systems evaluated in this study were: myristic acid (C 14:0 ) + palmitic acid (C 16:0 ), myristic acid (C 14:0 ) + stearic acid (C 18:0 ), and palmitic acid (C 16:0 ) + stearic acid (C 18:0 ), all measured at 50 mm Hg and with mole fractions between 0.0 and 1.0 in relation to the most volatile component of each diagram. The fugacity coefficients for the components in the vapor phase were calculated using the Hayden and O'Connell method [J.G. Hayden, J.P. O'Connell, Ind. Eng. Chem. Process Design Develop. 14 (3) (1975) 209-216] and the activity coefficients for the liquid phase were correlated with the traditional g E models (NRTL [H. Renon, J.M. Prausnitz, Aiche J. 14 (1968) 135-144], UNIQUAC [D.S. Abrams, J.M. Prausnitz, Aiche J. 21 (1975) 116-128], and Wilson [J.M. Prausnitz, N.L. Linchtenthaler, E.G. Azevedo, Molecular Thermodynamics of Fluid-phase Equilibria, River-Prentice Hall, Upper Saddle, 1999]). The sets of parameters were then compared in order to determine which adjustments best represented the VLE.

Excess heat capacity of the (Li1?xCax)F1+x liquid solution determined by differential scanning calorimetry and drop calorimetry

NARCIS (Netherlands)

Capelli, E.; Benes, O.; Konings, R.J.M.

2014-01-01

The work presents the measured heat capacity of the (Li1?xCax)F1+x liquid solution. Four samples with different compositions have been prepared and measured using a Differential Scanning Calorimeter. Since this technique was newly adopted for measuring encapsulated fluoride samples, some

Interaction between vitamin D 2 and magnesium in liposomes: Differential scanning calorimetry and FTIR spectroscopy studies

Science.gov (United States)

Toyran, Neslihan; Severcan, Feride

2007-08-01

Magnesium (Mg 2+) ion is of great importance in physiology by its intervention in 300 enzymatic systems, its role in membrane structure, its function in neuromuscular excitability and vitamin D metabolism and/or action. In the present study, the interaction of Mg 2+, at low (1 mole %) and high (7 mole %) concentrations with dipalmitoyl phosphatidylcholine (DPPC) liposomes has been studied in the presence and absence of vitamin D 2 (1 mole %) by using two noninvasive techniques, namely differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy. DSC studies reveal that the presence of vitamin D 2 in the pure or Mg 2+ (at both low and high concentrations) containing liposomes diminishes the pretransition. The calorimetric results also reveal that, inclusion of Mg 2+ (more significantly at high concentration) into pure or vitamin D 2 containing DPPC liposomes increases the main phase transition temperature. The investigation of the CH 2 symmetric, the CH 3 asymmetric, the C dbnd O stretching, and the PO2- antisymmetric double bond stretching bands in FTIR spectra with respect to changes occurring in the wavenumber and/or the bandwidth values as a function of temperature reveal that, inclusion of vitamin D 2 or Mg 2+ into pure DPPC liposomes orders and decreases the dynamics of the acyl chains in both gel and liquid-crystalline phases and does not induce hydrogen bond formation in the interfacial region. Furthermore, the dynamics of the head groups of the liposomes decreases in both phases. Our findings reveal that, simultaneous presence of vitamin D 2 and Mg 2+ alters the effect of each other, which is reflected as a decrease in the interactions between these two additives within the model membrane.

Using a Differential Scanning Calorimeter to Teach Phase Equilibria to Students of Igneous and Metamorphic Petrology

Science.gov (United States)

Maria, Anton H.; Millam, Evan L.; Wright, Carrie L.

2011-01-01

As an aid for teaching phase equilibria to undergraduate students of igneous and metamorphic petrology, we have designed a laboratory exercise that allows them to create a phase diagram from data produced by differential scanning calorimetry. By preparing and analyzing samples of naphthalene and phenanthrene, students acquire hands-on insight into…

Physical-chemical characterization and stability study of alpha-trypsin at ph 3.0 by differential scanning calorimetry

Energy Technology Data Exchange (ETDEWEB)

Santos, A.M.C.; Santana, M.A.; Gomide, F.T.F.; Oliveira, J.S.; Vilas Boas, F.A.S.; Santoro, M.M.; Teixera, K.N. [Universidade Federal de Minas Gerais (UFMG), Belo Horizonte, MG (Brazil). Inst. de Ciencias Biologicas (ICB). Dept. de Bioquimica e Imunologia; Miranda, A.A.C.; Biondi, I. [Universidade Estadual de Feira de Santana (UEFS), BA (Brazil). Dept. de Ciencias Biologicas; Vasconcelos, A.B.; Bemquerer, M.P. [EMBRAPA Recursos Geneticos e Biotecnologia, Brasilia, DF (Brazil). Parque Estacao Biologica (PqEB)

2008-07-01

Full text: {alpha}-Trypsin is a serine-protease with a polypeptide chain of 223 amino acid residues and six disulfide bridges. It is a globular protein with predominance of antiparallel {beta}-sheet secondary structure and it has two domains with similar structures. In the present work, a stability study of {alpha}-trypsin in the acid pH range was performed and physical-chemical denaturation parameters were measured by using differential scanning calorimetry (DSC). The {alpha}-trypsin has a shelf-life (t{sub 95%}) of about ten months at pH 3.0 and 4 deg C and its hydrolysis into the {psi}-trypsin isoform is negligible during six months as monitored by mass spectrometry (Micromass Q-ToF). The observed {delta}H{sub cal}/{delta}H{sub vH} ratio is close to unity for {alpha}-trypsin denaturation, which suggests the occurrence of a two-state transition, devoid of molten-globule intermediates. At pH 3.0, {alpha}-trypsin unfolded with T{sub m} 325.9 K and {delta}H= 99.10 kcal mol{sup -1}, and the change in heat capacity between the native and unfolded forms of the protein was estimated to be 1.96 {+-} 0.18 kcal mol{sup -1} K{sup -1}. The stability of {alpha}-trypsin calculated at 298 K and at pH 3.0 was {delta}G{sub U} = 6.10 kcal mol{sup -1}. These values are in the range expected for a small globular protein. These results show that the thermodynamic parameters for unfolding of {beta}-trypsin do not change substantially after its conversion to {alpha}-trypsin.

State of the water in crosslinked sulfonated poly(ether ether ketone). Two-dimensional differential scanning calorimetry correlation mapping

Energy Technology Data Exchange (ETDEWEB)

Al Lafi, Abdul G. [Department of Chemistry, Atomic Energy Commission, Damascus, P.O. Box 6091 (Syrian Arab Republic); Hay, James N., E-mail: cscientific9@aec.org.sy [The School of Metallurgy and Materials, College of Physical Sciences and Engineering, University of Birmingham, Edgbaston, Birmingham B15 2TT (United Kingdom)

2015-07-20

Highlights: • 2D-DSC mapping was applied to analyze the heat flow responses of hydrated crosslinked sPEEK. • Two types of loosely bond water were observed. • The first was bond to the sulfonic acid groups and increased with ion exchange capacity. • The second was attributed to the polar groups introduced by ions irradiation and increased with crosslinking degree. • DSC combined with 2D mapping provides a powerful tool for polymer structural determination. - Abstract: This paper reports the first application of two-dimensional differential scanning calorimetry correlation mapping, 2D-DSC-CM to analyze the heat flow responses of sulphonated poly(ether ether ketone), sPEEK, films having different ion exchange capacity and degrees of crosslinks. With the help of high resolution and high sensitivity of 2D-DSC-CM, it was possible to locate two types of loosely bound water within the structure of crosslinked sPEEK. The first was bound to the sulfonic acid groups and dependent on the ion exchange capacity of the sPEEK. The second was bound to other polar groups, either introduced by irradiation with ions and dependent on the crosslinking degree or present in the polymer such as the carbonyl groups or terminal units. The results suggest that the ability of the sulfonic acid groups in the crosslinked sPEEK membranes to adsorb water molecules is increased by crosslinking, probably due to the better close packing efficiency of the crosslinked samples. DSC combined with 2D correlation mapping provides a fast and powerful tool for polymer structural determination.

An evaluation of the transition temperature range of super-elastic orthodontic NiTi springs using differential scanning calorimetry.

Science.gov (United States)

Barwart, O; Rollinger, J M; Burger, A

1999-10-01

Differential scanning calorimetry (DSC) was used to determine the transition temperature ranges (TTR) of four types of super-elastic orthodontic nickel-titanium coil springs (Sentalloy). A knowledge of the TTR provides information on the temperature at which a NiTi wire or spring can assume superelastic properties and when this quality disappears. The spring types in this study can be distinguished from each other by their characteristic TTR during cooling and heating. For each tested spring type a characteristic TTR during heating (austenite transformation) and cooling (martensite transformation) was evaluated. The hysteresis of the transition temperature, found between cooling and heating, was 3.4-5.2 K. Depending on the spring type the austenite transformation started (As) at 9.7-17.1 degrees C and finished (Af) at 29.2-37 degrees C. The martensite transformation starting temperature (Ms) was evaluated at 32.6-25.4 degrees C, while Mf (martensite transformation finishing temperature) was 12.7-6.5 degrees C. The results show that the springs become super-elastic when the temperature increases and As is reached. They undergo a loss of super-elastic properties and a rapid decrease in force delivery when they are cooled to Mf. For the tested springs, Mf and As were found to be below room temperature. Thus, at room temperature and some degrees lower, all the tested springs exert super-elastic properties. For orthodontic treatment this means the maintenance of super-elastic behaviour, even when mouth temperature decreases to about room temperature as can occur, for example, during meals.

Cholesterol affects the interaction between an ionic liquid and phospholipid vesicles. A study by differential scanning calorimetry and nanoplasmonic sensing.

Science.gov (United States)

Russo, Giacomo; Witos, Joanna; Rantamäki, Antti H; Wiedmer, Susanne K

2017-12-01

The present work aims at studying the interactions between cholesterol-rich phosphatidylcholine-based lipid vesicles and trioctylmethylphosphonium acetate ([P 8881 ][OAc]), a biomass dissolving ionic liquid (IL). The effect of cholesterol was assayed by using differential scanning calorimetry (DSC) and nanoplasmonic sensing (NPS) measurement techniques. Cholesterol-enriched dipalmitoyl-phosphatidylcholine vesicles were exposed to different concentrations of the IL, and the derived membrane perturbation was monitored by DSC. The calorimetric data could suggest that the binding and infiltration of the IL are delayed in the vesicles containing cholesterol. To clarify our findings, NPS was applied to quantitatively follow the resistance of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine incorporating 0, 10, and 50mol% of cholesterol toward the IL exposure over time. The membrane perturbation induced by different concentrations of IL was found to be a concentration dependent process on cholesterol-free lipid vesicles. Moreover, our results showed that lipid depletion in cholesterol-enriched lipid vesicles is inversely proportional to the increasing amount of cholesterol in the vesicles. These findings support that cholesterol-rich lipid bilayers are less susceptible toward membrane disrupting agents as compared to membranes that do not incorporate any sterols. This probably occurs because cholesterol tightens the phospholipid acyl chain packing of the plasma membranes, increasing their resistance and reducing their permeability. Copyright © 2017 Elsevier B.V. All rights reserved.

Differential scanning calorimetry of the effects of temperature and humidity on phenol-formaldehyde resin cure

Science.gov (United States)

X.-M. Wang; B. Riedl; A.W. Christiansen; R.L. Geimer

1994-01-01

Phenol-formaldehyde (PF) resin is a widely used adhesive in the manufacture of wood composites. However, curing behaviour of the resin under various environmental conditions is not well known. A differential scanning calorimeter was employed to characterize the degree of resin cure in this study. Resin-impregnated glass cloth samples with varied moisture contents (0,31...

Heat capacity and transition behavior of sucrose by standard, fast scanning and temperature-modulated calorimetry

Energy Technology Data Exchange (ETDEWEB)

Magoń, A. [Department of Chemistry, University of Technology, 35-959 Rzeszów (Poland); Wurm, A.; Schick, C. [Department of Physics, University of Rostock, 18057 Rostock (Germany); Pangloli, Ph.; Zivanovic, S. [Department of Food Science and Technology, University of Tennessee, Knoxville, TN 37996 (United States); Skotnicki, M. [Department of Pharmaceutical Technology, Poznan University of Medical Sciences, 60-780 Poznań (Poland); Pyda, M., E-mail: mpyda@utk.edu [Department of Chemistry, University of Technology, 35-959 Rzeszów (Poland)

2014-08-10

Highlights: • Experimental, apparent heat capacity of sucrose was investigated by advanced thermal analysis. • Vibrational heat capacity of solid state was linked with a low temperature experimental heat capacity of sucrose. • Equilibrium melting parameters of sucrose were determined. • Decomposition, superheating of crystalline sucrose during melting process were presented. • TGA, DSC, TMDSC, and FSC are useful tools for characterization of sucrose. - Abstract: The heat capacity (C{sub p}) of crystalline and amorphous sucrose was determined using standard and quasi-isothermal temperature modulated differential scanning calorimetry. The results were combined with the published data determined by adiabatic calorimetry, and the C{sub p} values are now reported for the wide 5–600 K range. The experimental C{sub p} of solid sucrose at 5–300 K was used to calculate the vibrational, solid C{sub p} based on the vibrational molecular motions. The calculated solid and liquid C{sub p} together with the transition parameters for equilibrium conditions were used as references for detailed quantitative thermal analysis of crystalline and amorphous sucrose. Melting temperature (T{sub m}) of the crystalline sucrose was identified in a broad 442–465 K range with a heat of fusion of 40–46 J/mol determined at heating rates 0.5–20 K/min, respectively. The equilibrium T{sub m} and heat of fusion of crystalline sucrose were estimated at zero heating rate as T{sup o}{sub m} = 424.4 K and ΔH{sup o}{sub f} = 32 kJ/mol, respectively. The glass transition temperature (T{sub g}) of amorphous sucrose was at 331 K with a change in C{sub p} of 267 J/(mol K) as it was estimated from reversing heat capacity by quasi-isothermal TMDSC on cooling. At heating rates less than 30 K/min, thermal decomposition occurred during melting, while at extreme rate of 1000 K/s, degradation was not observed. Data obtained by fast scanning calorimetry (FSC) at 1000 K/s, showed that T{sub m} was

Compatibilidad química del piracetam determinada por calorimetría diferencial de barrido Chemical compatibility of piracetam determined by differential scanning calorimetry

Directory of Open Access Journals (Sweden)

Luis Octavio Martínez Álvarez

2013-03-01

Full Text Available Introducción: en la primera etapa de preformulación de un medicamento se seleccionan los excipientes y es importante la realización de los estudios de compatibilidad química entre el ingrediente activo farmacéutico (IFA y excipientes. Una de las técnicas más rápidas para realizar dichos estudios es la Calorimetría diferencial de barrido (DSC, y como técnica complementaria la Termogravimetría (TG. Objetivo: empleando DSC y TG, se realiza un estudio de compatibilidad química entre IFA y excipientes preseleccionados, para comprobar la existencia o no de interacción química. Métodos: el equipo empleado fue el TA3000Mettler, aco­plado a la celda DSC20 y al horno TG50. El IFA utilizado fue Piracetam, y los excipientes: Kollidon VA 64, Estearato de magnesio, Celulosa microcristalina, Polietilenglicol 20 000 y Aerosil. Dichos excipientes se caracterizaron por DSC al igual que el IFA, al cual se le detectó la transición física de fusión. Para el estudio de compatibilidad se prepararon mezclas físicas binarias en una relación de concentración 1:1 Resultados: la figura 1 muestra la detección del punto de fusión por DSC del IFA. Se obtuvieron dos transiciones endotérmicas, comprobándose por TG cuál era la de fusión. La figura 2 muestra los termogramas de las mezclas formadas entre IFA y excipientes. Conclusiones: no se detectó aparición de nuevos picos, por lo que se infiere que no hay incompatibilidad química entre las sustancias estudiadas y se recomienda el uso de los excipientes para el desarrollo de la formulación farmacéutica.Introduction: the first phase of the drug preformulation comprises the selection of excipients and the conduction of studies on chemical compatibility between pharmacologically active ingredient and the excipients. One of the quickest techniques is the differential scanning calorimetry and the supplementary technique called thermogravimetic analysis. Objective: to conduct a chemical compatibility

Crystallization kinetics of Fe-B based amorphous alloys studied in-situ using X-rays diffraction and differential scanning calorimetry

Directory of Open Access Journals (Sweden)

Santos D.R. dos

2001-01-01

Full Text Available The crystallization processes for the amorphous metallic alloys Fe74B17Si2Ni4Mo3 and Fe86B6Zr7Cu1 (at. % were investigated using X-rays diffraction measurements performed in-situ during Joule-heating, with simultaneous monitoring of the electrical resistance. We determined the main structural transitions and crystalline phases formed during heating, and correlated these results to the observed resistance variations. As the annealing current is increased, the resistance shows an initial decrease due to stress relaxation, followed by a drop to a minimum value due to massive nucleation and growth of alpha-Fe nanocrystals. Further annealing causes the formation of small fractions of Fe-B, B2Zr or ZrO2, while the resistance increases due to temperature enhancement. In situ XRD measurements allowed the identification of metastable phases, as the gamma-Fe phase which occurs at high temperatures. The exothermal peaks observed in the differential scanning calorimetry (DSC for each alloy corroborate the results. We also have performed DSC measurements with several heating rates, which allowed the determination of the Avrami exponent and crystallization activation energy for each alloy. The obtained activation energies (362 and 301 kJ/mol for Fe-B-Zr-Cu; 323 kJ/mol for Fe-B-Si-Ni-Mo are comparable to reported values for amorphous iron alloys, while the Avrami exponent values (n = 1.0 or n = 1.2 are consistent with diffusion controlled crystallization processes with nucleation rates close to zero.

Quantifying low amorphous or crystalline amounts of alpha-lactose-monohydrate using X-ray powder diffraction, near-infrared spectroscopy, and differential scanning calorimetry.

Science.gov (United States)

Fix, I; Steffens, K J

2004-05-01

Efficient and accurate quantification of low amorphous and crystalline contents within pharmaceutical materials still remains a challenging task in the pharmaceutical industry. Since X-ray powder diffraction (XRPD) equipment has improved in recent years, our aim was 1) to investigate the possibility of substantially lowering the detection limits of amorphous or crystalline material to about 1% or 0.5% w/w respectively by applying conventional Bragg Brentano optics, combined with a fast and simple evaluation technique; 2) to perform these measurements within a short time to make it suitable for routine analysis; and 3) to subject the same data sets to a partial least squares regression (PLSR) in order to investigate whether it is possible to improve accuracy and precision compared to the standard integration method. Near-infrared spectroscopy (NIRS) and differential scanning calorimetry (DSC) were chosen as reference method. As model substance, alpha lactose monohydrate was chosen to create calibration curves based on predetermined mixtures of highly crystalline and amorphous substance. In contrast to DSC, XRPD and NIRS revealed an excellent linearity, precision, and accuracy with the percent of crystalline amount and a detectability down to about 0.5% w/w. Chemometric evaluation (partial least squares regression) applied to the XRPD data further improved the quality of our calibration.

Vibrational spectroscopic characterisation of salmeterol xinafoate polymorphs and a preliminary investigation of their transformation using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry

International Nuclear Information System (INIS)

Ali, Hassan Refat H.; Edwards, Howell G.M.; Hargreaves, Michael D.; Munshi, Tasnim; Scowen, Ian J.; Telford, Richard J.

2008-01-01

Knowledge and control of the polymorphic phases of chemical compounds are important aspects of drug development in the pharmaceutical industry. Salmeterol xinafoate, a long acting β-adrenergic receptor agonist, exists in two polymorphic Forms, I and II. Raman and near infrared spectra were obtained of these polymorphs at selected wavelengths in the range of 488-1064 nm; significant differences in the Raman and near-infrared spectra were apparent and key spectral marker bands have been identified for the vibrational spectroscopic characterisation of the individual polymorphs which were also characterised with X ray diffractometry. The solid-state transition of salmeterol xinafoate polymorphs was studied using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry isothermally between transitions. This method assisted in the unambiguous characterisation of the two polymorphic forms by providing a simultaneous probe of both the thermal and vibrational data. The study demonstrates the value of a rapid in situ analysis of a drug polymorph which can be of potential value for at-line in-process control

Vibrational spectroscopic characterisation of salmeterol xinafoate polymorphs and a preliminary investigation of their transformation using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry

Energy Technology Data Exchange (ETDEWEB)

Ali, Hassan Refat H. [Chemical and Forensic Sciences/University Analytical Centre, School of Life Sciences, University of Bradford, Richmond Road, Bradford BD7 1DP (United Kingdom); Edwards, Howell G.M. [Chemical and Forensic Sciences/University Analytical Centre, School of Life Sciences, University of Bradford, Richmond Road, Bradford BD7 1DP (United Kingdom)], E-mail: H.G.M.Edwards@bradford.ac.uk; Hargreaves, Michael D.; Munshi, Tasnim; Scowen, Ian J.; Telford, Richard J. [Chemical and Forensic Sciences/University Analytical Centre, School of Life Sciences, University of Bradford, Richmond Road, Bradford BD7 1DP (United Kingdom)

2008-07-14

Knowledge and control of the polymorphic phases of chemical compounds are important aspects of drug development in the pharmaceutical industry. Salmeterol xinafoate, a long acting {beta}-adrenergic receptor agonist, exists in two polymorphic Forms, I and II. Raman and near infrared spectra were obtained of these polymorphs at selected wavelengths in the range of 488-1064 nm; significant differences in the Raman and near-infrared spectra were apparent and key spectral marker bands have been identified for the vibrational spectroscopic characterisation of the individual polymorphs which were also characterised with X ray diffractometry. The solid-state transition of salmeterol xinafoate polymorphs was studied using simultaneous in situ portable Raman spectroscopy and differential scanning calorimetry isothermally between transitions. This method assisted in the unambiguous characterisation of the two polymorphic forms by providing a simultaneous probe of both the thermal and vibrational data. The study demonstrates the value of a rapid in situ analysis of a drug polymorph which can be of potential value for at-line in-process control.

The effect of increasing membrane curvature on the phase transition and mixing behavior of a dimyristoyl-sn-glycero-3-phosphatidylcholine/distearoyl-sn-glycero-3-phosphatidylcholine lipid mixture as studied by Fourier transform infrared spectroscopy and differential scanning calorimetry

DEFF Research Database (Denmark)

Brumm, T.; Jørgensen, Kent; Mouritsen, Ole G.

1996-01-01

The phase transition behavior of a lipid bilayer of dimyristoyl-sn-glycero-3-phosphalidylcholine/distearoyl-sn- glycero-3-phosphatidylcholine (DMPC-d54/DSPC) (1:1) on a solid support with varying curvatures was investigated with differential scanning calorimetry, infrared spectroscopy, and model...... of the liquidus point can be understood as a reduction of the lateral pressure in the bilayer with increasing curvature. The shift of the solidus line is interpreted as a result of the increased demixing of the two components in the two-phase region with increasing curvature due to lowering of the lateral...

Influence of bending mode on the mechanical properties of nickel-titanium archwires and correlation to differential scanning calorimetry measurements.

Science.gov (United States)

Brauchli, Lorenz M; Keller, Heidi; Senn, Christiane; Wichelhaus, Andrea

2011-05-01

Nickel-titanium orthodontic archwires are used with bonded appliances for initial leveling. However, precise bending of these archwires is difficult and can lead to changes within the crystal structure of the alloy, thus changing the mechanical properties unpredictably. The aim of this study was to evaluate different bending methods in relation to the subsequent mechanical characteristics of the alloy. The mechanical behaviors of 3 archwires (Copper NiTi 35°C [Ormco, Glendora, Calif], Neo Sentalloy F 80 [GAC International, Bohemia, NY], and Titanol Low Force [Forestadent, Pforzheim, Germany]) were investigated after heat-treatment in a dental furnace at 550-650°C, treatment with an electrical current (Memory-Maker, Forestadent), and cold forming. In addition, the change in A(f) temperature was registered by means of differential scanning calorimetry. Heat-treatment in the dental furnace as well as with the Memory-Maker led to widely varying force levels for each product. Cold forming resulted in similar or slightly reduced force levels when compared to the original state of the wires. A(f) temperatures were in general inversely proportional to force levels. Archwire shape can be modified by using either chair-side technique (Memory-Maker, cold forming) because the superelastic behavior of the archwires is not strongly affected. However it is important to know the specific changes in force levels induced for each individual archwire with heat-treatment. Cold forming resulted in more predictable forces for all products tested. Therefore, cold forming is recommended as a chair-side technique for the shaping of NiTi archwires. Copyright © 2011 American Association of Orthodontists. Published by Mosby, Inc. All rights reserved.

Conformational study of red kidney bean (Phaseolus vulgaris L.) protein isolate (KPI) by tryptophan fluorescence and differential scanning calorimetry.

Science.gov (United States)

Yin, Shou-Wei; Tang, Chuan-He; Yang, Xiao-Quan; Wen, Qi-Biao

2011-01-12

Fluorescence and differential scanning calorimetry (DSC) were used to study changes in the conformation of red kidney bean (Phaseolus vulgaris L.) protein isolate (KPI) under various environmental conditions. The possible relationship between fluorescence data and DSC characteristics was also discussed. Tryptophan fluorescence and fluorescence quenching analyses indicated that the tryptophan residues in KPI, exhibiting multiple fluorophores with different accessibilities to acrylamide, are largely buried in the hydrophobic core of the protein matrix, with positively charged side chains close to at least some of the tryptophan residues. GdnHCl was more effective than urea and SDS in denaturing KPI. SDS and urea caused variable red shifts, 2-5 nm, in the emission λ(max), suggesting the conformational compactness of KPI. The result was further supported by DSC characteristics that a discernible endothermic peak was still detected up to 8 M urea or 30 mM SDS, also evidenced by the absence of any shift in emission maximum (λ(max)) at different pH conditions. Marked decreases in T(d) and enthalpy (ΔH) were observed at extreme alkaline and/or acidic pH, whereas the presence of NaCl resulted in higher T(d) and ΔH, along with greater cooperativity of the transition. Decreases in T(d) and ΔH were observed in the presence of protein perturbants, for example, SDS and urea, indicating partial denaturation and decrease in thermal stability. Dithiothreitol and N-ethylmaleimide have a slight effect on the thermal properties of KPI. Interestingly, a close linear relationship between the T(d) (or ΔH) and the λ(max) was observed for KPI in the presence of 0-6 M urea.

Correlation between Temperature-dependent Fatigue Resistance and Differential Scanning Calorimetry Analysis for 2 Contemporary Rotary Instruments.

Science.gov (United States)

Arias, Ana; Macorra, José C; Govindjee, Sanjay; Peters, Ove A

2018-04-01

The aim of this study was to assess differences in cyclic fatigue (CF) life of contemporary heat-treated nickel-titanium rotary instruments at room and body temperatures and to document corresponding phase transformations. Forty Hyflex EDM (H-EDM) files (Coltene, Cuyahoga Falls, OH [#25/.08, manufactured by electrical discharge machining]) and 40 TRUShape (TS) files (Dentsply Tulsa Dental Specialties, Tulsa, OK [#25/.06v, manufactured by grinding and shape setting]) were divided into 2 groups (n = 20) for CF resistance tests in a water bath either at room (22°C ± 0.5°C) or body temperature (37°C ± 0.5°C). Instruments were rotated in a simulated canal (angle = 60°, radius = 3 mm, and center of the curvature 5 mm from the tip) until fracture occurred. The motor was controlled by an electric circuit that was interrupted after instrument fracture. The mean half-life and beta and eta Weibull parameters were determined and compared. Two instruments of each brand were subjected to differential scanning calorimetry (DSC). While TS instruments lasted significantly longer at room temperature (mean life = 234.7 seconds; 95% confidence interval [CI], 209-263.6) than at body temperature (mean life = 83.2 seconds; 95% CI, 76-91.1), temperature did not affect H-EDM behavior (room temperature mean life = 725.4 seconds; 95% CI, 658.8-798.8 and body temperature mean life = 717.9 seconds; 95% CI, 636.8-809.3). H-EDM instruments significantly outlasted TS instruments at both temperatures. At body temperature, TS was predominantly austenitic, whereas H-EDM was martensitic or in R-phase. TS was in a mixed austenitic/martensitic phase at 22°C, whereas H-EDM was in the same state as at 37°C. H-EDM had a longer fatigue life than TS, which showed a marked decrease in fatigue life at body temperature; neither the life span nor the state of the microstructure in the DSC differed for H-EDM between room or body temperature. Copyright © 2017 American Association of

The heat capacity of polyethylene fibers measured by multi-frequency temperature-modulated calorimetry

International Nuclear Information System (INIS)

Pyda, M.; Nowak-Pyda, E.; Wunderlich, B.

2006-01-01

The apparent heat capacity of polyethylene fibers in the melting region was measured by quasi-isothermal, temperature-modulated differential scanning calorimetry (TMDSC) and compared with results from standard differential scanning calorimetry (DSC) and the solid and liquid thermodynamic heat capacity as references from the ATHAS Data Bank. Using a multi-frequency, complex sawtooth modulation in the quasi-isothermal mode disclosed for the first time that the uncorrected apparent heat capacity C p =A Φ /(A T s ω) of the liquid polyethylene fiber increases with increasing frequency (A Φ is the differential heat-flow rate and A T s is the sample temperature). The frequency-dependent heat capacity cannot be represented by the expression: C p =A Φ /(A T s νω)[1+(τνω) 2 ] 0.5 because of a negative τ 2 . The results were later confirmed by independent measurements on single sinusoidal quasi-isothermal TMDSC on the same material. The error is caused by shrinking of the fiber, which deforms the sample pan

Novel Technique for Quantitative Fast Scanning Calorimetry on Electrospun Fibers

Science.gov (United States)

Thomas, David; Govinna, Nelaka; Schick, Christoph; Cebe, Peggy

Fast scanning chip calorimetry allows for the study of polymers which have rapid nucleation and/or crystallization kinetics, or degrade within their melting range. Heating rates used, up to 4000 K/s, allow studies of hetero and homogeneous nucleation at time scales inaccessible with conventional calorimeters, whose rates are typically alcohol (PVA) were chosen in the development of a new methodology to obtain quantitative fast scanning thermal data from electrospun nanofibers using a Flash DSC1. The structure of nanofibers requires special methods to load nanogram-sized samples onto a UFSC1 sensor. Fibers were directly spun onto TEM grids which provide a durable substrate to support bundles of nanofibers and possess excellent thermal conductivity allowing for a strong, repeatable signal and ensure good sample to sensor contact. As spun samples were held isothermally at temperatures ranging from Tg to Tm then heated at 2,000 K/s to assess as-spun crystallinity and cold crystallization behaviors. Above Tm the fibers break up into micro- and nano-droplets. On these samples, melt crystallization experiments were performed to study nucleation and crystallization of polymer confined to nanodroplet morphology. NSF DMR-1608125.

Introduction of Differential Scanning Calorimetry in a General Chemistry Laboratory Course: Determination of Thermal Properties of Organic Hydrocarbons

Science.gov (United States)

D'Amelia, Ronald; Franks, Thomas; Nirode, William F.

2007-01-01

In first-year general chemistry undergraduate courses, thermodynamics and thermal properties such as melting points and changes in enthalpy ([Delta]H) and entropy ([Delta]S) of phase changes are frequently discussed. Typically, classical calorimetric methods of analysis are used to determine [Delta]H of reactions. Differential scanning calorimetry…

Characterization of Synthesized and Commercial Forms of Magnesium Stearate Using Differential Scanning Calorimetry, Thermogravimetric Analysis, Powder X-Ray Diffraction, and Solid-State NMR Spectroscopy.

Science.gov (United States)

Delaney, Sean P; Nethercott, Matthew J; Mays, Christopher J; Winquist, Nickolas T; Arthur, Donia; Calahan, Julie L; Sethi, Manish; Pardue, Daniel S; Kim, Junghyun; Amidon, Gregory; Munson, Eric J

2017-01-01

Magnesium stearate is the salt of a complex mixture of fatty acids, with the majority being stearate and palmitate. It has multiple crystalline forms and, potentially, an amorphous form. Magnesium stearate is used in the pharmaceutical manufacturing industry as a powder lubricant, and typically is added at low levels (∼1%) during the manufacturing process and blended for a relatively short time (∼5 min). Proper levels and mixing times are needed, as too short a mixing time or too small a quantity will result in improper lubrication, and too much can negatively impact dissolution rates. The complex mixture of multiple fatty acids and crystalline forms in magnesium stearate leads to variability between commercial sources, and switching between sources can impact both the amount of lubricant and mixing time needed for proper lubrication. In order to better understand the complex nature of magnesium stearate, a variety of analytical techniques were used to characterize both synthesized and commercial magnesium stearate samples. The results show that correlation among differential scanning calorimetry, thermogravimetric analysis, solid-state NMR spectroscopy, and other techniques provides a unique insight into the forms of magnesium stearate. Finally, the ability to monitor form changes of magnesium stearate in an intact tablet using solid-state NMR spectroscopy is shown. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

Ionic liquids. Combination of combustion calorimetry with high-level quantum chemical calculations for deriving vaporization enthalpies.

Science.gov (United States)

Emel'yanenko, Vladimir N; Verevkin, Sergey P; Heintz, Andreas; Schick, Christoph

2008-07-10

In this work, the molar enthalpies of formation of the ionic liquids [C2MIM][NO3] and [C4MIM][NO3] were measured by means of combustion calorimetry. The molar enthalpy of fusion of [C2MIM][NO3] was measured using differential scanning calorimetry. Ab initio calculations of the enthalpy of formation in the gaseous phase have been performed for the ionic species using the G3MP2 theory. We have used a combination of traditional combustion calorimetry with modern high-level ab initio calculations in order to obtain the molar enthalpies of vaporization of a series of the ionic liquids under study.

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)

Energy Technology Data Exchange (ETDEWEB)

Rodriguez, Carmen P.; Pierce, David A.; Schweiger, Michael J.; Kruger, Albert A.; Chun, Jaehun; Hrma, Pavel R.

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 mass 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.

Kinetics of solid-gas reactions characterized by scanning AC nano-calorimetry with application to Zr oxidation

International Nuclear Information System (INIS)

Xiao, Kechao; Lee, Dongwoo; Vlassak, Joost J.

2014-01-01

Scanning AC nano-calorimetry is a recently developed experimental technique capable of measuring the heat capacity of thin-film samples of a material over a wide range of temperatures and heating rates. Here, we describe how this technique can be used to study solid-gas phase reactions by measuring the change in heat capacity of a sample during reaction. We apply this approach to evaluate the oxidation kinetics of thin-film samples of zirconium in air. The results confirm parabolic oxidation kinetics with an activation energy of 0.59 ± 0.03 eV. The nano-calorimetry measurements were performed using a device that contains an array of micromachined nano-calorimeter sensors in an architecture designed for combinatorial studies. We demonstrate that the oxidation kinetics can be quantified using a single sample, thus enabling high-throughput mapping of the composition-dependence of the reaction rate.

Polarized differential-phase laser scanning microscope

International Nuclear Information System (INIS)

Chou Chien; Lyu, C.-W.; Peng, L.-C.

2001-01-01

A polarized differential-phase laser scanning microscope, which combines a polarized optical heterodyne Mach-Zehnder interferometer and a differential amplifier to scan the topographic image of a surface, is proposed. In the experiment the differential amplifier, which acts as a PM-AM converter, in the experiment, converting phase modulation (PM) into amplitude modulation (AM). Then a novel, to our knowledge, phase demodulator was proposed and implemented for the differential-phase laser scanning microscope. An optical grating (1800 lp/mm) was imaged. The lateral and the depth resolutions of the imaging system were 0.5 μm and 1 nm, respectively. The detection accuracy, which was limited by the reflectivity variation of the test surface, is discussed

ceramics by differential scanning calorimetry

Indian Academy of Sciences (India)

Administrator

tilled water. These solutions were mixed, stirred, filtered and slowly added into a dilute ammonium hydrate solu- tion to obtain gel-like precipitates. These gels were washed with distilled water until pH = 7 and then washed several times in analytically ... chromate, barium carbonate and strontium carbonate sup- plied by the ...

Exploring ultrastability in nanostructured glassy polymer films by fast-scanning calorimetry.

Science.gov (United States)

Chowdhury, Mithun; Wang, Yucheng; Jeong, Hyuncheol; Cangialosi, Daniele; Priestley, Rodney

A decade ago ultra-stable small molecule glass formers were discovered. Since then a significant amount of research has been devoted to traverse down the energy landscape of such glass formers via physical vapor deposition (PVD). Matrix assisted pulsed laser evaporation (MAPLE) has the known ability to produce vapour deposited nanostructured polymer glass with exceptional kinetic stability. We explored the role of deposition temperature/ growth rate on thermodynamic and kinetic stabilities of poly (methyl methacrylate) (PMMA) films, deposited over a fast-scanning calorimetry sensor. We found in general any MAPLE deposited glass is kinetically more stable than bulk polymer and its spin-coated film. Moreover slow growth rate and optimum temperature during MAPLE deposition can additionally lead to thermodynamically stable (low-energy) glass. The role of interfaces formed through dramatic nanostructuring and packing of nanoglobules (removal of void space) may have additional role on such ultrastability. NSF-MRSEC through PCCM (Grant: DMR-1420541).

Continuous gradient temperature Raman spectroscopy and differential scanning calorimetry of N-3DPA and DHA from -100 to 10°C.

Science.gov (United States)

Broadhurst, C Leigh; Schmidt, Walter F; Nguyen, Julie K; Qin, Jianwei; Chao, Kuanglin; Aubuchon, Steven R; Kim, Moon S

2017-04-01

Docosahexaenoic acid (DHA, 22:6n-3) is exclusively utilized in fast signal processing tissues such as retinal, neural and cardiac. N-3 docosapentaenoic acid (n-3DPA, 22:5n-3), with just one less double bond, is also found in the marine food chain yet cannot substitute for DHA. Gradient temperature Raman spectroscopy (GTRS) applies the temperature gradients utilized in differential scanning calorimetry (DSC) to Raman spectroscopy, providing a straightforward technique to identify molecular rearrangements that occur near and at phase transitions. Herein we apply GTRS and both conventional and modulated DSC to n-3DPA and DHA from -100 to 20°C. Three-dimensional data arrays with 0.2°C increments and first derivatives allowed complete assignment of solid, liquid and transition state vibrational modes. Melting temperatures n-3DPA (-45°C) and DHA (-46°C) are similar and show evidence for solid-state phase transitions not seen in n-6DPA (-27°C melt). The C6H2 site is an elastic marker for temperature perturbation of all three lipids, each of which has a distinct three dimensional structure. N-3 DPA shows the spectroscopic signature of saturated fatty acids from C1 to C6. DHA does not have three aliphatic carbons in sequence; n-6DPA does but they occur at the methyl end, and do not yield the characteristic signal. DHA appears to have uniform twisting from C6H2 to C12H2 to C18H2 whereas n-6DPA bends from C12 to C18, centered at C15H2. For n-3DPA, twisting is centered at C6H2 adjacent to the C2-C3-C4-C5 aliphatic moiety. These molecular sites are the most elastic in the solid phase and during premelting. Copyright © 2017 Elsevier B.V. All rights reserved.

Differential scanning calorimetric study of HTPB based composite propellants in presence of nano ferric oxide

Energy Technology Data Exchange (ETDEWEB)

Patil, Prajakta R.; Krishnamurthy, V.N.; Joshi, Satyawati S. [Department of Chemistry, University of Pune, Pune 411007 (India)

2006-12-15

A comparative study of the thermal decomposition of ammonium perchlorate (AP)/hydroxy terminated polybutadiene (HTPB) based composite propellants has been carried out in presence and absence of nano iron oxide at different heating rates in a dynamic nitrogen atmosphere using differential scanning calorimetry. The pronounced effect was a lowering of the high temperature decomposition by 49 C. A higher heat release up to 40% was observed in presence of nano ferric oxide (3.5 nm). The kinetic parameters were evaluated using the Kissinger method. The increase of the rate constant in the catalyzed propellant confirmed the enhancement of the catalytic activity of ammonium perchlorate. The scanning electron micrographs of nano Fe{sub 2}O{sub 3} incorporated in HTPB revealed a well-separated characteristic necklace-like structure of {alpha}-Fe{sub 2}O{sub 3} particles at high magnification. (Abstract Copyright [2006], Wiley Periodicals, Inc.)

Non-isothermal crystallization kinetics and fragility of (Cu46Zr47Al7)97Ti3 bulk metallic glass investigated by differential scanning calorimetry

International Nuclear Information System (INIS)

Zhu, Man; Li, Junjie; Yao, Lijuan; Jian, Zengyun; Chang, Fang’e; Yang, Gencang

2013-01-01

Highlights: • Non-isothermal crystallization kinetics of (Cu 46 Zr 47 Al 7 ) 97 Ti 3 BMGs was studied. • Two-stage of crystallization process is confirmed by DSC. • The nucleation process is difficult than growth process during crystallization. • The second crystallization process is the most sensitive to heating rate. • Kinetic fragility index is evaluated suggesting it is an intermediate glass. - Abstract: In this paper, bulk metallic glasses with the composition of (Cu 46 Zr 47 Al 7 ) 97 Ti 3 were prepared by copper mold casting technique. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) were used to investigate its structure and non-isothermal crystallization kinetics. DSC traces revealed that it undergoes two-stage crystallization. The activation energies corresponding to the characteristic temperatures have been calculated, and the results reveal that the as-cast alloys have a good thermal stability in thermodynamics. Based on Kissinger equation, the activation energies for glass transition, the first and second crystallization processes were obtained as 485 ± 16 kJ/mol, 331 ± 7 kJ/mol and 210 ± 3 kJ/mol, respectively, suggesting that the nucleation process is more difficult than the grain growth process. The fitting curves using Lasocka's empirical relation show that the influence of the heating rate for crystallization is larger than glass transition. Furthermore, the kinetic fragility for (Cu 46 Zr 47 Al 7 ) 97 Ti 3 bulk metallic glasses is evaluated. Depending on the fragility index, (Cu 46 Zr 47 Al 7 ) 97 Ti 3 bulk metallic glasses should be considered as “intermediate glasses”

A modified differential scanning calorimetry for determination of cell volumetric change during the freezing process.

Science.gov (United States)

Luo, Dawei; Han, Xu; He, Liqun; Cui, Xiangdong; Cheng, Shuxia; Lu, Caicheng; Liu, Jianghan; Gao, Dayong

2002-01-01

A modified analytical and experimental method using differential scanning calorimeter (DSC) was developed to determine the cell volume change during the freezing process. Two cell types were used in the study: human platelets and erythrocytes (red blood cells). Isotonic cell suspensions with different cytocrits were prepared and used in the DSC experiments. Low cooling rates were used to avoid intracellular ice formation. Cell suspensions were cooled from room temperature to -40 degrees C. Latent heat release from the freezing of cell suspensions was shown to be a linear function of cytocrit. From slope and intercept of the linear function, cell volume change was determined based on a developed theoretical model. From experimental data and theoretical analyses, it was revealed that (a) the final volume of a human platelet at -40 degrees C was 33.7% of its isotonic volume, and 15.2% of the original (at isotonic condition) intracellular water remained unfrozen inside platelets, and (b) the final volume of human erythrocyte at -40 degrees C was 50.0% of its isotonic volume, and 30.3% of the original intracellular water was kept inside cells as residual unfrozen water.

From Trioleoyl glycerol to extra virgin olive oil through multicomponent triacylglycerol mixtures: Crystallization and polymorphic transformation examined with differential scanning calorimetry and X-ray diffration techniques.

Science.gov (United States)

Bayés-García, L; Calvet, T; Cuevas-Diarte, M A; Ueno, S

2017-09-01

The polymorphic crystallization and transformation behavior of extra virgin olive oil (EVOO) was examined by using differential scanning calorimetry (DSC) and X-ray diffraction with both laboratory-scale (XRD) and synchrotron radiation source (SR-XRD). The complex behavior observed was studied by previously analyzing mixtures composed by its main 2 to 6 triacylglycerol (TAG) components. Thus, component TAGs were successively added to simulate EVOO composition, until reaching a 6 TAGs mixture, composed by trioleoyl glycerol (OOO), 1-palmitoyl-2,3-dioleoyl glycerol (POO), 1,2-dioleoyl-3-linoleoyl glycerol (OOL), 1-palmitoyl-2-oleoyl-3-linoleoyl glycerol (POL), 1,2-dipalmitoyl-3-oleoyl glycerol (PPO) and 1-stearoyl-2,3-dioleoyl glycerol (SOO). Molten samples were cooled from 25°C to -80°C at a controlled rate of 2°C/min and subsequently heated at the same rate. The polymorphic behavior observed in multicomponent TAG mixtures was interpreted by considering three main groups of TAGs with different molecular structures: triunsaturated OOO and OOL, saturated-unsaturated-unsaturated POO, POL and SOO, and saturated-saturated-unsaturated PPO. As confirmed by our previous work, TAGs belonging to the same structural group displayed a highly similar polymorphic behavior. EVOO exhibited two different β'-2L polymorphic forms (β' 2 -2L and β' 1 -2L), which transformed into β'-3L when heated. Equivalent polymorphic pathways were detected when the same experimental conditions were applied to the 6 TAG components mixture. Hence, minor components may not exert a strong influence in this case. Copyright © 2017 Elsevier Ltd. All rights reserved.

Investigation of magnetocaloric effect in La0.45Pr0.25Ca0.3MnO3 by magnetic, differential scanning calorimetry and thermal analysis

International Nuclear Information System (INIS)

Aparnadevi, M.; Barik, S.K.; Mahendiran, R.

2012-01-01

We investigated magnetocaloric effect in La 0.45 Pr 0.25 Ca 0.3 MnO 3 by direct methods (changes in temperature and latent heat) and indirect method (magnetization isotherms). This compound undergoes a first-order paramagnetic to ferromagnetic transition with T C =200 K upon cooling. The paramagnetic phase becomes unstable and it transforms into a ferromagnetic phase under the application of magnetic field, which results in a field-induced metamagnetic transition (FIMMT). The FIMMT is accompanied by release of latent heat and temperature of the sample as evidenced from differential scanning calorimetry and thermal analysis experiments. A large magnetic entropy change of ΔS m =−7.2 J kg −1 K −1 at T=212.5 K and refrigeration capacity of 228 J kg −1 are found for a field change of ΔH=5 T. It is suggested that destruction of magnetic polarons and growth of ferromagnetic phase accompanied by a lattice volume change with increasing magnetic field is responsible for the large magnetocaloric effect in this compound. - Highlights: ► We report magnetic entropy change measured by indirect and direct methods in La 0.45 Pr 0.25 Ca 0.3 MnO 3. ► Anomalous field-induced induced metamagnetic transition is found in the paramagnetic state. ► A large reversible magnetic entropy change (ΔS m =7.2 J kg −1 K −1 for ΔH=5 T). ► A large refrigeration capacity (RC=228 J kg −1 ). ► Collapse of magnetic polarons is suggested as possible origin of the large MCE.

Interactions in interesterified palm and palm kernel oils mixtures. II – Microscopy and Differential Scanning Calorimetry

Directory of Open Access Journals (Sweden)

Grimaldi, Renato

2001-12-01

Full Text Available Palm oil (PO and palm kernel oil (PKO compositions (100/0, 80/20, 60/40, 50/50, 40/60, 20/80 and 0/100 were interesterified in laboratory scale under predetermined conditions (0.4% sodium metoxide, 20 minutes, 100ºC. The fourteen samples, before and after interesterification, were characterized by Polarized Light Microscopy and Differential Scanning Calorimetry (DSC. Results showed the effect of various factors on the form and width of crystals. The mean area of crystals revealed the increase of crystals when PKO was added, with values varying from 2.7 x 10E3 µm2 to PO and 1.8 x 10E6 µm2 to PKO. After interesterification, the crystal widths were lower at PO/PKO 100/0, 80/20, 60/40, 20/80 fractions and were higher to anothers. The beta-prime polimorphic form was observed in the pure palm oil sample. The results showed in melting curves, onset values from –19.6ºC to more unsaturated peaks until 20.7ºC to more saturated ones. The higher values to more saturated peak in a melting curve to palm oil, 38.7 J.g-1 before and 48.4 J.g-1 after interesterification, showed a mores table saturated group. I n a genera l way, t h e interesterification promoted an increase of crystallization rate and a better compatibility between PO/PKO fractions.Fueron interesterificados en el laboratorio mezclas de aceite de palma (PO y aceite de palmiste (PKO en diferentes proporciones (100/0, 80/20, 60/40, 50/50, 40/60, 20/80 y 0/100 bajo condiciones predeterminadas (0.4% metoxido de sodio, 20 minutos, 100ºC. Las catorce muestras fueron caracterizadas antes y después de la interesterificación por Microscopía de Luz Polarizada y por Calorimetría Diferencial de Barrido (DSC. Los resultados mostraron el efecto de varios factores sobre la forma y anchura de los cristales. El área media de los cristales revela el aumento de tamaño de los mismos cuando aumenta la proporción de PKO, con valores que varían entre 2.7 x 10E3 µm2 para PO y 1.8 x 10E

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.

Science.gov (United States)

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.

The use of differential scanning calorimetry for the evaluation of dental materials. I. Cements, cavity lining materials and anterior restorative materials.

Science.gov (United States)

McCabe, J F; Wilson, H J

1980-03-01

Thermal changes occurring during the setting of restorative materials have been measured accurately using a differential scanning calorimeter. The results were used to evaluate setting characteristics. The heat of reaction and rate of heat output may be significant in determining thermal damage to the pulp. The heat capacity is related to thermal insulation properties. These properties have been determined and their effect on the efficacy of restorative materials discussed.

Adiabatic differential scanning calorimetric study of divalent cation induced DNA - DPPC liposome formulation compacted for gene delivery

Directory of Open Access Journals (Sweden)

Erhan Süleymanoglu

2004-11-01

Full Text Available Complexes between nucleic acids and phospholipid vesicles have been developed as stable non-viral gene delivery vehicles. Currently employed approach uses positively charged lipid species and a helper zwitterionic lipid, the latter being applied for the stabilization of the whole complex. However, besides problematic steps during their preparation, cationic lipids are toxic for cells. The present work describes some energetic issues pertinent to preparation and use of neutral lipid-DNA self-assemblies, thus avoiding toxicity of lipoplexes. Differential scanning calorimetry data showed stabilization of polynucleotide helix upon its interaction with liposomes in the presence of divalent metal cations. It is thus possible to suggest this self-assembly as an improved formulation for use in gene delivery.

Nucleation behavior of melted Bi films at cooling rates from 101 to 104 K/s studied by combining scanning AC and DC nano-calorimetry techniques

International Nuclear Information System (INIS)

Xiao, Kechao; Vlassak, Joost J.

2015-01-01

Highlights: • We proposed a general data reduction scheme that combines scanning AC and DC calorimetry results for the study of reaction kinetics. • Calorimetry measurements at cooling rates ranging from 30 K/s to 20,000 K/s were achieved. • Upon initial melting, the Bi thin-film sample breaks up into thousands of isolated islands, and highly repeatable nucleation behavior is observed. • The nucleation rate of melted Bi is calculated, which can be well described by classical nucleation theory over a wide range of cooling rates. - Abstract: We study the nucleation behavior of undercooled liquid Bi at cooling rates ranging from 10 1 to 10 4 K/s using a combination of scanning DC and AC nano-calorimetry techniques. Upon initial melting, the Bi thin-film sample breaks up into silicon nitride-coated isolated islands. The number of islands in a typical sample is sufficiently large that highly repeatable nucleation behavior is observed, despite the stochastic nature of the nucleation process. We establish a data reduction technique to evaluate the nucleation rate from DC and AC calorimetry results. The results show that the driving force for the nucleation of melted Bi is well described by classical nucleation theory over a wide range of cooling rates. The proposed technique provides a unique and efficient way to examine nucleation kinetics with cooling rates over several orders of magnitude. The technique is quite general and can be used to evaluate reaction kinetics in other materials

A real time analysis of the self-assembly process using thermal analysis inside the differential scanning calorimeter instrument.

Science.gov (United States)

Roy, Debmalya; Shastri, Babita; Mukhopadhyay, K

2012-07-12

The supramolecular assembly of the regioregular poly-3-hexylthiophene (rr-P3HT) in solution has been investigated thoroughly in the past. In the current study, our focus is on the enthalpy of nanofiber formation using thermal analysis techniques by performing the self-assembly process inside the differential scanning calorimetry (DSC) instrument. Thermogravimetric analysis (TGA) was carried out to check the concentration of the solvent during the self-assembly process of P3HT in p-xylene. Ultraviolet visible (UV-vis) spectophotometric technique, small-angle X-ray scattering (SAXS) experiment, atomic force microscopic (AFM), and scanning electron microscopic (SEM) images were used to characterize the different experimental yields generated by cooling the reaction mixture at desired temperatures. Comparison of the morphologies of self-assembled products at different fiber formation temperatures gives us an idea about the possible crystallization parameters which could affect the P3HT nanofiber morphology.

Electrical conductivity, differential scanning calorimetry, X-ray diffraction, and 7Li nuclear magnetic resonance studies of n-CxH(2x+1)OSO3Li (x = 12, 14, 16, 18, and 20)

International Nuclear Information System (INIS)

Hirakawa, Satoru; Morimoto, Yoshiaki; Honda, Hisashi

2015-01-01

Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C x H (2x+1) OSO 3 Li (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 (2x+1) OSO 3 Na and n-C x H (2x+1) OSO 3 K (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 (ΔS). For n-C 18 H 37 OSO 3 Li and n-C 20 H 41 OSO 3 Li salts, each melting point produced a small ΔS mp value compared with the total entropy change in the solid phases (ΔS tr1 +ΔS 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. 7 Li NMR spectra of n-C 18 H 37 OSO 3 Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals

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)

Science.gov (United States)

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.

Differential scanning calorimetric study of the binding between native DNA and its primary water of hydration.

Science.gov (United States)

Marlowe, R. L.; Lukan, A. M.; Lee, S. A.; Anthony, L.; Rupprecht, A.

1996-03-01

Differential scanning calorimetry was used to measure the binding strength between calf-thymus DNA and its primary water of hydration. The specific heat of wet-spun films was found to have a broad endothermic transition near 80 ^oC and a sharp exothermic transition near 250 ^oC. The broad transition is believed to be mainly due to the breaking of the bonds of the strongly bound water of hydration. This transition was found to be reversible, as expected. Kissinger analysis indicates that the activation barrier for breaking the bonds of these water molecules is about 0.6 eV. The sharp transition appeared to be an indication of a thermal decomposition of the DNA. Samples taken above this transition lost mass, showed evidence of having melted, and had turned black in color. This transition is irreversible.

Method for HEPA filter leak scanning with differentiating aerosol detector

Energy Technology Data Exchange (ETDEWEB)

Kovach, B.J.; Banks, E.M.; Wikoff, W.O. [NUCON International, Inc., Columbus, OH (United States)

1997-08-01

While scanning HEPA filters for leaks with {open_quotes}Off the Shelf{close_quote} aerosol detection equipment, the operator`s scanning speed is limited by the time constant and threshold sensitivity of the detector. This is based on detection of the aerosol density, where the maximum signal is achieved when the scanning probe resides over the pinhole longer than several detector time-constants. Since the differential value of the changing signal can be determined by observing only the first small fraction of the rising signal, using a differentiating amplifier will speed up the locating process. The other advantage of differentiation is that slow signal drift or zero offset will not interfere with the process of locating the leak, since they are not detected. A scanning hand-probe attachable to any NUCON{reg_sign} Aerosol Detector displaying the combination of both aerosol density and differentiated signal was designed. 3 refs., 1 fig.

High-pressure differential scanning microcalorimeter.

Science.gov (United States)

Senin, A A; Dzhavadov, L N; Potekhin, S A

2016-03-01

A differential scanning microcalorimeter for studying thermotropic conformational transitions of biopolymers at high pressure has been designed. The calorimeter allows taking measurements of partial heat capacity of biopolymer solutions vs. temperature at pressures up to 3000 atm. The principles of operation of the device, methods of its calibration, as well as possible applications are discussed.

Silk I and Silk II studied by fast scanning calorimetry

Energy Technology Data Exchange (ETDEWEB)

Cebe, Peggy; Partlow, Benjamin P.; Kaplan, David L.; Wurm, Andreas; Zhuravlev, Evgeny; Schick, Christoph

2017-06-01

Using fast scanning calorimetry (FSC), we investigated the glass transition and crystal melting of samples of B. mori silk fibroin containing Silk I and/or Silk II crystals. Due to the very short residence times at high temperatures during such measurements, thermal decomposition of silk protein can be significantly suppressed. FSC was performed at 2000 K/s using the Mettler Flash DSC1 on fibroin films with masses around 130–270 ng. Films were prepared with different crystalline fractions (ranging from 0.26 to 0.50) and with different crystal structures (Silk I, Silk II, or mixed) by varying the processing conditions. These included water annealing at different temperatures, exposure to 50% MeOH in water, or autoclaving. The resulting crystal structure was examined using wide angle X-ray scattering. Degree of crystallinity was evaluated from Fourier transform infrared (FTIR) spectroscopy and from analysis of the heat capacity increment at the glass transition temperature. Silk fibroin films prepared by water annealing at 25 °C were the least crystalline and had Silk I structure. FTIR and FSC studies showed that films prepared by autoclaving or 50% MeOH exposure were the most crystalline and had Silk II structure. Intermediate crystalline fraction and mixed Silk I/Silk II structures were found in films prepared by water annealing at 37 °C. FSC results indicate that Silk II crystals exhibit endotherms of narrower width and have higher mean melting temperature Tm(II) = 351 ± 2.6 °C, compared to Silk I crystals which melt at Tm(I) = 292 ± 3.8 °C. Films containing mixed Silk I/Silk II structure showed two clearly separated endothermic peaks. Evidence suggests that the two types of crystals melt separately and do not thermally interconvert on the extremely short time scale (0.065 s between onset and end of melting) of the FSC experiment.

Measuring the temperature dependent thermal diffusivity of geomaterials using high-speed differential scanning calorimetry

Science.gov (United States)

von Aulock, Felix W.; Wadsworth, Fabian B.; Vasseur, Jeremie; Lavallée, Yan

2016-04-01

Heat diffusion in the Earth's crust is critical to fundamental geological processes, such as the cooling of magma, heat dissipation during and following transient heating events (e.g. during frictional heating along faults), and to the timescales of contact metamorphosis. The complex composition and multiphase nature of geomaterials prohibits the accurate modeling of thermal diffusivities and measurements over a range of temperatures are sparse due to the specialized nature of the equipment and lack of instrument availability. We present a novel method to measure the thermal diffusivity of geomaterials such as minerals and rocks with high precision and accuracy using a commercially available differential scanning calorimeter (DSC). A DSC 404 F1 Pegasus® equipped with a Netzsch high-speed furnace was used to apply a step-heating program to corundum single crystal standards of varying thicknesses. The standards were cylindrical discs of 0.25-1 mm thickness with 5.2-6 mm diameter. Heating between each 50 °C temperature interval was conducted at a rate of 100 °C/min over the temperature range 150-1050 °C. Such large heating rates induces temperature disequilibrium in the samples used. However, isothermal segments of 2 minutes were used during which the temperature variably equilibrated with the furnace between the heating segments and thus the directly-measured heat-flow relaxed to a constant value before the next heating step was applied. A finite-difference 2D conductive heat transfer model was used in cylindrical geometry for which the measured furnace temperature was directly applied as the boundary condition on the sample-cylinder surfaces. The model temperature was averaged over the sample volume per unit time and converted to heat-flow using the well constrained thermal properties for corundum single crystals. By adjusting the thermal diffusivity in the model solution and comparing the resultant heat-flow with the measured values, we obtain a model

Investigation of magnetocaloric effect in La{sub 0.45}Pr{sub 0.25}Ca{sub 0.3}MnO{sub 3} by magnetic, differential scanning calorimetry and thermal analysis

Energy Technology Data Exchange (ETDEWEB)

Aparnadevi, M; Barik, S K [Department of Physics, 2 Science Drive 3, National University of Singapore, Lower Kent Ridge Road, Singapore-117 452 (Singapore); Mahendiran, R [Department of Physics, 2 Science Drive 3, National University of Singapore, Lower Kent Ridge Road, Singapore-117 452 (Singapore)

2012-10-15

We investigated magnetocaloric effect in La{sub 0.45}Pr{sub 0.25}Ca{sub 0.3}MnO{sub 3} by direct methods (changes in temperature and latent heat) and indirect method (magnetization isotherms). This compound undergoes a first-order paramagnetic to ferromagnetic transition with T{sub C}=200 K upon cooling. The paramagnetic phase becomes unstable and it transforms into a ferromagnetic phase under the application of magnetic field, which results in a field-induced metamagnetic transition (FIMMT). The FIMMT is accompanied by release of latent heat and temperature of the sample as evidenced from differential scanning calorimetry and thermal analysis experiments. A large magnetic entropy change of {Delta}S{sub m}=-7.2 J kg{sup -1} K{sup -1} at T=212.5 K and refrigeration capacity of 228 J kg{sup -1} are found for a field change of {Delta}H=5 T. It is suggested that destruction of magnetic polarons and growth of ferromagnetic phase accompanied by a lattice volume change with increasing magnetic field is responsible for the large magnetocaloric effect in this compound. - Highlights: Black-Right-Pointing-Pointer We report magnetic entropy change measured by indirect and direct methods in La{sub 0.45}Pr{sub 0.25}Ca{sub 0.3}MnO{sub 3.} Black-Right-Pointing-Pointer Anomalous field-induced induced metamagnetic transition is found in the paramagnetic state. Black-Right-Pointing-Pointer A large reversible magnetic entropy change ({Delta}S{sub m}=7.2 J kg{sup -1} K{sup -1} for {Delta}H=5 T). Black-Right-Pointing-Pointer A large refrigeration capacity (RC=228 J kg{sup -1}). Black-Right-Pointing-Pointer Collapse of magnetic polarons is suggested as possible origin of the large MCE.

Usefulness of Thallium Scan for Differential Diagnosis of Breast Mass

Energy Technology Data Exchange (ETDEWEB)

Bae, Sang Kyun; Yum, Ha Yong; Lee, Chung Han; Choi, Kyung Hyun [Kosin University College of Medicine, Pusan (Korea, Republic of)

1994-07-15

The purpose of this study is to evaluate thallium scanning as a potential test in differentiating malignant from benign lesions of breast. Thirty-one female patients underwent thallium scan of the breast. After intravenous injection of 74-111 MBq(2-3 mCi)of thallium-201, anterior and lateral images were obtained. We compared thallium scans with pathological results. Of 11 patients with breast cancers, 10 cases (90.9%) were detected using thallium scan. Thallium scan obtained in one patient who had breast cancer but received several cycles of chemotherapy did not show thallium uptake. The smallest detectable cancer was 1.5 cm in diameter. In contrast, there is no thallium accumulation in breasts of 17 of 20 patients with benign disease (85%), Three cases of 13 fibrocystic disease show thallium uptake in their breast. In conclusion, thallium scan is an effective test in differentiating benign from malignant lesion.

Usefulness of Thallium Scan for Differential Diagnosis of Breast Mass

International Nuclear Information System (INIS)

Bae, Sang Kyun; Yum, Ha Yong; Lee, Chung Han; Choi, Kyung Hyun

1994-01-01

The purpose of this study is to evaluate thallium scanning as a potential test in differentiating malignant from benign lesions of breast. Thirty-one female patients underwent thallium scan of the breast. After intravenous injection of 74-111 MBq(2-3 mCi)of thallium-201, anterior and lateral images were obtained. We compared thallium scans with pathological results. Of 11 patients with breast cancers, 10 cases (90.9%) were detected using thallium scan. Thallium scan obtained in one patient who had breast cancer but received several cycles of chemotherapy did not show thallium uptake. The smallest detectable cancer was 1.5 cm in diameter. In contrast, there is no thallium accumulation in breasts of 17 of 20 patients with benign disease (85%), Three cases of 13 fibrocystic disease show thallium uptake in their breast. In conclusion, thallium scan is an effective test in differentiating benign from malignant lesion.

Calorimetry

International Nuclear Information System (INIS)

Pope, B.

1983-01-01

An overall review of properties of various types of calorimeters is given, with special attention given to the challenges of high luminosity and high energy. The calorimeters described include continuous calorimeters, scintillation sampling calorimetry, gas sampling calorimetry, and liquid ionization calorimeters. Next explored are some limiting factors involved in experiments at high luminosities (or at high energies), and some examples are offered of detectors capable of operating at the highest luminosities (energies). Specific areas where substantial research and development work is needed are itemized

Temperature modulated differential scanning calorimetry. Modelling and applications

International Nuclear Information System (INIS)

Jiang, Z.

2000-01-01

The research focused on the TMDSC technique with respect to both theoretical problems and applications. The modelling has been performed to address the effects of heat transfer on the quantitative measurement of TMDSC experiments. A procedure has been suggested to correct the effect on the phase angle obtained by dynamic TMDSC. The effects under quasi-isothermal conditions have been investigated using improved models in terms of various heat transfer interface qualities, sample properties and sensor properties. The contributions of the sensor's properties to the heat transfer are, for the first time, separated from the overall effects. All the modelling results are compared with the corresponding experimental data and they are in good agreement. Ripples and fluctuations on the experimental signals during some transitions have been simulated using a simple model, and then, been shown to be artefacts of the Fourier transformation process. The applications of TMDSC to both research and commercial samples are reported in terms of differing either the experimental conditions or the thermal history of the sample for the studies of the glass transition, cold crystallisation, the melting transition, the clearing transition of a liquid crystal polymer, and the vitrification of an epoxy resin under quasi-isothermal conditions. The results show that the interpretations of some quantities obtained by TMDSC to some physical transitions still need to be clarified by further work. The applications also show the abilities of TMDSC for combining the sensitivity of a measurement at high instantaneous heating with the resolution obtained by measuring at a low underlying heating and measuring the heat capacity of the sample and its variation under the quasi-isothermal conditions. The frequency dependent complex heat capacity during the glass transition provides a window to measure the apparent activation energy of the transition, which is different from the window used by conventional DSC. Some shortcomings of TMDSC have been noticed in both modelling and application work. Firstly, any experiments for purpose of either understanding or the quantitative measurements of TMDSC output quantities should be performed under carefully selected conditions which can satisfy the linear response assumption. Secondly, some signals in particular those associated with kinetic processes may not be fully sampled by TMDSC due to the limit of the observing window of a modulation. Thirdly, the TMDSC evaluation procedure introduces mathematical artefacts into the output signals. As a consequence, it is preferable to include as many temperature modulations as possible within any transition being studied in order obtain good quality experimental signals by eliminating or minimising these artefacts. (author)

Detection of irradiated food by differential scanning calorimetry

International Nuclear Information System (INIS)

Nesvadba, P.; Kent, M.

1991-01-01

It has been showed that the freezing point of chicken is depressed on irradiation and that this can serve as a possible method of detection of irradiated chicken. The purposed of the present work was to see whether other foods (cod, mushroom) show the freezing point depression

Analytical methods for lignin characterization - Differential scanning calorimetry

NARCIS (Netherlands)

Koullas, D.P.; Koukios, E.G.; Avgerinos, E.; Abaecherli, A.; Gosselink, R.; Vasile, C.; Lehnen, R.; Saake, B.; Suren, J.

2006-01-01

Results of a round robin on lignin thermal analyses are reported. Six laboratories have conducted thermal analyses of four lignin types to determine their cp values and softening points, and to study the thermal behaviour, materials endo- and exotherms included. The lignin types examined were wood

Characterization of the molecular distribution of drugs in glassy solid dispersions at the nano-meter scale, using differential scanning calorimetry and gravimetric water vapour sorption techniques.

Science.gov (United States)

van Drooge, D J; Hinrichs, W L J; Visser, M R; Frijlink, H W

2006-03-09

The molecular distribution in fully amorphous solid dispersions consisting of poly(vinylpyrrolidone) (PVP)-diazepam and inulin-diazepam was studied. One glass transition temperature (T(g)), as determined by temperature modulated differential scanning calorimetry (TMDSC), was observed in PVP-diazepam solid dispersions prepared by fusion for all drug loads tested (10-80 wt.%). The T(g) of these solid dispersions gradually changed with composition and decreased from 177 degrees C for pure PVP to 46 degrees C for diazepam. These observations indicate that diazepam was dispersed in PVP on a molecular level. However, in PVP-diazepam solid dispersions prepared by freeze drying, two T(g)'s were observed for drug loads above 35 wt.% indicating phase separation. One T(g) indicated the presence of amorphous diazepam clusters, the other T(g) was attributed to a PVP-rich phase in which diazepam was dispersed on a molecular level. With both the value of the latter T(g) and the DeltaC(p) of the diazepam glass transition the concentrations of molecular dispersed diazepam could be calculated (27-35 wt.%). Both methods gave similar results. Water vapour sorption (DVS) experiments revealed that the PVP-matrix was hydrophobised by the incorporated diazepam. TMDSC and DVS results were used to estimate the size of diazepam clusters in freeze dried PVP-diazepam solid dispersions, which appeared to be in the nano-meter range. The inulin-diazepam solid dispersions prepared by spray freeze drying showed one T(g) for drug loads up to 35 wt.% indicating homogeneous distribution on a molecular level. However, this T(g) was independent of the drug load, which is unexpected because diazepam has a lower T(g) than inulin (46 and 155 degrees C, respectively). For higher drug loads, a T(g) of diazepam as well as a T(g) of the inulin-rich phase was observed, indicating the formation of amorphous diazepam clusters. From the DeltaC(p) of the diazepam glass transition the amount of molecularly dispersed

Electrical conductivity, differential scanning calorimetry, X-ray diffraction, and {sup 7}Li nuclear magnetic resonance studies of n-C{sub x}H{sub (2x+1)}OSO{sub 3}Li (x = 12, 14, 16, 18, and 20)

Energy Technology Data Exchange (ETDEWEB)

Hirakawa, Satoru [Yokohama City University, Graduate School of Nanobioscience (Japan); Morimoto, Yoshiaki [Yokohama City University, International College of Arts and Sciences (Japan); Honda, Hisashi, E-mail: hhonda@yokohama-cu.ac.jp [Yokohama City University, Graduate School of Nanobioscience (Japan)

2015-04-15

Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C {sub x}H{sub (2x+1)}OSO{sub 3}Li (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 {sub x}H{sub (2x+1)}OSO{sub 3}Na and n-C {sub x}H{sub (2x+1)}OSO{sub 3}K (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 (ΔS). For n-C {sub 18}H{sub 37}OSO{sub 3}Li and n-C {sub 20}H{sub 41}OSO{sub 3}Li salts, each melting point produced a small ΔS{sub mp} value compared with the total entropy change in the solid phases (ΔS{sub tr1}+ΔS{sub tr2}). Additionally, Li {sup +} 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. {sup 7}Li NMR spectra of n-C {sub 18}H{sub 37}OSO{sub 3}Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li {sup +} ions are localized at asymmetric sites in the crystals.

Calorimetry of non-reacting systems

CERN Document Server

McCullough, John P

2013-01-01

Experimental Thermodynamics, Volume 1: Calorimetry of Non-Reacting Systems covers the heat capacity determinations for chemical substances in the solid, liquid, solution, and vapor states, at temperatures ranging from near the absolute zero to the highest at which calorimetry is feasible.This book is divided into 14 chapters. The first four chapters provide background information and general principles applicable to all types of calorimetry of non-reacting systems. The remaining 10 chapters deal with specific types of calorimetry. Most of the types of calorimetry treated are developed over a c

Thallium 201 thyroid scan: differential diagnosis of benign and malignant nodules

International Nuclear Information System (INIS)

Oh, Jong Sub; Kim, Byong Geun; Park, Byung Ran; Kim, Se Jong; Ko, Kang Seok; Kim, Min Joong; Ji, Joo Yun

1995-01-01

To evaluate useful findings and diagnostic value of TI-201 thyroid scan in differentiating benign from malignant nodules. We studied 77 cold thyroid nodules proven histologically(27 malignant and 50 benign). Early (5-15 min) and delayed images(3-5 hours) were obtained after intravenous injection of thallium 201. In these nodules, we retrospectively analyzed the degree of TI-201 uptake in early and delayed images, histopathologic type, size, and presence or absence of cystic change in the sonograms of 22 malignant nodules. Useful finding for diagnosis of malignant nodules was strong uptake of TI-201 in early and delayed images(specificity: 98%, sensitivity: 63%, positive predictive value: 94.4%). Useful finding for benign nodules was no uptake of TI-201 in delayed image(specificity: 88.9%, sensitivity: 68%, positive predictive value: 91.9%). The accuracy of TI-201 thyroid scan in differentiating benign from malignant nodules was 66.2%. The nodules with strong TI-201 uptake in early image and low TI-201 uptake in delayed image were malignant in 29.4%. Cystic changes were found in 40% of malignant nodules with atypical TI-201 uptake. TI-201 thyroid scan showed high specificity in follicular neoplasm and adenomatous goiter in which differentiation of benignancy and malignancy is difficult with only cytologic examination. We consider that TI-201 thyroid scan is valuable in differentiating benign from malignant nodules and when combined with fine needle aspiration and ultrasound examination, it will enable more accurate differential diagnosis between benign and malignant thyroid nodules

DETERMINATION OF HYDROGEN DESORBED THROUGH THERMAL CALORIMETRY IN A HIGH STRENGTH STEEL

Directory of Open Access Journals (Sweden)

Carolina A. Asmus

2014-03-01

Full Text Available The following study aims to quantify the release activation energy (Ea of hydrogen (H from lattice sites, reversible or irreversible, where the H can be trapped. Moreover, enthalpy changes associated with the main hydrogen (H trapping sites can be analyzed by means of differential scanning calorimetry (DSC. In this technique, the peak temperature measurement is determined at two different heating rates, 3ºC/min y 5ºC/min, from ambient temperature to 500°C. In order to simulate severe conditions of hydrogen income into resulfurized high strength steel, electrolytic permeation tests were performed on test tubes suitable for fatigue tests. Sometimes during charging, H promoters were aggregated to electrolytic solution. Subsequently, the test tubes were subjected to flow cycle fatigue tests. Finally, irreversible trap which anchor more strongly H atoms are MnS inclusions. Its role on hydrogen embrittlement during fatigue tests is conclusive.

Variants and pitfalls on radioiodine scans in pediatric patients with differentiated thyroid carcinoma

Energy Technology Data Exchange (ETDEWEB)

Mostafa, Mohamed; Vali, Reza; Chan, Jeffrey; Omarkhail, Yusuaf; Shammas, Amer [University of Toronto, Nuclear Medicine Division, Department of Medical Imaging, The Hospital for Sick Children, Toronto, Ontario (Canada)

2016-10-15

Potentially false-positive findings on radioiodine scans in children with differentiated thyroid carcinoma can mimic functioning thyroid tissue and functioning thyroid carcinomatous tissue. Such false-positive findings comprise variants and pitfalls that can vary slightly in children as compared with adults. To determine the patterns and frequency of these potential false-positive findings on radioiodine scans in children with differentiated thyroid carcinoma. We reviewed a total of 223 radioiodine scans from 53 pediatric patients (mean age 13.3 years, 37 girls) with differentiated thyroid carcinoma. Focal or regional activity that likely did not represent functioning thyroid tissue or functioning thyroid carcinomatous tissue were categorized as variants or pitfalls. The final diagnosis was confirmed by reviewing the concurrent and follow-up clinical data, correlative ultrasonography, CT scanning, serum thyroglobulin and antithyroglobulin antibody levels. We calculated the frequency of these variants and pitfalls from diagnostic and post-therapy radioiodine scans. The most common variant on the radioiodine scans was the thymic activity (24/223, 10.8%) followed by the cardiac activity (8/223, 3.6%). Salivary contamination and star artifact, caused by prominent thyroid remnant, were the most important observed pitfalls. Variants and pitfalls that mimic functioning thyroid tissue or functioning thyroid carcinomatous tissue on radioiodine scan in children with differentiated thyroid carcinoma are not infrequent, but they decrease in frequency on successive radioiodine scans. Potential false-positive findings can be minimized with proper knowledge of the common variants and pitfalls in children and correlation with clinical, laboratory and imaging data. (orig.)

[Significance and mechanism of MSCT perfusion scan on differentiation of NSCLC].

Science.gov (United States)

Liu, Jin-Kang; Hu, Cheng-Ping; Zhou, Mo-Ling; Zhou, Hui; Xiong, Zeng; Xia, Yu; Chen, Wei

2009-06-01

To determine the significance of MSCT perfusion scan on differentiation of NSCLC and to investigate its possible mechanisms. Forty four NSCLC patients underwent CT perfusion scan by MSCT. Among them, 22 cases were selected to detected the two-dimensional tumor microvascular architecture phenotype (2D-TMAP), the relationships between CT perfusion parameters (BF, BV, PEI, TIP), and the differentiation of NSCLC were analysed by using the correlation analysis and trend test. Spearman correlation analysis was used to study the relationships between CT perfusion parameters, differentiation, and 2D-TMAP. The total BF, BV and PEI decreased with decreasing differentiation of NSCLC (P<0.05). The total PEI showed a positive correlation with the total MVD (P<0.05). There were negative correlations between the surrounding area BF, the total BF, BV, and PEI, the uncomplete lumen of the surrounding area MVD, and expression of PCNA, respectively (P<0.05). There were positive correlations between degree of differentiation and the uncomplete lumen of the surrounding area MVD (P<0.05). It was the same as degree of differentiation and expression of PCNA, VEGF, respectively. There were positive correlations between the uncomplete lumen of the surrounding area MVD and expression of VEGF, ephrinB2, EphB4, and PCNA, respectively (P<0.05). Perfusion parameters reflect the difference of density of vassels with mature functional lumen. Careful evaluation of the differences of blood flow pattern in pulmonary space-occupying lesions by MSCT perfusion scan can be used to identify the degree of NSCLC differentiation.

Optical methods and differential scanning calorimetry as a potential tool for discrimination of olive oils (extra virgin and mix with vegetable oils)

Science.gov (United States)

Nikolova, Kr.; Yovcheva, T.; Marudova, M.; Eftimov, T.; Bodurov, I.; Viraneva, A.; Vlaeva, I.

2016-03-01

Eleven samples from olive oil have been investigated using four physical methods - refractive index measurement, fluorescence spectra, color parameters and differential scanning colorimetry. In pomace olive oil (POO) and extra virgin olive oil (EVOO) the oleic acid (65.24 %-78.40 %) predominates over palmitic (10.47 %-15.07 %) and linoleic (5.26 %-13.92 %) acids. The fluorescence spectra contain three peaks related to oxidation products at about λ = (500-540) nm, chlorophyll content at about λ = (675-680) nm and non determined pigments at λ = (700-750) nm. The melting point for EVOO and POO is between -1 °C and -6 °C. In contrast, the salad olive oils melt between -24 °C and -30 °C. The refractive index for EVOO is lower than that for mixed olive oils. The proposed physical methods could be used for fast and simple detection of vegetable oils in EVOO without use of chemical substances. The experimental results are in accordance with those obtained by chemical analysis.

Scanning differential polarization microscope: Its use to image linear and circular differential scattering

International Nuclear Information System (INIS)

Mickols, W.; Maestre, M.F.

1988-01-01

A differential polarization microscope that couples the sensitivity of single-beam measurement of circular dichroism and circular differential scattering with the simultaneous measurement of linear dichroism and linear differential scattering has been developed. The microscope uses a scanning microscope stage and single-point illumination to give the very shallow depth of field found in confocal microscopy. This microscope can operate in the confocal mode as well as in the near confocal condition that can allow one to program the coherence and spatial resolution of the microscope. This microscope has been used to study the change in the structure of chromatin during the development of sperm in Drosophila

Melt behaviour, crystallinity and morphology of poly(p-dioxanone)

NARCIS (Netherlands)

Pezzin, APT; van Ekenstein, GOR; Duek, EAR

The melt behaviour of poly(p-dioxanone) (PPD) has been studied by differential scanning calorimetry (DSC). Crystallinity and morphology were evaluated by modulated differential scanning calorimetry (MDSC) and polarizing optical microscopy. The melting curves showed two melting endotherms, a higher

Development of Resistive Micromegas for Sampling Calorimetry

Science.gov (United States)

Geralis, T.; Fanourakis, G.; Kalamaris, A.; Nikas, D.; Psallidas, A.; Chefdeville, M.; Karyotakis, I.; Koletsou, I.; Titov, M.

2018-02-01

Resistive micromegas is proposed as an active element for sampling calorimetry. Future linear collider experiments or the HL-LHC experiments can profit from those developments for Particle Flow Calorimetry. Micromegas possesses remarkable properties concerning gain stability, reduced ion feedback, response linearity, adaptable sensitive element granularity, fast response and high rate capability. Recent developments on Micromegas with a protective resistive layer present excellent results, resolving the problem of discharges caused by local high charge deposition, thanks to its RC-slowed charge evacuation. Higher resistivity though, may cause loss of the response linearity at high rates. We have scanned a wide range of resistivities and performed laboratory tests with X-rays that demonstrate excellent response linearity up to rates of (a few) times 10MHz/cm2, with simultaneous mitigation of discharges. Beam test studies at SPS/CERN with hadrons have also shown a remarkable stability of the resistive Micromegas and low currents for rates up to 15MHz/cm2. We present results from the aforementioned studies confronted with MC simulation

Design of Test Wrapper Scan Chain Based on Differential Evolution

Directory of Open Access Journals (Sweden)

Aijun Zhu

2013-08-01

Full Text Available Integrated Circuit has entered the era of design of the IP-based SoC (System on Chip, which makes the IP core reuse become a key issue. SoC test wrapper design for scan chain is a NP Hard problem, we propose an algorithm based on Differential Evolution (DE to design wrapper scan chain. Through group’s mutation, crossover and selection operations, the design of test wrapper scan chain is achieved. Experimental verification is carried out according to the international standard benchmark ITC’02. The results show that the algorithm can obtain shorter longest wrapper scan chains, compared with other algorithms.

Recent developments in silicon calorimetry

International Nuclear Information System (INIS)

Brau, J.E.

1990-11-01

We present a survey of some of the recent calorimeter applications of silicon detectors. The numerous attractive features of silicon detectors are summarized, with an emphasis on those aspects important to calorimetry. Several of the uses of this technology are summarized and referenced. We consider applications for electromagnetic calorimetry, hadronic calorimetry, and proposals for the SSC

IMPLICATIONS OF GLOBAL AND LOCAL MOBILITY IN AMORPHOUS EXCIPIENTS AS DETERMINED BY DSC AND TM DSC

OpenAIRE

Ion Dranca; Tudor Lupascu

2009-01-01

The paper explores the use of differential scanning calorimetry (DSC) and temperature modulated differential scanning calorimetry (TM DSC) to study α- and β- processes in amorphous sucrose and trehalose. The real part of the complex heat capacity is evaluated at the frequencies, f, from 5 to 20mHz. β-relaxations were studied by annealing glassy samples at different temperatures and subsequently heating at different rates in a differential scanning calorimeter.

Gravimetric analysis and differential scanning calorimetric studies on glycerin-induced skin hydration.

Science.gov (United States)

Lee, Ae-Ri Cho; Moon, Hee Kyung

2007-11-01

A thermal gravimetric analysis (TGA) and a differential scanning calorimetry (DSC) were carried out to characterize the water property and an alteration of lipid phase transition of stratum corneum (SC) by glycerin. In addition, the relationship between steady state skin permeation rate and skin hydration in various concentrations of glycerin was investigated. Water vapor absorption-desorption was studied in the hairless mouse stratum corneum. Dry SC samples were exposed to different conc. of glycerin (0-50%) followed by exposure to dry air and the change in weight property was monitored over time by use of TGA. In DSC study, significant decrease in DeltaH of the lipid transition in 10% glycerin and water treated sample: the heat of lipid transition of normal, water, 10% glycerin treated SC were 6.058, 4.412 and 4.316 mJ/mg, respectively. In 10% glycerin treated SCs, the Tc of water shifts around 129 degrees C, corresponding to the weakly bound secondary water. In 40% glycerin treated SC, the Tc of water shifts to 144 degrees C corresponding to strongly bound primary water. There was a good correlation between the hydration property of the skin and the steady state skin flux with the correlation coefficient (r2=0.94). As the hydration increased, the steady state flux increased. As glycerin concentration increased, hydration property decreased. High diffusivity induced by the hydration effect of glycerin and water could be the major contributing factor for the enhanced skin permeation of nicotinic acid (NA).

Modulated differential photoacoustic cell to study the gelatinization in a starch-water suspension

Science.gov (United States)

Villada, J. A.; Herrera, W.; Espinosa-Arbeláez, D. G.; Mosquera, J. C.; Rodríguez-García, M. E.

2014-06-01

In this paper the design and implementation of a novel Differential Photoacoustic Cell (DPC) system is presented. The system was used to study the thermo optic transition in water-starch suspension called gelatinization. The melting temperature of Gallium was used to calibrate the temperature of the system. Both temperature values for starch gelatinization and gallium melting were agreed with those obtained using differential scanning calorimetry (DSC). The results show that this system is suitable to study other thermal processes in food or any thermal transition at low temperature.

Modulated differential photoacoustic cell to study the gelatinization in a starch-water suspension

Directory of Open Access Journals (Sweden)

J. A. Villada

2014-06-01

Full Text Available In this paper the design and implementation of a novel Differential Photoacoustic Cell (DPC system is presented. The system was used to study the thermo optic transition in water-starch suspension called gelatinization. The melting temperature of Gallium was used to calibrate the temperature of the system. Both temperature values for starch gelatinization and gallium melting were agreed with those obtained using differential scanning calorimetry (DSC. The results show that this system is suitable to study other thermal processes in food or any thermal transition at low temperature.

Gas phase enthalpies of formation of nitrobenzamides using combustion calorimetry and thermal analysis

International Nuclear Information System (INIS)

Ximello, Arturo; Flores, Henoc; Rojas, Aarón; Adriana Camarillo, E.; Patricia Amador, M.

2014-01-01

Graphical abstract: - Highlights: • Formation enthalpies of the nitrobenzamides were derived from combustion calorimetry. • Enthalpies of vaporisation and sublimation were calculated by thermogravimetry. • From gas phase enthalpies of formation the stability of the isomers is studied. • Stability of isomers is not driven by a steric hindrance between functional groups. - Abstract: The standard molar energies of combustion of 2-nitrobenzamide, 3-nitrobenzamide and 4-nitrobenzamide were determined with an isoperibolic, static-bomb, combustion calorimeter. From the combustion results, the standard molar enthalpies of combustion and formation for these compounds in the condensed phase at T = 298.15 K were derived. Subsequently, to determine the enthalpies of sublimation, the vapour pressure data as a function of the temperature for the compounds under investigation were estimated using thermogravimetry by applying Langmuir’s equation, and the enthalpies of vaporisation were derived. Standard enthalpies of fusion were measured by differential scanning calorimetry then added to those of vaporisation to obtain reliable results for the enthalpy of sublimation. From the combustion and sublimation data, the gas phase enthalpies of formation were determined to be (−138.9 ± 3.5) kJ · mol −1 , (−122.9 ± 2.9) kJ · mol −1 and (−108.5 ± 3.7) kJ · mol −1 for the ortho, meta and para isomers of nitrobenzamide, respectively. The meaning of these results with regard to the enthalpic stability of these molecular structures is discussed herein

Differential scanning fluorimetry illuminates silk feedstock stability and processability

Czech Academy of Sciences Publication Activity Database

Dicko, C.; Kasoju, Naresh; Hawkins, N.; Vollrath, F.

2016-01-01

Roč. 12, č. 1 (2016), s. 255-262 ISSN 1744-683X R&D Projects: GA MŠk(CZ) EE2.3.30.0029 Institutional support: RVO:61389013 Keywords : differential scanning fluorimetry * biomaterials * silk fibroin Subject RIV: CE - Biochemistry Impact factor: 3.889, year: 2016

Analysis of Siderite Thermal Decomposition by Differential Scanning Calorimetry

Science.gov (United States)

Bell, M. S.; Lin, I.-C.; McKay, D. S.

2000-01-01

Characterization of carbonate devolitilization has important implications for atmospheric interactions and climatic effects related to large meteorite impacts in platform sediments. On a smaller scale, meteorites contain carbonates which have witnessed shock metamorphic events and may record pressure/temperature histories of impact(s). ALH84001 meteorite contains zoned Ca-Mg-Fe-carbonates which formed on Mars. Magnetite crystals are found in the rims and cores of these carbonates and some are associated with void spaces leading to the suggestion by Brearley et al. that the crystals were produced by thermal decomposition of the carbonate at high temperature, possibly by incipient shock melting or devolitilization. Golden et al. recently synthesized spherical Mg-Fe-Ca-carbonates from solution under mild hydrothermal conditions that have similar carbonate compositional zoning to those of ALH84001. They have shown experimental evidence that the carbonate-sulfide-magnetite assemblage in ALH84001 can result from a multistep inorganic process involving heating possibly due to shock events. Experimental shock studies on calcium carbonate prove its stability to approx. 60 GPa, well in excess of the approx. 45 GPa peak pressures indicated by other shock features in ALH84001. In addition, Raman spectroscopy of carbonate globules in ALH84001 indicates no presence of CaO and MgO. Such oxide phases should be found associated with the magnetites in voids if these magnetites are high temperature shock products, the voids resulting from devolitilization of CO2 from calcium or magnesium carbonate. However, if the starting material was siderite (FeCO3), thermal breakdown of the ALH84001 carbonate at 470 C would produce iron oxide + CO2. As no documentation of shock effects in siderite exists, we have begun shock experiments to determine whether or not magnetite is produced by the decomposition of siderite within the < 45GPa pressure window and by the resultant thermal pulse to approx. 600 C experienced by ALH84001. Here, we report thermal and compositional characterization of unshocked siderite and its transition to magnetite. Additional information is contained in the original extended abstract.

IMPLICATIONS OF GLOBAL AND LOCAL MOBILITY IN AMORPHOUS EXCIPIENTS AS DETERMINED BY DSC AND TM DSC

Directory of Open Access Journals (Sweden)

Ion Dranca

2009-12-01

Full Text Available The paper explores the use of differential scanning calorimetry (DSC and temperature modulated differential scanning calorimetry (TM DSC to study α- and β- processes in amorphous sucrose and trehalose. The real part of the complex heat capacity is evaluated at the frequencies, f, from 5 to 20mHz. β-relaxations were studied by annealing glassy samples at different temperatures and subsequently heating at different rates in a differential scanning calorimeter.

Comparison of thallium-201 scan and Tc-99m sestamibi scan in the differential diagnosis of breast mass

Energy Technology Data Exchange (ETDEWEB)

Cho, Ihn Ho; Won, Kyu Jang; Lee, Hyung Woo; Lee, Soon Jung [College of Medicine, Yonsei Univ., Seoul (Korea, Republic of)

1999-02-01

We performed this study to compare Tl-201 and Tc-99m MIBI scans for the differentiation of malignant from benign breast mass. Thirty-eight female patients underwent Tl-201 breast scan and thirty-two of them also underwent Tc-99m MIBI scan of the breast. After intravenous injection of 74-111 MBq of Tl-201, early (10 minutes) and delayed (3 hours) images were obtained. Then, 555-740 MBq of Tc-99m MIBI was injected and images after 30 minutes were obtained. We compared Tl-201 and Tc-99m MIBI scans with pathologic results. Twenty-three patients were confirmed to have infiltrating duct carcinoma and fifteen patients to have benign breast mass by excisonal biopsy. The sensitivity of early and delayed Tl-201 scan and Tc-99m MIBI scan in the detection of malignant breast lesion were 100% (23/23), 82% (18/22), and 90% (18/20), respectively. The sensitivity of early Tl-201 scan was significantly higher than that of delayed Tl-201 scan, (p<0.05). The specificity of early and delayed Tl-201 scan and Tc-99m MIBI scan were 73% (11/15), 73% (11/15) and 83% (10/12), respectively (p: not significant). Three patients out of nine with fibroadenoma and one patient with atypical duct hyperplasia were false positive in both early and delayed Tl-201 scans. The size of fibroadenoma with false positive in early and delayed Tl-201 scan (4 cases) was larger than that of 11 fibroadenoma with true negative scan (p<0.01). Metastatic axillary lymph node involvement was present in fifteen patients. The sensitivity to detect metastatic nodes was 38% (5/13) for early Tl-201 images, 15% (2/13) for delayed Tl-201 images, 58% (7/12) for Tc-99m MIBI planar images and 67% (4/6) for Tc-99m MIBI SPECT. The sensitivity of Tc-99m MIBI planar or SPECT was significantly higher than that of delayed Tl-201 images (p<0.05). Early Tl-201 and Tc-99m MIBI scan are useful noninvasive methods to differentiate malignant from benign mass of breast. Tc-99m MIBI scan was sensitive in detecting axillary lymph node

Lattice defect investigation of nanostructured ECAP-Cu by means of x-ray line profile analysis, calorimetry and electrical resistometry

International Nuclear Information System (INIS)

Schafler, E.; Steiner, G.; KEXrber, M.; Zehetbauer, M.J.; Korznikova, E.

2005-01-01

Full text: Cu rods have been deformed by Equal Channel Angular Pressing (ECAP) up to shear strains γ ∼ 5 while applying various deformation paths A, B c and C. ECAP processed materials show a microstructure with grain sizes in the nanometer range and a high density of lattice defects. X-ray Bragg Profile Analyses (XPA), Differential Scanning Calorimetry (DSC) as well as Residual Electrical Resistivity (RER) measurements have been performed, in order to detect the densities of various deformation induced lattice defects and/or their arrangements. The results have been analyzed in terms of annealing of deformation induced dislocations and vacancies (vacancy agglomerates). Compared to conventional cold work procedures, deformation by ECAP achieves a strongly enhanced concentration of vacancy type defects. (author)

Structure of water in mesoporous organosilica by calorimetry and inelastic neutron scattering

Science.gov (United States)

Levy, Esthy; Kolesnikov, Alexander I.; Li, Jichen; Mastai, Yitzhak

2009-01-01

In this paper, we describe the preparation of mesoporous organosilica samples with hydrophilic or hydrophobic organic functionality inside the silica channel. We synthesized mesoporous organosilica of identical pore sizes based on two different organic surface functionality namely hydrophobic (based on octyltriethoxysilane OTES) and hydrophilic (3-aminopropyltriethoxysilane ATES) and MCM-41 was used as a reference system. The structure of water/ice in those porous silica samples have been investigated over a range temperatures by differential scanning calorimetry (DSC) and inelastic neutron scattering (INS). INS study revealed that water confined in hydrophobic mesoporous organosilica shows vibrational behavior strongly different than bulk water. It consists of two states: water with strong and weak hydrogen bonds (with ratio 1:2.65, respectively), compared to ice-Ih. The corresponding O-O distances in these water states are 2.67 and 2.87 Ǻ, which strongly differ compared to ice-Ih (2.76 Ǻ). INS spectra for water in hydrophilic mesoporous organosilica ATES show behavior similar to bulk water, but with greater degree of disorder.

Scintillator plate calorimetry

International Nuclear Information System (INIS)

Price, L.E.

1990-01-01

Calorimetry using scintillator plates or tiles alternated with sheets of (usually heavy) passive absorber has been proven over multiple generations of collider detectors. Recent detectors including UA1, CDF, and ZEUS have shown good results from such calorimeters. The advantages offered by scintillator calorimetry for the SSC environment, in particular, are speed (<10 nsec), excellent energy resolution, low noise, and ease of achieving compensation and hence linearity. On the negative side of the ledger can be placed the historical sensitivity of plastic scintillators to radiation damage, the possibility of nonuniform response because of light attenuation, and the presence of cracks for light collection via wavelength shifting plastic (traditionally in sheet form). This approach to calorimetry is being investigated for SSC use by a collaboration of Ames Laboratory/Iowa State University, Argonne National Laboratory, Bicron Corporation, Florida State University, Louisiana State University, University of Mississippi, Oak Ridge National Laboratory, Virginia Polytechnic Institute and State University, Westinghouse Electric Corporation, and University of Wisconsin

Evaluation of glass transition temperature and dynamic mechanical properties of autopolymerized hard direct denture reline resins.

Science.gov (United States)

Takase, Kazuma; Watanabe, Ikuya; Kurogi, Tadafumi; Murata, Hiroshi

2015-01-01

This study assessed methods for evaluation of glass transition temperature (Tg) of autopolymerized hard direct denture reline resins using dynamic mechanical analysis and differential scanning calorimetry in addition to the dynamic mechanical properties. The Tg values of 3 different reline resins were determined using a dynamic viscoelastometer and differential scanning calorimeter, and rheological parameters were also determined. Although all materials exhibited higher storage modulus and loss modulus values, and a lower loss tangent at 37˚C with a higher frequency, the frequency dependence was not large. Tg values obtained by dynamic mechanical analysis were higher than those by differential scanning calorimetry and higher frequency led to higher Tg, while more stable Tg values were also obtained by that method. These results suggest that dynamic mechanical analysis is more advantageous for characterization of autopolymerized hard direct denture reline resins than differential scanning calorimetry.

Silk I and Silk II studied by fast scanning calorimetry.

Science.gov (United States)

Cebe, Peggy; Partlow, Benjamin P; Kaplan, David L; Wurm, Andreas; Zhuravlev, Evgeny; Schick, Christoph

2017-06-01

Using fast scanning calorimetry (FSC), we investigated the glass transition and crystal melting of samples of B. mori silk fibroin containing Silk I and/or Silk II crystals. Due to the very short residence times at high temperatures during such measurements, thermal decomposition of silk protein can be significantly suppressed. FSC was performed at 2000K/s using the Mettler Flash DSC1 on fibroin films with masses around 130-270ng. Films were prepared with different crystalline fractions (ranging from 0.26 to 0.50) and with different crystal structures (Silk I, Silk II, or mixed) by varying the processing conditions. These included water annealing at different temperatures, exposure to 50%MeOH in water, or autoclaving. The resulting crystal structure was examined using wide angle X-ray scattering. Degree of crystallinity was evaluated from Fourier transform infrared (FTIR) spectroscopy and from analysis of the heat capacity increment at the glass transition temperature. Silk fibroin films prepared by water annealing at 25°C were the least crystalline and had Silk I structure. FTIR and FSC studies showed that films prepared by autoclaving or 50%MeOH exposure were the most crystalline and had Silk II structure. Intermediate crystalline fraction and mixed Silk I/Silk II structures were found in films prepared by water annealing at 37°C. FSC results indicate that Silk II crystals exhibit endotherms of narrower width and have higher mean melting temperature T m (II)=351±2.6°C, compared to Silk I crystals which melt at T m (I)=292±3.8°C. Films containing mixed Silk I/Silk II structure showed two clearly separated endothermic peaks. Evidence suggests that the two types of crystals melt separately and do not thermally interconvert on the extremely short time scale (0.065s between onset and end of melting) of the FSC experiment. Silkworm silk is a naturally occurring biomaterial. The fibroin component of silk forms two types of crystals. Silk properties depend upon the

Simultaneous Synchrotron WAXD and Fast Scanning (Chip) Calorimetry: On the (Isothermal) Crystallization of HDPE and PA11 at High Supercoolings and Cooling Rates up to 200 °C s(-1).

Science.gov (United States)

Baeten, Dorien; Mathot, Vincent B F; Pijpers, Thijs F J; Verkinderen, Olivier; Portale, Giuseppe; Van Puyvelde, Peter; Goderis, Bart

2015-06-01

An experimental setup, making use of a Flash DSC 1 prototype, is presented in which materials can be studied simultaneously by fast scanning calorimetry (FSC) and synchrotron wide angle X-ray diffraction (WAXD). Accumulation of multiple, identical measurements results in high quality, millisecond WAXD patterns. Patterns at every degree during the crystallization and melting of high density polyethylene at FSC typical scanning rates from 20 up to 200 °C s(-1) are discussed in terms of the temperature and scanning rate dependent material crystallinities and crystal densities. Interestingly, the combined approach reveals FSC thermal lag issues, for which can be corrected. For polyamide 11, isothermal solidification at high supercooling yields a mesomorphic phase in less than a second, whereas at very low supercooling crystals are obtained. At intermediate supercooling, mixtures of mesomorphic and crystalline material are generated at a ratio proportional to the supercooling. This ratio is constant over the isothermal solidification time. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fast-Scan DSC and its role in pharmaceutical physical form characterisation and selection.

Science.gov (United States)

Ford, James L; Mann, Timothy E

2012-04-01

Conventional rate Differential Scanning Calorimetry (DSC) has been used for many years as a tool in the analysis of pharmaceutical materials. In recent years an extension of the technique to include fast heating and cooling rates has become more prevalent. Broadly termed Fast-Scan DSC, this review examines the current applications of this technique to the characterisation and selection of pharmaceutical materials. Its increasing use encompasses the characterisation of amorphousness in crystalline materials, the characterisation of polymorphs and polymorphic transitions, the solubility of drugs in polymers, and characterisation of dosage forms. Notwithstanding the advantages of analytical speed in analytical turnover, the review emphasises the advantages of Fast-Scan DSC in its sensitivity which allows the separation of overlapping thermal events, the reduction it provides in degradation during the scanning process and its role in determining solubility in waxy and polymeric based systems. A comparison of the uses of Fast-Scan DSC to modulated DSC techniques and localised thermal analysis is also given. © 2011 Elsevier B.V. All rights reserved.

A differential scanning calorimetric study of the effects of metal ions, substrate/product, substrate analogues and chaotropic anions on the thermal denaturation of yeast enolase 1.

Science.gov (United States)

Brewer, J M; Wampler, J E

2001-03-14

The thermal denaturation of yeast enolase 1 was studied by differential scanning calorimetry (DSC) under conditions of subunit association/dissociation, enzymatic activity or substrate binding without turnover and substrate analogue binding. Subunit association stabilizes the enzyme, that is, the enzyme dissociates before denaturing. The conformational change produced by conformational metal ion binding increases thermal stability by reducing subunit dissociation. 'Substrate' or analogue binding additionally stabilizes the enzyme, irrespective of whether turnover is occurring, perhaps in part by the same mechanism. More strongly bound metal ions also stabilize the enzyme more, which we interpret as consistent with metal ion loss before denaturation, though possibly the denaturation pathway is different in the absence of metal ion. We suggest that some of the stabilization by 'substrate' and analogue binding is owing to the closure of moveable polypeptide loops about the active site, producing a more 'closed' and hence thermostable conformation.

Calorimetry

International Nuclear Information System (INIS)

McDonald, J.C.

1978-01-01

The techniques and equipment currently employed for calorimetric dosimetry have been briefly surveyed and the status of some recent measurements presented. The problems which remain to be investigated are: the thermal defect, the suitability of A-150 plastic as a material for heavy charged particle calorimetry and calorimeter designs that are appropriate for specific radiation situations, including cryogenic calorimeters

Apparent heat capacity measurements and thermodynamic functions of D(−)-fructose by standard and temperature-modulated calorimetry

International Nuclear Information System (INIS)

Magoń, A.; Pyda, M.

2013-01-01

Highlights: ► Experimental, apparent heat capacity of fructose was investigated by advanced thermal analysis. ► Equilibrium melting parameters of fructose were determined. ► Decomposition, superheating of crystalline fructose during melting process were presented. ► TGA, DSC, and TMDSC are useful tools for characterisation of fructose. - Abstract: The qualitative and quantitative thermal analyses of crystalline and amorphous D(−)-fructose were studied utilising methods of standard differential scanning calorimetry (DSC), quasi-isothermal temperature-modulated differential scanning calorimetry (quasi-isothermal TMDSC), and thermogravimetric analysis (TGA). Advanced thermal analysis of fructose was performed based on heat capacity. The apparent total and apparent reversing heat capacities, as well as phase transition parameters were examined on heating and cooling. The melting temperature, T m , of crystalline D(−)-fructose shows a heating rate dependency, which increases with raising the heating rate and leads to superheating. The equilibrium melting temperatures: T m ∘ (onset) = 370 K and T m ∘ (peak) = 372 K, and the equilibrium enthalpy of fusion Δ fus H ° = 30.30 kJ · mol −1 , of crystalline D(−)-fructose were estimated on heating for the results at zero heating rate. Anomalies in the heat capacity in the liquid state of D(−)-fructose, assigned as possible tautomerisation equilibrium, were analysed by DSC and quasi-isothermal TMDSC, both on heating and cooling. Thermal stability of crystals in the region of the melting temperature was examined by TGA and quasi-isothermal TMDSC. Melting, mutarotation, and degradation processes occur simultaneously and there are differences in values of the liquid heat capacity of D(−)-fructose with varied thermal history, measured by quasi-isothermal TMDSC. Annealing of amorphous D(−)-fructose between the glass transition temperature, T g , and the melting temperature, T m , also leads to

Differential Aging Signals in Abdominal CT Scans.

Science.gov (United States)

Orlov, Nikita V; Makrogiannis, Sokratis; Ferrucci, Luigi; Goldberg, Ilya G

2017-12-01

Changes in the composition of body tissues are major aging phenotypes, but they have been difficult to study in depth. Here we describe age-related change in abdominal tissues observable in computed tomography (CT) scans. We used pattern recognition and machine learning to detect and quantify these changes in a model-agnostic fashion. CT scans of abdominal L4 sections were obtained from Baltimore Longitudinal Study of Aging (BLSA) participants. Age-related change in the constituent tissues were determined by training machine classifiers to differentiate age groups within male and female strata ("Younger" at 50-70 years old vs "Older" at 80-99 years old). The accuracy achieved by the classifiers in differentiating the age cohorts was used as a surrogate measure of the aging signal in the different tissues. The highest accuracy for discriminating age differences was 0.76 and 0.72 for males and females, respectively. The classification accuracy was 0.79 and 0.71 for adipose tissue, 0.70 and 0.68 for soft tissue, and 0.65 and 0.64 for bone. Using image data from a large sample of well-characterized pool of participants dispersed over a wide age range, we explored age-related differences in gross morphology and texture of abdominal tissues. This technology is advantageous for tracking effects of biological aging and predicting adverse outcomes when compared to the traditional use of specific molecular biomarkers. Application of pattern recognition and machine learning as a tool for analyzing medical images may provide much needed insight into tissue changes occurring with aging and, further, connect these changes with their metabolic and functional consequences. Published by Elsevier Inc.

Thermodynamics of ion binding to phosphatidic acid bilayers. Titration calorimetry of the heat of dissociation of DMPA.

Science.gov (United States)

Blume, A; Tuchtenhagen, J

1992-05-19

The heat of dissociation of the second proton of 1,2-dimyristoylphosphatidic acid (DMPA) was studied as a function of temperature using titration calorimetry. The dissociation of the second proton of DMPA was induced by addition of NaOH. From the calorimetric titration experiment, the intrinsic pK0 for the dissociation reaction could be determined by applying the Gouy-Chapman theory. pK0 decreases with temperature from ca. 6.2 at 11 degrees C to 5.4 at 54 degrees C. From the total heat of reaction, the dissociation enthalpy, delta Hdiss, was determined by subtracting the heat of neutralization of water and the heat of dilution of NaOH. In the temperature range between 2 and 23 degrees C, delta Hdiss is endothermic with an average value of ca. 2.5 kcal.mol-1 and shows no clear-cut temperature dependence. In the temperature range between 23 and 52 degrees C, delta Hdiss calculated after subtraction of the heat of neutralization and dilution is not the true dissociation enthalpy but includes contributions from the phase transition enthalpy, delta Htrans, as the pH jump induces a transition from the gel to the liquid-crystalline phase. The delta Cp for the reaction enthalpy observed in this temperature range is positive. Above 53 degrees C, the pH jump induces again only the dissociation of the second proton, and the bilayers stay in the liquid-crystalline phase. In this temperature range, delta Hdiss seems to decrease with temperature. The thermodynamic data from titration calorimetry and differential scanning calorimetry as a function of pH can be combined to construct a complete enthalpy-temperature diagram of DMPA in its two ionization states.

Crystallization of Polymers Investigated by Temperature-Modulated DSC

OpenAIRE

Maria Cristina Righetti

2017-01-01

The aim of this review is to summarize studies conducted by temperature-modulated differential scanning calorimetry (TMDSC) on polymer crystallization. This technique can provide several advantages for the analysis of polymers with respect to conventional differential scanning calorimetry. Crystallizations conducted by TMDSC in different experimental conditions are analysed and discussed, in order to illustrate the type of information that can be deduced. Isothermal and non-isothermal crystal...

Intercomparative tests on phase change materials characterisation with differential scanning calorimeter

International Nuclear Information System (INIS)

Lazaro, Ana; Peñalosa, Conchita; Solé, Aran; Diarce, Gonzalo; Haussmann, Thomas; Fois, Magali; Zalba, Belén; Gshwander, Stefan; Cabeza, Luisa F.

2013-01-01

Highlights: ► Advances in intercomparative tests of enthalpy of phase change material (PCM). ► Enthalpy of PCM determined by DSC is influenced by certain factors. ► The influence factors were identified. ► A methodology to avoid these influences for heating measurements is proposed. ► Forthcoming steps are focused on calibration and cooling measurements. - Abstract: For the correct design of thermal storage systems using phase change materials (PCMs) in any application, as well as for their simulation, it is essential to characterise the materials from thermophysical and rheological standpoints (phase change enthalpy, thermal conductivity in solid and liquid phases, viscosity and density in function of temperature). Taking advantage of the different research groups facilities available in two international networks: within the IEA (International Energy Agency), the ECES Implementing Agreement (Energy Conservation through Energy Storage IA) and SHC Programme (Solar Heating and Cooling) Task 42/Annex 24 “Compact Thermal Energy Storage – Material Development for System Integration”, and the COST Action TU0802 “Next generation cost effective phase change materials for increased energy efficiency in renewable energy systems in buildings (NeCoE-PCM)” a set of Round Robin Tests (RRTs) was proposed. The objective was to come to comparable results for PCMs using Differential Scanning Calorimetry (DSC) to determine their melting enthalpy as well as their melting and solidification behaviour. The first RRT was without defining the procedure, the second one with a predefined procedure for the measurements, but not for calibration and the third one with a predefined procedure for calibration, for the measurements and also for the data evaluation. This paper presents the conclusions after the three RRT. The main conclusion of the paper is that enthalpy in function of temperature determined using a dynamic method for DSC can be influenced by certain reasons

Characterization of Two Different Clay Materials by Thermogravimetry (TG), Differential Scanning Calorimetry (DSC), Dilatometry (DIL) and Mass Spectrometry (MS) - 12215

Energy Technology Data Exchange (ETDEWEB)

Post, Ekkehard [NETZSCH Geraetebau GmbH, Wittelsbacherstrasse 42, 95100 Selb (Germany); Henderson, Jack B. [NETZSCH Instruments North America, LLC, 129 Middlesex Turnpike, Burlington, MA 01803 (United States)

2012-07-01

An illitic clay containing higher amounts of organic materials was investigated by dilatometry, thermogravimetry and differential scanning calorimetric. The evolved gases were studied during simultaneous TG-DSC (STA) and dilatometer measurements with simultaneous mass spectrometry in inert gas and oxidizing atmosphere. The dilatometer results were compared with the STA-MS results which confirmed and explained the reactions found during heating of the clay, like dehydration, dehydroxylation, shrinkage, sintering, quartz phase transition, combustion or pyrolysis of organics and the solid state reactions forming meta-kaolinite and mullite. The high amount of organic material effects in inert gas atmosphere most probably a reduction of the oxides which leads to a higher mass loss than in oxidizing atmosphere. Due to this reduction an additional CO{sub 2} emission at around 1000 deg. C was detected which did not occur in oxidizing atmosphere. Furthermore TG-MS results of a clay containing alkali nitrates show that during heating, in addition to water and CO{sub 2}, NO and NO{sub 2} are also evolved, leading to additional mass loss steps. These types of clays showed water loss starting around 100 deg. C or even earlier. This relative small mass loss affects only less shrinkage during the expansion of the sample. The dehydroxylation and the high crystalline quartz content result in considerable shrinkage and expansion of the clay. During the usual solid state reaction where the clay structure collapses, the remaining material finally shrinks down to a so-called clinker. With the help of MS the TG steps can be better interpreted as the evolved gases are identified. With the help of the MS it is possible to distinguish between CO{sub 2} and water (carbonate decomposition, oxidation of organics or dehydration/dehydroxylation). The MS also clearly shows that mass number 44 is found during the TG step of the illitic clay at about 900 deg. C in inert gas, which was interpreted

Calorimetry for the SSC

Energy Technology Data Exchange (ETDEWEB)

Gordon, H.A.; Grannis, P.D.

1984-01-01

The activities related to calorimetry at Snowmass took place in three main areas. These were: (1) The performance criteria for SSC calorimetry, including the requirements on hermeticity, shower containment, segmentation and time resolution. The use of calorimetric means of particle identification was studied. (2) The study of triggering methods using calorimeter energy, angle and timing information. (3) A review of a wide variety of calorimeter materials for absorber and sampling, as well as several means of obtaining the readout of the energy deposits. 48 references, 10 figures, 1 table.

Calorimetry for the SSC

International Nuclear Information System (INIS)

Gordon, H.A.; Grannis, P.D.

1984-01-01

The activities related to calorimetry at Snowmass took place in three main areas. These were: (1) The performance criteria for SSC calorimetry, including the requirements on hermeticity, shower containment, segmentation and time resolution. The use of calorimetric means of particle identification was studied. (2) The study of triggering methods using calorimeter energy, angle and timing information. (3) A review of a wide variety of calorimeter materials for absorber and sampling, as well as several means of obtaining the readout of the energy deposits. 48 references, 10 figures, 1 table

Differential phase microscope and micro-tomography with a Foucault knife-edge scanning filter

Science.gov (United States)

Watanabe, N.; Hashizume, J.; Goto, M.; Yamaguchi, M.; Tsujimura, T.; Aoki, S.

2013-10-01

An x-ray differential phase microscope with a Foucault knife-edge scanning filter was set up at the bending magnet source BL3C, Photon Factory. A reconstructed phase profile from the differential phase image of an aluminium wire at 5.36 keV was fairly good agreement with the numerical simulation. Phase tomography of a biological specimen, such as an Artemia cyst, could be successfully demonstrated.

Application of calorimetry in evaluation of phase transformations in the selected hypoeutectic silumins

Directory of Open Access Journals (Sweden)

J. Szymszal

2009-04-01

Full Text Available The investigations of phase transformations described in this study were carried out on hypoeutectic alloys from the Al-Si during heating and cooling. The determination and analysis of characteristic temperature values from the solidification range was made by the DSC method in calorimetric investigations carried out on a high-temperature multi HTC Setaram scanning calorimeter. Applying the lever rule, the phase composition of the examined slumins was calculated and compared with the results of DSC calorimetry.

Theory of calorimetry

CERN Document Server

Zielenkiewicz, Wojciech

2004-01-01

The purpose of this book is to give a comprehensive description of the theoretical fundamentals of calorimetry. The considerations are based on the relations deduced from the laws and general equations of heat exchange theory and steering theory.

Calorimetry end-point predictions

International Nuclear Information System (INIS)

Fox, M.A.

1981-01-01

This paper describes a portion of the work presently in progress at Rocky Flats in the field of calorimetry. In particular, calorimetry end-point predictions are outlined. The problems associated with end-point predictions and the progress made in overcoming these obstacles are discussed. The two major problems, noise and an accurate description of the heat function, are dealt with to obtain the most accurate results. Data are taken from an actual calorimeter and are processed by means of three different noise reduction techniques. The processed data are then utilized by one to four algorithms, depending on the accuracy desired to determined the end-point

Solid-Liquid Equilibria for the Binary Mixtures 1,4-Xylene + Ethylbenzene and 1,4-Xylene + Toluene

DEFF Research Database (Denmark)

Huyghe, Raphaël; Rasmussen, Peter; Thomsen, Kaj

2004-01-01

Solid-liquid equilibrium (SLE) data for the binary mixtures 1,4-xylene + ethylbenzene, and 1,4-xylene + toluene have been measured using differential scanning calorimetry (DSC) in the temperature range from 133.15 K to 293.15 K.......Solid-liquid equilibrium (SLE) data for the binary mixtures 1,4-xylene + ethylbenzene, and 1,4-xylene + toluene have been measured using differential scanning calorimetry (DSC) in the temperature range from 133.15 K to 293.15 K....

Characterization of thermal reaction of aluminum/copper (II) oxide/poly(tetrafluoroethene) nanocomposite by thermogravimetric analysis, differential scanning calorimetry, mass spectrometry and X-ray diffraction

International Nuclear Information System (INIS)

Li, Xiangyu; Yang, Hongtao; Li, Yan-chun

2015-01-01

Highlights: • The thermal reaction properties of the Al/CuO/PTFE nanocomposite were investigated. • The Al/PTFE and CuO/PTFE nanocomposites were prepared and tested for comparison. • TG/DSC–MS and XRD analysis were performed. • PTFE is oxidizing Al and reducing CuO during the thermal decomposition. - Abstract: The application of fluoropolymers as reactive agent in energetic materials have attracted significant interest recently. In this study, the thermal reaction properties of the aluminum nanoparticles/copper (II) oxide nanoparticles/poly(tetrafluoroethene) (Al-NPs/CuO-NPs/PTFE) nanocomposite (mass ratio of Al-NPs/CuO-NPs/PTFE = 20/60/20) were investigated by means of thermogravimetry/differential scanning calorimetry–mass spectrometry (TG/DSC–MS) and X-ray diffraction (XRD) analyses. The Al-NPs/PTFE (mass ratio of Al-NPs/PTFE = 50/50) and CuO-NPs/PTFE (mass ratio of CuO-NPs/PTFE = 75/25) nanocomposites were also prepared and tested for comparison. It is observed that PTFE is acting as both oxidizer and reducer during the thermal decomposition process of Al-NPs/CuO-NPs/PTFE nanocomposites. Before 615 °C, PTFE is oxidized by CuO-NPs and oxidizing Al-NPs, resulting mass reduction. After 615 °C, the excessive aluminum and copper (I)/copper (II) oxide will proceed the exothermic condensed phase reaction.

The CLEO-III Trigger: Calorimetry and tracking

International Nuclear Information System (INIS)

Bergfeld, T.J.; Gollin, G.D.; Haney, M.J.

1996-01-01

The CLEO-III Trigger provides a trigger decision every 42ns, with a latency of approximately 2.5μs. This paper describes the pipelined signal processing and pattern recognition schemes used by the calorimeter, and the axial and stereo portions of the drift chamber, to provide the information necessary to make these decisions. Field programmable gate arrays are used extensively to provide cluster filtering and location sorting for calorimetry, and path finding for tracking. Analog processing is also employed in the calorimetry to provide additional leverage on the problem. Timing information is extracted from both calorimetry and tracking

Study of asphaltene precipitation by Calorimetry

DEFF Research Database (Denmark)

Verdier, Sylvain Charles Roland; Plantier, Frédéric; Bessières, David

2007-01-01

Can calorimetry bring new input to the Current understanding of asphaltene precipitation? In this work, two types of precipitation were studied by means of calorimetry: addition of n-heptane into asphaltene solutions and temperature/pressure variations on a recombined live oil. The first series...... of experiments showed that weak forces determine precipitation. Indeed, isothermal titration calorimetry could not detect any clear signal although this technique can detect low-energy transitions such as liquid-liquid equilibrium and rnicellization. The second series of tests proved that precipitation caused...... by T and P variations is exothermic for this system. Furthermore, the temperature-induced precipitation is accompanied by an increase in the apparent thermal expansivity. Therefore, it seems that these two phase transitions exhibit different calorimetric behaviours and they may not be as similar...

Chemical kinetics on thermal decompositions of cumene hydroperoxide in cumene studied by calorimetry: An overview

Energy Technology Data Exchange (ETDEWEB)

Duh, Yih-Shing, E-mail: yihshingduh@yahoo.com.tw [Department of Occupation Safety and Health, Jen-Teh Junior College of Medicine, Nursing and Management, Miaoli, 35664, Taiwan, ROC (China); Department of Safety, Health and Environmental Engineering, National United University, No. 1 Lien-Da, Miaoli, 36052, Taiwan, ROC (China)

2016-08-10

Highlights: • Chemical kinetics on thermal decompositions of CHP are conducted and summarized. • Kinetics agrees well between data from DSC and adiabatic calorimetry. • Ea is determined to be about 120 kJ mol{sup −1} by various calorimetry. • LogA (A in s{sup −1}) is determined to be about 11.8 by various calorimetry. - Abstract: Study on chemical kinetics related to the thermal decomposition of cumene hydoperoxide (CHP) in cumene is summarized in this work. It is of great importance to gather and compare the differences between these kinetic parameters for further substantial applications in the chemical industry and process safety. CHP has been verified to possess an autocatalytic behavior by using microcalorimetry (such as TAM and C-80) operated at isothermal mode in the temperature range from 70 °C to 120 °C. However, it exhibits a reaction of n-th order detected by non-isothermal DSC scanning and adiabatic calorimeter. By the isothermal aging tests, activation energy and frequency factor in logA(s{sup −1}) were averaged to be (117.3 ± 5.9) kJ mol{sup −1}and (11.4 ± 0.3), respectively. Kinetic parameters acquired from data of interlaboratories by using heat-flow calorimetry, the averaged activation energy and frequency factor in logA(s{sup −1}) were (119.3 ± 11.3) kJ mol{sup −1}and (12.0 ± 0.2), respectively. On the analogy of results from adiabatic calorimetry, the activation energy and frequency factor in logA(s{sup −1}) were respectively averaged to be (122.4 ± 9.2) kJ mol{sup −1}and (11.8 ± 0.8). Five sets of kinetic models in relation to autocatalytic reactions are collected and discussed as well.

Calorimetry

International Nuclear Information System (INIS)

Anon.

1982-01-01

We have divided this study of calorimetry at the SLC into five topics: physics with calorimeters, readout geometries, performance of existing detectors, calorimeter technologies, and new calorimeter designs. The first topic is a review of the Z 0 physics in which calorimetry would be important. We discuss the Monte Carlo model and the general features of the events which it generates. We consider how the physics affects the design of the electromagnetic and hadron calorimeters in energy resolution, segmentation, solid angle coverage, and general performance. The two ways of reading out a calorimeter, strips and towers, are the basis of the second topic. We discuss a model which makes quantitative comparisons of these two schemes, with particular reference to electromagnetic calorimeters. These programs should be useful in other studies of calorimeter performance as well. There are six detectors at PEP and SPEAR with calorimetric elements. The third topic is a review of their performance at present energies and an evaluation of the problems which would arise at SLC energies. The new technologies which may be mature enough for use in an SLC detector are considered as the fourth topic. Some are now being built into anti pp detectors, others are in test beam stages, and others are still bright ideas. We review ten techniques and include references for further pursuit. The last section combines the physics goals, readout schemes, and present and future techniques into sensible calorimeter designs which sharpen the issues. Six models resulted. We discuss their strengths, weaknesses, feasibility, and rough costs

Direct calorimetry of free-moving eels with manipulated thyroid status

Science.gov (United States)

van Ginneken, Vincent; Ballieux, Bart; Antonissen, Erik; van der Linden, Rob; Gluvers, Ab; van den Thillart, Guido

2007-02-01

In birds and mammals, the thyroid gland secretes the iodothyronine hormones of which tetraiodothyronine (T4) is less active than triiodothyronine (T3). The action of T3 and T4 is calorigenic and is involved in the control of metabolic rate. Across all vertebrates, thyroid hormones also play a major role in differentiation, development and growth. Although the fish thyroidal system has been researched extensively, its role in thermogenesis is unclear. In this study, we measured overall heat production to an accuracy of 0.1 mW by direct calorimetry in a free-moving European eel ( Anguilla anguilla L.) with different thyroid status. Hyperthyroidism was induced by injection of T3 and T4, and hypothyroidism was induced with phenylthiourea. The results show for the first time at the organismal level, using direct calorimetry, that neither overall heat production nor overall oxygen consumption in eels is affected by hyperthyroidism. Therefore, we conclude that the thermogenic metabolism-stimulating effect of thyroid hormones (TH) is not present with a cold-blooded fish species like the European eel. This supports the concept that TH does not stimulate thermogenesis in poikilothermic species.

DMSO-induced dehydration of DPPC membranes studied by x-ray diffraction, small angle neutron scattering and calorimetry

International Nuclear Information System (INIS)

Kiselev, M.A.; Kiselev, A.M.; Lesieur, P.; Grabielle-Madelmond, C.; Ollivon, M.

1998-01-01

The properties of dimethyl sulfoxide (DMSO), a cryoprotector well known for its biological and therapeutic applications, were investigated on lipid membranes by x-ray diffraction, differential scanning calorimetry (DSC) and small angle neutron scattering (SANS). The DSC study of water freezing and melting of ice was performed in the ternary system which consists of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC)/DMSO/water system. The influence of DMSO on the DPPC membrane structure was established in the excess of solvent in the region of DMSO mole fraction from 0.0 to 1.0. The methods applied demonstrated the differences in the membrane structure in three sub-regions of DMSO mole fraction (X DMSO ) from 0.0 to 0.3 for the first, from 0.3 to 0.9 for the second, and from 0.9 to 1.0 for the third sub-region. The results for 0.0 ≤ X DMSO ≤ 0.3 can be explained in the framework of DMSO-induced dehydration of intermembrane space

Thermodynamics of mercaptopurine dehydration.

Science.gov (United States)

Niazi, S

1978-04-01

The hydrate form of mercaptopurine was shown to undergo peritectic decomposition of its water molecule, localized dissolution, and dehydration around 125 degrees. The anhydrate form was prepared by a thermal method, whose effectiveness was confirmed by X-ray diffraction, NMR spectroscopy, and differential scanning calorimetry. The activation energy for mercaptopurine dehydration calculated by various methods ranged from 45.74 to 63.04 kcal/mole. The dehydration enthalpy was calculated to be 8.27 kcal/mole by differential scanning calorimetry. The solution enthalpy for the hydrate was calculated to be 4.85 kcal/mole from its saturation solubility and differential scanning calorimetry. Anhydrate solubility in water was calculated based on initial dissolution rate data since the anhydrate converts to hydrate in aqueous media. The high degree of stability against interconversion of the hydrate and anhydrate forms and the higher solubility of the anhydrate suggest that use of the anhydrate might improve mercaptopurine bioavailability.

Liquid ionization calorimetry: review and preview

International Nuclear Information System (INIS)

Fabjan, C.W.

1995-01-01

The experimental requirements at existing and planned accelerators, and new facilities for underground or space-borne experimentation have stimulated a wide-ranging R and D programme in liquid ionization calorimetry. Precision sampling calorimetry is approaching ''crystal'' energy resolution whilst their rate capabilities will be able to cope with the highest LHC luminosities. (Quasi)-homogeneous noble-liquid calorimeters are under construction or in the planning stage to address some of the most fundamental physics questions. (orig.)

Calorimetry at industrial electron accelerators

DEFF Research Database (Denmark)

Miller, Arne; Kovacs, A.

1985-01-01

Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials such as grap......Calorimetry is a convenient way to measure doses at industrial electron accelerators, where high absorbed doses (1-100 kGy) are delivered at dose rates of 102-105 Gy s-1 or even higher. Water calorimeters have been used for this purpose for several years, but recently other materials...

Phase behavior and micellar properties of carboxylic acid end group modified pluronic surfactants

NARCIS (Netherlands)

Custers, J.P.A.; Broeke, van den L.J.P.; Keurentjes, J.T.F.

2007-01-01

The micellar behavior of three different carboxylic acid end standing (CAE) surfactants has been characterized using conductometry, differential scanning calorimetry, isothermal titration calorimetry, and dynamic light scattering. The CAE surfactants are modified high molecular weight Pluronic

Re-evaluation of differential phase contrast (DPC) in a scanning laser microscope using a split detector as an alternative to differential interference contrast (DIC) optics.

Science.gov (United States)

Amos, W B; Reichelt, S; Cattermole, D M; Laufer, J

2003-05-01

In this paper, differential phase imaging (DPC) with transmitted light is implemented by adding a suitable detection system to a standard commercially available scanning confocal microscope. DPC, a long-established method in scanning optical microscopy, depends on detecting the intensity difference between opposite halves or quadrants of a split photodiode detector placed in an aperture plane. Here, DPC is compared with scanned differential interference contrast (DIC) using a variety of biological specimens and objective lenses of high numerical aperture. While DPC and DIC images are generally similar, DPC seems to have a greater depth of field. DPC has several advantages over DIC. These include low cost (no polarizing or strain-free optics are required), absence of a double scanning spot, electronically variable direction of shading and the ability to image specimens in plastic dishes where birefringence prevents the use of DIC. DPC is also here found to need 20 times less laser power at the specimen than DIC.

Calorimetry energy measurement in particle physics

CERN Document Server

Wigmans, Richard

2017-01-01

Particle physics is the science that pursues the age-old quest for the innermost structure of matter and the fundamental interactions between its constituents. Modern experiments in this field rely increasingly on calorimetry, a detection technique in which the particles of interest are absorbed in the detector. Calorimeters are very intricate instruments. Their performance characteristics depend on subtle, sometimes counter-intuitive design details. This book, written by one of the world's foremost experts, is the first comprehensive text on this topic. It provides a fundamental and systematic introduction to calorimetry. It describes the state of the art in terms of both the fundamental understanding of calorimetric particle detection, and the actual detectors that have been or are being built and operated in experiments. The last chapter discusses landmark scientific discoveries in which calorimetry has played an important role. This book summarizes and puts into perspective the work described in some 900...

Forward calorimetry in the upgraded UA1 experiment

International Nuclear Information System (INIS)

Alvarez-Taviel, F.J.; Diez-Hedo, F.; Doncel, P.; Marquina, M.A.; Rodrigo, T.; Bacci, C.; Petrolo, E.; Tusi, A.; Ferrando, A.; Givernaud, A.; Rubbia, C.; Vuillemin, V.

1989-01-01

The major improvement in the upgraded UA1 calorimetry at the Santi ppS is the general use of ionization chambers filled with tetramethylpentane (TMP) as a detection medium interspersed with uranium plates as absorber. To achieve overall uniformity of detection down to very small angles, an identical solution is proposed for the forward calorimetry. Forward calorimetry is essential for good total and missing energy measurement at high luminosity in view of the increasing rate of multiple collisions. Both designs for forward and very forward calorimeters are presented along with expected resolutions. (orig.)

An autosampling differential scanning calorimeter instrument for studying molecular interactions.

Science.gov (United States)

Plotnikov, Valerian; Rochalski, Andrew; Brandts, Michael; Brandts, John F; Williston, Samuel; Frasca, Verna; Lin, Lung-Nan

2002-11-01

A new ultrasensitive differential scanning calorimeter (DSC) instrument is described, which utilizes autosampling for continuous operation. High scanning rates to 250 deg/h with rapid cooling and equilibration between scans facilitates higher sample throughput up to 50 samples during each 24 h of unattended operation. The instrument is suited for those pharmaceutical applications where higher throughput is important, such as screening drug candidates for binding constant or screening solution conditions for stability of liquid protein formulations. Results are presented on the binding of five different anionic inhibitors to ribonuclease A, which included cytidine 2'-monophosphate (2'CMP), 3'CMP, uridine 3'-monophosphate, pyrophosphate, and phosphate. Binding constants K(B) (or dissociation constants K(d)) are obtained from the shift in the transition temperature T(M) for ribonuclease thermal unfolding in the presence of ligand relative to the transition temperature in the absence of ligand. Measured binding constants ranged from 155 M(-1) (K(d) = 6.45 mM) for the weak-binding phosphate anion to 13100 M(-1) (K(d) = 76.3 microM) for the strongest binding ligand, 2'CMP. The DSC method for measuring binding constants can also be extended to ultratight interactions involving either ligand-protein or protein-protein binding.

Diagnostic I-131 scintigraphy in patients with differentiated thyroid cancer. No additional value of higher scan dose

International Nuclear Information System (INIS)

Phan, T.T.H.; Tol, K.M. van; Links, T.P.; Piers, D.A.; Vries, E.G.E. de; Dullaart, R.P.F.; Jager, P.L.

2004-01-01

After initial treatment with total thyroidectomy and radio iodine ablation, most follow-up protocols for patients with differentiated thyroid carcinoma contain cyclic diagnostic I-131 imaging and serum thyroglobulin (Tg) measurements. The applied diagnostic I-131 doses vary between 37 and 370 MBq. The aim of this study was to determine the yield of a diagnostic scan with 370 MBq I-131 in patients with a negative diagnostic scan with 74 MBq I-131. Retrospective evaluation of 158 patients who received a high-dose diagnostic scan with 370 MBq I-131 because of a negative low-dose diagnostic scan with 74 MBq I-131. Special attention was paid to the patients with positive high-dose diagnostic scanning and undetectable serum Tg levels after thyroid hormone withdrawal. In 127 (80%) of patients the 370 MBq I-131 scan was negative, just like the preceding low-dose scan. In 31 (20%) of patients abnormal uptake was present on the 370 MBq diagnostic scan. In 19 of these 31 patients serum Tg was undetectable. In 15/19 the high-dose diagnostic scan proved either false positive or demonstrated clinically irrelevant minor ablation rests. In only four patients (2.5%) did the high-dose diagnostic scans reveal possibly relevant uptake caused by residual differentiated thyroid cancer. In 98% of patients a 370 MBq dose of I-131 for diagnostic whole-body scintigraphy (WBS) had no additional value. The combination of a low-dose diagnostic I-131 scan using only 74 MBq combined with a serum Tg level measurement proved sufficient for correct clinical decision making regarding whether the patient requires additional I-131 therapy. (authors)

Calorimetry and thermal methods in catalysis

CERN Document Server

Auroux, Aline

2013-01-01

The book is about calorimetry and thermal analysis methods, alone or linked to other techniques, as applied to the characterization of catalysts, supports and adsorbents, and to the study of catalytic reactions in various domains: air and wastewater treatment, clean and renewable energies, refining of hydrocarbons, green chemistry, hydrogen production and storage. The book is intended to fill the gap between the basic thermodynamic and kinetics concepts acquired by students during their academic formation, and the use of experimental techniques such as thermal analysis and calorimetry to answ

Melting and thermal history of poly(hydroxybutyrate-co-hydroxyvalerate) using step-scan DSC

International Nuclear Information System (INIS)

Gunaratne, L.M.W.K.; Shanks, R.A.

2005-01-01

Melting behaviour and crystal morphology of poly(3-hydroxybutyrate) (PHB) and its copolymer of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) with various hydroxyvalerate (HV) contents [5 wt.% (PHB5HV), 8 wt.% (PHB8HV) and 12 wt.% (PHB12HV)] have been investigated by conventional DSC, step-scan differential scanning calorimetry (SDSC) and hot-stage polarised optical microscopy (HSPOM). Crystallisation behaviour of PHB and its copolymers were investigated by SDSC. Thermal properties were investigated after different crystallisation treatments, fast, medium and slow cooling. Multiple melting peak behaviour was observed for all polymers. SDSC data revealed that PHB and its copolymers undergo melting-recrystallisation-remelting during heating, as evidenced by exothermic peaks in the IsoK baseline (non-reversing signal). An increase in degree of crystallinity due to significant melt-recrystallisation was observed for slow-cooled copolymers. PHB5HV showed different crystal morphologies for various crystallisation conditions. SDSC proved a convenient and precise method for measurement of the apparent thermodynamic specific heat (reversing signal) HSPOM results showed that the crystallisation rates and sizes of spherulites were significantly reduced as crystallisation rate increased

Calorimetry at the SSC

International Nuclear Information System (INIS)

Wigmans, R.

1987-09-01

The state of the art, and our present understanding of the basic limitations in hadron calorimetry, are briefly described. The various options for SSC calorimeters are discussed, and the R and D needed for the ones that look most promising is outlined. 13 refs.; 8 figs

DMSO-induced dehydration of DPPC membranes studied by x-ray diffraction, small angle neutron scattering and calorimetry

Energy Technology Data Exchange (ETDEWEB)

Kiselev, M A; Kiselev, A M [Frank Laboratory of Neutron Physics, Joint Institute for Nuclear Research, Dubna (Russian Federation); Lesieur, P [LURE, Universite Paris-Sud, Bat. 209-D, F91405 Orsay cedex, (France); Grabielle-Madelmond, C; Ollivon, M [Physico-Chimie des systemes polyphases, URA 1218 du CNRS, Faculte de Pharmacie, tour B, F-92296, Chatenay Malabry (France)

1998-12-01

The properties of dimethyl sulfoxide (DMSO), a cryoprotector well known for its biological and therapeutic applications, were investigated on lipid membranes by x-ray diffraction, differential scanning calorimetry (DSC) and small angle neutron scattering (SANS). The DSC study of water freezing and melting of ice was performed in the ternary system which consists of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC)/DMSO/water system. The influence of DMSO on the DPPC membrane structure was established in the excess of solvent in the region of DMSO mole fraction from 0.0 to 1.0. The methods applied demonstrated the differences in the membrane structure in three sub-regions of DMSO mole fraction (X{sub DMSO}) from 0.0 to 0.3 for the first, from 0.3 to 0.9 for the second, and from 0.9 to 1.0 for the third sub-region. The results for 0.0 {<=} X{sub DMSO} {<=} 0.3 can be explained in the framework of DMSO-induced dehydration of intermembrane space 11 refs., 7 figs. Submitted to the Conference `ISSRNS`98`, 15-20 Jun 1998, Ustron-Jaszowiec, Poland

Investigating Freezing Point Depression and Cirrus Cloud Nucleation Mechanisms Using a Differential Scanning Calorimeter

Science.gov (United States)

Bodzewski, Kentaro Y.; Caylor, Ryan L.; Comstock, Ashley M.; Hadley, Austin T.; Imholt, Felisha M.; Kirwan, Kory D.; Oyama, Kira S.; Wise, Matthew E.

2016-01-01

A differential scanning calorimeter was used to study homogeneous nucleation of ice from micron-sized aqueous ammonium sulfate aerosol particles. It is important to understand the conditions at which these particles nucleate ice because of their connection to cirrus cloud formation. Additionally, the concept of freezing point depression, a topic…

Determination of Differential Enthalpy and Isotherm by Adsorption Calorimetry

Directory of Open Access Journals (Sweden)

V. Garcia-Cuello

2008-01-01

Full Text Available An adsorption microcalorimeter for the simultaneous determination of the differential heat of adsorption and the adsorption isotherm for gas-solid systems are designed, built, and tested. For this purpose, a Calvet heat-conducting microcalorimeter is developed and is connected to a gas volumetric unit built in stainless steel to record adsorption isotherms. The microcalorimeter is electrically calibrated to establish its sensitivity and reproducibility, obtaining K=154.34±0.23 WV−1. The adsorption microcalorimeter is used to obtain adsorption isotherms and the corresponding differential heats for the adsorption of CO2 on a reference solid, such as a NaZSM-5 type zeolite. Results for the behavior of this system are compared with those obtained with commercial equipment and with other studies in the literature.

Liquid Argon Calorimetry with LHC-Performance Specifications

CERN Multimedia

2002-01-01

% RD-3 Liquid Argon Calorimetry with LHC-Performance Specifications \\\\ \\\\Good electromagnetic and hadronic calorimetry will play a central role in an LHC detector. Among the techniques used so far, or under development, the liquid argon sampling calorimetry offers high radiation resistence, good energy resolution (electromagnetic and hadronic), excellent calibration stability and response uniformity. Its rate capabilities, however, do not yet match the requirements for LHC. \\\\ \\\\The aim of this proposal is to improve the technique in such a way that high granularity, good hermiticity and adequate rate capabilities are obtained, without compromising the above mentioned properties. To reach this goal, we propose to use a novel structure, the $^{\\prime\\prime}$accordion$^{\\prime\\prime}$, coupled to fast preamplifiers working at liquid argon temperature. Converter and readout electrodes are no longer planar and perpendicular to particles, as usual, but instead they are wiggled around a plane containing particles. ...

Fluoride substitution in LiBH₄; destabilization and decomposition

DEFF Research Database (Denmark)

Richter, Bo; Ravnsbaek, Dorthe B.; Sharma, Manish

2017-01-01

Fluoride substitution in LiBH4 is studied by investigation of LiBH4-LiBF4 mixtures (9:1 and 3:1). Decomposition was followed by in situ synchrotron radiation X-ray diffraction (in situ SR-PXD), thermogravimetric analysis and differential scanning calorimetry with gas analysis (TGA/DSC-MS) and in ......Fluoride substitution in LiBH4 is studied by investigation of LiBH4-LiBF4 mixtures (9:1 and 3:1). Decomposition was followed by in situ synchrotron radiation X-ray diffraction (in situ SR-PXD), thermogravimetric analysis and differential scanning calorimetry with gas analysis (TGA...

Physiochemical properties of the complex of myricetin and ...

African Journals Online (AJOL)

visible spectrometry (UV), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and x-ray diffractometry (XRD). Results: The content of myricetin in the complex prepared in ...

Physical characterisation of endodontic instruments in NiTi alloy

International Nuclear Information System (INIS)

Torrisi, L.

2000-01-01

NiTi based endodontic instruments are investigated in functionality and wear. The instrument surfaces have been studied applying Auger electron spectroscopy, mechanical analysis, differential-scanning calorimetry, wear tests, and scanning electron microscopy. (orig.)

Sericeous thyroglobulin and whole body thyroid scan in patients with differentiated thyroid cancer

International Nuclear Information System (INIS)

Mendoza, G.; Cano, R.; Morales, R.; Huanca, M.; Postigo, J.; Farfan, J.

1994-01-01

Thyroid cancer is the most frequent malignant tumor among endocrine diseases. it has an incidence of 1,87 cases per hundred thousand habitants. Thyroglobulin is an iodo glycoprotein useful in the follow-up of patients with differentiated thyroid carcinoma. Total body scan is a well established method to localize distant functioning metastases. We report the concordance of this two methods in 22 patients attending to the Nuclear Medicine Center and proceeding from the Head and Neck Department of INEN, which had undergone total thyroidectomy, received a I-131 ablative dose, performed a total body scan and determined the thyroglobulin concentration fourteen were female patients and the same number were accounted as high risk patients. We conclude for the studied population, that an excellent correlation between thyroglobulin and scans was noted and that 6,5 ng/ml will be used as a cut-off point for the thyroglobulin determination. (authors). 40 refs., 5 tabs

Differentiating intraparenchymal hemorrhage from contrast extravasation on post-procedural noncontrast CT scan in acute ischemic stroke patients undergoing endovascular treatment

Energy Technology Data Exchange (ETDEWEB)

Payabvash, Seyedmehdi [Zeenat Qureshi Stroke Institute, Minneapolis, MN (United States); University of Minnesota, Department of Radiology, Minneapolis, MN (United States); Qureshi, Mushtaq H.; Khan, Shayaan M.; Khan, Mahnoor; Majidi, Shahram; Pawar, Swaroop; Qureshi, Adnan I. [Zeenat Qureshi Stroke Institute, Minneapolis, MN (United States)

2014-09-15

This study aimed to identify the imaging characteristics that can help differentiate intraparenchymal hemorrhage from benign contrast extravasation on post-procedural noncontrast CT scan in acute ischemic stroke patients after endovascular treatment. We reviewed the clinical and imaging records of all acute ischemic stroke patients who underwent endovascular treatment in two hospitals over a 3.5-year period. The immediate post-procedural CT scan was evaluated for the presence of hyperdense lesion(s). The average attenuation of the lesion(s) was measured. Intraparenchymal hemorrhage was defined as a persistent hyperdensity visualized on follow-up CT scan, 24 h or greater after the procedure. Of the 135 patients studied, 74 (55 %) patients had hyperdense lesion(s) on immediate post-procedural CT scan. Follow-up scans confirmed the diagnosis of intraparenchymal hemorrhage in 20 of these 74 patients. A receiver operating characteristic analysis showed that the average attenuation of the most hyperdense lesion can differentiate intraparenchymal hemorrhage from contrast extravasation with an area under the curve of 0.78 (p = 0.001). An average attenuation of <50 Hounsfield units (HU) in the most visually hyperattenuating hyperdense lesion had 100 % specificity and 56 % sensitivity for identification of contrast extravasations. Petechial hyperdensity was seen in 46/54 (85 %) patients with contrast extravasation versus 9/20 (45 %) patients with intraparenchymal hemorrhage on the immediate post-procedural CT scan (p < 0.001). An average attenuation <50 HU of the most hyperattenuating hyperdense parenchymal lesion on immediate post-procedural CT scan was very specific for differentiating contrast extravasation from intraparenchymal hemorrhage in acute ischemic stroke patients after endovascular treatment. (orig.)

Differentiating intraparenchymal hemorrhage from contrast extravasation on post-procedural noncontrast CT scan in acute ischemic stroke patients undergoing endovascular treatment

International Nuclear Information System (INIS)

Payabvash, Seyedmehdi; Qureshi, Mushtaq H.; Khan, Shayaan M.; Khan, Mahnoor; Majidi, Shahram; Pawar, Swaroop; Qureshi, Adnan I.

2014-01-01

This study aimed to identify the imaging characteristics that can help differentiate intraparenchymal hemorrhage from benign contrast extravasation on post-procedural noncontrast CT scan in acute ischemic stroke patients after endovascular treatment. We reviewed the clinical and imaging records of all acute ischemic stroke patients who underwent endovascular treatment in two hospitals over a 3.5-year period. The immediate post-procedural CT scan was evaluated for the presence of hyperdense lesion(s). The average attenuation of the lesion(s) was measured. Intraparenchymal hemorrhage was defined as a persistent hyperdensity visualized on follow-up CT scan, 24 h or greater after the procedure. Of the 135 patients studied, 74 (55 %) patients had hyperdense lesion(s) on immediate post-procedural CT scan. Follow-up scans confirmed the diagnosis of intraparenchymal hemorrhage in 20 of these 74 patients. A receiver operating characteristic analysis showed that the average attenuation of the most hyperdense lesion can differentiate intraparenchymal hemorrhage from contrast extravasation with an area under the curve of 0.78 (p = 0.001). An average attenuation of <50 Hounsfield units (HU) in the most visually hyperattenuating hyperdense lesion had 100 % specificity and 56 % sensitivity for identification of contrast extravasations. Petechial hyperdensity was seen in 46/54 (85 %) patients with contrast extravasation versus 9/20 (45 %) patients with intraparenchymal hemorrhage on the immediate post-procedural CT scan (p < 0.001). An average attenuation <50 HU of the most hyperattenuating hyperdense parenchymal lesion on immediate post-procedural CT scan was very specific for differentiating contrast extravasation from intraparenchymal hemorrhage in acute ischemic stroke patients after endovascular treatment. (orig.)

Indirect measurement of the magnetocaloric effect using a novel differential scanning calorimeter with magnetic field

DEFF Research Database (Denmark)

Jeppesen, Stinus; Linderoth, Søren; Pryds, Nini

2008-01-01

A simple and high-sensitivity differential scanning calorimeter (DSC) unit operating under magnetic field has been built for indirect determination of the magnetocaloric effect. The principle of the measuring unit in the calorimeter is based on Peltier elements as heat flow sensors. The high...

Estudo termoanalítico de comprimidos revestidos contendo captopril através de termogravimetria (TG e calorimetria exploratória diferencial (DSC Thermal analysis study of captopril coated tablets by thermogravimetry (TG and differential scanning calorimetry (DSC

Directory of Open Access Journals (Sweden)

Giovana Carolina Bazzo

2005-09-01

Full Text Available No presente trabalho foram desenvolvidos comprimidos de captopril revestidos com hidroxipropilmetilcelulose (HPMC, Opadry®, polivinilpirrolidona (PVP, Eudragit® E e goma laca. Foi realizado estudo termoanalítico do fármaco e das formulações através de termogravimetria (TG e calorimetria exploratória diferencial (DSC. Através da análise das curvas DSC verificou-se que não houve a ocorrência de interação entre o fármaco e os excipientes lactose, celulose microcristalina, croscarmelose sódica, Aerosil® e talco, utilizados na formulação do comprimido. Através desta técnica detectou-se a possibilidade de interação entre captopril e estearato de magnésio. De acordo com os resultados obtidos através de DSC não foram observadas alterações na cristalinidade do fármaco decorrentes dos processos de compressão e revestimento. A termogravimetria foi utilizada para o estudo da cinética de degradação do captopril e dos comprimidos. Os parâmetros cinéticos foram determinados através do método de Ozawa. Os resultados demonstraram que não houve alteração da estabilidade térmica do captopril na forma de comprimido. A formulação revestida com HPMC foi a que apresentou maior estabilidade térmica, quando comparada às demais formulações de revestimento.In the present study, captopril coated tablets with hydroxypropylmethylcellulose (HPMC, Opadry®, polyvinylpirrolidone (PVP, Eudragit® and shellac were produced. Differential scanning calorimetry (DSC and thermogravimetry (TG were used to evaluate the thermal properties of the drug and the formulations. On the basis of DSC results, captopril was found to be compatible with lactose, microcrystalline cellulose, sodium croscarmellose, Aerosil® and talc. Some possibility of interaction between drug-excipient was observed with magnesium stearate. However, additional techniques to confirm the results obtained are needed. There was no influence of mechanical treatment (tableting

Impregnation of mesoporous silica for catalyst preparation studied with differential scanning calorimetry

NARCIS (Netherlands)

Eggenhuisen, T.M.; van Steenbergen, M.J.; Talsma, H.; de Jongh, P.E.; de Jong, K.P.

2009-01-01

Aqueous impregnation of mesoporous silica as a first step in catalyst preparation was studied to investigate the distribution of the metal-precursor solution over the support. The degree of pore-filling after impregnation was determined using the freezing point depression of confined liquids. A

Enzyme-catalyzed and binding reaction kinetics determined by titration calorimetry.

Science.gov (United States)

Hansen, Lee D; Transtrum, Mark K; Quinn, Colette; Demarse, Neil

2016-05-01

Isothermal calorimetry allows monitoring of reaction rates via direct measurement of the rate of heat produced by the reaction. Calorimetry is one of very few techniques that can be used to measure rates without taking a derivative of the primary data. Because heat is a universal indicator of chemical reactions, calorimetry can be used to measure kinetics in opaque solutions, suspensions, and multiple phase systems and does not require chemical labeling. The only significant limitation of calorimetry for kinetic measurements is that the time constant of the reaction must be greater than the time constant of the calorimeter which can range from a few seconds to a few minutes. Calorimetry has the unique ability to provide both kinetic and thermodynamic data. This article describes the calorimetric methodology for determining reaction kinetics and reviews examples from recent literature that demonstrate applications of titration calorimetry to determine kinetics of enzyme-catalyzed and ligand binding reactions. A complete model for the temperature dependence of enzyme activity is presented. A previous method commonly used for blank corrections in determinations of equilibrium constants and enthalpy changes for binding reactions is shown to be subject to significant systematic error. Methods for determination of the kinetics of enzyme-catalyzed reactions and for simultaneous determination of thermodynamics and kinetics of ligand binding reactions are reviewed. Copyright © 2015 Elsevier B.V. All rights reserved.

Low cost, microcontroller based heating device for multi-wavelength differential scanning fluorimetry.

Science.gov (United States)

Hoeser, Jo; Gnandt, Emmanuel; Friedrich, Thorsten

2018-01-23

Differential scanning fluorimetry is a popular method to estimate the stability of a protein in distinct buffer conditions by determining its 'melting point'. The method requires a temperature controlled fluorescence spectrometer or a RT-PCR machine. Here, we introduce a low-budget version of a microcontroller based heating device implemented into a 96-well plate reader that is connected to a standard fluorescence spectrometer. We demonstrate its potential to determine the 'melting point' of soluble and membranous proteins at various buffer conditions.

WA80 BGO calorimetry electronics

International Nuclear Information System (INIS)

Wintenberg, A.L.; Britton, C.L. Jr.; Ericson, M.N.; Maples, R.A.; Young, G.R.; Awes, T.C.

1991-01-01

This paper describes instrumentation designed for BGO scintillator-based calorimetry of particles covering a very wide range of energies (from less than 50 MeV to 50 GeV). The instrumentation was designed to have a measurement accuracy of 0.1% over as much of the energy range as possible so the energy resolution of BGO would be the limiting factor. Two 1.5-cm 2 photodiodes were used per 2.5 cm x 2.5 cm x 25 cm BGO crystal. Both a charge-sensitive preamplifier and a pulse processor were developed specifically for the needs of the WA80 experiment. The preamplifier was designed for high detector capacitance (100 to 700 pF), low integral and differential non-linearity and low power consumption (200 mW). The pulse processor is a time-invariant shaping amplifier with integral peak-detect-and-hold and automatic gain selection circuits. The amplifier use quasi-triangular shaping with 4 μs peaking time, and the hold circuit is gated with a fast first level trigger. The system has more than 20 bits of effective resolution when used with an external 12-bit ADC. Results from beam tests at CERN are presented. 6 refs., 5 figs., 1 tab

Detectors for Linear Colliders: Calorimetry at a Future Electron-Positron Collider (3/4)

CERN Multimedia

CERN. Geneva

2010-01-01

Calorimetry will play a central role in determining the physics reach at a future e+e- collider. The requirements for calorimetry place the emphasis on achieving an excellent jet energy resolution. The currently favoured option for calorimetry at a future e+e- collider is the concept of high granularity particle flow calorimetry. Here granularity and a high pattern recognition capability is more important than the single particle calorimetric response. In this lecture I will describe the recent progress in understanding the reach of high granularity particle flow calorimetry and the related R&D efforts which concentrate on test beam demonstrations of the technological options for highly granular calorimeters. I will also discuss alternatives to particle flow, for example the technique of dual readout calorimetry.

Thermoanalytical Investigation of Terazosin Hydrochloride

Directory of Open Access Journals (Sweden)

Mona Mohamed Abdel-Moety

2013-02-01

Full Text Available Purpose: Thermal analysis (TGA, DTG and DTA and differential scanning calorimetry (DSC have been used to study the thermal behavior of terazosin hydrochloride (TER. Methods: Thermogravimetric analysis (TGA/DTG, differential thermal analysis (DTA and differential scanning calorimetry (DSC were used to determine the thermal behavior and purity of the used drug. Thermodynamic parameters such as activation energy (E*, enthalpy (H*, entropy (S* and Gibbs free energy change of the decomposition (G* were calculated using different kinetic models. Results: The purity of the used drug was determined by differential scanning calorimetry (99.97% and specialized official method (99.85% indicating to satisfactory values of the degree of purity. Thermal analysis technique gave satisfactory results to obtain quality control parameters such as melting point (273 ºC, water content (7.49% and ash content (zero in comparison to what were obtained using official method: (272 ºC, (8.0% and (0.02% for melting point, water content and ash content, respectively. Conclusion: Thermal analysis justifies its application in quality control of pharmaceutical compounds due to its simplicity, sensitivity and low operational costs. DSC data indicated that the degree of purity of terazosin hydrochloride is similar to that found by official method.

A systematic study on the use of ultrasound energy for the synthesis of nickel-metal organic framework compounds

NARCIS (Netherlands)

Sargazi, G.; Afzali, D.; Daldosso, N.; Kazemian, H.; Chauhan, N.P.S.; Sadeghian, Z.; Tajerian, T.; Ghafarinazari, A.; Mozafari, M.

2015-01-01

A nickel metal-organic framework (Ni-MOF) was successfully synthesized using ultrasound irradiation. Further to this, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR), Thermo-Gravimetric Analysis (TGA), Differential Scanning Calorimetry

Calorimetry at the SSC

International Nuclear Information System (INIS)

Wigmans, R.

1988-01-01

The state of the art, and the present understanding of the basic limitations in hadron calorimetry, are briefly described. The various options for SSC calorimeters are discussed, and the R ampersand D needed for the ones that look most promising is outlined. The most promising candidates are (1) lead/scintillating fibers and (2) lead (or uranium)/TMS (or other warm liquids)

Measurement of the thermophysical properties of industrial liquid metallic alloys by non-contact calorimetry under reduced gravity

International Nuclear Information System (INIS)

Wunderlich, R.K.; Fecht, H.-J.

2001-01-01

Full Text: The numerical modeling of casting and solidification is becoming of increased importance in industrial process design. While the numerical algorithms have made large progress towards real process design and optimization, there is a pronounced lack of precise thermophysical input data. This lack is caused by the high chemical reactivity of many metallic alloys in the liquid phase making conventional measurement techniques such as differential thermal analysis difficult if at all possible to apply. In this contribution we report about a project planning to use containerless electromagnetic processing under reduced gravity conditions for thermophysical property measurement of industrially relevant alloys. Alloys of interest are, among others, Ti-alloys, Ni-base superalloys, and steels. In preparation of this project, a survey among leading European industries was conducted revealing properties such as melting range, fraction solid/liquid, specific heat capacity, enthalpy, as well as density, viscosity and surface tension as properties most in need. Non-contact calorimetry of electromagnetically levitated specimens was developed for an investigation of the thermophysical properties of Zr-alloys in the liquid phase. These methods have been applied successfully under reduced gravity conditions on board spacelab to the measurement of the specific heat capacity by modulation calorimetry, the enthalpy of fusion, the total hemispherical emissivity and for an effective thermal conductivity. Specific examples from these experiments demonstrating the applicability of these methods for quantitative calorimetry as well as application at higher Biot numbers will be discussed. New developments include modulation calorimetry in the two phase region for the measurement of the fraction solid. (author)

Physicochemical Characterization of Inclusion Complex of Catechin ...

African Journals Online (AJOL)

Its physicochemical properties were investigated by ultravioletvisible spectrometry (UV), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). Results: The characteristic UV absorption peaks for catechin, the physical ...

Calorimetry and thermodynamics of living systems

International Nuclear Information System (INIS)

Lamprecht, Ingolf

2003-01-01

Calorimetry of living systems and classical thermodynamics developed in parallel, from Lavoisier's early ice calorimeter experiments on guinea pigs, followed by Dubrunfaut's macrocalorimetric research of fermentation processes and Atwater-Rosa's whole-body calorimetry on humans and domestic animals, to the introduction of the famous Tian-Calvet instrument that found entrance into so many different fields of biology. In this work, six examples of living-system calorimetry and thermodynamics are presented. These are: (i) glycolytic oscillations far off the thermodynamic equilibrium; (ii) growth and energy balances in fermenting and respiring yeast cultures; (iii) direct and indirect calorimetric monitoring of electrically stimulated reptile metabolism; (iv) biologic and climatic factors influencing the temperature constancy and distribution in the mound of a wood ant colony as an example of a complex ecological system; (v) energetic considerations on the clustering of European honeybees in winter as a means to save energy and stored food as well as for their Japanese counterparts in defending against hornet predators; and (vi) energetic and evolutionary aspects of the mass specific entropy production rate, the so-called bound dissipation or psiu-function. The examples presented here are just a very personal selection of living systems from a broad spectrum at all levels of complexity. Common for all of them is that they were investigated calorimetrically on the background of classical and irreversible thermodynamics

Continuing Studies on Lead/Scintillating Fibres Calorimetry (LFC)

CERN Multimedia

2002-01-01

Starting from the results obtained in the framework of the LAA Project~2B, we propose a continuation of the R&D on lead/scintillating fibres calorimetry (``spaghetti calorimetry''), including further tests on the old calorimeter prototypes and the construction and testing of new prototypes. The main results we pursue concern the performances of a projective calorimeter built with new, cheaper, techniques and the radiation hardness of the scintillating fibres, the optimization of a preshower detector system is also studied.

Crystallinity changes in wheat starch during the bread-making process: Starch crystallinity in the bread crust

NARCIS (Netherlands)

Primo-Martín, C.; Nieuwenhuijzen, N.H. van; Hamer, R.J.; Vliet, T. van

2007-01-01

The crystallinity of starch in crispy bread crust was quantified using several different techniques. Confocal scanning laser microscopy (CSLM) demonstrated the presence of granular starch in the crust and remnants of granules when moving towards the crumb. Differential scanning calorimetry (DSC)

Crystallinity changes in wheat starch during the bread-making process: starch crystallinity in the bread crust

NARCIS (Netherlands)

Primo-Martin, C.; Nieuwenhuijzen, van N.H.; Hamer, R.J.; Vliet, van T.

2007-01-01

The crystallinity of starch in crispy bread crust was quantified using several different techniques. Confocal scanning laser microscopy (CSLM) demonstrated the presence of granular starch in the crust and remnants of granules when moving towards the crumb. Differential scanning calorimetry (DSC)

Scintillating-fibre calorimetry

International Nuclear Information System (INIS)

Livan, M.; Vercesi, V.; Wigmans, R.

1995-01-01

In the past decade, calorimetry based on scintillating plastic fibres as active elements was developed from a conceptual idea to a mature detector technology, which is nowadays widely applied in particle physics experiments. This development and the performance characteristics of representative calorimeters, both for the detection of electromagnetic and hadronic showers, are reviewed. We also discuss new information on shower development processes in dense matter and its application to calorimetric principles that has emerged from some very thorough studies that were performed in the framework of this development. (orig.)

Application of prediction of equilibrium to servo-controlled calorimetry measurements

International Nuclear Information System (INIS)

Mayer, R.L. II

1987-01-01

Research was performed to develop an endpoint prediction algorithm for use with calorimeters operating in the digital servo-controlled mode. The purpose of this work was to reduce calorimetry measurement times while maintaining the high degree of precision and low bias expected from calorimetry measurements. Data from routine operation of two calorimeters were used to test predictive models at each stage of development against time savings, precision, and robustness criteria. The results of the study indicated that calorimetry measurement times can be significantly reduced using this technique. The time savings is, however, dependent on parameters in the digital servo-control algorithm and on packaging characteristics of measured items

Triacylglycerol and melting profiles of milk fat from several species

NARCIS (Netherlands)

Smiddy, M.A.; Huppertz, T.; Ruth, van S.M.

2012-01-01

Gas chromatography and differential scanning calorimetry (DSC) were used to differentiate the fats of cow, goat, sheep, water buffalo, donkey, horse and camel milk (n = 20 for each species). Principal component analysis of triacylglycerol (TAG) composition allowed classification into groups

Material characterization of a polyester resin system for the pultrusion process

DEFF Research Database (Denmark)

Baran, Ismet; Akkerman, Remko; Hattel, Jesper Henri

2014-01-01

In the present work, the chemo-rheology of an industrial ‘‘orthophthalic’’ polyester system specifically prepared for a pultrusion process is characterized. The curing behaviour is first characterized using the differential scanning calorimetry (DSC). Isothermal and dynamic scans are performed...

Formulation of Sustained-Release Matrix Tablets Using Cross ...

African Journals Online (AJOL)

MK and the formulations were also characterized by scanning electron microscopy (SEM), Fourier transform infra-red spectroscopy (FTIR) and differential scanning calorimetry (DSC). Results: Tablets with MK showed higher mean dissolution time (MDT) and lower dissolution efficiency than those prepared with karaya gum.

Bulletin of Materials Science | Indian Academy of Sciences

Indian Academy of Sciences (India)

Therefore, to study the development of β -phase in films, stretching is achieved by spinning and crystallization temperature is adjusted by means of baking. PVDF films are characterized using Fourier transform infrared spectroscopy, X-ray diffraction, differential scanning calorimetry, and scanning electronmicroscopy.

Application of prediction of equilibrium to servo-controlled calorimetry measurements

International Nuclear Information System (INIS)

Mayer, R.L. II.

1987-01-01

Research was performed to develop an endpoint prediction algorithm for use with calorimeters operating in the digital servo-controlled mode. The purpose of this work was to reduce calorimetry measurement times while maintaining the high degree of precision and low bias expected from calorimetry measurements. Data from routine operation of two calorimeters were used to test predictive models at each stage of development against time savings, precision, and robustness criteria. The results of the study indicated that calorimetry measurement times can be significantly reduced using this technique. The time savings is, however, dependent on parameters in the digital servo-control algorithm and on packaging characteristics of measured items. 7 refs., 4 figs., 1 tab

The use of calorimetry for plutonium assay

International Nuclear Information System (INIS)

Mason, J.A.

1982-12-01

Calorimetry is a technique for measuring the thermal power of heat-producing substances. The technique may be applied to the measurement of plutonium-bearing materials which evolve heat as a result of alpha and beta decay. A calorimetric measurement of the thermal power of a plutonium sample, combined with a knowledge or measurement of the plutonium isotopic mass ratios of the sample provides a convenient and accurate, non-destructive measure of the total plutonium mass of the sample. The present report provides a description, and an assessment of the calorimetry technique applied to the assay of plutonium-bearing materials. Types and characteristics of plutonium calorimeters are considered, as well as calibration and operating procedures. The instrumentation used with plutonium calorimeters is described and the use of computer control for calorimeter automation is discussed. A critical review and assessment of plutonium calorimetry literature since 1970 is presented. Both fuel element and plutonium-bearing material calorimeters are considered. The different types of plutonium calorimeters are evaluated and their relative merits are discussed. A combined calorimeter and gamma-ray measurement assay system is considered. The design principles of plutonium assay calorimeters are considered. An automatic, computer-based calorimeter control system is proposed in conjunction with a general plutonium assay calorimeter design. (author)

New crystals for dual-readout calorimetry

Czech Academy of Sciences Publication Activity Database

Akchurin, N.; Bedeschi, F.; Cardini, A.; Carosi, R.; Ciapetti, G.; Ferrari, R.; Franchino, S.; Fraternali, M.; Gaudio, G.; Hauptman, J.; Incagli, M.; Korzhik, M.; Lacava, F.; La Rotonda, L.; Livan, M.; Meoni, E.; Nikl, Martin; Pinci, D.; Policicchio, A.; Popescu, S.; Scuri, F.; Sill, A.; Vandelli, W.; Vedda, A.; Venturelli, T.; Voena, C.; Volobouev, I.; Wigmans, R.

2009-01-01

Roč. 604, č. 3 (2009), s. 512-526 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10100521 Keywords : calorimetry * Cherenkov light * high-Z scintillating crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.317, year: 2009

Preparation, characterization and in vitro study of biocompatible ...

African Journals Online (AJOL)

The morphology and crystalline structure of lyophilized hydrogels were investigated by scanning electron microscopy (SEM) and wide-angle diffractometry, respectively while the surface functional groups were analyzed by FT-IR. The thermal behavior was also studied by means of differential scanning calorimetry and ...

Effect of Sucrose Esters on the Physicochemical Properties of Wheat ...

African Journals Online (AJOL)

In addition, the structure and thermodynamic properties of the modified starch were analyzed by Fourier transform infrared spectroscopy (FITR), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). Results: The properties of wheat starch changed greatly by adding different sucrose esters to their ...

Formulation and Evaluation of Spray-Dried Esomeprazole ...

African Journals Online (AJOL)

HP

(FTIR), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Results: The microspheres were discrete, spherical, and showed good drug entrapment efficiency. (60.5 - 92.3 %). FTIR and DSC results indicate that the drug was compatible with the polymers used. Amongst all the formulations, ...

Formulation and Evaluation of Spray-Dried Esomeprazole ...

African Journals Online (AJOL)

evaluated for their micromeritic properties and in vitro release. as well as by Fourier transform infrared (FTIR), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). Results: The microspheres were discrete, spherical, and showed good drug entrapment efficiency (60.5 - 92.3 %). FTIR and DSC ...

Phase Identification of Cu-In Alloys with 45 and 41.25 at.% In Compositions

DEFF Research Database (Denmark)

Baqué, Laura; Torrado, D.; Aurelio, G.

2014-01-01

In this work, the thermal stability of Cu-In alloys with 45.0 and 41.2 at.% In nominal compositions was investigated by differential scanning calorimetry (DSC), scanning electron microscopy, wavelength dispersive spectroscopy, and in-situ synchrotron x-ray powder diffraction (S-PXRD) over...

Characterization and thermal stability of uranium peroxides by thermogravimetry and differential scanning calorimetry

International Nuclear Information System (INIS)

Souza Junior, P.T. de; Abrao, A.

1982-01-01

The characterization and thermal behaviour of uranium peroxide samples prepared by precipitation with hydrogen peroxide from uranyl nitrate solution is described. The latter was obtained by dissolution of ammonium diuranate and ammonium uranyl tricarbonate. TG and DTG curves were recorded in the temperature range from room temperature to 700 0 C. DSC curves were recorded from room temperature to 600 0 C. The heating rate was 5 0 C/min. Based upon the DTG curves of a great number of samples, the uranium peroxides were classified in five groups. The collected information was used to recognise the temperature at which the peroxide decomposes and to know its sequential conversion to UO 3 and U 3 O 8 , the evolution of molecules of water of crystallization and absorption, and the elimination of occluded nitrate ions. The results allowed to conclude that no NH + 4 nor H 2 O 2 molecules were occluded by uranium peroxide. The stoichiometric composition of representative samples for the five groups is indicated. (Author) [pt

Applications of Modulated Temperature Differential Scanning Calorimetry to Polymer Blends and Related Systems

Science.gov (United States)

Hourston, Douglas J.; Song, Mo

It has been shown in this chapter that the MTDSC technique is a very useful tool in the study of several aspects of polymer blends and related materials including structured latexes and interpenetrating polymer networks. It is important to note that the dC p/dT versus temperature signal may be used not only qualitatively as a sensitive detector of transitions impossible to spot by other thermal techniques such as conventional DSC and DMTA, but it may also be used to significant advantage in a quantitative way. It has been shown that it is sensitive to the diffuse interface between phases. Thus, from dC p/dT versus temperature signals, the weight fraction of the diffuse interface can be quantified. There are many situations where this will prove to be very valuable.

Physicochemical Characterization of Inclusion Complex of Catechin ...

African Journals Online (AJOL)

with catechin, and characterize the physicochemical properties of the inclusion complex of catechin and ... microscopy (SEM), X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). ... complexes with bioactive compounds.

Application of calorimetry and thermodynamics to critical problems in materials science

International Nuclear Information System (INIS)

Atake, Tooru

2009-01-01

Calorimetry and thermodynamic studies have long been playing a very important role in the research fields of fundamental science and technology. Some topics and examples of thermodynamics studies are given, and the details are explained on the basis of the present author's experience, focusing attention to application of adiabatic calorimetry and thermodynamics to solve critical problems in materials science: (1) condensed gas calorimetry and third law entropy, (2) phase transition and polymorphism in simple molecular crystals, (3) incommensurate phase transitions, (4) particle size effects on the phase transitions in ferroelectric/ferroelastic crystals, (5) relaxor ferroelectrics and multi-ferroics, and some other topics in materials science and technology

Formulation and in vitro Evaluation of Eudragit® Microspheres of ...

African Journals Online (AJOL)

The prepared microspheres were characterized for their micromeritic properties and drug loading, as well by fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry, x-ray powder diffractometry and scanning electron microscopy. The in vitro release studies were performed in pH 6.8, phosphate buffer ...

Formulation and evaluation of matrix microspheres for simultaneous ...

African Journals Online (AJOL)

The prepared microspheres were characterized for their micromeritic properties and drug loading, as well as by infrared spectroscopy (IR), differential scanning calorimetry (DSC), x-ray powder diffractometry (XRD) and scanning electron microscopy (SEM). The in vitro release studies were performed in pH 7.4, phosphate ...

Morphological characteristic of the conventional and melt-spun Al-10Ni-5.6Cu (in wt.%) alloy

Energy Technology Data Exchange (ETDEWEB)

Karakoese, Ercan [Erciyes University, Institute of Science and Technology, Department of Physics, 38039 Kayseri (Turkey); Keskin, Mustafa, E-mail: keskin@erciyes.edu.tr [Erciyes University, Faculty of Arts and Sciences, Department of Physics, 38039 Kayseri (Turkey)

2009-12-15

The Al-10Ni-5.6Cu alloy was prepared by conventional casting and further processed melt-spinning technique. The resulting conventional cast and melt-spun ribbons were characterized using X-ray diffraction, optical microscopy, scanning electron microscopy together with energy dispersive spectroscopy, differential scanning calorimetry and microhardness techniques. The X-ray diffraction analysis indicated that ingot samples were {alpha}-Al, intermetallic Al{sub 3}Ni and Al{sub 2}Cu phases. The optical microscopy and scanning electron microscopy results show that the microstructures of rapidly solidified ribbons are clearly different from their ingot alloy. Al-10Ni-5.6Cu ribbons reveal a very fine cellular structure with intermetallic Al{sub 3}Ni particles. Moreover, at high solidification rates the melt-spun ribbons have a polygonal structure dispersed in a supersaturated aluminum matrix. The differential scanning calorimetry measurements revealed that exothermic reaction was between 290 deg. C and 440 deg. C which are more pronounced in the ternary Al-10Ni-5.6Cu alloy.

Morphological characteristic of the conventional and melt-spun Al-10Ni-5.6Cu (in wt.%) alloy

International Nuclear Information System (INIS)

Karakoese, Ercan; Keskin, Mustafa

2009-01-01

The Al-10Ni-5.6Cu alloy was prepared by conventional casting and further processed melt-spinning technique. The resulting conventional cast and melt-spun ribbons were characterized using X-ray diffraction, optical microscopy, scanning electron microscopy together with energy dispersive spectroscopy, differential scanning calorimetry and microhardness techniques. The X-ray diffraction analysis indicated that ingot samples were α-Al, intermetallic Al 3 Ni and Al 2 Cu phases. The optical microscopy and scanning electron microscopy results show that the microstructures of rapidly solidified ribbons are clearly different from their ingot alloy. Al-10Ni-5.6Cu ribbons reveal a very fine cellular structure with intermetallic Al 3 Ni particles. Moreover, at high solidification rates the melt-spun ribbons have a polygonal structure dispersed in a supersaturated aluminum matrix. The differential scanning calorimetry measurements revealed that exothermic reaction was between 290 deg. C and 440 deg. C which are more pronounced in the ternary Al-10Ni-5.6Cu alloy.

Characterization of Microemulsions Prepared using Isopropyl ...

African Journals Online (AJOL)

HP

subjected to further characterization by polarized light microscopy, differential scanning calorimetry. (DSC) ... preparation and phase inversion. The aim .... propanol, D = butanol, E = pentanol .... and water-soluble compounds in triglycerides. In.

Liquid argon calorimetry for the SSC

International Nuclear Information System (INIS)

Gordon, H.A.

1990-01-01

Liquid argon calorimetry is a mature technique. However, adapting it to the challenging environment of the SSC requires a large amount of R ampersand D. The advantages of the liquid argon approach are summarized and the issues being addressed by the R ampersand D program are described. 18 refs

MDCT in the Differentiation of Adrenal Masses: Comparison between Different Scan Delays for the Evaluation of Intralesional Washout

Directory of Open Access Journals (Sweden)

Giuseppe Angelelli

2013-01-01

Full Text Available Purpose. To evaluate the accuracy of the washout in the differential diagnosis between adenomas and nonadenomas and to compare the obtained results in delayed CT scans at 5, 10 and 15 minutes. Methods. Fifty patients with adrenal masses were prospectively evaluated. CT scans were performed by using a 320-row MDCT device, before and after injection of contrast material. In 25 cases, delayed scans were performed at 5′ and 10′ (group 1, while in the remaining 25, at 5′ and 15′ (group 2. Absolute and relative wash-out percentage values (APW and RPW were calculated. Results. Differential diagnosis between adenomas and nonadenomas was obtained in 48/50 (96% cases, with sensitivity, specificity, and accuracy values of 96%, 95%, and 96%, respectively. In group 1, APW and RPW values were, respectively, 69.8% and 67.2% at 5′ and 75.9% and 73.5% at 10′ for adenomas and 25.1% and 15.8% at 5′ and 33.5% and 20.5% at 10′ for nonadenomas. In group 2, APW and RPW values were 63% and 54.6% at 5′ and 73.8% and 65.5% at 15′ for adenomas and 22% and 12.5% at 5′ and 35.5% and 19.9% at 15′ for nonadenomas. Conclusions. The evaluation of the wash-out values in CT scans performed at 5′, 10′, and 15′ provides comparable diagnostic results. CT scans performed at 5′ are, therefore, to be preferred, since they reduce the examination time and patient discomfort.

Pseudo-self-organized topological phases in glassy selenides for IR photonics

Energy Technology Data Exchange (ETDEWEB)

Shpotyuk, O. [Lviv Institute of Materials of Scientific Research Company ' ' Carat' ' 202, Stryjska str., 79031 Lviv (Ukraine); Institute of Physics of Jan Dlugosz University 13/15, al. Armii Krajowej, 42201 Czestochowa (Poland); Golovchak, R. [Lviv Institute of Materials of Scientific Research Company ' ' Carat' ' 202, Stryjska str., 79031 Lviv (Ukraine)

2011-09-15

Network-forming cluster approach is applied to As-Se and Ge-Se glasses to justify their tendency to self-organization. It is shown that reversibility windows determined by temperature-modulated differential scanning calorimetry using short-term aged or as-prepared samples do not necessary coincide with self-organized phase in these materials. The obtained results testify also pseudo-self-organization phenomenon in Ge-Se glasses: over-constrained outrigger raft structural units built of two edge- and four corner-shared tetrahedra are interconnected via optimally-constrained {identical_to}Ge-Se-Se-Ge{identical_to} bridges within the range of compositions identified previously as self-organized phase by temperature modulated differential scanning calorimetry technique. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

Crystallization of Polymers Investigated by Temperature-Modulated DSC

Directory of Open Access Journals (Sweden)

Maria Cristina Righetti

2017-04-01

Full Text Available The aim of this review is to summarize studies conducted by temperature-modulated differential scanning calorimetry (TMDSC on polymer crystallization. This technique can provide several advantages for the analysis of polymers with respect to conventional differential scanning calorimetry. Crystallizations conducted by TMDSC in different experimental conditions are analysed and discussed, in order to illustrate the type of information that can be deduced. Isothermal and non-isothermal crystallizations upon heating and cooling are examined separately, together with the relevant mathematical treatments that allow the evolution of the crystalline, mobile amorphous and rigid amorphous fractions to be determined. The phenomena of ‘reversing’ and ‘reversible‘ melting are explicated through the analysis of the thermal response of various semi-crystalline polymers to temperature modulation.

What does calorimetry and thermodynamics of living cells tell us?

Science.gov (United States)

Maskow, Thomas; Paufler, Sven

2015-04-01

This article presents and compares several thermodynamic methods for the quantitative interpretation of data from calorimetric measurements. Heat generation and absorption are universal features of microbial growth and product formation as well as of cell cultures from animals, plants and insects. The heat production rate reflects metabolic changes in real time and is measurable on-line. The detection limit of commercially available calorimetric instruments can be low enough to measure the heat of 100,000 aerobically growing bacteria or of 100 myocardial cells. Heat can be monitored in reaction vessels ranging from a few nanoliters up to many cubic meters. Most important the heat flux measurement does not interfere with the biological process under investigation. The practical advantages of calorimetry include the waiver of labeling and reactants. It is further possible to assemble the thermal transducer in a protected way that reduces aging and thereby signal drifts. Calorimetry works with optically opaque solutions. All of these advantages make calorimetry an interesting method for many applications in medicine, environmental sciences, ecology, biochemistry and biotechnology, just to mention a few. However, in many cases the heat signal is merely used to monitor biological processes but only rarely to quantitatively interpret the data. Therefore, a significant proportion of the information potential of calorimetry remains unutilized. To fill this information gap and to motivate the reader using the full information potential of calorimetry, various methods for quantitative data interpretations are presented, evaluated and compared with each other. Possible errors of interpretation and limitations of quantitative data analysis are also discussed. Copyright © 2014 Elsevier Inc. All rights reserved.

Low-temperature heat capacity and thermodynamic functions of vitamin B12

International Nuclear Information System (INIS)

Knyazev, A.V.; Smirnova, N.N.; Plesovskikh, A.S.; Shushunov, A.N.; Knyazeva, S.S.

2014-01-01

Graphical abstract: - Highlights: • Temperature dependence of heat capacity of vitamin B 12 has been measured by precision adiabatic vacuum calorimetry. • The thermodynamic functions of the vitamin B 12 have been determined for the range from T → 0 to 343 K. • The character of heterodynamics of structure was detected. • The thermal stability of cyanocobalamin was studied by differential scanning calorimetry. - Abstract: In the present work temperature dependence of heat capacity of vitamin B 12 (cyanocobalamin) has been measured for the first time in the range from 6 to 343 K by precision adiabatic vacuum calorimetry. Based on the experimental data, the thermodynamic functions of the vitamin B 12 , namely, the heat capacity, enthalpy H°(T) − H°(0), entropy S°(T) − S°(0) and Gibbs function G°(T) − H°(0) have been determined for the range from T → 0 to 343 K. The value of the fractal dimension D in the function of multifractal generalization of Debye's theory of the heat capacity of solids was estimated and the character of heterodynamics of structure was detected. The thermal stability of cyanocobalamin was also studied by differential scanning calorimetry

Bulletin of Materials Science | Indian Academy of Sciences

Indian Academy of Sciences (India)

The in vitro degradation behaviour of poly(glycolic acid) (PGA) and its composite films containing poly(DL-lactic acid) (PDLLA) and poly(DL-lactic-co-glycolic acid) (PDLGA) were investigated via mass loss, scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). All the films were prepared by ...

Microstructures and mechanical properties of Mg–Zn–Zr–Dy ...

Indian Academy of Sciences (India)

Microstructures and phase compositions of as-cast and extruded ZK60–Dy ( = 0–5) alloys were analysed by optical microscope, scanning electron microscope, X-ray diffraction and differential scanning calorimetry. Meanwhile, the tensile mechanical property was tested.With increasing Dy content, Mg–Zn–Dy new phase ...

Mechanical, Dielectric, and Spectroscopic Characteristics of "Micro/Nanocellulose + Oxide" Composites

Science.gov (United States)

Nedielko, Maksym; Hamamda, Smail; Alekseev, Olexander; Chornii, Vitalii; Dashevskii, Mykola; Lazarenko, Maksym; Kovalov, Kostiantyn; Nedilko, Sergii G.; Tkachov, Sergii; Revo, Sergiy; Scherbatskyi, Vasyl

2017-02-01

The set of composite materials that consist of micro/nanocellulose and complex K2Eu(MoO4)(PO4) luminescent oxide particles was prepared. The composites were studied by means of scanning electron microscopy, XRD analysis, dilatometry, differential scanning calorimetry and thermogravimetric analysis, and dielectric and luminescence spectroscopy.

Studies on sampling and homogeneous dual readout calorimetry with meta-crystals

CERN Document Server

Mavromanolakis, G; Lecoq, P

2011-01-01

The meta-crystals concept is an approach that consists of using both undoped and properly doped heavy crystal fibers of identical material as the active medium of a calorimeter. The undoped fibers behave as Cherenkov radiators while the doped ones behave as scintillators. A dual readout calorimeter can be built with its sensitive volume composed of a mixture of both types of crystals. In addition if the calorimeter is adequately finely segmented it can also function as a particle flow calorimeter at the same time. In this way one could possibly combine the advantages of both the particle flow concept and the dual readout scheme. We discuss the approach of dual readout calorimetry with meta-crystals made of Lutetium Aluminium Garnet (LuAG). We brie fly present studies on the material development and first testbeam activities and then focus on performance expectation studies based on simulation. We discuss in more detail the results from generic systematic scannings of the design parameters of a dual readout ca...

Laser-flash calorimetry

International Nuclear Information System (INIS)

Takahashi, Y.; Nakamura, J.-I.

1982-01-01

The heat capacity of vanadium has been measured by laser-flash calorimetry in the temperature region from 80 to 1000 K. The results are compared with available low- and high-temperature heat capacities, and revised thermodynamic values of vanadium are given. No heat-capacity anomaly has been found in the pure vanadium sample over the temperature range investigated, while a small heat-capacity discontinuity, less than 1.2 J.K -1 .mol -1 , has been observed at 220 to 230 K on the same sample but electropolished before measurement. This anomaly disappeared after annealing at 1000 K in vacuo for 1 h and is attributable to the introduction of a small amount of hydrogen during electropolishing. (author)

Relative value of thallium-201 and iodine-131 scans in the detection of recurrence or distant metastasis of well differentiated thyroid carcinoma

International Nuclear Information System (INIS)

Lin Jen-Der; Weng Hsiao-Fen; Lu Wen-Tsoung; Kao Pan-Fu; Huang Miau-Ju

1998-01-01

Radioactive iodine ( 131 I) has been found to be more sensitive and more specific than thallium-201 for the detection of distant metastases and thyroid remnants in the neck in cases of well-differentiated thyroid carcinoma. 201 Tl has been deemed particularly useful in localizing metastases or recurrence in patients with a negative 131 I scan and abnormal levels of serum thyroglobulin (Tg). This study aimed to: (1) determine the value of 201 Tl imaging in localizing metastases or recurrence in patients with well-differentiated thyroid carcinoma, and (2) evaluate the false-positive and false-negative results of 131 I and 201 Tl scintigraphy. Sixty-two thyroid remnant ablated patients who underwent simultaneous postoperative 201 Tl and 131 I scans and and serum Tg determinations were evaluated. Fifty patients had papillary thyroid carcinomas and 12 had follicular thyroid carcinomas. 201 Tl imaging was performed before the 131 I studies. Of the 62 patients who underwent 201 Tl imaging studies, 24 were found to have positive results, with local recurrence or distant metastases. Patients with positive results in the 201 Tl imaging studies tended to be older, were mor often male, had higher Tg levels and had a higher recurrence rate. Of these 24 patients, ten had negative diagnostic or therapeutic 131 I scans. Concurrently, serum Tg levels were less than 5 ng/ml in five of these ten patients. Three patients were deemed false positive by 201 Tl scans; one had a parotid tumour, one a periodontal abscess and one lung metastasis. Among the 38 patients with negative 201 Tl scans, 11 had positive findings on 131 I scans. Three had distant metastases: two with lung metastases and one with bone metastases. Patients with false-positive results on 131 I scans included those with biliary tract stones, ovarian cysts, and breast secretion. Of the 27 patients with negative 201 Tl and 131 I scans, 15 had elevated serum Tg levels. Among these, local recurrence followed by lung

Bilayers of phosphatidyldiacylglycerol and phosphatidylcholesterol give 31P-NMR spectra characteristic for hexagonal and isotropic phases

NARCIS (Netherlands)

Noggle, J.H.; Marecek, J.F.; Mandal, S.B.; Venetie, R. van; Rogers, J.; Jain, M.K.; Ramirez, F.

1982-01-01

Aqueous dispersions of phosphatidyldiacylglycerol and phosphatidylcholesterol are shown to form bilayers by differential scanning calorimetry, diphenylhexatriene fluorescence polarization, and electron microscopy; however, 31P-nuclear magnetic resonance spectra of these dispersions are

Reprint of “Heat capacity and transition behavior of sucrose by standard, fast scanning and temperature-modulated calorimetry”

Energy Technology Data Exchange (ETDEWEB)

Magoń, A. [Department of Chemistry, University of Technology, 35-959 Rzeszów (Poland); Wurm, A.; Schick, C. [Department of Physics, University of Rostock, 18057 Rostock (Germany); Pangloli, Ph.; Zivanovic, S. [Department of Food Science and Technology, University of Tennessee, Knoxville, TN 37996 (United States); Skotnicki, M. [Department of Pharmaceutical Technology, Poznan University of Medical Sciences, 60-780 Poznań (Poland); Pyda, M., E-mail: mpyda@utk.edu [Department of Chemistry, University of Technology, 35-959 Rzeszów (Poland)

2015-03-10

Highlights: • Experimental, apparent heat capacity of sucrose was investigated by advanced thermal analysis. • Vibrational heat capacity of solid state was linked with a low temperature experimental heat capacity of sucrose. • Equilibrium melting parameters of sucrose were determined. • Decomposition, superheating of crystalline sucrose during melting process were presented. • TGA, DSC, TMDSC, and FSC are useful tools for characterization of sucrose. - Abstract: The heat capacity (C{sub p}) of crystalline and amorphous sucrose was determined using standard and quasi-isothermal temperature modulated differential scanning calorimetry. The results were combined with the published data determined by adiabatic calorimetry, and the C{sub p} values are now reported for the wide 5–600 K range. The experimental C{sub p} of solid sucrose at 5–300 K was used to calculate the vibrational, solid C{sub p} based on the vibrational molecular motions. The calculated solid and liquid C{sub p} together with the transition parameters for equilibrium conditions were used as references for detailed quantitative thermal analysis of crystalline and amorphous sucrose. Melting temperature (T{sub m}) of the crystalline sucrose was identified in a broad 442–465 K range with a heat of fusion of 40–46 J/mol determined at heating rates 0.5–20 K/min, respectively. The equilibrium T{sub m} and heat of fusion of crystalline sucrose were estimated at zero heating rate as T{sup o}{sub m} = 424.4 K and ΔH{sup o}{sub f} = 32 kJ/mol, respectively. The glass transition temperature (T{sub g}) of amorphous sucrose was at 331 K with a change in C{sub p} of 267 J/(mol K) as it was estimated from reversing heat capacity by quasi-isothermal TMDSC on cooling. At heating rates less than 30 K/min, thermal decomposition occurred during melting, while at extreme rate of 1000 K/s, degradation was not observed. Data obtained by fast scanning calorimetry (FSC) at 1000 K/s, showed that T{sub m} was

Thermochemical and phase diagram studies of the Bi-Ni-Sn system

Czech Academy of Sciences Publication Activity Database

Milcheva, N.; Brož, P.; Buršík, Jiří; Vassilev, G.P.

2012-01-01

Roč. 534, APR (2012), s. 41-50 ISSN 0040-6031 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0068 Institutional research plan: CEZ:AV0Z20410507 Keywords : differential scanning calorimetry * scanning electron microscopy * solders Subject RIV: BJ - Thermodynamics Impact factor: 1.989, year: 2012

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

Science.gov (United States)

Koruza, J.; Tellier, J.; Malič, B.; Bobnar, V.; Kosec, M.

2010-12-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 °C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 °C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 °C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 °C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

Phase transitions of sodium niobate powder and ceramics, prepared by solid state synthesis

International Nuclear Information System (INIS)

Koruza, J.; Tellier, J.; Malic, B.; Bobnar, V.; Kosec, M.

2010-01-01

Phase transitions of sodium niobate, prepared by the solid state synthesis method, were examined using dielectric measurements, differential scanning calorimetry, and high temperature x-ray diffraction, in order to contribute to the clarification of its structural behavior below 400 deg. C. Four phase transitions were detected in the ceramic sample using dielectric measurements and differential scanning calorimetry and the obtained temperatures were in a good agreement with previous reports for the transitions of the P polymorph. The anomaly observed by dielectric measurements in the vicinity of 150 deg. C was frequency dependent and could be related to the dynamics of the ferroelectric nanoregions. The phase transitions of the as-synthesized NaNbO 3 powder were investigated using differential scanning calorimetry and high temperature x-ray diffraction. The results show the existence of the Q polymorph at room temperature, not previously reported for the powder, which undergoes a transition to the R polymorph upon heating through a temperature region between 265 and 326.5 deg. C. This transition is mainly related to the displacement of Na into a more symmetric position and a minor change in the tilting system. The structures at room temperature, 250, 300, and 420 deg. C were refined by the Rietveld method and the evolution of the tilting system of the octahedral network and cationic displacement are reported.

Evaluation of optimized magnetic resonance perfusion imaging scanning time window after contrast agent injection for differentiating benign and malignant breast lesions.

Science.gov (United States)

Dong, Jie; Wang, Dawei; Ma, Zhenshen; Deng, Guodong; Wang, Lanhua; Zhang, Jiandong

2017-03-01

The aim of the study was evaluate the 3.0 T magnetic resonance (MR) perfusion imaging scanning time window following contrast injection for differentiating benign and malignant breast lesions and to determine the optimum scanning time window for increased scanner usage efficiency and reduced diagnostic adverse risk factors. A total of 52 women with breast abnormalities were selected for conventional MR imaging and T1 dynamic-enhanced imaging. Quantitative parameters [volume transfer constant (K trans ), rate constant (K ep ) and extravascular extracellular volume fraction (V e )] were calculated at phases 10, 20, 30, 40 and 50, which represented time windows at 5, 10, 15, 20 and 25 min, respectively, following injection of contrast agent. The association of the parameters at different phases with benign and malignant tumor diagnosis was analyzed. MR perfusion imaging was verified as an effective modality in the diagnosis of breast malignancies and the best scanning time window was identified: i) Values of K trans and K ep at all phases were statistically significant in differentiating benign and malignant tumors (P0.05); ii) values of V e in benign tumors increased with phase number, but achieved no obvious changes at different phases in malignant tumors; iii) the optimum scanning time window of breast perfusion imaging with 3.0 T MR was between phases 10 and 30 (i.e., between 5 and 15 min after contrast agent injection). The variation trend of V e values at different phases may serve as a diagnostic reference for differentiating benign and malignant breast abnormalities. The most efficient scanning time window was indicated to be 5 min after contrast injection, based on the observation that the V e value only had statistical significance in diagnosis at stage 10. However, the optimal scanning time window is from 5 to 15 min following the injection of contrast agent, since that the variation trend of V e is able to serve as a diagnostic reference.

Value of whole body 123I scan for detection of metastasis in patients with well-differentiated thyroid carcinoma

International Nuclear Information System (INIS)

Takahashi, Naoya; Odano, Ikuo; Sugita, Tadashi; Sato, Yoko; Sakai, Kunio

1995-01-01

To evaluate the utility of 123 I whole body scan for detection of metastasis in patients with well-differentiated thyroid carcinoma, post-therapy whole body 131 I images in 55 cases were compared with pre-therapy 123 I images using diagnostic dose (74 MBq). The post-therapy studies were performed 7 days after administration of therapeutic doses (3.33-7.77 GBq) of 131 I. The pre-therapy scans showed 30 lesions (71.4%) of 42 lesions which were shown by 131 I post-therapy scans. The diagnostic accuracy of 123 I whole body scans was considered to be nearly the same as the images obtained by 131 I using diagnostic dose. 123 I has short-life and an optimum gamma ray energy for scintigraphy. It makes radiation dose to patients lower than that of 131 I. Therefore, we recommend pre-therapy 131 I image using diagnostic dose is replaced by 123 I image. (author)

Thermodynamics of biphasic lanthanide extraction by tripodal diglycolamide: a solution calorimetry study

NARCIS (Netherlands)

Ansari, S.A.; Mohapatra, P.K.; Verboom, Willem; Rao, L.

2016-01-01

Isothermal titration calorimetry was employed for the direct measurement of the enthalpy of extraction (ΔHextr) of Eu(NO3)3 by using a tripodal diglycolamide (T-DGA) ligand dissolved in n-dodecane containing 5% (v/v) 2-decanol. The enthalpy of extraction obtained by titration calorimetry was in good

Effect of Body Position on Energy Expenditure of Preterm Infants as Determined by Simultaneous Direct and Indirect Calorimetry.

Science.gov (United States)

Bell, Edward F; Johnson, Karen J; Dove, Edwin L

2017-04-01

Background  Indirect calorimetry is the standard method for estimating energy expenditure in clinical research. Few studies have evaluated indirect calorimetry in infants by comparing it with simultaneous direct calorimetry. Our purpose was (1) to compare the energy expenditure of preterm infants determined by these two methods, direct calorimetry and indirect calorimetry; and (2) to examine the effect of body position, supine or prone, on energy expenditure. Study Design  We measured energy expenditure by simultaneous direct (heat loss by gradient-layer calorimeter corrected for heat storage) and indirect calorimetry (whole-body oxygen consumption and carbon dioxide production) in 15 growing preterm infants during two consecutive interfeeding intervals, once in the supine position and once in the prone position. Results  The mean energy expenditure for all measurements in both positions did not differ significantly by the method used: 2.82 (standard deviation [SD] 0.42) kcal/kg/h by direct calorimetry and 2.78 (SD 0.48) kcal/kg/h by indirect calorimetry. The energy expenditure was significantly lower, by 10%, in the prone than in the supine position, whether examined by direct calorimetry (2.67 vs. 2.97 kcal/kg/h, p  Direct calorimetry and indirect calorimetry gave similar estimates of energy expenditure. Energy expenditure was 10% lower in the prone position than in the supine position. Thieme Medical Publishers 333 Seventh Avenue, New York, NY 10001, USA.

Functional imaging in differentiating bronchial masses: an initial experience with a combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan.

Science.gov (United States)

Kumar, Arvind; Jindal, Tarun; Dutta, Roman; Kumar, Rakesh

2009-10-01

To evaluate the role of combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan in differentiating bronchial tumors observed in contrast enhanced computed tomography scan of chest. Prospective observational study. Place of study: All India Institute of Medical Sciences, New Delhi, India. 7 patients with bronchial mass detected in computed tomography scan of the chest were included in this study. All patients underwent (18)F-FDG PET-CT scan, (68)Ga DOTA-TOC PET-CT scan and fiberoptic bronchoscope guided biopsy followed by definitive surgical excision. The results of functional imaging studies were analyzed and the results are correlated with the final histopathology of the tumor. Histopathological examination of 7 bronchial masses revealed carcinoid tumors (2 typical, 1 atypical), inflammatory myofibroblastic tumor (1), mucoepidermoid carcinoma (1), hamartoma (1), and synovial cell sarcoma (1). The typical carcinoids had mild (18)F-FDG uptake and high (68)Ga DOTA-TOC uptake. Atypical carcinoid had moderate uptake of (18)F-FDG and high (68)Ga DOTA-TOC uptake. Inflammatory myofibroblastic tumor showed high uptake of (18)F-FDG and no uptake of (68)Ga DOTA-TOC. Mucoepidermoid carcinoma showed mild (18)F-FDG uptake and no (68)Ga DOTA-TOC uptake. Hamartoma showed no uptake on either scans. Synovial cell sarcoma showed moderate (18)F-FDG uptake and mild focal (68)Ga DOTA-TOC uptake. This initial experience with the combined use of (18)F-FDG and (68)Ga DOTA-TOC PET-CT scan reveals different uptake patterns in various bronchial tumors. Bronchoscopic biopsy will continue to be the gold standard; however, the interesting observations made in this study merits further evaluation of the utility of the combination of (18)F-FDG PET-CT scan and (68)Ga DOTA-TOC PET-CT scan in larger number of patients with bronchial masses.

Scintillating glasses for total absorption dual readout calorimetry

Energy Technology Data Exchange (ETDEWEB)

Bonvicini, V. [INFN, Trieste; Driutti, A. [Udine U.; Cauz, D. [Udine U.; Pauletta, G. [Udine U.; Rubinov, P. [Fermilab; Santi, L. [Udine U.; Wenzel, H. [Fermilab

2012-01-01

Scintillating glasses are a potentially cheaper alternative to crystal - based calorimetry with common problems related to light collection, detection and processing. As such, their use and development are part of more extensive R&D aimed at investigating the potential of total absorption, combined with the readout (DR) technique, for hadron calorimetry. A recent series of measurements, using cosmic and particle beams from the Fermilab test beam facility and scintillating glass with the characteristics required for application of the DR technique, serve to illustrate the problems addressed and the progress achieved by this R&D. Alternative solutions for light collection (conventional and silicon photomultipliers) and signal processing are compared, the separate contributions of scintillation and Cherenkov processes to the signal are evaluated and results are compared to simulation.

Substernal thyroid carcinoma detected by 67Ga scan in a patient with normal 131I scan

International Nuclear Information System (INIS)

Kim, e.E.; Maruyama, Y.; Deland, F.H.

1978-01-01

A patient with a superior mediastinal mass on an admission chest radiograph was initially evaluated by an 131 I thyroid scan which failed to demonstrate a substernal thyroid. However, the tomographic 67 Ga scan clearly showed an abnormal uptake in the area corresponding to the mass lesion on radiographic examination. Subsequent resection and biopsy of the substernal mass revealed a poorly differentiated follicular carcinoma with foci of anaplastic carcinoma. The differential diagnosis of the anterior mediastinal mass and the usefullness of the tomographic gallium scan are briefly discussed

Composition dependence of spontaneous crystallization of phosphosilicate glass melts during cooling

DEFF Research Database (Denmark)

Liu, S.J.; Zhu, C.F.; Zhang, Y.F.

2012-01-01

Crystallization behavior of alumino-phospho-silicate melts during cooling is studied by means of the differential scanning calorimetry, X-ray diffractometry and viscometry. The results show a pronounced impact of alkaline earth oxide, alkali oxide and fluoride on the crystal type and crystallizat......Crystallization behavior of alumino-phospho-silicate melts during cooling is studied by means of the differential scanning calorimetry, X-ray diffractometry and viscometry. The results show a pronounced impact of alkaline earth oxide, alkali oxide and fluoride on the crystal type...... and crystallization degree. It is found that adding NaF into the studied compositions slightly decreases melt fragility and improves both the glass-forming ability and melt workability. This effect is associated with the unique structural role of NaF compared to the other modifier oxides. It is also found...

Relative value of thallium-201 and iodine-131 scans in the detection of recurrence or distant metastasis of well differentiated thyroid carcinoma

Energy Technology Data Exchange (ETDEWEB)

Lin Jen-Der; Weng Hsiao-Fen; Lu Wen-Tsoung [Division of Endocrinology and Metabolism, Chang Gung Memorial Hospital (Taiwan, Province of China); Kao Pan-Fu; Huang Miau-Ju [Department of Nuclear Medicine, Chang Gung Memorial Hospital, Taiwan (Taiwan, Province of China)

1998-07-01

Radioactive iodine ({sup 131}I) has been found to be more sensitive and more specific than thallium-201 for the detection of distant metastases and thyroid remnants in the neck in cases of well-differentiated thyroid carcinoma. {sup 201}Tl has been deemed particularly useful in localizing metastases or recurrence in patients with a negative {sup 131}I scan and abnormal levels of serum thyroglobulin (Tg). This study aimed to: (1) determine the value of {sup 201}Tl imaging in localizing metastases or recurrence in patients with well-differentiated thyroid carcinoma, and (2) evaluate the false-positive and false-negative results of {sup 131}I and {sup 201}Tl scintigraphy. Sixty-two thyroid remnant ablated patients who underwent simultaneous postoperative {sup 201}Tl and {sup 131}I scans and and serum Tg determinations were evaluated. Fifty patients had papillary thyroid carcinomas and 12 had follicular thyroid carcinomas. {sup 201}Tl imaging was performed before the {sup 131}I studies. Of the 62 patients who underwent {sup 201}Tl imaging studies, 24 were found to have positive results, with local recurrence or distant metastases. Patients with positive results in the {sup 201}Tl imaging studies tended to be older, were mor often male, had higher Tg levels and had a higher recurrence rate. Of these 24 patients, ten had negative diagnostic or therapeutic {sup 131}I scans. Concurrently, serum Tg levels were less than 5 ng/ml in five of these ten patients. Three patients were deemed false positive by {sup 201}Tl scans; one had a parotid tumour, one a periodontal abscess and one lung metastasis. Among the 38 patients with negative {sup 201}Tl scans, 11 had positive findings on {sup 131}I scans. Three had distant metastases: two with lung metastases and one with bone metastases. Patients with false-positive results on {sup 131}I scans included those with biliary tract stones, ovarian cysts, and breast secretion. Of the 27 patients with negative {sup 201}Tl and {sup 131}I

Monte Carlo studies of uranium calorimetry

International Nuclear Information System (INIS)

Brau, J.; Hargis, H.J.; Gabriel, T.A.; Bishop, B.L.

1985-01-01

Detailed Monte Carlo calculations of uranium calorimetry are presented which reveal a significant difference in the responses of liquid argon and plastic scintillator in uranium calorimeters. Due to saturation effects, neutrons from the uranium are found to contribute only weakly to the liquid argon signal. Electromagnetic sampling inefficiencies are significant and contribute substantially to compensation in both systems. 17 references

Orientation of HDPE inclusions within solid-state drawn rubber-modified isotactic polypropylene: DSC insight

Czech Academy of Sciences Publication Activity Database

Sližová, M.; Raab, Miroslav

2013-01-01

Roč. 130, č. 1 (2013), s. 603-609 ISSN 0021-8995 Institutional support: RVO:61389013 Keywords : blends * differential scanning calorimetry * structure-property relations Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.640, year: 2013

Investigation and characterization of the nanoscale precipitation sequence and their kinetics in Al–1.0% Mg{sub 2}Si–0.4 wt% Si–0.5Cu (wt%) alloy

Energy Technology Data Exchange (ETDEWEB)

Ali, Atif Mossad, E-mail: atifali@kku.edu.sa [Department of Physics, Faculty of Science, Assiut University, Assiut 71516 (Egypt); Department of Physics, Faculty of Science, King Khalid University, Abha (Saudi Arabia); Gaber, Abdel-Fattah [Department of Physics, Faculty of Science, Assiut University, Assiut 71516 (Egypt); Matsuda, Kenji; Ikeno, Susumu [Department of Materials Science and Technology, Faculty of Engineering, Toyama University (Japan)

2014-10-15

Nonisothermal differential scanning calorimetry technique has been applied on Al–0.63 mass% Mg–0.77 mass% Si–0.5 mass% Cu alloy. Seven reaction peaks have been observed from differential scanning calorimetry (DSC). High resolution transmission electron microscopic (HRTEM) investigation has also been carried out for specimens heated with the same heating rate to the peak temperatures of the corresponding processes in the differential scanning calorimetry scans in order to characterize the developed precipitates at these temperatures. As per our results obtained from DSC and HRTEM investigations, the precipitation sequence can be written as: α{sub sss} → Si–Mg–vacancy clusters → GP zones → β″-phase and random precipitates → type C and/or Q′-phase → predominant Q′-phase + a few β(Mg{sub 2}Si)-phase and Si precipitates. In addition to that, the activation energies associated with the precipitation of β″ and Q′ were found close to the diffusion energies of Si and Mg in Al matrix. This result suggests that the diffusion of the solute atoms to form the precipitates is the appropriate mechanism of controlling both types of precipitates. - Highlights: • The behavior of the DSC scans is characterized by seven reaction processes. • HRTEM observations showed that the formed GP zones are lath shaped precipitates. • The crystal structure of β″-precipitates is monoclinic. • Excess Si stabilizes both random and β″ precipitates to higher temperatures. • The crystal analysis of C and/or Q′ precipitates exhibits a hexagonal structure.

Thermal Properties of Alkyl-Triethylammonium bis{(Trifluoromethyl)Sulfonyl}Imide Ionic Liquids

Czech Academy of Sciences Publication Activity Database

Machanová, Karolina; Wagner, Zdeněk; Andresová, Adéla; Rotrekl, Jan; Boisset, A.; Jacquemin, J.; Bendová, Magdalena

2015-01-01

Roč. 44, 3-4 (2015), s. 790-810 ISSN 0095-9782 Institutional support: RVO:67985858 Keywords : ionic liquids * differential scanning calorimetry * mathematical gnostics Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.256, year: 2015

Design and Characterization of Liquidlike POSS-Based Hybrid Nanomaterials Synthesized via Ionic Bonding and Their Interactions with CO 2

KAUST Repository

Petit, Camille; Lin, Kun-Yi Andrew; Park, Ah-Hyung Alissa

2013-01-01

relevant to CO2 capture, in particular thermal stability, swelling, viscosity, as well as their interactions with CO 2, were investigated using thermogravimetric analyses, differential scanning calorimetry, and NMR and ATR FT-IR spectroscopies. The results

Heat capacity measurements on ThO2 by temperature modulated differential scanning calorimetry (TMDSC)

International Nuclear Information System (INIS)

Venkatakrishnan, R.; Nagarajan, K.; Vasudeva Rao, P.R.

2001-01-01

Heat capacity measurements were carried out on ThO 2 in the temperature range 330-820 K by using temperature modulated DSC. An underlying heating rate of 5 K. min -1 , a temperature modulation with an amplitude of 0.398K and a period of 150s were used for these measurements. The heat capacity values are within ± 2-4% of the literature data. (author)

Low-temperature heat capacity and thermodynamic functions of vitamin B{sub 12}

Energy Technology Data Exchange (ETDEWEB)

Knyazev, A.V., E-mail: knyazevav@gmail.com; Smirnova, N.N.; Plesovskikh, A.S.; Shushunov, A.N.; Knyazeva, S.S.

2014-04-01

Graphical abstract: - Highlights: • Temperature dependence of heat capacity of vitamin B{sub 12} has been measured by precision adiabatic vacuum calorimetry. • The thermodynamic functions of the vitamin B{sub 12} have been determined for the range from T → 0 to 343 K. • The character of heterodynamics of structure was detected. • The thermal stability of cyanocobalamin was studied by differential scanning calorimetry. - Abstract: In the present work temperature dependence of heat capacity of vitamin B{sub 12} (cyanocobalamin) has been measured for the first time in the range from 6 to 343 K by precision adiabatic vacuum calorimetry. Based on the experimental data, the thermodynamic functions of the vitamin B{sub 12}, namely, the heat capacity, enthalpy H°(T) − H°(0), entropy S°(T) − S°(0) and Gibbs function G°(T) − H°(0) have been determined for the range from T → 0 to 343 K. The value of the fractal dimension D in the function of multifractal generalization of Debye's theory of the heat capacity of solids was estimated and the character of heterodynamics of structure was detected. The thermal stability of cyanocobalamin was also studied by differential scanning calorimetry.

LIQUID COAL CHARACTERISTIC ANALYSIS WITH FOURIER TRANSFORM INFRA RED (FTIR AND DIFFERENTIAL SCANNING CALORIMETER (DSC

Directory of Open Access Journals (Sweden)

ATUS BUKU

2017-02-01

Full Text Available The aim of this study is to identify the value of compounds contained in liquid coal by using Fourier Transform Infra-Red (FTIR and Differential Scanning Calorimeter (DSC. FTIR was used to analyse the components contained in liquid coal, while the DSC is done to observe the heat reaction to the environment. Based on the Fourier Transform Infra-Red (FTIR test results it is shown that the compound contained in the liquid Coal consisting of alkanes, alkenes and alkyne. These compounds are similar compounds. The alkanes, alkenes and alkynes compounds undergo complete combustion reaction with oxygen and would produce CO2 and water vapour [H2O (g]. If incomplete combustion occurs, the reaction proceeds in the form of Carbon Monoxide CO gas or solid carbon andH2O. Combustion reaction that occurs in all these three compounds also produces a number of considerable energy. And if it has higher value of Carbon then the boiling point would be higher. From the Differential Scanning Calorimetric (DSC test results obtained some of the factors that affect the reaction speed, which are the temperature, the reaction mixture composition, and pressure. Temperature has a profound influence in coal liquefaction, because if liquid coal heated with high pressure, the carbon chain would break down into smaller chains consisting of aromatic chain, hydro-aromatic, or aliphatic. This then triggers a reaction between oil formation and polymerization reactions to form solids (char.

Characterization of early-age hydration processes in lime-ceramic binders using isothermal calorimetry, X-ray diffraction and scanning electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Jerman, Miloš; Tydlitát, Vratislav; Keppert, Martin; Čáchová, Monika; Černý, Robert, E-mail: cernyr@fsv.cvut.cz

2016-06-10

Highlights: • Early age hydration processes in lime-ceramic binders are analyzed within a wide range of component ratios. • The applied waste ceramic dust exhibits partial hydraulic properties, ettringite and calcite are formed. • Transition from tobermorite- to jennite-like structures is identified by SEM within the first 48 h. • The highest specific hydration heat after 300 h, 63 J/g, is measured for the binder containing 70% ceramic. • Substantial effect of the heat of wetting is observed, ranging from 10 J/g for lime to 3.9 J/g for ceramic. - Abstract: Early-age hydration processes in a lime-ceramic-water system are analyzed within the whole range of possible lime/ceramic ratios. The isothermal calorimetry shows a substantial effect of the heat of wetting on the total heat evolved, ranging from 10 J/g for lime to 3.9 J/g for ceramic. The highest specific hydration heat of 63 J/g during the analyzed 300-h hydration period exhibits the blended binder containing 70% ceramic and 30% lime which correlates well with the highest compressive and bending strengths of the paste prepared using this blend. Portlandite, ettringite and calcite are the main phases identified by the X-ray diffraction analysis after the hydration of ceramic-rich blends. According to the results of scanning electron microscopy, the initial course of pozzolanic reaction is for this type of binders characterized by the transition from tobermorite-like calcium-silicate-hydrate structures into jennite-like structures within the first 48 h. Blends with the ceramic content lower than 70% show a high portion of portlandite, calcite is present in low amount, and the jennite-like structures are observed after 48 h, following the initial formation of components with a very high Ca content. The favorable properties of the ceramic-rich blended binders can be explained by the partial hydraulic character of the ceramic. With the specific hydration heat of 29 J/g after 300 h and compressive strength

Characterization of early-age hydration processes in lime-ceramic binders using isothermal calorimetry, X-ray diffraction and scanning electron microscopy

International Nuclear Information System (INIS)

Jerman, Miloš; Tydlitát, Vratislav; Keppert, Martin; Čáchová, Monika; Černý, Robert

2016-01-01

Highlights: • Early age hydration processes in lime-ceramic binders are analyzed within a wide range of component ratios. • The applied waste ceramic dust exhibits partial hydraulic properties, ettringite and calcite are formed. • Transition from tobermorite- to jennite-like structures is identified by SEM within the first 48 h. • The highest specific hydration heat after 300 h, 63 J/g, is measured for the binder containing 70% ceramic. • Substantial effect of the heat of wetting is observed, ranging from 10 J/g for lime to 3.9 J/g for ceramic. - Abstract: Early-age hydration processes in a lime-ceramic-water system are analyzed within the whole range of possible lime/ceramic ratios. The isothermal calorimetry shows a substantial effect of the heat of wetting on the total heat evolved, ranging from 10 J/g for lime to 3.9 J/g for ceramic. The highest specific hydration heat of 63 J/g during the analyzed 300-h hydration period exhibits the blended binder containing 70% ceramic and 30% lime which correlates well with the highest compressive and bending strengths of the paste prepared using this blend. Portlandite, ettringite and calcite are the main phases identified by the X-ray diffraction analysis after the hydration of ceramic-rich blends. According to the results of scanning electron microscopy, the initial course of pozzolanic reaction is for this type of binders characterized by the transition from tobermorite-like calcium-silicate-hydrate structures into jennite-like structures within the first 48 h. Blends with the ceramic content lower than 70% show a high portion of portlandite, calcite is present in low amount, and the jennite-like structures are observed after 48 h, following the initial formation of components with a very high Ca content. The favorable properties of the ceramic-rich blended binders can be explained by the partial hydraulic character of the ceramic. With the specific hydration heat of 29 J/g after 300 h and compressive strength

Crystal structure transformation in potassium acrylate

Science.gov (United States)

Pai Verneker, V. R.; Vasanthakumari, R.

1983-10-01

Potassium acrylate undergoes a reversible phase transformation around 335°K with an activation energy of 133 kcal/mole. Differential scanning calorimetry and high temperature X-ray powder diffraction techniques have been used to probe this phenomenon.

The thermal properties of a carbon nanotube-enriched epoxy: Thermal conductivity, curing, and degradation kinetics

KAUST Repository

Ventura, Isaac Aguilar; Rahaman, Ariful; Lubineau, Gilles

2013-01-01

conductivity, and degradation kinetics were studied. Introducing the MWCNTs increased the curing activation energy as revealed by differential scanning calorimetry. The final thermal conductivity of the 0.5 and 1.0 wt % MWCNT-enriched epoxy samples measured

Preformulation compatibility screening of dika fat-drug mixtures ...

African Journals Online (AJOL)

Differential scanning calorimetry (DSC) was used as screening technique for assessing compatibility between dika fat and drug substances. Dika fat was found to be compatible with aspirin, ascorbic acid, paracetamol, sulphanilamide, phenylpropanolamine hydrochloride, bromopheniramine maleate, chlorpheniramire ...

Hydroxychalcone and Hydroxypropyl-β-Cyclodextrin

African Journals Online (AJOL)

stability of the complex was measured by thermogravimetric/differential scanning calorimetry (TG/DSC). Results: The ... has approved the application of HP-β-CD in food, ... diagrams as in Eq 1. .... The financial support provided by the Program.

Magnetic-field-controlled negative differential conductance in scanning tunneling spectroscopy of graphene npn junction resonators

Science.gov (United States)

Li, Si-Yu; Liu, Haiwen; Qiao, Jia-Bin; Jiang, Hua; He, Lin

2018-03-01

Negative differential conductance (NDC), characterized by the decreasing current with increasing voltage, has attracted continuous attention for its various novel applications. The NDC typically exists in a certain range of bias voltages for a selected system and controlling the regions of NDC in curves of current versus voltage (I -V ) is experimentally challenging. Here, we demonstrate a magnetic-field-controlled NDC in scanning tunneling spectroscopy of graphene npn junction resonators. The magnetic field not only can switch on and off the NDC, but also can continuously tune the regions of the NDC in the I -V curves. In the graphene npn junction resonators, magnetic fields generate sharp and pronounced Landau-level peaks with the help of the Klein tunneling of massless Dirac fermions. A tip of scanning tunneling microscope induces a relatively shift of the Landau levels in graphene beneath the tip. Tunneling between the misaligned Landau levels results in the magnetic-field-controlled NDC.

Experimental study of the energetics of tetradentate N2O2 Schiff bases derived from salicylaldehyde

International Nuclear Information System (INIS)

Ribeiro da Silva, Maria D.M.C.; Goncalves, Jorge M.; Silva, Ana L.R.; Silva, Adelina M.R.O.A.; Oliveira, Paula C.F.C.; Ribeiro da Silva, Manuel A.V.

2004-01-01

The standard (p 0 = 0.1 MPa) molar enthalpies of formation, at T = 298.15 K, in the gaseous phase of two Schiff bases, N,N'-bis(salicylaldehydo)ethylenediimine and N,N'-bis(salicylaldehydo)tetramethylenediimine, were determined from their enthalpies of combustion and sublimation, obtained by static bomb calorimetry in oxygen and by the Knudsen effusion technique, respectively. The enthalpies of fusion of both compounds have been determined by differential scanning calorimetry

Isothermal Titration Calorimetry in the Student Laboratory

Science.gov (United States)

Wadso, Lars; Li, Yujing; Li, Xi

2011-01-01

Isothermal titration calorimetry (ITC) is the measurement of the heat produced by the stepwise addition of one substance to another. It is a common experimental technique, for example, in pharmaceutical science, to measure equilibrium constants and reaction enthalpies. We describe a stirring device and an injection pump that can be used with a…

Liquid Crystalline Perylene diimides : Architecture and Charge Carrier Mobilities

NARCIS (Netherlands)

Struijk, C.W.; Sieval, A.B.; Dakhorst, J.E.J.; Dijk, van M.; Kimkes, P.; Koehorst, R.B.M.; Donker, H.

2000-01-01

The phase behavior of three N-alkyl-substituted perylene diimide derivatives is examined by differential scanning calorimetry and polarized optical microscopy. The occurrence of multiple phase transitions indicates several crystalline and several liquid crystalline phases. X-ray diffraction

Creep recovery of metallic glass Fe-Ni-B after longtime stress-annealing

NARCIS (Netherlands)

Jurikova, A; Csach, K; Miskuf, J; Ocelik, Vaclav

2004-01-01

The creep strain recovery of magnetic soft material - amorphous metallic glass Fe-Ni-B after a longtime stress-annealing at different temperatures below the crystallization temperature was described using differential scanning calorimetry and dilatometry. Several deformation energy accumulations

Characterization of Digestion Resistance Sweet Potato Starch ...

African Journals Online (AJOL)

Purpose: To analyze the physicochemical properties and in vitro digestibility of sweet potato starchphosphodiester prepared using sodium trimetaphosphate. Methods: The physicochemical properties of sweet potato starch phosphodiester were analyzed by using infrared spectrometry (IR), differential scanning calorimetry ...

Gradient temperature Raman spectroscopy identifies flexible sites in proline and alanine peptides

Science.gov (United States)

Continuous thermo dynamic Raman spectroscopy (TDRS) applies the temperature gradients utilized in differential scanning calorimetry (DSC) to Raman spectroscopy, providing a straightforward technique to identify molecular rearrangements that occur just prior to phase transitions. Herein we apply TDRS...

Annealing properties of potato starches with different degrees of phosphorylation

DEFF Research Database (Denmark)

Muhrbeck, Per; Svensson, E

1996-01-01

Changes in the gelatinization temperature interval and gelatinization enthalpy with annealing time at 50 degrees C were followed for a number of potato starch samples, with different degrees of phosphorylation, using differential scanning calorimetry. The gelatinization temperature increased...

Sadhana | Indian Academy of Sciences

Indian Academy of Sciences (India)

Changes in polymer foils used in food packaging tested by using differential scanning calorimetry ... A third-order active-R filter with feedforward input signal ... Time-variant power spectral analysis of heart-rate time series by autoregressive ...

Differential magnetic force microscope imaging.

Science.gov (United States)

Wang, Ying; Wang, Zuobin; Liu, Jinyun; Hou, Liwei

2015-01-01

This paper presents a method for differential magnetic force microscope imaging based on a two-pass scanning procedure to extract differential magnetic forces and eliminate or significantly reduce background forces with reversed tip magnetization. In the work, the difference of two scanned images with reversed tip magnetization was used to express the local magnetic forces. The magnetic sample was first scanned with a low lift distance between the MFM tip and the sample surface, and the magnetization direction of the probe was then changed after the first scan to perform the second scan. The differential magnetic force image was obtained through the subtraction of the two images from the two scans. The theoretical and experimental results have shown that the proposed method for differential magnetic force microscope imaging is able to reduce the effect of background or environment interference forces, and offers an improved image contrast and signal to noise ratio (SNR). © Wiley Periodicals, Inc.

Water calorimetry: The heat defect

International Nuclear Information System (INIS)

Klassen, N.V.; Ross, C.K.

1997-01-01

Domen developed a sealed water calorimeter at NIST to measure absorbed dose to water from ionizing radiation. This calorimeter exhibited anomalous behavior using water saturated with gas mixtures of H 2 O 2 . Using computer simulations of the radiolysis of water, the authors show that the observed behavior can be explained if, in the gas mixtures, the amount-of-substance of H 2 and of O 2 differed significantly from 50%. The authors also report the results of simulations for other dilute aqueous solutions that are used for water calorimetry--pure water, air-saturated water, and H 2 -saturated water. The production of H 2 O 2 was measured for these aqueous solutions and compared to simulations. The results indicate that water saturated with a gas mixture containing an amount-of-substance of H 2 of 50% and of O 2 of 50% is suitable for water calorimetry if the water is stirred and is in contact with a gas space of similar volume. H 2 -saturated water does not require a gas space but O 2 contamination must be guarded against. The lack of a scavenger for OH radicals in pure water means that, depending on the water purity, some pure water might require a large priming dose to remove reactive impurities. The experimental and theoretical problems associated with air-saturated water and O 2 -saturated water in water calorimeters are discussed

The physics of compensating calorimetry and the new CALOR89 code system

International Nuclear Information System (INIS)

Gabriel, T.A.; Brau, J.E.; Bishop, B.L.

1989-03-01

Much of the understanding of the physics of calorimetry has come from the use of excellent radiation transport codes. A new understanding of compensating calorimetry was introduced four years ago following detailed studies with a new CALOR system. Now, the CALOR system has again been revised to reflect a better comprehension of high energy nuclear collisions by incorporating a modified high energy fragmentation model from FLUKA87. This revision will allow for the accurate analysis of calorimeters at energies of 100's of GeV. Presented in this paper is a discussion of compensating calorimetry, the new CALOR system, the revisions to HETC, and recently generated calorimeter related data on modes of energy deposition and secondary neutron production (E < 50 MeV) in infinite iron and uranium blocks. 38 refs., 5 figs., 5 tabs

Evaluation of dynamic enhanced CT scanning in the differentiation of adrenal lipid-poor adenomas with metastases

International Nuclear Information System (INIS)

Fang Xiangming; Hu Chunhong; Hu Xiaoyun; Chen Hongwei; Wu Liyuan; Zou Xinnong; Qian Pingyan

2006-01-01

Objective: To evaluate dynamic enhanced CT in differentiating adrenal metastases from adrenal lipid-poor adenomas(ALPA). Methods: Both plain and dynamic enhanced CT scanning was performed in 9 metastases with 13 masses and 28 lipid-poor adenoma with 30 masses. The types of time-density curve according to peak time(PT) and relative washout percentage(Washr) besides shape, size, margin, internal structure, surrounding status and enhanced pattern of each lesion were measuerd and compared between the two groups of metastases and ALPA. Results: There is difference between metastases and ALPA in the aspects of shape, density, neighboring structure and the type of enhancement. The type of TDC of matastases was characterized by fast-washin and fast-washout, which was quite differed from the type of TDC of ALPA characterized by fast-washin and slow-washout. According to this, the sensitiveity and specificity for differentiating metastases from ALPA were 96.7%, 92.3%. Conclusion: The types of TDC of dynamic enhanced CT is of great value in differentiating metastases from ALPA. (authors)

Investigation of polarized-proton target materials by differential calorimetry: preliminary results

International Nuclear Information System (INIS)

Hill, D.A.; Hill, J.J.

1980-01-01

A simple differential calorimeter was designed and operated for an investigation of the thermodynamic properties of polarized target materials. The calibration and use of the calorimeter are discussed, after a brief exposition of our motivation for this work. The results of a preliminary study of target materials is presented with emphasis on the relevance of the glass state to dynamic polarization in chemically-doped targets

Primary crystallization in Al-rich metallic glasses at unusually low temperatures

International Nuclear Information System (INIS)

Bokeloh, J.; Boucharat, N.; Roesner, H.; Wilde, G.

2010-01-01

The initial stage of the primary crystallization reaction and the glass transition of the marginal metallic glass Al 89 Y 6 Fe 5 were investigated by conventional differential scanning calorimetry (DSC) and modulated differential scanning calorimetry (MDSC), microcalorimetry, X-ray diffraction (XRD) and transmission electron microscopy. A sharp onset of the primary crystallization was found by microcalorimetry and XRD studies at temperatures which were 120 deg. C below the primary crystallization peak observed in conventional DSC. A systematic MDSC study of annealed samples revealed a wide spectrum of glass transition onsets, which show a strong dependence on the annealing conditions. In addition, the glass transition onsets can be linked to the initial stage of the primary crystallization. The spectrum of glass transition onsets observed is discussed with respect to the occurrence of phase separation preceding the nucleation and growth of dendritic aluminium nanocrystals.

Value of 201Tl imaging in predicting therapeutic 131I uptake in patients with thyroglobulin-positive but 131I scan-negative differentiated thyroid carcinoma

International Nuclear Information System (INIS)

Conlu, R.A.O.; Obaldo, J.M.

2004-01-01

Background: Serum thyroglobulin assay and 131Iodine (1311) whole body scan are considered complementary in detecting malignant thyroid tissue or metastases. A large number of patients, however, are encountered presenting with scan-negative, thyroglobulin-positive differentiated thyroid carcinoma posing a dilemma in therapeutic management. One of the first alternative scanning agents to be employed is 201Thallium (201Tl). Recent studies have demonstrated its usefulness in identifying lesions that are not visualized with traditional 131I whole body scan. It is not clear, however, whether 201Tl scan helps in the decision-making for subsequent 131I therapy. This study was conducted to determine if 201Tl scan can predict therapeutic 131I uptake and to define the clinical role of 201Tl scanning in these patients. Methods and results: A total of 12 patients (20-63 y/o), 5 males and 7 females, underwent surgery for differentiated thyroid cancer and all had serum thyroglobulin values above 10 ng/ml and normal TPO autoantibodies. Pre-therapy 131I scan using 111 MBq (3mCi) of 131I were obtained. As required for inclusion, all patients had negative pre-therapy scan and negative TPO autoantibody results and underwent 20lTl scanning within 3 weeks. All patients were given 131I therapy (3.7-5.5 GBq or 100-150 mCi) between one to two months after 201Tl scanning. Within a week after therapy, all patients underwent whole body 1311 scanning. 201Tl imaging demonstrated thyroid remnants in 9 out of 12 patients having positive 201Tl scan but negative pre-therapy 1311 scan. However, only 2 of the positive 201Tl scans showed 131I uptake post-therapy (positive predictive value of 20%). None of the subjects presented with a negative 201Tl scan and a positive post-therapy 131I scan. Conclusion: Our study suggests that evidence of remnants or metastases on 201Tl scanning may be an inappropriate basis for the decision to proceed with 131I therapy. The role of 20lTl imaging in this subset of

Papel del agua en la gelatinización delalmidón de maíz: estudio por calorimetríadiferencial de barrido Role of water in maize starch gelatinization: an study by Differential Scanning Calorimetry

Directory of Open Access Journals (Sweden)

P. Pineda–Gómez

2010-06-01

Full Text Available El comportamiento térmico del almidón de maíz (Sigma Aldrich se estudió através de calorimetría diferencial de barrido (DSC. El pico endotérmico observadoen el perfil DSC se asocia al proceso de transición de gelatinizacióndel almidón. La fase inicial del proceso y el rango en el que éste ocurre, está gobernada principalmente por la concentración del almidón en solución. Enesta investigación se demuestra que los parámetros relacionados con el métodode observación, en un análisis de DSC influyen al momento de determinar lagelatinización del almidón de maíz. De esta forma, la temperatura del picode transición, la entalpía de gelatinización y el intervalo de temperatura degelatinización son los parámetros en estudio cuando se varía la humedad dela muestra y velocidad de calentamiento con un tamaño de grano homogéneo.Para los análisis, se tomaron valores de humedad de 60, 65, 70, 75 y 80%(p/p, para una velocidad de calentamiento de 2, 5 y 10◦C/min. De igualmodo, para un valor fijo de humedad (80%, se utilizó una velocidad de calentamientode 2, 5, 7, 10 y 15◦C/min. Los resultados indican que la cantidad deagua influye significativamente sobre la entalpía de gelatinización del proceso,pero la temperatura del pico Tp de la endoterma se mantiene constante. Elvalor de la entalpía disminuye a medida que la cantidad de agua aumenta.Las variaciones también son dependientes de la rapidez con que se efectúa latransformación. Los análisis permitieron corroborar, que esta transición en elalmidón es dependiente de factores extrínsecos durante el proceso. Este conocimientosobre la gelatinización del almidón es útil para optimizar procesosindustriales derivados de éste.The thermal behavior of corn starch (Sigma Aldrich was studied by differential scanning calorimetry (DSC. The endothermic peak in the DSC thermogram is associated to the starch gelatinization transition process. Initial phase of process and range in

Differentiation of Aedes aegypti and Aedes notoscriptus (Diptera: Culicidae) eggs using scanning electron microscopy.

Science.gov (United States)

Faull, Katherine J; Williams, Craig R

2016-05-01

Aedes notoscriptus and Aedes aegypti are both peri-domestic, invasive container-breeding mosquitoes. While the two potential arboviral vectors are bionomically similar, their sympatric distribution in Australia is limited. In this study, analyses of Ae. aegypti and Ae. notoscriptus eggs were enabled using scanning electron microscopy. Significant variations in egg length to width ratio and outer chorionic cell field morphology between Ae. aegypti and Ae. notoscriptus enabled distinction of the two species. Intraspecific variations in cell field morphology also enabled differentiation of the separate populations of both species, highlighting regional and global variation. Our study provides a comprehensive comparative analysis of inter- and intraspecific egg morphological and morphometric variation between two invasive container-breeding mosquitoes. The results indicate a high degree of intraspecific variation in Ae. notoscriptus egg morphology when compared to the eggs of Ae. aegypti. Comparative morphological analyses of Ae. aegypti and Ae. notoscriptus egg attributes using SEM allows differentiation of the species and may be helpful in understanding egg biology in relation to biotope of origin. Copyright © 2016 Elsevier Ltd. All rights reserved.

Kinetics of the subtransition in dipalmitoylphosphatidylcholine

International Nuclear Information System (INIS)

Tristram-Nagle, S.; Wiener, M.C.; Yang, C.P.; Nagle, J.F.

1987-01-01

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 0 C. After incubation at 0.1 0 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, the authors show that these two peaks merge into one at slow scanning rates with a common equilibrium transition temperature of 13.8 0 C, in agreement with equilibrium calorimetry and dilatometry. For incubation temperatures above 4.6 0 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. They suggest that higher incubation temperatures (near 5 0 C) are preferable for forming the stable subgel phase, and they present a colliding domain picture that indicates why this may be so. The results in D 2 O 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

Kinetics of the subtransition in dipalmitoylphosphatidylcholine.

Science.gov (United States)

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.

Crystallization processes in Ge2Sb2Se4Te glass

Czech Academy of Sciences Publication Activity Database

Svoboda, R.; Bezdička, Petr; Gutwirth, J.; Malek, J.

2015-01-01

Roč. 61, JAN (2015), s. 207-214 ISSN 0025-5408 Institutional support: RVO:61388980 Keywords : Chalcogenides * Glass es * Differential scanning calorimetry (DSC) * X-ray diffraction * Crystal structure Subject RIV: CA - Inorganic Chemistry Impact factor: 2.435, year: 2015

Thermal stability study of crystalline and novel spray-dried amorphous nilotinib hydrochloride

NARCIS (Netherlands)

Herbrink, Maikel; Vromans, Herman; Schellens, Jan Hm; Beijnen, Jos H; Nuijen, Bastiaan

2018-01-01

The thermal characteristics and the thermal degradation of crystalline and amorphous nilotinib hydrochloride (NH) were studied. The spray drying technique was successfully utilized for the amorphization of NH and was evaluated by spectroscopic techniques and differential scanning calorimetry (DSC).

Investigation of thermodynamic properties of magnesium chloride amines by HPDSC and TG. For application in a high-lift high-temperature chemical heat pump

NARCIS (Netherlands)

Bevers, E.R.T.; Oonk, H.A.J.; Haije, W.G.; Ekeren, P.J. van

2007-01-01

The formation as well as the decomposition of magnesium chloride ammonia complexes was studied by high-pressure differential scanning calorimetry (HPDSC) and thermogravimetric analysis (TG). HPDSC runs were performed under constant ammonia pressure conditions to determine the transition temperatures

Continuous gradient temperature Raman spectroscopy of oleic and linoleic acids from -100 to 50°C

Science.gov (United States)

Gradient Temperature Raman spectroscopy (GTRS) applies the temperature gradients utilized in differential scanning calorimetry (DSC) to Raman spectroscopy, providing a straightforward technique to identify molecular rearrangements that occur near and at phase transitions. Herein we apply GTRS and DS...

Fast sampling calorimetry with solid argon ionization chambers

International Nuclear Information System (INIS)

Clark, E.; Linn, S.; Piekarz, H.; Wahl, H.; Womersley, J.; Hansen, S.; Hurh, P.; Rivetta, C.; Sanders, R.; Schmitt, R.; Stanek, R.; Stefanik, A.

1992-01-01

A proposal for the fast sampling calorimetry with solid argon as active medium and the preliminary results from the solid argon test cell are presented. The proposed test calorimeter module structure, the signal routing and the mechanical and cryogenic arrangements are also discussed

Thermal decomposition of natural polysaccharides: Chitin and chitosan

Directory of Open Access Journals (Sweden)

Kuchina Yu.A.

2015-03-01

Full Text Available The results of the thermal analysis of shrimp’s chitin and chitosan have been presented (samples of polysaccharide differed by the deacetylation degree have been studied. The thermal analysis has been carried out by differential thermogravimetry and differential scanning calorimetry. Activation energy of process of chitin and chitosan thermal destruction has been calculated

Evaluation of the amorphous content of lactose by solution calorimetry and Raman spectroscopy.

Science.gov (United States)

Katainen, Erja; Niemelä, Pentti; Harjunen, Päivi; Suhonen, Janne; Järvinen, Kristiina

2005-11-15

Solution calorimetry can be used to determine the amorphous content of a compound when the solubility and dissolution rate of the compound in the chosen solvent are reasonably high. Sometimes, it can be difficult find a solvent in which a sample is freely soluble. The present study evaluated the use of solution calorimetry for the assessment of the amorphous content of a sample that is poorly soluble in a solvent. Physical mixtures of lactose and spray-dried lactose samples (the amorphous content varied from 0 to 100%) were analyzed by a solution calorimeter and the results were compared with Raman spectroscopy determinations. The heat of solvation of the samples was determined by solution calorimetry in organic solvents MeOH, EtOH, ACN, THF, acetone (400mg sample/100ml solvent). Lactose is virtually insoluble in ACN, THF and acetone and very slightly soluble in EtOH and MeOH. The amorphous content of the samples could not be determined by solution calorimetry in EtOH, ACN, THF or acetone. However, an excellent correlation was observed between the heat of solvation and the amorphous content of the samples in MeOH. Furthermore, the heat of solvation values of the samples in MeOH showed a linear correlation with the Raman quantifications. Therefore, our results demonstrate that solution calorimetry may represent a rapid and simple method for determining the amorphous content also in samples that are not freely soluble in the solvent.

Methodology of hot nucleus calorimetry and thermometry produced by nuclear reactions around Fermi energies; Methodologie de la calorimetrie et de la thermometrie des noyaux chauds formes lors de collisions nucleaires aux energies de Fermi

Energy Technology Data Exchange (ETDEWEB)

Vient, E

2006-12-15

This work deals with the calorimetry and thermometry of hot nuclei produced in collisions Xe + Sn between 25 and 100 MeV/u. The apparatus for hot nucleus physical characterization is the 4{pi} detector array Indra. This study was made by using the event generators Gemini, Simon and Hipse and a data-processing filter simulating the complete operation of the multi-detector. The first chapter presents the different ways of producing hot nuclei. In the second and third chapters, the author presents a critical methodological study of calorimetry and thermometry applied to hot nuclei, different methods are reviewed, their accuracy and application range are assessed. All the calorimetry methods rely on the assumption that we are able to discriminate decay products of the hot nucleus from evaporated particles. In the fourth chapter, the author gives some ways of improving calorimetry characterization of the hot nucleus. An alternative method of calorimetry is proposed in the fifth chapter, this method is based on the experimental determination of an evaporation probability that is deduced from the physical characteristics of the particles present in a restricted domain of the space of velocities.

Synthesis and mesomorphic properties of a triphenylene-based ...

African Journals Online (AJOL)

A new triphenylene liquid crystal material with six rod-shape bisazobenzene moieties as the peripheral units has been synthesized and characterized by spectroscopic methods. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and, X-ray diffraction.

Structural changes in polytetrafluoroethylene molecular chains upon sliding against steel

NARCIS (Netherlands)

Shen, J.T.; Pei, Y.T.; Hosson, J.Th.M. De

In this work, the influence of dry sliding between a steel counterpart ball and polytetrafluoroethylene (PTFE) plate sample on the transformation of PTFE molecular structure is investigated. With X-ray diffraction, differential scanning calorimetry, Fourier transform infrared (FT-IR) spectroscopy

Thermal analysis on parchments I: DSC and TGA combined approach for heat damage assessment

DEFF Research Database (Denmark)

Fessas, D.; Signorelli, M.; Schiraldi, A.

2006-01-01

Ancient, new and artificially aged parchments were investigated with both differential scanning calorimetry (DSC) and thermogravimetry (TGA). Criteria to define a quantitative ranking of the damage experienced by the bulk collagen of historical parchments were assessed. A damage-related correlation...

Nanospheres with a smectic hydrophobic core and an amorphous PEG hydrophilic shell: structural changes and implications for drug delivery

Energy Technology Data Exchange (ETDEWEB)

Murthy, N. Sanjeeva [New Jersey Center for Biomaterials; Rutgers; The State University of New Jersey; Piscataway; USA; Zhang, Zheng [New Jersey Center for Biomaterials; Rutgers; The State University of New Jersey; Piscataway; USA; Borsadia, Siddharth [New Jersey Center for Biomaterials; Rutgers; The State University of New Jersey; Piscataway; USA; Kohn, Joachim [New Jersey Center for Biomaterials; Rutgers; The State University of New Jersey; Piscataway; USA

2018-01-01

The structural changes in nanospheres with a crystalline core and an amorphous diffuse shell were investigated by small-angle neutron scattering (SANS), small-, medium-, and wide-angle X-ray scattering (SAXS, MAXS and WAXS), and differential scanning calorimetry (DSC).

Microstructure and molecular interaction in glycerol plasticized chitosan/poly(vinyl alcohol) blending films

Science.gov (United States)

Poly (vinyl alcohol) (PVA)/chitosan (CS) blended films plasticized by glycerol were investigated using mechanical testing, atomic force microscopy (AFM), differential scanning calorimetry (DSC) and FTIR spectroscopy, with primary emphasis on the effects of the glycerol content and the molecular weig...

Note on the glass transition temperature of poly(vinylphenol)

Czech Academy of Sciences Publication Activity Database

Kratochvíl, Jaroslav; Šturcová, Adriana; Sikora, Antonín; Dybal, Jiří

2009-01-01

Roč. 45, č. 6 (2009), s. 1851-1856 ISSN 0014-3057 Institutional research plan: CEZ:AV0Z40500505 Keywords : Poly(4-vinylphenol) * glass transition temperature * differential scanning calorimetry Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.310, year: 2009

Use of instrumental methods in the investigation of low temperature tolerance of soil algae and cyanobacteria

Czech Academy of Sciences Publication Activity Database

Lukešová, Alena; Worland, M. R.; Kaftan, David; Lukeš, Martin

2004-01-01

Roč. 3, č. 1 (2004), s. 82-85 ISSN 1336-1120 Grant - others:Evropská unie(XE) QLRI-CT--2001-01645 Institutional research plan: CEZ:AV0Z6066911 Keywords : cryomicroscopy * cryopreservation * differential scanning calorimetry Subject RIV: EH - Ecology, Behaviour

The Effect of Polymer Molecular Weight on Citrate Crosslinked ...

African Journals Online (AJOL)

SEM), dissolution studies and differential scanning calorimetry (DSC) for surface ... Conclusion: The citrate-crosslinked chitosan films can be modulated to vary swelling and drug release at pH 3.5 and 6.2; this feature makes them useful tools for ...

Synthesis of Well-Defined Polyethylene-Based 3-Miktoarm Star Copolymers and Terpolymers

KAUST Repository

Zhang, Zhen; Altaher, Maryam; Zhang, Hefeng; Wang, De; Hadjichristidis, Nikolaos

2016-01-01

by 1H NMR, high temperature gel permeation chromatography (HT-GPC), and differential scanning calorimetry (DSC). The synthetic method is a general one and can be used for the synthesis of complex PE-based architectures by combination with other living

Vendor Testing of Sensitive Compounds in Simulated Dry Sludge

International Nuclear Information System (INIS)

Dworjanyn, L.O.

1999-01-01

This assessment covers thermal screening, differential scanning calorimetry, and impact sensitivity testing on Mercury Fulminate, and mixtures of the fulminate in dry inorganic sludge, which is present in large quantities in a number of storage tanks at Westinghouse Savannah River

Structural Changes in Deformed Soft Magnetic Ni-Based Metallic Glass

NARCIS (Netherlands)

Jurikova, A.; Csach, K.; Miskuf, J.; Ocelik, V.

The effects of intensive plastic deformation of the soft magnetic metallic glass Ni Si 13 on the structural relaxation were examined. The enthalpy changes studied by differential scanning calorimetry revealed that the intensive plastic deformation was associated with the partial structural

Systematic investigation of lard polymorphism using combined DSC and time-resolved synchrotron X-ray diffraction

NARCIS (Netherlands)

Kalnin, D.J.E.; Lesieur, P.; Artzner, F.; Keller, G.; Ollivon, M.

2005-01-01

The polymorphic behavior of lard was systematically investigated by differential scanning calorimetry (DSC) while simultaneously monitoring the formation of the different crystal forms with X-ray diffraction (XRDT). To interpret the complex polymorphic evolution of the sample analyzed by regular

Noninvasive differential diagnosis of dental periapical lesions in cone-beam CT scans

Energy Technology Data Exchange (ETDEWEB)

Okada, Kazunori, E-mail: kazokada@sfsu.edu [Department of Computer Science, San Francisco State University, San Francisco, California 94132 (United States); Rysavy, Steven [Biomedical and Health Informatics Program, University of Washington, Seattle, Washington 98195 (United States); Flores, Arturo [Computer Science and Engineering, University of California, San Diego, California 92093 (United States); Linguraru, Marius George [Sheikh Zayed Institute for Pediatric Surgical Innovation, Children’s National Medical Center, Washington, DC 20010 and Departments of Radiology and Pediatrics, George Washington University, Washington, DC 20037 (United States)

2015-04-15

Purpose: This paper proposes a novel application of computer-aided diagnosis (CAD) to an everyday clinical dental challenge: the noninvasive differential diagnosis of periapical lesions between periapical cysts and granulomas. A histological biopsy is the most reliable method currently available for this differential diagnosis; however, this invasive procedure prevents the lesions from healing noninvasively despite a report that they may heal without surgical treatment. A CAD using cone-beam computed tomography (CBCT) offers an alternative noninvasive diagnostic tool which helps to avoid potentially unnecessary surgery and to investigate the unknown healing process and rate for the lesions. Methods: The proposed semiautomatic solution combines graph-based random walks segmentation with machine learning-based boosted classifiers and offers a robust clinical tool with minimal user interaction. As part of this CAD framework, the authors provide two novel technical contributions: (1) probabilistic extension of the random walks segmentation with likelihood ratio test and (2) LDA-AdaBoost: a new integration of weighted linear discriminant analysis to AdaBoost. Results: A dataset of 28 CBCT scans is used to validate the approach and compare it with other popular segmentation and classification methods. The results show the effectiveness of the proposed method with 94.1% correct classification rate and an improvement of the performance by comparison with the Simon’s state-of-the-art method by 17.6%. The authors also compare classification performances with two independent ground-truth sets from the histopathology and CBCT diagnoses provided by endodontic experts. Conclusions: Experimental results of the authors show that the proposed CAD system behaves in clearer agreement with the CBCT ground-truth than with histopathology, supporting the Simon’s conjecture that CBCT diagnosis can be as accurate as histopathology for differentiating the periapical lesions.

Noninvasive differential diagnosis of dental periapical lesions in cone-beam CT scans

International Nuclear Information System (INIS)

Okada, Kazunori; Rysavy, Steven; Flores, Arturo; Linguraru, Marius George

2015-01-01

Purpose: This paper proposes a novel application of computer-aided diagnosis (CAD) to an everyday clinical dental challenge: the noninvasive differential diagnosis of periapical lesions between periapical cysts and granulomas. A histological biopsy is the most reliable method currently available for this differential diagnosis; however, this invasive procedure prevents the lesions from healing noninvasively despite a report that they may heal without surgical treatment. A CAD using cone-beam computed tomography (CBCT) offers an alternative noninvasive diagnostic tool which helps to avoid potentially unnecessary surgery and to investigate the unknown healing process and rate for the lesions. Methods: The proposed semiautomatic solution combines graph-based random walks segmentation with machine learning-based boosted classifiers and offers a robust clinical tool with minimal user interaction. As part of this CAD framework, the authors provide two novel technical contributions: (1) probabilistic extension of the random walks segmentation with likelihood ratio test and (2) LDA-AdaBoost: a new integration of weighted linear discriminant analysis to AdaBoost. Results: A dataset of 28 CBCT scans is used to validate the approach and compare it with other popular segmentation and classification methods. The results show the effectiveness of the proposed method with 94.1% correct classification rate and an improvement of the performance by comparison with the Simon’s state-of-the-art method by 17.6%. The authors also compare classification performances with two independent ground-truth sets from the histopathology and CBCT diagnoses provided by endodontic experts. Conclusions: Experimental results of the authors show that the proposed CAD system behaves in clearer agreement with the CBCT ground-truth than with histopathology, supporting the Simon’s conjecture that CBCT diagnosis can be as accurate as histopathology for differentiating the periapical lesions

Noninvasive differential diagnosis of dental periapical lesions in cone-beam CT scans.

Science.gov (United States)

Okada, Kazunori; Rysavy, Steven; Flores, Arturo; Linguraru, Marius George

2015-04-01

This paper proposes a novel application of computer-aided diagnosis (CAD) to an everyday clinical dental challenge: the noninvasive differential diagnosis of periapical lesions between periapical cysts and granulomas. A histological biopsy is the most reliable method currently available for this differential diagnosis; however, this invasive procedure prevents the lesions from healing noninvasively despite a report that they may heal without surgical treatment. A CAD using cone-beam computed tomography (CBCT) offers an alternative noninvasive diagnostic tool which helps to avoid potentially unnecessary surgery and to investigate the unknown healing process and rate for the lesions. The proposed semiautomatic solution combines graph-based random walks segmentation with machine learning-based boosted classifiers and offers a robust clinical tool with minimal user interaction. As part of this CAD framework, the authors provide two novel technical contributions: (1) probabilistic extension of the random walks segmentation with likelihood ratio test and (2) LDA-AdaBoost: a new integration of weighted linear discriminant analysis to AdaBoost. A dataset of 28 CBCT scans is used to validate the approach and compare it with other popular segmentation and classification methods. The results show the effectiveness of the proposed method with 94.1% correct classification rate and an improvement of the performance by comparison with the Simon's state-of-the-art method by 17.6%. The authors also compare classification performances with two independent ground-truth sets from the histopathology and CBCT diagnoses provided by endodontic experts. Experimental results of the authors show that the proposed CAD system behaves in clearer agreement with the CBCT ground-truth than with histopathology, supporting the Simon's conjecture that CBCT diagnosis can be as accurate as histopathology for differentiating the periapical lesions.

PHOTOACTIVE POLYACRYLONITRILE FIBERS COATED BY NANO-SIZED TITANIUM DIOXIDE: SYNTHESIS, CHARACTERIZATION, THERMAL INVESTIGATION

OpenAIRE

MOAFI, HADI FALLAH; FALLAH SHOJAIE, ABDOLLAH; ALI ZANJANCHI, MOHAMMAD

2011-01-01

Anatase nanocrystals were successfully synthesized and deposited onto polyacrylonitrile fibers with photocatalytic self-cleaning activity using the sol-gel process at low temperature. The original and treated samples have been characterized by several techniques such as scanning electron microscopy, fourier transform infrared spectroscopy, x-ray diffraction, diffuse reflectance spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The TiO2 nanoparticles, have been fo...

Nano-CL-20/HMX Cocrystal Explosive for Significantly Reduced Mechanical Sensitivity

OpenAIRE

An, Chongwei; Li, Hequn; Ye, Baoyun; Wang, Jingyu

2017-01-01

Spray drying method was used to prepare cocrystals of hexanitrohexaazaisowurtzitane (CL-20) and cyclotetramethylene tetranitramine (HMX). Raw materials and cocrystals were characterized using scanning electron microscopy, X-ray diffraction, differential scanning calorimetry, Raman spectroscopy, and Fourier transform infrared spectroscopy. Impact and friction sensitivity of cocrystals were tested and analyzed. Results show that, after preparation by spray drying method, microparticles were sph...

Isothermal Titration Calorimetry Can Provide Critical Thinking Opportunities

Science.gov (United States)

Moore, Dale E.; Goode, David R.; Seney, Caryn S.; Boatwright, Jennifer M.

2016-01-01

College chemistry faculties might not have considered including isothermal titration calorimetry (ITC) in their majors' curriculum because experimental data from this instrumental method are often analyzed via automation (software). However, the software-based data analysis can be replaced with a spreadsheet-based analysis that is readily…

Iota-carrageenan/chitosan/gelatin scaffold for the osteogenic differentiation of adipose-derived MSCs in vitro.

Science.gov (United States)

Li, Junjie; Yang, Boguang; Qian, Yufeng; Wang, Qiyu; Han, Ruijin; Hao, Tong; Shu, Yao; Zhang, Yabin; Yao, Fanglian; Wang, Changyong

2015-10-01

In this study, we have developed ι-carrageenan/chitosan/gelatin (CCG) scaffold containing multiple functional groups (-NH2 , -OH, -COOH, and -SO3 H) to resemble the native extracellular matrix (ECM), using the ion-shielding technology and ultrasonic dispersion method. Fourier transform infrared spectroscopy (FTIR) of the CCG scaffolds suggests that the formation of CCG network involves electrostatic interactions between ι-carrageenan (ι-CA) and chitosan/gelatin, and the covalent cross-linking among amino groups of chitosan and/or gelatin. Scanning electron microscopic (SEM) observation reveals that the porous structure of scaffolds can be modulated by the ratio of ι-CA to chitosan/gelatin. The swelling ratio of the hydrogels increases as the ι-CA contents increase. Using differential scanning calorimetry, we found that the double helix structure of ι-CA is only stabilized at low contents of ι-CA in the CCG scaffolds (e.g., 5 wt %). The scaffolds containing 5% ι-CA showed the best protein adsorption capacity (4.46 ± 0.63 μg protein/mg scaffold) and elastic modulus (5.37 ± 1.03 MPa). In addition, the CCG scaffolds exhibit excellent support for adipose-derived mesenchymal stem cells (ADMSCs) attachment and proliferation, and they can improve the osteogenic differentiation and neovascularization capacities of ADMSCs. Overall, we conclude that the CCG may represent an ideal scaffold material for bone tissue engineering. © 2014 Wiley Periodicals, Inc.

CALOR2012 XVth International Conference on Calorimetry in High Energy Physics

Energy Technology Data Exchange (ETDEWEB)

Akchurin, Nural .

2015-05-04

The International Conferences on Calorimetry in High Energy Physics, or the CALOR series, have always been where the calorimeter experts come together to review the state of calorimetry and bring forth new ideas every two years. The fteenth conference, CALOR2012, in Santa Fe was no exception. Although they were built roughly a decade ago, we are now witnessing the exceptional power of the LHC calorimeters and the crucial role they have been playing in the discovery of the 125 GeV Higgs-like boson. As we ruminate on the coming generation of experiments at the next (linear) collider and on the upgrades at the LHC, we are heartened by the substantial advances we made in calorimetry in the last decade. These advances will certainly help uncover new physics in the years to come, not only at colliders but also in astroparticle experiments that take advantage of natural elements such as air, water, and ice. The proceedings were published by the IOP in Journal of Physics, Vol 404 2011. The conference web site is calor2012.ttu.edu.

A new tool for an old job: Using fixed cell scanning calorimetry to investigate dilute aqueous solutions

International Nuclear Information System (INIS)

Woolley, E.M.

2007-01-01

The development of fixed twin cell temperature scanning calorimeters has enabled the more efficient determination of heat capacities of dilute aqueous solutions with a precision comparable to that of the Picker flow heat capacity calorimeters developed nearly 40 years ago. Experiments require less than 0.5 cm 3 of solution, and results can be obtained routinely over the temperature range (278 to 395) K at pressures up to a few bars. Multiple scanning of samples by both increasing and decreasing temperature allows assessment of instrument drift, solute stability, and reproducibility of results. Chemical calibration is essential to take full advantage of the precision and sensitivity of the calorimeters. The calorimetric output is a direct measure of the difference in heat capacity per unit volume of a solution and of a reference liquid, usually water. Thus, densities of the solution and reference liquid are needed to transform the results into heat capacities per unit mass of solution. Examples of solutes that have been investigated include a variety of inorganic and organic compounds that dissolve to give simple ionic or neutral species, or that produce complexes or species that exist in equilibrium distributions that can change as the temperature is scanned. Appropriate selection of the results from experiments on combinations of solutes allows calculation of standard state (zero concentration) thermodynamic quantities for chemical processes and reactions over the ranges of temperature scanned at the solution compositions investigated. Results for a few specific systems are presented and discussed for some representative classes of solutes that have been investigated in our laboratory since 1998

Investigation of Kinetic Hydrate Inhibition Using a High Pressure Micro Differential Scanning Calorimeter

DEFF Research Database (Denmark)

Daraboina, Nagu; Malmos, Christine; von Solms, Nicolas

2013-01-01

of hydrate growth. Additionally, hydrate formed in the presence of inhibitor decomposed at higher temperatures compared to pure water, indicating that while hydrate formation is initially inhibited; once hydrates form, they are more stable in the presence of inhibitor. Overall, this method proved a viable......Methane hydrate formation and decomposition were investigated in the presence of the kinetic inhibitor (Luvicap EG) and synergist (polyethylene oxide; PEO) using a high pressure micro-differential scanning calorimeter (HP-μDSC) with both temperature ramping and isothermal temperature programs....... These investigations were performed using small samples in four different capillary tubes in the calorimeter cell. When the isothermal method was employed, it was found that Luvicap EG significantly delays the hydrate nucleation time as compared to water. The results obtained from the ramping method demonstrated...

Differential diagnosis between adrenal adenomas and non-adenomas with gadolinium MR in delayed scans: another diagnostic possibility

International Nuclear Information System (INIS)

Mondello, Eduardo J.; Eyheremendy, Eduardo P.; Stoisa, Daniela

2001-01-01

Purpose: To determine the value of measuring delayed post gadolinium signal intensity by displaying a curve, to make the differential diagnosis between adrenal adenomas and non-adenomas, and compare it to chemical shift MR imaging and unenhanced/delayed contrast enhanced CT. Material and methods: Nine adrenal masses have been evaluated by unenhanced/delayed contrast enhanced CT, chemical shift MR imaging and Dynamic Scan at 5, 15, 30 minutes or more, with measurement curves. The 'in phase' imaging have been compared to the 'out phase' ones. Results: Adenomas have shown drop of the curve at 30 minutes of the contrast injection. Non-adenomas have conserved an ascending curve with the same delay. Conclusion: Gadolinium-enhanced MR imaging at delayed scans can characterize adrenal masses as adenomas or non-adenomas. This technique could be considered as a new complementary diagnostic method. (author)

77 FR 5768 - Application(s) for Duty-Free Entry of Scientific Instruments

Science.gov (United States)

2012-02-06

... California, Davis, NEAT ORU, One Shields Ave. Davis, CA 95616. Instrument: Alexsys 1000 Calorimeter... where such solvents are molten. Conventional differential scanning calorimeters, made by other companies... sensitive detector that is essential for solution calorimetry. Justification for Duty-Free Entry: There are...

In Situ Stability of Substrate-Associated Cellulases Studied by DSC

DEFF Research Database (Denmark)

Borch, Kim; Cruys-Bagger, Nicolaj; Badino, Silke Flindt

2014-01-01

This work shows that differential scanning calorimetry (DSC) can be used to monitor the stability of substrate-adsorbed cellulases during long-term hydrolysis of insoluble cellulose. Thermal transitions of adsorbed enzyme were measured regularly in subsets of a progressing hydrolysis, and the size...

Miscibility and specific interactions in blends of poly(n-vinyl-2-pyrrolidone) and acid functional polyester resins.

NARCIS (Netherlands)

Senatore, D.; Berix, M.J.A.; Laven, J.; Benthem, van R.A.T.M.; With, de G.; Mezari, B.; Magusin, P.C.M.M.

2008-01-01

Miscibility and intermol. interactions of novel blends of poly(N-vinyl-2-pyrrolidone) (PVP) and acid functional polyester resins (APE) were studied by use of Differential Scanning Calorimetry (DSC), Attenuated Total Reflectance Fourier Transform IR (ATR-FTIR), Cross-Polarization Magic Angle Spinning

In-vitro Characterization of Optimized Multi-Unit Dosage Forms of ...

African Journals Online (AJOL)

The optimized formulation was characterized with Differential Scanning Calorimetry and Fourier-Transform Infrared Spectroscopy. Results showed that the optimized MU tablets gave dissolution profile that was comparable with that of the designed model. The following were the dissolution parameters of the optimized MU ...

Using IR spectroscopy and multivariate curve resolution to elucidate mechanism of heat-induced decomposition of an organic complex

DEFF Research Database (Denmark)

Karpushkin, Evgeny; Gvozdik, Nataliya; Kucheryavskiy, Sergey V.

the opportunity to carry out simultaneous thermogravimetry/differential scanning calorimetry analysis and IR/Raman/mass spectrometry investigation of the evolving gaseous products. However, elucidation of the mechanism of the reactions occurring upon heat- ing is not completely straightforward, due to a number...

Resonance – Journal of Science Education | Indian Academy of ...

Indian Academy of Sciences (India)

Home; Journals; Resonance – Journal of Science Education; Volume 14; Issue 8. Differential Scanning Calorimetry: Fundamental Overview. Kevin Lukas Peter K LeMaire. Classroom Volume 14 Issue 8 August 2009 pp 807-817. Fulltext. Click here to view fulltext PDF. Permanent link:

Morphology in binary blends of poly(vinyl methyl ether) and epsilon-caprolactone-trimethylene carbonate diblock copolymer

NARCIS (Netherlands)

Luyten, MC; Bogels, EJF; vanEkenstein, GORA; tenBrinke, G; Bras, W; Komanschek, BE; Ryan, AJ

The morphology of symmetric diblock copolymer of epsilon-caprolactone (PCL) and trimethylene carbonate (PTMC), in blends with poly(vinyl methyl ether) (PVME) is investigated with (modulated) differential scanning calorimetry (d.s.c.), time resolved small angle (SAXS) and wide angle (WAXS) X-ray

Dicyclomine-loaded Eudragit®-based Microsponge with Potential ...

African Journals Online (AJOL)

Methods: Dicyclomine-loaded, Eudragit-based microsponges were prepared using a quasi-emulsion solvent diffusion method. The compatibility of the drug with formulation components was established by differential scanning calorimetry (DSC) and Fourier transform infra-red (FTIR). Process parameters were modulated to ...

Preparation, Characterization and Antibacterial Properties of Silver ...

African Journals Online (AJOL)

electron microscopy (SEM), differential scanning calorimetry (DSC), dynamic light scattering (DLS) and laser Doppler electrophoresis (LDE). The antibacterial ... silver nanoparticles. The size of the nanoparticles can be modulated by varying both chitosan MW and process conditions such as temperature and stirring speed.

Morphology in binary blends of poly(vinyl methyl ether) and ε-caprolactone-trimethylene carbonate diblock copolymer

NARCIS (Netherlands)

Luyten, M.C.; Bögels, E.J.F.; Alberda van Ekenstein, G.O.R.; Brinke, G. ten; Bras, W.; Komanschek, B.E.; Ryan, A.J.

1997-01-01

The morphology of symmetric diblock copolymer of ε-caprolactone (PCL) and trimethylene carbonate (PTMC), in blends with poly(vinyl methyl ether) (PVME) is investigated with (modulated) differential scanning calorimetry (d.s.c.), time resolved small angle (SAXS) and wide angle (WAXS) X-ray

Fulltext PDF

Indian Academy of Sciences (India)

Admin

(See article on p.782). T Ramakrishnan. (1922–2008). ( Illustration: Subhankar Biswas ). Front Cover. Back Cover. 737. Information and Announcements. Classics. The Control of. Tuberculosis: A. Continuous Game of. Snakes and Ladders. T Ramakrishnan and. P Chandrasekhar. Differential Scanning. Calorimetry: Funda-.

Khảo sát sự tạo mixel của một số Copolyme Pluronic

DEFF Research Database (Denmark)

Hùng, Nguyễn Quốc; Hvidt, Søren; Batsberg, Walther

2009-01-01

The micellization of several Pluronics (PEO-PPO-PEO triblock copolymers) was investigated by Differential Scanning Calorimetry (DSC). These copolymers were also characterized and purified by liquid chromatography. The PEO/PPO compositions of Pluronics were determined by 1H-NMR. The thermograms from...

Preparation of Tetramethylguanidine-Functionalized Mesoporous ...

African Journals Online (AJOL)

The catalyst was characterized by various techniques including Diffuse Reflectance FTIR, 13C NMR, elemental analysis and simultaneous thermogravimetric and differential scanning calorimetry analyses. It was then screened in the epoxidation of electron deficient alkenes. The results obtained show that indeed the ...

Functional eladic containing triglycerides: Synthesis, physical properties, and solution behavior

Science.gov (United States)

The enthalpy of fusion (Hf) for a number of symmetrical and asymmetrical triacylgylcerides as mixtures in soybean oil (TAGs) were determined by melting point data (MPD), differential scanning calorimetry (DSC), and effective carbon numbers (ECN). Pure triacylgylcerides were mixed with soybean oil an...

Solid-state interactions between trimethoprim and parabens

DEFF Research Database (Denmark)

Pedersen, S.; Kristensen, H. G.; Cornett, Claus

1994-01-01

by differential scanning calorimetry, X-ray powder diffraction, Fourier transform infrared spectroscopy, and solid-state C-13-NMR. Interactions between trimethoprim and 4-hydroxybenzoic acid and its ethyl,propyl and butyl esters were not observed. The nature of the trimethoprim and methyl parahydroxybenzoate...

An Integrated Approach to Thermal Analysis of Pharmaceutical Solids

Science.gov (United States)

Riley, Shelley R. Rabel

2015-01-01

A three-tiered experiment for undergraduate Instrumental Analysis students is presented in which students characterize the solid-state thermal behavior of an active pharmaceutical ingredient (acetaminophen) and excipient (a-lactose hydrate) using differential scanning calorimetry, thermogravimetric analysis, and thermal microscopy. Students are…

Lindane Suppresses the Lipid-bilayer Permeability in Main Transition Region

DEFF Research Database (Denmark)

Sabra, Mads Christian; Jørgensen, Kent; Mouritsen, Ole G.

1996-01-01

The effects of a small molecule, the insecticide lindane, on unilamellar DMPC bilayers in the phase transition region, have been studied by means of differential scanning calorimetry and fluorescence spectroscopy. The calorimetric data show that increasing concentrations of lindane broaden the tr...

COPOLYMER BLENDS OF STYRENE AND ORTHO-FLUOROSTYRENE

NARCIS (Netherlands)

TENBRINKE, G; KARASZ, FE

1991-01-01

The traditional method, using differential scanning calorimetry, to study phase behaviour in blends containing styrene and fluorinated styrene is hampered by the fact that the glass transition temperatures of fluorinated polystyrenes are almost independent of the degree of fluorination. To deal with

Structural relaxation of Ni-Si-B amorphous ribbon

NARCIS (Netherlands)

Jurikova, A.; Csach, K.; Miskuf, J.; Ocelik, V.

The structural relaxation of the Ni-Si-B amorphous ribbon was studied by means of differential scanning calorimetry and thermomechanical analysis. It was shown that considerable length changes associated with reversible structural relaxation were revealed after a previous creep applied at higher

Internal Structure Quality Control of Solid Pharmaceuticals. A Comparative Study

Directory of Open Access Journals (Sweden)

Imre Silvia

2016-03-01

Full Text Available Objective: The aim of the study was a comparative investigation by spectral and thermal analysis in order to asses a number of characteristics of different varieties ofrawmaterials of ursodeoxycholic acid and ibuprofen. The different dissolution behavior of two ursodeoxycholic acid pharmaceutical product by crystallinity pattern was investigated. Methods: Raw materials of ursodeoxycholic acid and ibuprofen were used. IR spectroscopy, differential scanning calorimetry and X-Ray Diffraction Analysis were applied. Results: The results show no crystallinitydifferences for different batches of the tested drugs. No solid solid transition was proved during sample preparation for transmission IR analysis. Conclusions: A combination of two more affordabletests by IR spectrometry and differential scanning calorimetry lead to the same results as X-Ray diffraction analysis for crystallinity similarity assessment of the studied substances. The dissolution differences of test drugs were not related to the polymorphism of the raw materials.

High-purity Cu nanocrystal synthesis by a dynamic decomposition method

Science.gov (United States)

Jian, Xian; Cao, Yu; Chen, Guozhang; Wang, Chao; Tang, Hui; Yin, Liangjun; Luan, Chunhong; Liang, Yinglin; Jiang, Jing; Wu, Sixin; Zeng, Qing; Wang, Fei; Zhang, Chengui

2014-12-01

Cu nanocrystals are applied extensively in several fields, particularly in the microelectron, sensor, and catalysis. The catalytic behavior of Cu nanocrystals depends mainly on the structure and particle size. In this work, formation of high-purity Cu nanocrystals is studied using a common chemical vapor deposition precursor of cupric tartrate. This process is investigated through a combined experimental and computational approach. The decomposition kinetics is researched via differential scanning calorimetry and thermogravimetric analysis using Flynn-Wall-Ozawa, Kissinger, and Starink methods. The growth was found to be influenced by the factors of reaction temperature, protective gas, and time. And microstructural and thermal characterizations were performed by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and differential scanning calorimetry. Decomposition of cupric tartrate at different temperatures was simulated by density functional theory calculations under the generalized gradient approximation. High crystalline Cu nanocrystals without floccules were obtained from thermal decomposition of cupric tartrate at 271°C for 8 h under Ar. This general approach paves a way to controllable synthesis of Cu nanocrystals with high purity.

Particle flow calorimetry at the international linear collider

Indian Academy of Sciences (India)

Particle flow calorimetry at the international linear ... It is widely believed that the most promising strategy for achieving a jet ... this level of performance for two main reasons. Firstly ... (i) Tracking: For the studies presented in this paper, the track pattern ... that particles propagating outward from the interaction region will cross ...

Hadronic shower development in iron-scintillator tile calorimetry

Czech Academy of Sciences Publication Activity Database

Amaral, P.; Amorim, A.; Anderson, K.; Lokajíček, Miloš; Němeček, Stanislav

2000-01-01

Roč. 443, - (2000), s. 51-70 ISSN 0168-9002 R&D Projects: GA MPO RP-4210/69 Institutional research plan: CEZ:AV0Z1010920 Keywords : ATLAS Iron-Scintillator * hadron calorimeter * shower parametrisation * calorimetry * computer data analysis Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 0.964, year: 2000

Optimization of crystals for applications in dual-readout calorimetry

Czech Academy of Sciences Publication Activity Database

Akchurin, N.; Bedeschi, F.; Cardini, A.; Carosi, R.; Ciapetti, G.; Fasoli, M.; Ferrari, R.; Franchino, S.; Fraternali, M.; Gaudio, G.; Hauptman, J.; Incagli, M.; Lacava, F.; La Rotonda, L.; Lee, S.; Livan, M.; Meoni, E.; Nikl, Martin; Pinci, D.; Policicchio, A.; Popescu, S.; Scuri, F.; Sill, A.; Susinno, G.; Vandelli, W.; Vedda, A.; Venturelli, T.; Voena, C.; Volobouev, I.; Wigmans, R.

2010-01-01

Roč. 621, 1-3 (2010), 212-221 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10100521 Keywords : calorimetry * Cherenkov light * High-Z scintillating crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.142, year: 2010

Optical fibre temperature sensor technology and potential application in absorbed dose calorimetry

International Nuclear Information System (INIS)

Allen, P.D.; Hargrave, N.J.

1992-09-01

Optical fibre based sensors are proposed as a potential alternative to the thermistors traditionally used as temperature sensors in absorbed dose calorimetry. The development of optical fibre temperature sensor technology over the last ten years is reviewed. The potential resolution of various optical techniques is assessed with particular reference to the requirements of absorbed dose calorimetry. Attention is drawn to other issues which would require investigation before the development of practical optical fibre sensors for this purpose could occur. 192 refs., 5 tabs., 4 figs

Comparison of thallium-201, Tc-99m MIBI and I-131 scan in the follow-up assessment after I-131 ablative therapy in differentiated thyroid cancer

International Nuclear Information System (INIS)

Kwon, Jae Sung; Lee, Sung Keun; Kim, Doe Min; Park, Sae Jong; Jang, Kyong Sun; Kim, Eun Sil; Kim, Chong Soon

1999-01-01

We conducted a comparative study to evaluate the diagnostic values of Tl-201, Tc-99m MIBI and I-131 scans in the follow-up assessment after ablative I-131 therapy in differentiated thyroid cancer. The study population consisted of 20 patients who underwent surgical removal of thyroid cancer and ablative radioactive iodine therapy, and followed by one or more times of I-131 retreatment (33 cases). In all patients, Tl-201, Tc-99m MIBI, diagnostic and therapeutic I-131 scans were performed and the results were analyzed retrospectively. Also serum thyroglobulin levels were measured in all patients. The final diagnosis of recurrent or metastatic thyroid cancer was determined by clinical, biochemical, radiologic and/or biopsy findings. Positive rates (PR) of Tc-99m MIBI, Tl-201, diagnostic and therapeutic I-131 scans in detecting malignant thyroid tissue lesions were 70% (19/27), 54% (15/28), 35% (17/48) and 63% (30/48), respectively. The PR in the group of 20 cases (28 lesions) who underwent concomitant Tl-201 and I-131 scans were in the order of therapeutic 131 scan 71%, Tl-201 scan 54% and diagnostic I-131 scan 36%. There was no statistically significant difference between Tl-201 and diagnostic I-131 scans (p>0.05). In the group of 20 cases (27 lesions) who underwent concomitant Tc-99m MIBI and I-131 scans, the PR were in the order of Tc-99m MIBI scan 70%, I-131 therapeutic scan 52% and I-131 diagnostic scan 33%. The PR of Tc-99m MIBI was significantly higher than that of diagnostic I-131 scan (p<0.05). Tc-99m MIBI scan is superior to diagnostic I-131 scan in detecting recurrent or metastatic thyroid cancer following ablation therapy in patients with differentiated thyroid cancer. Tl-201 scan did not showed significantly higher positive rate than diagnostic I-131 scan. Instead of diagnostic I-131 scan before the I-131 retreatment, Tc-99m MIBI scan without discontinuing thyroid hormone replacement would be a prudent and effective approach in the management of these

Observations of crystallization and melting in poly(ethylene oxide)/poly(methyl methacrylate) blends by hot-stage atomic-force microscopy

NARCIS (Netherlands)

Pearce, R.; Vancso, Gyula J.

1998-01-01

The binary blend of poly(ethylene oxide)/atactic poly(methyl methacrylate) is examined using hot-stage atomic-force microscopy (AFM) in conjunction with differential scanning calorimetry and optical microscopy. It was found possible to follow in real time the melting process, which reveals itself to

Phase separation phenomena in solutions of poly(2,6-dimethyl-1,4-phenylene oxide). IV. Thermodynamic parameters for solutions in a series of homologous solvents: Toluene to hexylbenzene

NARCIS (Netherlands)

Koenhen, D.M.; Bakker, A.; Broens, L.; van den Berg, J.W.A.; Smolders, C.A.

1984-01-01

Melting-point curves for solutions of poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) in a series of homologous solvents (toluene to n-hexylbenzene) have been obtained from visual and differential scanning calorimetry measurements. The measured melting points were used to calculate thermodynamic

Characterization of an alkali-treated grass fiber by thermogravimetric and X-ray crystallographic analysis

NARCIS (Netherlands)

De, D.; De, Debapriya

2008-01-01

The thermal behavior of grass fiber was characterized by means of thermogravimetric analysis and differential scanning calorimetry analysis. The results proved that the removal of water-soluble matter improved the thermal behavior of grass fiber over that of unleached fiber, and this was further

Revised final report for tank 241-AN-101, grab samples 1AN-95-1 through 1AN-95-7. Revision 1

International Nuclear Information System (INIS)

Esch, R.A.

1996-01-01

Six supernate grab samples and one field blank were taken from tank 241-AN-101. This report documents analyses performed in support of the Safety Screening program: differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), density by specific gravity (Sp.G.), and total alpha activity (AT)

Interactions in a blend of two polymers greatly differing in glass transition temperature

Czech Academy of Sciences Publication Activity Database

Kratochvíl, Jaroslav; Šturcová, Adriana; Sikora, Antonín; Dybal, Jiří

2011-01-01

Roč. 49, č. 14 (2011), s. 1031-1040 ISSN 0887-6266 Institutional research plan: CEZ:AV0Z40500505 Keywords : differential scanning calorimetry (DSC) * fouriertransform infrared spectroscopy (FT-IR) * glass transition temperature Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.531, year: 2011

Development of Chitosan Acetate Films for Transdermal Delivery of ...

African Journals Online (AJOL)

Methods: Chitosan acetate was chemically modified with acetaldehyde and the solution was prepared with 1 % acetic acid, in which was dissolved propranolol hydrochloride, was cast as films in Petri dish and characterised by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and ...

High molecular weight poly(L-lactide) and poly(ethylene oxide) blends : Thermal characterization and physical properties

NARCIS (Netherlands)

Nijenhuis, AJ; Colstee, E; Grijpma, DW; Pennings, AJ

1996-01-01

The miscibility of high molecular weight poly(L-lactide) (PLLA) with high molecular weight poly(ethylene oxide) (PEG) was studied by differential scanning calorimetry. Ail blends containing up to 50 weight% PEO showed single glass transition temperatures. The PLLA and PEO melting temperatures were

Design of lipid matrix particles for fenofibrate

DEFF Research Database (Denmark)

Xia, Dengning; Cui, Fude; Gan, Yong

2014-01-01

The effect of polymorphism of glycerol monostearate (GMS) on drug incorporation and release from lipid matrix particles (LMPs) was investigated using fenofibrate as a model drug. X-ray powder diffraction and differential scanning calorimetry were used to study the polymorphism change of GMS and t...

A novel cardanol-based antioxidant and its application in vegetable oils and biodiesel

Science.gov (United States)

A novel antioxidant, epoxidized cardanol (ECD), derived from cardanol has been synthesized and characterized by FT-IR, 1H-NMR and 13C-NMR. Oxidative stability of ECD in vegetable oils and biodiesel was evaluated by the pressurized differential scanning calorimetry and Rancimat methods, respectively....

The Synthesis of Novel Enclathration Compounds : Bis(9-amino-9 ...

African Journals Online (AJOL)

The stability of the clathrate complexes has been investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Competition experiments were carried out with the compounds that successfully hosted solvent molecules in order to determine their relative affinity for these solvents. One of the ...

Physicochemical properties of nanoparticles titania from alcohol ...

African Journals Online (AJOL)

The synthesized TiO2 were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal analysis (thermogravimetric analysis, TGA, and differential scanning calorimetry, DSC), and surface area Brunauer–Emmett–Teller (BET) method. The photocatalytic activity of TiO2 nanoparticles was ...

Inclusion Mechanism and Heat Stability of the Complex of 4 ...

African Journals Online (AJOL)

The physicochemical properties of the complex were evaluated by Fourier transform infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD) while the heat stability of the complex was measured by thermogravimetric/differential scanning calorimetry (TG/DSC). Results: The stability constants of the complexes were ...

Second amorphous-to-crystalline phase transformation in Cu60Ti20Zr20 bulk metallic glass

DEFF Research Database (Denmark)

Cao, Q.P.; Li, J.F.; Zhang, P.N.

2007-01-01

The second amorphous-to-crystalline phase transformation in Cu60Ti20Zr20 bulk metallic glass was investigated by differential scanning calorimetry and x-ray diffractometry. The difference of the Gibbs free energies between the amorphous phase and the crystalline products during the transformation...

Glass transition and the rigid amorphous phase in semicrystalline blends of bacterial polyhydroxybutyrate PHB with low molecular mass atactic R,S-PHB-diol

NARCIS (Netherlands)

Hoehne, G.W.H.

2004-01-01

The glass transition and the crystallinity of blends of isotactic bacterial PHB and low molecular mass atactic R, S-PHB-diols was investigated by means of differential scanning calorimetry (DSC), temperature-modulated DSC and dielectric spectroscopy. It was found that (i) Tg of crystallized blends

Synthesis and membrane behavior of a new class of unnatural phospholipid analogs useful as phospholipase A2 degradable liposomal drug carriers

DEFF Research Database (Denmark)

Andresen, Thomas Lars; Jørgensen, Kent

2005-01-01

A new and unnatural type of lipid analogs with the phosphocholine and phosphoglycerol head groups linked to the C-2 position of the glycerol moiety have been synthesized and the thermodynamic lipid membrane behavior has been investigated using differential scanning calorimetry. From the heat capa...

Thermodynamic Impact of Abasic Sites on Simulated Translesion DNA Synthesis

Czech Academy of Sciences Publication Activity Database

Malina, Jaroslav; Brabec, Viktor

2014-01-01

Roč. 20, č. 25 (2014), s. 7566-7570 ISSN 0947-6539 R&D Projects: GA ČR(CZ) GAP205/11/0856 Institutional support: RVO:68081707 Keywords : abasic sites * differential scanning calorimetry * DNA Subject RIV: BO - Biophysics Impact factor: 5.731, year: 2014

Evaluation of Poly(2-Ethyl-2-Oxazoline) Containing Copolymer Networks of Varied Composition as Sustained Metoprolol Tartrate Delivery Systems

OpenAIRE

Kostova, Bistra; Ivanova, Sijka; Balashev, Konstantin; Rachev, Dimitar; Christova, Darinka

2014-01-01

Segmented copolymer networks (SCN) based on poly(2-ethyl-2-oxazoline) and containing 2-hydroxyethyl methacrylate, 2-hydroxypropyl acrylate, and/or methyl methacrylate segments have been evaluated as potential sustained release systems of the water soluble cardioselective β-blocker metoprolol tartrate. The structure and properties of the drug carriers were investigated by differential scanning calorimetry, attenuated total reflectance Fourier transform infrared spectroscopy, scanning electron ...

Slit-scanning differential phase-contrast mammography: first experimental results

Science.gov (United States)

Roessl, Ewald; Daerr, Heiner; Koehler, Thomas; Martens, Gerhard; van Stevendaal, Udo

2014-03-01

The demands for a large field-of-view (FOV) and the stringent requirements for a stable acquisition geometry rank among the major obstacles for the translation of grating-based, differential phase-contrast techniques from the laboratory to clinical applications. While for state-of-the-art Full-Field-Digital Mammography (FFDM) FOVs of 24 cm x 30 cm are common practice, the specifications for mechanical stability are naturally derived from the detector pixel size which ranges between 50 and 100 μm. However, in grating-based, phasecontrast imaging, the relative placement of the gratings in the interferometer must be guaranteed to within micro-meter precision. In this work we report on first experimental results on a phase-contrast x-ray imaging system based on the Philips MicroDose L30 mammography unit. With the proposed approach we achieve a FOV of about 65 mm x 175 mm by the use of the slit-scanning technique. The demand for mechanical stability on a micrometer scale was relaxed by the specific interferometer design, i.e., a rigid, actuator-free mount of the phase-grating G1 with respect to the analyzer-grating G2 onto a common steel frame. The image acquisition and formation processes are described and first phase-contrast images of a test object are presented. A brief discussion of the shortcomings of the current approach is given, including the level of remaining image artifacts and the relatively inefficient usage of the total available x-ray source output.

Calorimetry exchange program annual data report for 1992

International Nuclear Information System (INIS)

Barnett, T.M.

1992-01-01

The goals of the Calorimetry Sample Exchange Program are: discuss measurement differences; review and improve analytical measurements and methods; discuss new measurement capabilities; provide data to DOE on measurement capabilities to evaluate shipper-receiver differences; provide characterized or standard materials as necessary for exchange participants; and provide a measurement control program for plutonium analysis. A sample of PuO 2 powder is available at each participating site for NDA measurement, including either or both calorimetry and high-resolution gamma-ray spectroscopy, the elements which are typically combined to provide a calorimetric assay of plutonium. The facilities measure the sample as frequently and to the level of precision which they desire, and then submit the data to the Exchange for analysis. The data report includes summary tables for each measurement and charts showing the performance of each laboratory. Comparisons are made to the accepted values for the exchange sample and to data previously reported by that laboratory. This information is presented, in the form of quarterly and annual reports, intended for use by Exchange participants in measurement control programs, or to indicate when bias corrections may be appropriate. No attempt, however, has been made to standardize methods or frequency of data collection, calibration, or operating procedures. Direct comparisons between laboratories may, therefore, be misleading since data have not been collected to the same precision or for the same time periods. A meeting of the participants of the Calorimetry Exchange is held annually at EG ampersand G Mound Applied Technologies. The purposes of this meeting are to discuss measurement differences, problems, and new measurement capabilities, and to determine the additional activities needed to fulfill the goals of the Exchange. This document provides data for 1992

Enhancing the early differential diagnosis of plateau iris and pupillary block using a-scan ultrasonography.

Directory of Open Access Journals (Sweden)

Yu-Yen Chen

Full Text Available To distinguish the frequently misdiagnosed plateau iris eyes from pupillary block group and normal group, we compared the ocular biometrical parameters of them by A-scan ultrasongraphy.In total, we retrospectively reviewed general characteristics and ocular findings including ocular biometric measurements of 71 normal, 39 plateau iris, and 83 pupillary block eyes.The normal controls, plateau iris group and pupillary block group were significantly different in age, but not in gender. The anterior chamber depth tended to decrease and the lens thickness tended to increase from normal to plateau iris to pupillary block eyes. Compared to those of plateau iris group, the pupillary block group had significantly shallower anterior chamber depth (2.90mm vs. 2.33mm; p<0.001, thicker lens (4.77mm vs. 5.11mm; p<0.001, shorter axial length (23.16mm vs. 22.63mm; p<0.001, smaller relative lens position (2.28 vs. 2.16; p<0.001 and larger lens/axial length factor (2.06 vs. 2.26; p<0.001. However, when comparing plateau iris and normal eyes, only axial length and lens/axial length factor were significantly different (23.16 vs. 23.54; p<0.05 and 2.06 vs. 1.96; p<0.05.Measured by A-scan ultrasonography, the ocular biometrics of plateau iris were significantly different from those of pupillary block eyes. However, our A-scan ultrasongraphy generally found no significant biometric differences between plateau iris and normal eyes. These findings suggest that while A-scan ultrasonography might be used as a practical tool for differentiating plateau iris and papillary block eyes, a more meticulous gonioscopy and other assessments may be necessary to distinguish plateau iris from normal eyes.

Determination of the oxidizing property: proposal of an alternative method based on differential scanning calorimetry

International Nuclear Information System (INIS)

Gigante, L.; Dellavedova, M.; Pasturenzi, C.; Lunghi, A.; Mattarella, M.; Cardillo, P.

2008-01-01

Determination of chemical-physical and hazardous properties of substances is a very important matter in the chemical industry, considering the growing attention of public opinion regarding safety and eco-compatibility aspects of products. In the present work, attention was focused on characterization of oxidizing properties. In case of solid compounds, the current method (Dir 84/449/CEE 6) compares the maximum combustion rate of the examined substance to the maximum combustion rate of a reference mixture. This method shows a lot of disvantages and does not provide a quantitative result. In the following work an alternative method, based on DSC measurements, is proposed for the determination of oxidizing properties. [it

Determination of melting point of vegetable oils and fats by differential scanning calorimetry (DSC technique.

Directory of Open Access Journals (Sweden)

Nassu, Renata Tieko

1999-02-01

Full Text Available Melting point of fats is used to characterize oils and fats and is related to their physical properties, such as hardness and thermal behaviour. The present work shows the utilization of DSC technique on the determination of melting point of fats. In a comparison with softening point (AOCS method Cc 3-25, DSC values were higher than those obtained by AOCS method. It has occurred due to the fact that values obtained by DSC technique were taken when the fat had melted completely. DSC was also useful for determining melting point of liquid oils, such as soybean and cottonseed ones.

El punto de fusión de grasas es usado para caracterizar aceites y grasas, y está relacionado con sus propiedades físicas, tales como dureza y comportamiento térmico. El presente trabajo muestra la utilización de la técnica de Calorimetría Diferencial de Barrido (DSC en la determinación del punto de fusión de grasas. En comparación con el punto de ablandamiento (AOCS método Cc 3-25, los valores de DSC fueron más altos que los obtenidos por los métodos de AOCS. Esto ha ocurrido debido al hecho que los valores obtenidos por la técnica de DSC fueron tomados cuando la grasa había fundido completamente. DSC fue también útil para determinar puntos de fusión de aceites líquidos, tales como los de soya y algodón.

The application of differential scanning calorimetry and ice nucleation spectrometry to ecophysiological studies of algae

Czech Academy of Sciences Publication Activity Database

Worland, M. R.; Lukešová, Alena

2001-01-01

Roč. 123, - (2001), s. 571-583 ISSN 1438-9134 Institutional research plan: CEZ:AV0Z6066911 Keywords : Antarctic * cold tolerance * terrestrial algae Subject RIV: EH - Ecology, Behaviour Impact factor: 0.488, year: 2000

Crystallization Kinetics of Nanocrystalline Materials by Combined X-ray Diffraction and Differential Scanning Calorimetry Experiments

Czech Academy of Sciences Publication Activity Database

Gil-González, E.; Perejón, A.; Sánchez-Jiménez, P. E.; Medina-Carrasco, S.; Kupčík, Jaroslav; Šubrt, Jan; Criado, J. M.; Pérez-Maqueda, L. A.

2018-01-01

Roč. 18, č. 5 (2018), s. 3107-3116 ISSN 1528-7483 Institutional support: RVO:61388980 Keywords : nanocrysalline alloys * combined X ray diffraction * crystallization kinetics Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 4.055, year: 2016

Differential scanning calorimetry as a screening technique in compatibility studies of acyclovir extended release formulations

International Nuclear Information System (INIS)

Barboza, Fernanda M.; Vecchia, Debora D.; Tagliari, Monika P.; Ferreira, Andrea Granada; Silva, Marcos A.S.; Stulzer, Hellen K.

2009-01-01

Acyclovir (ACV) has been investigated during the past years, mainly due to its antiviral activity. Assessment of possible incompatibility between an active component and different excipients along with the evaluation of thermal stability are crucial parts of a normal study prior to the final formulation setting of a medicine. Thermal analysis studies were used as important and complementary tools during pre-formulation to determine the compatibility of drug excipients with the purpose of developing an acyclovir extended release formulation. Fourier transform infrared spectroscopy and X-ray powder diffraction analyses were also realized. The results showed that ACV only exhibited interaction which could influence the stability of the product in the binary mixtures of ACV/magnesium stearate. (author)

Differential scanning calorimetry studies of Se85Te15–xPbx (x = 4, 6 ...

Indian Academy of Sciences (India)

Unknown

2000-06-14

Jun 14, 2000 ... Matusita's equation while 102–139 kJ/mol by modified Kissinger's equation. The Hruby number ... to n-type in Ge–Se–Pb system (Toghe et al 1987) is observed in spite ... determine the activation energy of structural relaxation.

Thermodynamics of translesion synthesis across a major DNA adduct of antitumor oxaliplatin: Differential scanning calorimetric study

Czech Academy of Sciences Publication Activity Database

Florian, Jakub; Brabec, Viktor

2012-01-01

Roč. 18, č. 6 (2012), s. 1634-1639 ISSN 0947-6539 R&D Projects: GA ČR(CZ) GD301/09/H004; GA ČR(CZ) GAP301/10/0598 Institutional research plan: CEZ:AV0Z50040702 Keywords : antitumor platinum * DNA * calorimetry Subject RIV: BO - Biophysics Impact factor: 5.831, year: 2012

Low Energy Scanned Electron-Beam Dose Distribution in Thin Layers

DEFF Research Database (Denmark)

McLaughlin, W. L.; Hjortenberg, P. E.; Pedersen, Walther Batsberg

1975-01-01

Thin radiochromic dye film dosimeters, calibrated by means of calorimetry, make possible the determination of absorbed-dose distributions due to low-energy scanned electron beam penetrations in moderately thin coatings and laminar media. For electrons of a few hundred keV, calibrated dosimeters...... of about 30–60 μm thickness may be used in stacks or interleaved between layers of materials of interest and supply a sufficient number of experimental data points throughout the depth of penetration of electrons to provide a depth-dose curve. Depth doses may be resolved in various polymer layers...... on different backings (wood, aluminum, and iron) for scanned electron beams (Emax = 400 keV) having a broad energy spectrum and diffuse incidence, such as those used in radiation curing of coatings, textiles, plastics, etc. Theoretical calculations of such distributions of energy depositions are relatively...

Integration and global analysis of isothermal titration calorimetry data for studying macromolecular interactions.

Science.gov (United States)

Brautigam, Chad A; Zhao, Huaying; Vargas, Carolyn; Keller, Sandro; Schuck, Peter

2016-05-01

Isothermal titration calorimetry (ITC) is a powerful and widely used method to measure the energetics of macromolecular interactions by recording a thermogram of differential heating power during a titration. However, traditional ITC analysis is limited by stochastic thermogram noise and by the limited information content of a single titration experiment. Here we present a protocol for bias-free thermogram integration based on automated shape analysis of the injection peaks, followed by combination of isotherms from different calorimetric titration experiments into a global analysis, statistical analysis of binding parameters and graphical presentation of the results. This is performed using the integrated public-domain software packages NITPIC, SEDPHAT and GUSSI. The recently developed low-noise thermogram integration approach and global analysis allow for more precise parameter estimates and more reliable quantification of multisite and multicomponent cooperative and competitive interactions. Titration experiments typically take 1-2.5 h each, and global analysis usually takes 10-20 min.

Clinical importance of technetium-99m-methoxyisobutylisonitrile (MIBI) scintigraphy in differentiated thyroid carcinoma patients with elevated thyroglobulin levels and negative I-131 scanning results

International Nuclear Information System (INIS)

Kuecuek, N.O.; Kulak, H.A.; Aras, G.

2006-01-01

The aim of this study was to evaluate the potential contribution of Tc-99m-MIBI scintigraphy to the follow-up of patients with differentiated thyroid carcinoma, who had elevated Tg levels and negative I-131 whole-body scan (WBS) results. In this retrospective study, we evaluated 28 patients with differentiated thyroid carcinoma, who had total or near total thyroidectomy followed by an ablative dose of I-131 at various time intervals (15 women, 13 men; mean age 43±17 years). All patients were treated with T4 suppression. After a mean follow-up period of 6.1 years (range 3-15) all patients were determined to have a high serum Tg concentrations (>2 ng/ml) and previous negative I-131 WBS results. All patients were examined for metastatic sites using Tc-99m-MIBI scan. Scans were visually evaluated for detecting lymph node metastases and/or local recurrence, lung metastases and skeletal metastases. Tc-99m-MIBI scan demonstrated lesions in 23 patients (83.3%). In five patients with negative Tc-99m-MIBI scan findings (FN results): Chest CT showed small-sized mediastinal LN metastases in 2 patients and lung metastases in another 2 patients (<1 cm); Neck CT showed small-sized cervical LN involvement in 1 patient. The sensitivity of detection for neck was 94.4%, for lung 63.6%, and for bone lesions 100%. For all scan sites taken together, the sensitivity of disease detection was 83.3%, the specificity was 50%, positive predictive value (PPV) was 96.2%, and finally negative predictive value (NPV) was 16.7%. We concluded that Tc-99m-MIBI scan should be considered as a supplementary scintigraphic method for the follow-up of patients with high serum Tg levels and negative I-131 WBS results, and it can help clinicians in making the decision to treat these patients. (author)

Martensitic nature of δ → γ allotropic transformation in plutonium

International Nuclear Information System (INIS)

Lopez, P.C.; Cost, J.R.; Axler, K.M.

1996-09-01

Isothermal and isoplethal studies using differential scanning calorimetry have been conducted to characterize the allotropic transformations of plutonium. The δ-γ transformation (upon cooling) was observed to have a classic martensitic nature. The work described herein is the first quantitative study of this phenomena in plutonium

Thermal and mechanical properties of multiple-component aliphatic degradable polyurethanes

Czech Academy of Sciences Publication Activity Database

Poreba, Rafal; Kredatusová, Jana; Hodan, Jiří; Serkis, Magdalena; Špírková, Milena

2015-01-01

Roč. 132, č. 16 (2015), 41872_1-41872_12 ISSN 0021-8995 R&D Projects: GA ČR(CZ) GA13-06700S Institutional support: RVO:61389013 Keywords : differential scanning calorimetry * mechanical properties * polyurethanes Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.866, year: 2015

Crystallization and melting behavior of multi-walled carbon nanotube-reinforced nylon-6 composites

NARCIS (Netherlands)

Phang, In Yee; Ma, Jianhua; Shen, Lu; Liu, Tianxi; Zhang, Wei-De

2006-01-01

The crystallization and melting behavior of neat nylon-6 (PA6) and multi-walled carbon nanotubes (MWNTs)/PA6 composites prepared by simple melt-compounding was comparatively studied. Differential scanning calorimetry (DSC) results show two crystallization exotherms (TCC, 1 and TCC, 2) for PA6/MWNTs

Synthesis of epoxidized cardanol and its antioxidative properties for vegetable oils and biodiesel

Science.gov (United States)

A novel antioxidant epoxidized cardanol (ECD), derived from cardanol, was synthesized and characterized by FT-IR, 1H-NMR and 13C-NMR. Oxidative stability of ECD used in vegetable oils and biodiesel was evaluated by pressurized differential scanning calorimetry (PDSC) and the Rancimat method, respect...

Preparation and characterization of PAN–KI complexed gel polymer

Indian Academy of Sciences (India)

The structural, miscibility and the chemical rapport between PAN and KI are investigated using X-ray diffraction, Fourier transform infrared spectroscopy and differential scanning calorimetry methods. The conductivity is enhanced with the increase in KI concentration and temperature. The maximum conductivity at 30 ∘ C is ...

Synthesis of lithium-manganese-oxide spinels: A study by thermal analysis

CSIR Research Space (South Africa)

Thackeray, MM

1994-12-01

Full Text Available The synthesis of lithium-manganese-oxide spinels by reaction of Li2CO3 and MnCO3 in air and under nitrogen to T(max) = 600°C has been investigated by thermogravimetric analysis and differential scanning calorimetry. When the reaction is conducted...

Thermochemical studies of 4-tert-butylbiphenyl and 4,4'-di-tert-butylbiphenyl

International Nuclear Information System (INIS)

Melkhanova, Svetlana V.; Pimenova, Svetlana M.; Chelovskaya, Nelly V.; Miroshnichenko, Eugenii A.; Pashchenko, Larisa L.; Nesterov, Igor A.; Naumkin, P.V.

2009-01-01

The standard massic energies of compounds of 4-tert-butylbiphenyl and 4,4'-di-tert-butylbiphenyl were measured at T = 298.15 K by static-bomb combustion calorimetry. The standard enthalpies of vaporization, fusion and sublimation were measured in a Calvet microcalorimeter, or by differential scanning calorimetry. The standard molar enthalpies of formation in the condensed and gaseous states were obtained from these data. The tert-butyl group increments for the substitution of one hydrogen atom in a position '4' in biphenyl molecule were calculated

Peningkatan Laju Disolusi Dispersi Padat Amorf Genistein dengan PVP K-30

Directory of Open Access Journals (Sweden)

Erizal Zaini

2017-12-01

Full Text Available Amorphous solid dispersions of a poorly water-soluble drug genistein in PVP K-30 were prepared by solvent co-evaporation technique using organic solvent methanol. Solid dispersions system was prepared with several variations of drug to polymer 2:1, 1:1 dan 1:2 w/w. Solid state properties of solid dispersion system were evaluated by powder X-ray diffraction, Fourier transform infrared spectroscopy, and differential scanning calorimetry, and microscopic SEM. Dissolution rate profile were conducted in distilled water medium by using dissolution tester apparatus type II USP. Base on X-ray diffractometry analysis, differential scanning calorimetry and microscopic SEM, crystalline phase of genistein decreased in crystallinity index and formation of amophous state. Dissolution rate profile showed that genistein in amorphous solid dispersion had a faster dissolution rate in comparison to intact genistein. This study proved that preparation of solid dispersion of genistein in PVP K-30 is an effective approach to improve dissolution rate of genistein.

Tritium inventory measurements by 'in-bed' gas flowing calorimetry

International Nuclear Information System (INIS)

Hayashi, T.; Suzuki, T.; Yamada, M.; Okuno, K.

1996-01-01

In order to establish the 'in-bed' tritium accounting technology for the ITER scale tritium storage system, a gas flowing calorimetry has been studied using a scaled ZrCo bed (25 g tritium capacity). The basic calorimetric characteristics, steady state temperature raise of He gas stream flowing through a secondary coil line fixed in the ZrCo tritide, was measured and correlated with the stored tritium inventory. The results shows that about 4 degrees raise of He stream temperature can be detected for each gram of tritium storage. The sensitivity of this calorimetry is about 0.05 g of tritium, calculated by 0.2 degrees of temperature sensor error. The accuracy is better than 0.25 g of tritium on 25 g storage, evaluated by 2 times of standard deviation from the repeat measurements. This accuracy of < 1% on full storage capacity is satisfied the target accountability to measure ± 1 gram of tritium on 100 g storage for ITER. 13 refs., 7 figs

Inherent limitations of fixed time servo-controlled radiometric calorimetry

International Nuclear Information System (INIS)

Wetzel, J.R.; Duff, M.F.; Lemming, J.F.

1987-01-01

There has been some interest in low precision, short run time calorimetry measurements. This type of calorimetry measurement has been proposed for use when high precision measurements are not required, for example, to screen scrap containers to determine if there is enough material to be measured more accurately of for confirmatory measurements that only require low precision results. The equipment needed to make these measurements is a servo-controlled calorimeter with a sample preequilibration bath. The preequilibration bath temperature is set to the internal temperature of the calorimeter running at a fixed servo-controlled wattage level. The sample power value is determined at a fixed time form the sample loading into the calorimeter. There are some limitations and areas of uncertainties in the use of data obtained by this method. Data collected under controlled conditions demonstrate the limitations. Sample packaging, preequilibration time, and item wattage were chosen as the variables most likely to be encountered in a plant environment

Inherent limitations of fixed-time, servo-controlled radiometric calorimetry

International Nuclear Information System (INIS)

Wetzel, J.R.; Lemming, J.F.; Duff, M.F.

1987-01-01

Interest has been shown in using fixed-time, servo-controlled calorimetry to shorten the measurement times for certain samples that require low precision values (3 to 5%). This type of calorimeter measurement could be particularly useful for screening scrap samples to determine whether there is a need for a more accurate measurement or for certain confirmatory measurements for which low precision numbers are sufficient. The equipment required for this type of measurement is a servo-controlled calorimeter and a preconditioning unit. Samples to be measured are placed in the preconditioning unit, which is maintained at the internal temperature of the calorimeter. The power value for the sample is determined at a fixed time after loading into the calorimeter, for example, 30 min. When a calorimeter is operated using a fixed cutoff time, there are additional sources of uncertainty that need to be considered. The major factors affecting the uncertainty of the calorimetry power values are discussed. 2 refs., 4 figs

In situ visualization of Ni-Nb bulk metallic glasses phase transition

OpenAIRE

Oreshkin, A. I.; Mantsevich, V. N.; Savinov, S. V.; Oreshkin, S. I.; Panov, V. I.; Yavari, A. R.; Miracle, D. B.; Louzguine-Luzgin, D. V.

2013-01-01

We report the results of the Ni-based bulk metallic glass structural evolution and crystallization behavior in situ investigation. The X-ray diffraction (XRD), transmission electron microscopy (TEM), nano-beam diffraction (NBD), differential scanning calorimetry (DSC), radial distribution function (RDF) and scanning probe microscopy/spectroscopy (STM/STS) techniques were applied to analyze the structure and electronic properties of Ni63.5Nb36.5 glasses before and after crystallization. It was...

Neck and whole-body scanning with 5-mCi dose of (123)I as diagnostic tracer in patients with well-differentiated thyroid cancer.

Science.gov (United States)

Gulzar, Z; Jana, S; Young, I; Bukberg, P; Yen, V; Naddaf, S; Abdel-Dayem, H M

2001-01-01

To determine whether a 5-mCi dose of 123I can be used as an effective radiotracer for assessing the presence of remnant thyroid tissue and for searching for metastatic lesions in patients with well-differentiated thyroid cancer as well as to attempt to ascertain whether a scan performed only at 4 hours is sufficient for accurate diagnosis and might replace the conventional protocol of scanning at both 4 hours and 24 hours. We prospectively studied 27 patients who had undergone near-total thyroidectomy and had a documented diagnosis of well-differentiated thyroid carcinoma. Patients underwent scanning after receiving a 5-mCi dose of 123I, at a time when they had discontinued thyroid replacement therapy and had a thyrotropin level in excess of 30 mIU/mL. Whole-body images at 4 hours and 24 hours were obtained and were compared with posttherapy scans obtained 5 to 7 days after administration of 131I. Scans were interpreted by two board-certified nuclear medicine physicians. Of the 27 patients, 2 (7.4%) showed discordance between the 123I scan performed at 24 hours and the posttherapy 131I scan. When 4-hour images after administration of 123I were compared with the posttherapy 131I scans, a discordance rate of 14.8% (4 of 27 patients) was noted. In addition, two of these four patients showed lesions on the 24-hour images that were not seen on the 4-hour images (one with new lung metastatic involvement and the other with a local recurrence in the lower neck area). The prognosis and treatment of these two patients were substantially changed by the result of the 24-hour images. On comparison of scans obtained after administration of a 5-mCi dose of 123I with those obtained after 131I therapy, we conclude that 5 mCi of 123I produces images that have excellent quality and resolution and also compare favorably with those obtained after 131I therapy. Furthermore, a decrease in the dose of 123I from 10 mCi to 5 mCi lowered the cost of the study without compromising the

Preparation of continuous alumina gel fibres by aqueous sol–gel ...

Indian Academy of Sciences (India)

Abstract. Continuous alumina gel fibres were prepared by sol–gel method. The spinning sol was prepared by mixing aluminum nitrate, lactic acid and polyvinylpyrrolidone with a mass ratio of 10:3:1·5. Thermogravimetry– differential scanning calorimetry (TG–DSC), Fourier transform infrared (FTIR) spectra, X-ray diffraction ...

Preparation and Characterization of Nitrendipine-loaded Eudragit ...

African Journals Online (AJOL)

The results of FTIR spectrometry, differential scanning calorimetry and x-ray diffractometry indicated the stable character of nitrendipne in drug-loaded microspheres and also revealed absence of drug-polymer interaction. The drug release profiles of the microspheres at pH 1.2 showed poor drug release characteristics while ...

Modulation of gephyrin-glycine receptor affinity by multivalency

DEFF Research Database (Denmark)

Maric, Hans-Michael; Kasaragod, Vikram Babu; Schindelin, Hermann

2014-01-01

. A 2 Å crystal structure of the C-terminal domain of gephyrin (GephE) in complex with a 15-residue peptide derived from the GlyR β-subunit defined the core binding site, which we targeted with the dimeric peptide. Biophysical analyses via differential scanning calorimetry (DSC), thermofluor...

Effect of Isotacticity of Linear Poly(N-isopropylacrylamide) on its ...

Indian Academy of Sciences (India)

decreased with the increase in the isotacticity of the polymer. Gelation ... microscopy (SEM), differential scanning calorimetry ... The gap between two paral- ... sidering degree of polymerization, x = 6) with benzyl ..... Apart from the blue shift, the absorbance value grad- ..... for Bethe lattice, n should have the value equal to.

Bulletin of Materials Science | Indian Academy of Sciences

Indian Academy of Sciences (India)

Blends of poly(ρ-dioxanone) (PPDO) and poly(L-lactic acid) (PLLA) in different proportions were prepared by solution co-precipitation. The nonisothermal crystallization behaviour of pure PPDO and PPDO/PLLA blends was investigated by differential scanning calorimetry. The Avrami, Ozawa and Mo models were used to ...

Changes in polymer foils used in food packaging tested by using ...

Indian Academy of Sciences (India)

This work is an experimental study of the differential scanning calorimetry characterisation of polymer materials used in food packaging materials, such as polypropylene (0.03 mm), polyethylene (0.1 and 0.03 mm), ... Faculty of Food Technology and Biotechnology, University of Zagreb, Pierottijeva 6, 10000 Zagreb, Croatia ...

Fundamentals of Melt infiltration for the Preparation of Supported Metal Catalysts.The Case of Co/SiO2 Fischer-Tropsch Synthesis

NARCIS (Netherlands)

Eggenhuisen, T.M.|info:eu-repo/dai/nl/313959498; den Breejen, J.P.|info:eu-repo/dai/nl/304837318; Verdoes, D.; de Jongh, P.E.|info:eu-repo/dai/nl/186125372; de Jong, K.P.|info:eu-repo/dai/nl/06885580X

2013-01-01

We explored melt infiltration of mesoporous silica supports to prepare supported metal catalysts with high loadings and controllable particle sizes. Melting of Co(NO3)2 ·6H2O in the presence of silica supports was studied in situ with differential scanning calorimetry. The melting point depression

Perfusion lung scanning: differentiation of primary from thromboembolic pulmonary hypertension

International Nuclear Information System (INIS)

Lisbona, R.; Kreisman, H.; Novales-Diaz, J.; Derbekyan, V.

1985-01-01

Of eight patients with pulmonary arterial hypertension, final diagnosis established by autopsy or angiography, four had primary hypertension and four hypertension from thromboembolism. The perfusion lung scan was distinctly different in the two groups. The lung scan in primary pulmonary hypertension was associated with nonsegmental, patchy defects of perfusion, while in thromboembolic hypertensives it was characterized by segmental and/or lobar defects of perfusion with or without subsegmental defects. The perfusion lung scan is a valuable, noninvasive study in the evaluation of the patient with pulmonary hypertension of undetermined cause and in the exclusion of occult large-vessel pulmonary thromboembolism

Isothermal calorimetry of enzymatic biodiesel reaction

DEFF Research Database (Denmark)

Fjerbæk Søtoft, Lene; Westh, Peter; Christensen, Knud Villy

2010-01-01

  Isothermal calorimetry ITC has been used to investigate enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by the immobilized lipase Novozym 435 at 40°C. The ITC-experiments clearly demonstrate the possibilities of investigating complex...... and composition change in the system, the heat of reaction at 40°C for the two systems has been determined to -9.8 ± 0.9 kJ/mole biodiesel formed from rapeseed oil and methanol, and - 9.3 ± 0.7 kJ/mole when rapeseed oil and ethanol is used....

Assessment of breast tumor size in electrical impedance scanning

International Nuclear Information System (INIS)

Kim, Sungwhan

2012-01-01

Electrical impedance scanning (EIS) is a newly introduced imaging technique for early breast cancer detection. In EIS, we apply a sinusoidal voltage between a hand-held electrode and a scanning probe placed on the breast skin to make current travel through the breast. We measure induced currents (Neumann data) through the scanning probe. In this paper, we investigate the frequency-dependent behavior of the induced complex potential and show how the frequency differential of the current measurement on the scanning probe reflects the contrast in complex conductivity values between surrounding and cancerous tissues. Furthermore, we develop the formula for breast tumor size using the frequency differential of the current measurement and provide its feasibility. (paper)

CMS Forward Calorimetry R&D

Energy Technology Data Exchange (ETDEWEB)

Bilki, Burak [Univ. of Iowa, Iowa City, IA (United States); Argonne National Lab. (ANL), Argonne, IL (United States)

2013-11-11

This is a technical scope of work (TSW) between the Fermi National Accelerator Laboratory (Fermilab) and the experimenters of the CMS Forward Calorimetry Taskforce (FCAL group) who have committed to participate in beam tests to be carried out during the 2013-2016 Fermilab Test Beam Facility program. The TSW is intended primarily for the purpose of recording expectations for budget estimates and work allocations for Fermilab, the funding agencies and the participating institutions. It reflects an arrangement that currently is satisfactory to the parties; however, it is recognized and anticipated that changing circumstances of the evolving research program will necessitate revisions. The parties agree to modify this scope of work to reflect such required adjustments. Actual contractual obligations will be set forth in separate documents.

Enthalpy of sublimation/vaporization of trans-cyclohexyl-1,4-diamine and cis-cyclohexyl-1,2-diamine

OpenAIRE

Tomé, Luciana I. N.; Rosado, Mário T. S.; Nunes, Sandra C. C.; Maria, Teresa M. R.; Canotilho, João; Eusébio, M. Ermelinda S.

2007-01-01

The molar enthalpy of sublimation, , of trans-cyclohexyl-1,4-diamine and the molar enthalpy of vaporization, , of cis-cyclohexyl-1,2-diamine, at the temperature 298.15 K, were determined by calorimetry. was obtained for the trans-isomer and for the cis form. The molar enthalpy of fusion of the first compound, at T = 342.1 K, was determined by differential scanning calorimetry. The molar enthalpy of vaporization of the 1,4-isomer was estimated by combining the value of the enthalpy of sublimat...

Thermochemical studies of 4-tert-butylbiphenyl and 4,4'-di-tert-butylbiphenyl

Energy Technology Data Exchange (ETDEWEB)

Melkhanova, Svetlana V. [Chemistry Department, Moscow State University, Leninskie Gory 1, Bl.3, Moscow 119992 (Russian Federation)], E-mail: melkhan@phys.chem.msu.ru; Pimenova, Svetlana M.; Chelovskaya, Nelly V. [Chemistry Department, Moscow State University, Leninskie Gory 1, Bl.3, Moscow 119992 (Russian Federation); Miroshnichenko, Eugenii A. [Institute of Chemical Physics RAS, Kosygina 4, Moscow 117977 (Russian Federation); Pashchenko, Larisa L. [Chemistry Department, Moscow State University, Leninskie Gory 1, Bl.3, Moscow 119992 (Russian Federation); Institute of Chemical Physics RAS, Kosygina 4, Moscow 117977 (Russian Federation); Nesterov, Igor A.; Naumkin, P.V. [Samara State Technical University, Galaktionovskaya 141, Samara 443010 (Russian Federation)

2009-05-15

The standard massic energies of compounds of 4-tert-butylbiphenyl and 4,4'-di-tert-butylbiphenyl were measured at T = 298.15 K by static-bomb combustion calorimetry. The standard enthalpies of vaporization, fusion and sublimation were measured in a Calvet microcalorimeter, or by differential scanning calorimetry. The standard molar enthalpies of formation in the condensed and gaseous states were obtained from these data. The tert-butyl group increments for the substitution of one hydrogen atom in a position '4' in biphenyl molecule were calculated.

A green approach towards adoption of chemical reaction model on 2,5-dimethyl-2,5-di-(tert-butylperoxy)hexane decomposition by differential isoconversional kinetic analysis

Energy Technology Data Exchange (ETDEWEB)

Das, Mitali; Shu, Chi-Min, E-mail: shucm@yuntech.edu.tw

2016-01-15

Highlights: • Thermally degraded DBPH products are identified. • An appropriate mathematical model was selected for decomposition study. • Differential isoconversional analysis was performed to obtain kinetic parameters. • Simulation on thermal analysis model was conducted for the best storage conditions. - Abstract: This study investigated the thermal degradation products of 2,5-dimethyl-2,5-di-(tert-butylperoxy) hexane (DBPH), by TG/GC/MS to identify runaway reaction and thermal safety parameters. It also included the determination of time to maximum rate under adiabatic conditions (TMR{sub ad}) and self-accelerating decomposition temperature obtained through Advanced Kinetics and Technology Solutions. The apparent activation energy (E{sub a}) was calculated from differential isoconversional kinetic analysis method using differential scanning calorimetry experiments. The E{sub a} value obtained by Friedman analysis is in the range of 118.0–149.0 kJ mol{sup −1}. The TMR{sub ad} was 24.0 h with an apparent onset temperature of 82.4 °C. This study has also established an efficient benchmark for a thermal hazard assessment of DBPH that can be applied to assure safer storage conditions.

Correlation between serum thyroglobulin levels and whole body scans in patients with differentiated thyroid carcinoma

International Nuclear Information System (INIS)

Hristova, N.; Piperkova, E.; Sergieva, S.; Tsingilev, D.; Fanariotov, D.; Kirilova, B.; Dimitrova, M.

1999-01-01

Postoperative follow-up study of patients with differentiated thyroid carcinoma (DTC) is currently based on periodic whole body scan (WBS) and serum thyroglobulin (Tg) assessment. The correlation between Tg levels measured and WB scans of 84 DTC patients is investigated. WBS are performed on a rotation gamma camera DIACAM (Siemens) at 48 and 72 hours after per os administration of 185-222 MBq 131 I. The levels of Tg are determined by IRMA method and kits of BYK, Germany. Normal Tg values are obtained at a control group of 27 patients free of thyroid disease. Increased Tg levels are found at 2 cases (4%) of the group of 50 patients with total thyroidectomy given 131 I without any evidence of recurrences or metastases. At the third group consisting of 18 patients with total thyroidectomy, following 131 I therapy and recurrences and/or metastases, increased Tg values were obtained in 8 cases or 44.4%. Also increased Tg levels were obtained at 4 from 16 patients (25%) subjected to total thyroidectomy but with a residual thyroid tissue proved by scintigraphy. In conclusion, a combination of both methods should be applied for improving the diagnostic and therapeutic results at the postoperative control of DTC patients

Preparation of nano-aluminum and studies on thermo-reaction properties

International Nuclear Information System (INIS)

Wei Sheng; Wang Chaoyang; Huang Yong; Wu Weidong; Tang Yongjian; Wei Jianjun

2002-01-01

The author presents the fabrication of nano-aluminum powders by evaporation-condensation method. The thermo gravimetric-differential scanning calorimetry technique is used to characterize the thermo-reaction properties between nano-aluminum powders and N 2 or Ar. The experiment results confirm the different thermo-reaction properties between block- and nano-aluminum

Polymer blends of poly(2-cyanoethyl vinyl ether) and poly(methyl methacrylate) with improved dielectric properties for flexible electronics

Czech Academy of Sciences Publication Activity Database

Piana, Francesco; Kredatusová, Jana; Paruzel, Bartosz; Pfleger, Jiří

2017-01-01

Roč. 11, č. 9 (2017), s. 731-737 ISSN 1788-618X R&D Projects: GA MŠk(CZ) LO1507 Institutional support: RVO:61389013 Keywords : polymer blends and alloys * dielectric properties * differential scanning calorimetry Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 2.983, year: 2016

Heat capacity measurements on Ybx Gd2–x Zr2 O7 (x= 0, 1, 2 ...

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science; Volume 32; Issue 6. Heat capacity measurements on YbGd2–Zr2O7 ( = 0, 1, 2) ceramics by differential scanning calorimetry. Zhan-Guo Liu Jia-Hu Ouyang Yu Zhou. Ceramics and Glasses Volume 32 Issue 6 December 2009 pp 603-606 ...

Investigation of solidification behavior of the Sn-rich ternary Sn–Bi–Zn alloys

Directory of Open Access Journals (Sweden)

S Mladenović

2017-03-01

Full Text Available Solidification properties and microstructure of six as-cast Sn–Bi–Zn alloys with 80 at.% of Sn and variable contents of Bi and Zn were experimentally investigated using the scanning electron microscopy (SEM with energy-dispersive X-ray spectroscopy (EDS and differential scanning calorimetry (DSC. The experimentally obtained results were compared with predicted phase equilibria according to the calculation of phase diagram (CALPHAD method and by the Scheil solidification simulation.

Synthesis and characterization of poly(glycerol citrate/sebacate)

International Nuclear Information System (INIS)

Brioude, Michel M.; Guimaraes, Danilo H.; Fiuza, Raigenis P.; Boaventura, Jaime S.; Jose, Nadia M.

2011-01-01

In this work were prepared and characterized the poly(glycerol citrate/sebacate) in three different ratios between acids. The polymers were prepared by a polycondensation reaction between glycerol and citric/sebacic acids and characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning differential calorimetry (DSC), scanning electron microscopy (SEM). The results showed that the polymers are polyesters and its crystallinity, thermal and morphological properties were modified by sebacic acid adding. (author)

Synthesis and characterization of poly(glycerol citrate/sebacate); Preparacao de caracterizacao do poli(glicerol citrato/sebacato)

Energy Technology Data Exchange (ETDEWEB)

Brioude, Michel M.; Guimaraes, Danilo H.; Fiuza, Raigenis P.; Boaventura, Jaime S.; Jose, Nadia M., E-mail: mbrioude@gmail.com [Universidade Federal da Bahia - UFBA, Instituto de Quimica, Salvador, BA (Brazil)

2011-07-01

In this work were prepared and characterized the poly(glycerol citrate/sebacate) in three different ratios between acids. The polymers were prepared by a polycondensation reaction between glycerol and citric/sebacic acids and characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning differential calorimetry (DSC), scanning electron microscopy (SEM). The results showed that the polymers are polyesters and its crystallinity, thermal and morphological properties were modified by sebacic acid adding. (author)

PREPARATION AND CHARACTERIZATION OF SOY PROTEIN ISOLATE(SPI)/MONTMORILLONITE(MMT) BIONANOCOMPOSITES

Institute of Scientific and Technical Information of China (English)

傅强

2009-01-01

The bionanocomposites of soy protein isolate(SPI)/montmorillonite(MMT) have been prepared successfully via simple melt mixing,in which MMT was used as nanofiller and glycerol was used as plasticizer.Their structures and properties were characterized with X-ray diffraction(XRD),differential scanning calorimetry(DSC),scanning electron microscopy(SEM),thermogravimetric analysis and tensile testing.XRD、TEM and SEM results indicated that the MMT layers could be easily intercalated by the SPI matrix even by si...

Indirect calorimetry: assessing animal response to heat and cold stress

NARCIS (Netherlands)

Gaughan, J.B.; Heetkamp, M.J.W.; Hendriks, P.

2015-01-01

Calorimetric thermal stress studies where indirect calorimetry is used as a tool to estimate energy expenditure have been undertaken since this technique was developed. Some examples of these studies are presented in this chapter. The measurement of gas exchange by means of an open-circuit

Scintillating Fibre Calorimetry at the LHC

CERN Multimedia

2002-01-01

Good electromagnetic and hadronic calorimetry will play a central role in an LHC detector. The lead/scintillating fibre calorimeter technique provides a fast signal response well matched to the LHC rate requirements. It can be made to give equal response for electrons and hadrons (compensation) with good electromagnetic and hadronic energy resolutions.\\\\ \\\\ The aim of this R&D proposal is to study in detail the aspects that are relevant for application of this type of calorimeter in an LHC environment, including its integration in a larger system of detectors, e.g.~projective geometry, radiation hardness, light detection, calibration and stability monitoring, electron/hadron separation.....

Enhancement of thermal stability of silver(I) acetylacetonate by platinum(II) acetylacetonate

Czech Academy of Sciences Publication Activity Database

Křenek, T.; Kovářík, T.; Pola, M.; Jakubec, Ivo; Bezdička, Petr; Bastl, Zdeněk; Pokorná, Dana; Urbanová, Markéta; Galíková, Anna; Pola, Josef

2013-01-01

Roč. 554, FEB (2013), s. 1-7 ISSN 0040-6031 Institutional support: RVO:61388980 ; RVO:61388955 ; RVO:67985858 Keywords : thermal gravimetric analysis * differential scanning calorimetry * silver(I) acetylacetonate * platinum(II) acetylacetonate * enhancement of thermal stability Subject RIV: CA - Inorganic Chemistry; CF - Physical ; Theoretical Chemistry (UFCH-W) Impact factor: 2.105, year: 2013

Influence of solvents on the habit modification of alpha lactose monohydrate single crystals

Science.gov (United States)

Parimaladevi, P.; Srinivasan, K.

2013-02-01

Restricted evaporation of solvent method was adopted for the growth of alpha lactose monohydrate single crystals from different solvents. The crystal habits of grown crystals were analysed. The form of crystallization was confirmed by powder x-ray diffraction analysis. Thermal behaviour of the grown crystals was studied by using differential scanning calorimetry.

An Experiment in Physical Chemistry: Polymorphism and Phase Stability in Acetaminophen (Paracetamol)

Science.gov (United States)

Myrick, Michael L.; Baranowski, Megan; Profeta, Luisa T. M.

2010-01-01

Differential scanning calorimetry analyses of two easily prepared polymorphs of acetaminophen (also known as paracetamol) are recorded. The density of the forms can be found in the literature. Rules for heats of transition, heats of fusion, and density, as well as methods for determining the solid-solid transition temperature between the forms,…

Preparation and Characterization of a Complex of Paeonol and ...

African Journals Online (AJOL)

thermogravimetric/differential scanning calorimetry (TG/DSC). Results: The phase-solubility results showed that paeonol formed a 1:1 stoichiometric complex with. HP-β-CD while UV and IR spectra suggested that HP-β-CD and paeonol in the complex interacted by a non-covalent bond. SEM and XRD indicate that the heat ...

Synthesis of a Self-Healing Polymer Based on Reversible Diels-Alder Reaction: An Advanced Undergraduate Laboratory at the Interface of Organic Chemistry and Materials Science

Science.gov (United States)

Weizman, Haim; Nielsen, Christian; Weizman, Or S.; Nemat-Nasser, Sia

2011-01-01

This laboratory experiment exposes students to the chemistry of self-healing polymers based on a Diels-Alder reaction. Students accomplish a multistep synthesis of a monomer building block and then polymerize it to form a cross-linked polymer. The healing capability of the polymer is verified by differential scanning calorimetry (DSC) experiments.…

Effect of gamma irradiation on thermophysical properties of plasticized starch and starch surfactant films

Science.gov (United States)

Cieśla, Krystyna; Watzeels, Nick; Rahier, Hubert

2014-06-01

In this work the influence of gamma irradiation on the thermomechanical properties of the films formed in potato starch-glycerol and potato starch-glycerol-surfactant systems were examined by Dynamic Mechanical Analysis, DMA, and Differential Scanning Calorimetry, DSC, and the results were correlated to the amount of the volatile fraction in the films.

The upgraded CDF front end electronics for calorimetry

Energy Technology Data Exchange (ETDEWEB)

Drake, G.; Frei, D.; Hahn, S.R.; Nelson, C.A.; Segler, S.L.; Stuermer, W.

1991-11-01

The front end electronics used in the calorimetry of the CDF detector has been upgraded to meet system requirements for higher expected luminosity. A fast digitizer utilizing a 2 {mu}Sec, 16 bit ADC has been designed and built. Improvements to the front end trigger circuitry have been implemented, including the production of 900 new front end modules. Operational experience with the previous system is presented, with discussion of the problems and performance goals.

The upgraded CDF front end electronics for calorimetry

International Nuclear Information System (INIS)

Drake, G.; Frei, D.; Hahn, S.R.; Nelson, C.A.; Segler, S.L.; Stuermer, W.

1991-11-01

The front end electronics used in the calorimetry of the CDF detector has been upgraded to meet system requirements for higher expected luminosity. A fast digitizer utilizing a 2 μSec, 16 bit ADC has been designed and built. Improvements to the front end trigger circuitry have been implemented, including the production of 900 new front end modules. Operational experience with the previous system is presented, with discussion of the problems and performance goals

A guide to automation techniques in calorimetry

International Nuclear Information System (INIS)

Renz, D.P.; Wetzel, J.R.; Breakall, K.L.; James, S.J.; Kasperski, P.W.

1992-01-01

Many improvements occurring in calorimetry measurement technology in the past few years will help current users of calorimeters to achieve better use of their existing systems. These include a more user friendly operator computer interface, a more detailed printout at the end of each run, improved data processing to eliminate operator error, and improved system monitoring to detect system or environmental problems. In addition, an electrical calibration heater has been developed to replace plutonium-238 heat standards for calibrating calorimeters, and several automation systems allow for easier and safer system operation

A High Strain-Rate Investigation of a Zr-Based Bulk Metallic Glass and an HTPB Polymer Composite

Science.gov (United States)

2011-03-01

The second order partial differential equation, 2 2 2 0 02 2 2 0 0 1 , where Eu u c x c t        , (2.1) governs the displacement, u, due...Liquidmetal, Inc. These plates were determined to be fully amorphous based on differential scanning calorimetry and X-ray diffraction in previous...Cambridge University Press, Cambridge, UK. 50 9. Pochhammer L. (1876) Uber Fortplanzungsgeschwindigkeiten kleiner Schwingungen in einem

Thermodynamic modeling of the Mg-Al-Ca system

Energy Technology Data Exchange (ETDEWEB)

Janz, A.; Groebner, J. [Clausthal University of Technology, Institute of Metallurgy, Robert-Koch-Str. 42, D-38678 Clausthal-Zellerfeld (Germany); Cao, H.; Zhu, J.; Chang, Y.A. [Department of Materials Science and Engineering, University of Wisconsin, 1509 University Ave., Madison, WI 53706 (United States); Schmid-Fetzer, R. [Clausthal University of Technology, Institute of Metallurgy, Robert-Koch-Str. 42, D-38678 Clausthal-Zellerfeld (Germany)], E-mail: schmid-fetzer@tu-clausthal.de

2009-02-15

A thermodynamic model has been developed that provides a quantitative description for a wide area of the Mg-Al-Ca system. All available experimental data plus new key experiments using differential scanning calorimetry/differential thermal analysis have been considered to create a dataset which reproduces the primary crystallizing phases, the extensive ternary solubilities of binary phases and the ternary C36 Laves phase. This enables validated thermodynamic calculations in various areas of this ternary system.

Immersion calorimetry as a tool to evaluate the catalytic performance of titanosilicate materials in the epoxidation of cyclohexene.

Science.gov (United States)

Vernimmen, Jarian; Guidotti, Matteo; Silvestre-Albero, Joaquin; Jardim, Erika O; Mertens, Myrjam; Lebedev, Oleg I; Van Tendeloo, Gustaaf; Psaro, Rinaldo; Rodríguez-Reinoso, Francisco; Meynen, Vera; Cool, Pegie

2011-04-05

Different types of titanosilicates are synthesized, structurally characterized, and subsequently catalytically tested in the liquid-phase epoxidation of cyclohexene. The performance of three types of combined zeolitic/mesoporous materials is compared with that of widely studied Ti-grafted-MCM-41 molecular sieve and the TS-1 microporous titanosilicate. The catalytic test results are correlated with the structural characteristics of the different catalysts. Moreover, for the first time, immersion calorimetry with the same substrate molecule as in the catalytic test reaction is applied as an extra means to interpret the catalytic results. A good correlation between catalytic performance and immersion calorimetry results is found. This work points out that the combination of catalytic testing and immersion calorimetry can lead to important insights into the influence of the materials structural characteristics on catalysis. Moreover, the potential of using immersion calorimetry as a screening tool for catalysts in epoxidation reactions is shown.

Laser Calorimetry Spectroscopy for ppm-level Dissolved Gas Detection and Analysis.

Science.gov (United States)

K S, Nagapriya; Sinha, Shashank; R, Prashanth; Poonacha, Samhitha; Chaudhry, Gunaranjan; Bhattacharya, Anandaroop; Choudhury, Niloy; Mahalik, Saroj; Maity, Sandip

2017-02-20

In this paper we report a newly developed technique - laser calorimetry spectroscopy (LCS), which is a combination of laser absorption spectroscopy and calorimetry - for the detection of gases dissolved in liquids. The technique involves determination of concentration of a dissolved gas by irradiating the liquid with light of a wavelength where the gas absorbs, and measuring the temperature change caused by the absorbance. Conventionally, detection of dissolved gases with sufficient sensitivity and specificity was done by first extracting the gases from the liquid and then analyzing the gases using techniques such as gas chromatography. Using LCS, we have been able to detect ppm levels of dissolved gases without extracting them from the liquid. In this paper, we show the detection of dissolved acetylene in transformer oil in the mid infrared (MIR) wavelength (3021 nm) region.

Determination of the enthalpy of formation of Ni-Al intermetallic compounds using differential scanning calorimetry technique

International Nuclear Information System (INIS)

Kubaski, Evaldo Toniolo; Capocchi, Jose Deodoro Trani; Cintho, Osvaldo Mitsuyuki

2010-01-01

The compositions Ni20Al80, Ni25Al75, Ni40Al60, Ni50Al50, Ni60Al40 and Ni75Al25 (at. %) were heated in a calibrated thermal analysis equipment. All runs were conducted at a heating rate of 10 deg C/min under a dynamic argon atmosphere. Each composition was heated until the completion of the corresponding exothermic reaction responsible for intermetallic compound formation, and, also heated to 1480 deg C. The products obtained were characterized using X ray diffraction in order to identify the intermetallic compounds that were synthesized. Moreover, the results were evaluated using variance analysis. As a result, enthalpies of formation of Ni 2 Al 3 and Ni 3 Al compounds were determined by means of this methodology. Experimental values were 167 kJ/mol and 93 kJ/mol for Ni 2 Al 3 and Ni 3 Al, respectively. The former is 18% lower than the value found on literature, while the latter is 6% greater. (author)

Forensic characterization of HDPE pipes by DSC.

Science.gov (United States)

Sajwan, Madhuri; Aggarwal, Saroj; Singh, R B

2008-03-05

The melting behavior of 28 high density polyethylene (HDPE) pipe samples manufactured and supplied by 13 different manufacturers in India was examined by 'differential scanning calorimetry (DSC)' to find out if this parameter could be used in differentiating between these HDPE pipe samples which are chemically the same and being manufactured by different manufacturer. The results indicate that the melting temperature may serve as the useful criteria for differentiating HDPE (i) pipe samples from different sources and (ii) samples of different diameter from the same source.

Comparison of calorimetry and destructive analytical measurement techniques for excess plutonium powders

International Nuclear Information System (INIS)

Welsh, T.L.

1996-01-01

In Dec. 1994, IAEA safeguards were initiated on inventory of Pu- bearing materials, originating from the US nuclear weapons complex, at vault 3 of DOE's Plutonium Finishing Plant at Hanford. Because of the diversity and heterogeneity of the Pu, plant operators have increasingly used calorimetry for accountability measurements. During the recent commencement of IAEA safeguards at vault 3, destructive (electrochemical titration) methods were used to determine Pu concentrations in subsamples of inventory items with widely ranging chemical purities. The Pu concentrations in the subsamples were determined and contribution of heterogeneity to total variability was identified. Measurement results, gathered by PFP and IAEA laboratories, showed total measurement variability for calorimetry to be comparable with or lower than those of sampling and chemical analyses

The Philosophy and Feasibility of Dual Readout Calorimetry

International Nuclear Information System (INIS)

Hauptman, John

2006-01-01

I will discuss the general physical ideas behind dual-readout calorimetry, their implementation in DREAM (Dual REAdout Module) with exact separation of scintillation and Cerenkov light, implementation with mixed light in DREAM fibers, anticipated implementation in PbWO4 crystals with applications to the 4th Concept detector and to CMS, use in high energy gamma-ray and cosmic ray astrophysics with Cerenkov and N2 fluorescent light, and implementation in the 4th Concept detector for muon identification

Synergies between electromagnetic calorimetry and PET

International Nuclear Information System (INIS)

Moses, William W.

2002-01-01

The instrumentation used for the nuclear medical imaging technique of Positron Emission Tomography (PET) shares many features with the instrumentation used for electromagnetic calorimetry. Both fields can certainly benefit from technical advances in many common areas, and this paper discusses both the commonalties and the differences between the instrumentation needs for the two fields. The overall aim is to identify where synergistic development opportunities exist. While such opportunities exist in inorganic scintillators, photodetectors, amplification and readout electronics, and high-speed computing, it is important to recognize that while the requirements of the two fields are similar, they are not identical, and so it is unlikely that advances specific to one field can be transferred without modification to the other

Coulometry and Calorimetry of Electric Double Layer Formation in Porous Electrodes

NARCIS (Netherlands)

Janssen, Mathijs; Griffioen, Elian; Biesheuvel, P. M.; Van Roij, René; Erné, Ben

2017-01-01

Coulometric measurements on salt-water-immersed nanoporous carbon electrodes reveal, at a fixed voltage, a charge decrease with increasing temperature. During far-out-of-equilibrium charging of these electrodes, calorimetry indicates the production of both irreversible Joule heat and reversible

Elementary martensitic transformation processes in Ni-rich NiTi single crystals with Ni4Ti3 precipitates

Czech Academy of Sciences Publication Activity Database

Michutta, J.; Somsen, Ch.; Yawny, A.; Dlouhý, Antonín; Eggeler, G.

2006-01-01

Roč. 54, č. 13 (2006), s. 3525-3542 ISSN 1359-6454 R&D Projects: GA ČR(CZ) GA106/05/0918 Institutional research plan: CEZ:AV0Z20410507 Keywords : multiple-step martensitic transformations * differential scanning calorimetry * in situ cooling transmission electron microscopy Subject RIV: JG - Metallurgy Impact factor: 3.549, year: 2006

Physical ageing in the above-bandgap photoexposured glassy arsenic selenides

Energy Technology Data Exchange (ETDEWEB)

Kozdras, A [Faculty of Physics of Opole University of Technology, 75, Ozimska str., Opole, PL-45370 (Poland); Golovchak, R [Lviv Scientific Research Institute of Materials of SRC ' Carat' , 202, Stryjska str., Lviv, UA-79031 (Ukraine); Shpotyuk, O [Lviv Scientific Research Institute of Materials of SRC ' Carat' , 202, Stryjska str., Lviv, UA-79031 (Ukraine)

2007-08-15

Physical ageing induced by above-bandgap light illumination is studied in glassy As-Se using differential scanning calorimetry. It is shown that measurable effect like to known short-term physical ageing is observed only in Se-rich glasses. The kinetics of this effect is compared with that caused by natural storage in a dark.

Physical ageing in the above-bandgap photoexposured glassy arsenic selenides

International Nuclear Information System (INIS)

Kozdras, A; Golovchak, R; Shpotyuk, O

2007-01-01

Physical ageing induced by above-bandgap light illumination is studied in glassy As-Se using differential scanning calorimetry. It is shown that measurable effect like to known short-term physical ageing is observed only in Se-rich glasses. The kinetics of this effect is compared with that caused by natural storage in a dark

Chemical and phase structure of poly cyanurate-polyurethane grafted semi interpenetrating polymer networks

International Nuclear Information System (INIS)

Fainleib, A.M.; Gomza, Yu.P.; Privalko, V.P.; Bershtein, V.A.; Carini, G.

2001-01-01

In this research the phase morphology and properties of dicyanate ester of bisphenol A (DCEBA) based poly cyanurate network (PCN) modified with linear polyurethane (LPU) were successfully studied by the combination of infra-red spectroscopy, small-angle X-ray scattering (SAXS), dynamic mechanical thermal analysis (DMTA), differential scanning calorimetry and laser-interferometric creep rate spectroscopy

Silver lead borate glasses doped with europium ions for phosphors

Indian Academy of Sciences (India)

From the differential scanning calorimetry studies, the glass transition temperatures ( T g )have been investigated and their values are ranging from 449 to 458 ∘ C. The investigation of Fourier transformer infraredspectra shows the presence of boron atoms in both BO 3 and BO 4 units in the glass network. In addition, it was ...

Ligand binding and thermostability of different allosteric states of the insulin zinc-hexamer

DEFF Research Database (Denmark)

Huus, Kasper; Havelund, Svend; Olsen, Helle B

2006-01-01

The influence of ligand binding and conformation state on the thermostability of hexameric zinc-insulin was studied by differential scanning calorimetry (DSC). The insulin hexamer exists in equilibrium between the forms T6, T3R3, and R6. Phenolic ligands induce and stabilize the T3R3- and R6-stat...

Deepika Bhandari

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science. Deepika Bhandari. Articles written in Bulletin of Materials Science. Volume 23 Issue 5 October 2000 pp 369-375 Glasses. Differential scanning calorimetry studies of Se85Te15–Pb ( = 4, 6, 8 and 10) glasses · N B Maharajan N S Saxena Deepika Bhandari Mousa M Imran ...

Evaluation of the quasi-isothermal method of modulated DSC for heat capacity measurement

International Nuclear Information System (INIS)

Venkata Krishnan, R.; Nagarajan, K.

2004-01-01

Heat capacity measurements were carried out on ThO 2 by Modulated Differential Scanning Calorimetry (MDSC) using quasi-isothermal method in the temperature range 323-723 K. The highest accuracy of the heat capacity data obtained by this method was ± 2-3% which is much lower than that reported in the literature. (author)

Addition compounds of yttrium and lanthanide perrhenates with tetramethylene sulphoxide

International Nuclear Information System (INIS)

Umeda, K.

1977-01-01

Adducts of lanthanide perrhenates with tetramethylene sulfoxide are prepared and characterized. The compounds having as general formula Ln(Re04) 3 .7.5 TMSO(ln=La-Lu and Y) are characterized by elemental analysis, infrared spectra, molar conductance measurements, x-ray powder patterns, differential scanning calorimetry curves, melting temperature range measurements and thermogravimetric analysis [pt

Lignin-coated cellulose nanocrystals as promising nucleating agent for poly(lactic acid)

Science.gov (United States)

Anju Gupta; William Simmons; Gregory T. Schueneman; Eric A. Mintz

2016-01-01

We report the effect of lignin-coated cellulose nanocrystals (L-CNCs) on the crystallization behavior of poly(lactic acid) (PLA). PLA/L-CNC nanocomposites were prepared by melt mixing, and the crystallization behavior of PLA was investigated using differential scanning calorimetry. Isothermal crystallization data were analyzed using Avrami and Lauritzen–Hoffman...

Thermal protection of electronic devices with the Nylon6/66-PEG nanofiber membranes

OpenAIRE

Li Ya; Li Xue-Weis; He Ji-Huan; Wang Ping

2014-01-01

Phase change materials for thermal energy storage have been widely applied to clothing insulation, electronic products of heat energy storage. The thermal storage potential of the nanofiber membranes was analyzed using the differential scanning calorimetry. Effect of microstructure of the membrane on energy storage was analyzed, and its applications to electronic devices were elucidated.

Computed tomography of liver tumors, 2. Differential diagnosis between hepatocellular carcinoma and metastatic hepatic tumor by dynamic CT scanning

Energy Technology Data Exchange (ETDEWEB)

Naito, Akira; Fukuoka, Haruhito; Kashiwado, Kouzou; Ichiki, Toshio; Makidono, Yoko [Hiroshima Red Cross Hospital (Japan)

1984-02-01

Differential diagnosis between hepatocellular carcinoma and metastatic hepatic tumor was attempted using dynamic CT scanning. Homogeneous and patchy types were peculiar to hepatocellular carcinoma, and ring-like type to metastatic hepatic tumor. However, with no enhancement, hepatocellular carcinoma could not be denied. Hepatocellular carcinoma was characterized by the enhancement shown on the early stage of dynamic CT. Ring enhancement was not visualized on dynamic CT but visualized on conventional contrast enhanced CT in hepatocellular carcinomas; it was visualized on conventional contrast enhanced CT and on dynamic CT in metastatic hepatic tumors.

Microstructure evolution, thermal stability and fractal behavior of water vapor flow assisted in situ growth poly(vinylcarbazole)-titania quantum dots nanocomposites

Science.gov (United States)

Mombrú, Dominique; Romero, Mariano; Faccio, Ricardo; Mombrú, Alvaro W.

2017-12-01

Here, we report a novel strategy for the preparation of TiO2 quantum dots fillers prepared from alkoxide precursor via in situ water vapor flow diffusion into poly(N-vinylcarbazole) host. A detailed characterization by means of infrared and Raman spectroscopy, X-ray powder diffraction, small angle X-ray scattering and differential scanning calorimetry is reported. The growth mechanism of both crystallites and particles was mostly governed by the classical coarsening reaction limited growth and the polymer host showed no detectable chemical modifications at the interface or active participation in the growing process. The main relevance of our strategy respect to the typical sol-gel growth in solution is the possibility of the interruption of the reaction by simple stopping the water vapor flow diffusion into the polymer host thus achieving good control in the nanoparticles size. The thermal stability and fractal behavior of our nanocomposites were also studied by differential scanning calorimetry and in situ small angle X-ray scattering versus temperature. Strong correlations between modifications in the fractal behavior and glass transition or fusion processes were observed for these nanocomposites.

Ultra-Fast Hadronic Calorimetry

Energy Technology Data Exchange (ETDEWEB)

Denisov, Dmitri [Fermilab; Lukić, Strahinja [VINCA Inst. Nucl. Sci., Belgrade; Mokhov, Nikolai [Fermilab; Striganov, Sergei [Fermilab; Ujić, Predrag [VINCA Inst. Nucl. Sci., Belgrade

2017-12-18

Calorimeters for particle physics experiments with integration time of a few ns will substantially improve the capability of the experiment to resolve event pileup and to reject backgrounds. In this paper time development of hadronic showers induced by 30 and 60 GeV positive pions and 120 GeV protons is studied using Monte Carlo simulation and beam tests with a prototype of a sampling steel-scintillator hadronic calorimeter. In the beam tests, scintillator signals induced by hadronic showers in steel are sampled with a period of 0.2 ns and precisely time-aligned in order to study the average signal waveform at various locations w.r.t. the beam particle impact. Simulations of the same setup are performed using the MARS15 code. Both simulation and test beam results suggest that energy deposition in steel calorimeters develop over a time shorter than 3 ns providing opportunity for ultra-fast calorimetry. Simulation results for an "ideal" calorimeter consisting exclusively of bulk tungsten or copper are presented to establish the lower limit of the signal integration window.

Thermodynamic properties of 1-phenylnaphthalene and 2-phenylnaphthalene

International Nuclear Information System (INIS)

Chirico, Robert D.; Steele, William V.; Kazakov, Andrei F.

2014-01-01

Highlights: • Heat capacities, vapor pressures, enthalpies of combustion, and densities were measured for 1-phenylnaphthalene (1-PhN). • Heat capacities and vapor pressures were measured for 2-phenylnaphthalene (2-PhN). • Independent ideal-gas entropies derived with the calorimetric results and statistical methods are in accord for 1-PhN. • 2-PhN showed glassy-crystal behavior in the solid state, and an entropy deficit is demonstrated. - Abstract: Measurements leading to the calculation of thermodynamic properties in the ideal-gas state for 1-phenylnaphthalene (Chemical Abstracts registry number [605-02-7]) and 2-phenylnaphthalene (Chemical Abstracts registry number [612-94-2]) are reported. Experimental methods for 1-phenylnaphthalene were adiabatic heat-capacity calorimetry, differential scanning calorimetry, inclined-piston manometry, comparative ebulliometry, vibrating-tube densitometry, and combustion calorimetry. For 2-phenylnaphthalene, the experimental methods were adiabatic heat-capacity calorimetry, differential scanning calorimetry, and comparative ebulliometry. Critical properties were estimated for both compounds. Molar thermodynamic functions (enthalpies, entropies, and Gibbs free energies) for the condensed and ideal-gas states were derived from the experimental studies at selected temperatures. Statistical calculations were performed based on molecular geometry optimization and vibrational frequencies calculated at the B3LYP/6-31+G(d, p) and B3LYP/cc-pVTZ levels of theory. Ideal-gas entropies derived with two the independent methods are shown to be in good accord for 1-phenylnaphthalene, but significant differences are apparent for 2-phenylnaphthalene. These differences are likely due to a disorder of unknown type in the crystals of 2-phenylnaphthalene at low temperatures, as evidenced by the presence of a glass-like transition in the measured heat capacities for the solid state. All experimental results are compared with property values

Investigations of Differential Scanning Techniques using Two Radionuclides

Energy Technology Data Exchange (ETDEWEB)

Cottrall, M. F.; French, Rosemary J.; Trott, N. G. [Institute of Cancer Research and Royal Marsden Hospital, Sutton, Surrey (United Kingdom)

1969-01-15

In the development of scanning procedures difficulties sometimes arise because a particular radiopharmaceutical, which is selectively concentrated in an organ of interest, is also widely distributed in neighbouring sites in the body. Investigations have been made of a method which involves the use of a second radioactive substance to label such sites. By means of suitable electrical circuits fitted to a conventional mechanical scanner (Picker Magnascanner III), a direct colour scan of the organ under study can be obtained. Signals from the two radionuclides are distinguished by pulse-height analysis and used to operate the colour shift mechanism. Experimental studies with phantoms and clinical trials are reported. An analysis of the statistical limitations of the technique is given, including a discussion of the most suitable operating conditions for particular pairs of radionuclides. Illustrations include the use of {sup 75}Se selenomethionine and {sup 99m}Tc sulphur colloid or {sup 198}Au colloid in the delineation of the pancreas, and reference is also made to work with {sup 18}F, {sup 99m}Tc, {sup 133m}In and {sup 197}Hg, which are used in various chemical forms to visualize specific types of tumours in vascular surroundings labelled with other suitable tracers. Some discussion of the dosimetry of these procedures is made, since the extent to which the technique can be applied may be limited by the activities which can be administered. However, successful results are being obtained using activities within the range generally accepted for single radionuclide scanning procedures. For example, the pancreas can be successfully visualised using 250 {mu}Ci {sup 75}Se selenomethionine in combination with 1 mCi {sup 99m}TC sulphur colloid. (author)

A reference device for evaluating the thermal behavior of installed multilayered wall containing a phase change material

International Nuclear Information System (INIS)

Pagliolico, S.L.; Sassi, G.; Cascone, Y.; Bongiovanni, R.M.

2015-01-01

Highlights: • Thermal analysis of installed wallboards embedding phase change material layer. • Simple devices and real conditions for thermal analysis toward a standardization. • Scanning calorimetric measurements as initial condition for data regression. • Bias correction of calorimetric measurements data by installation factors. • Practical approach to identify a reliable thermal curve for capacitive wallboards. - Abstract: Thermal inertia of lightweight building envelopes can be improved including phase change materials in multilayered wallboards. The thermal modeling of buildings for design purposes needs a robust description of the thermal properties of installed phase change materials. A standard method would improve the thermal characterization of commercial products. The aim of the study is to develop a simple methodology to obtain reliable thermal data for phase change materials integrated in multilayered wallboards. The methodology modifies differential scanning calorimetry measurements on phase change material by installation factors to obtain the apparent specific heat vs. temperature for the wallboard layer embedding phase change material. Simple cubic cells were realized as reference devices to simulate a confined environment. A dynamic model of heat transfer was developed to simulate the thermal behavior of devices. Installation factors were calculated by regression of the monitored temperatures inside and outside the devices operating under real environmental conditions. The apparent specific heat of phase change material, measured by differential scanning calorimetry at different rates, resulted in a spread of curves vs. temperature. Mean curves were used as initial condition for regression. The mean calculation method did not significantly affect the installed resulted curve. A unique curve of apparent specific heat vs. temperature best fit data measured over a wide range of experimental devices and conditions. Good regression

Energetics of sodium-calcium exchanged zeolite A.

Science.gov (United States)

Sun, H; Wu, D; Guo, X; Shen, B; Navrotsky, A

2015-05-07

A series of calcium-exchanged zeolite A samples with different degrees of exchange were prepared. They were characterized by powder X-ray diffraction (XRD) and differential scanning calorimetry (DSC). High temperature oxide melt drop solution calorimetry measured the formation enthalpies of hydrated zeolites CaNa-A from constituent oxides. The water content is a linear function of the degree of exchange, ranging from 20.54% for Na-A to 23.77% for 97.9% CaNa-A. The enthalpies of formation (from oxides) at 25 °C are -74.50 ± 1.21 kJ mol(-1) TO2 for hydrated zeolite Na-A and -30.79 ± 1.64 kJ mol(-1) TO2 for hydrated zeolite 97.9% CaNa-A. Dehydration enthalpies obtained from differential scanning calorimetry are 32.0 kJ mol(-1) H2O for hydrated zeolite Na-A and 20.5 kJ mol(-1) H2O for hydrated zeolite 97.9% CaNa-A. Enthalpies of formation of Ca-exchanged zeolites A are less exothermic than for zeolite Na-A. A linear relationship between the formation enthalpy and the extent of calcium substitution was observed. The energetic effect of Ca-exchange on zeolite A is discussed with an emphasis on the complex interactions between the zeolite framework, cations, and water.

Clinical and CT scan pictures of cerebral cysticercosis

Energy Technology Data Exchange (ETDEWEB)

Singounas, E.G.; Krassanakis, K.; Karvounis, P.C. (Evangelismos Hospital, Athens (Greece))

1982-01-01

The clinical presentations and CT scan pictures of four patients harbouring big cysticercus cysts are described. The value of CT scanning in detecting these cysts is emphasized, and also the fact that these cysts can behave as space-occyping lesions, which must be differentiated from other cystic formations.

Subsite binding energies of an exo-polygalacturonase using isothermal titration calorimetry

Science.gov (United States)

Thermodynamic parameters for binding of a series of galacturonic acid oligomers to an exo-polygalacturonase, RPG16 from Rhizopus oryzae, were determined by isothermal titration calorimetry. Binding of oligomers varying in chain length from two to five galacturonic acid residues is an exothermic proc...

Monolithic front-end preamplifiers for a broad range of calorimetry applications

Energy Technology Data Exchange (ETDEWEB)

Radeka, V.; Rescia, S. [Brookhaven National Lab., Upton, NY (United States); Manfredi, P.F.; Speziali, V. [Pavia Univ. (Italy). Dipt. di Elettronica]|[INFN--Sezzione di Milano, Milano (Italy)

1993-12-31

The present paper summarizes the salient results of a research and development activity in the area of low noise preamplifiers for different applications in calorimetry. Design target for all circuits considered here are low noise, ability to cope with broad energy ranges and radiation hardness.

N S Saxena

Indian Academy of Sciences (India)

Home; Journals; Bulletin of Materials Science. N S Saxena. Articles written in Bulletin of Materials Science. Volume 23 Issue 5 October 2000 pp 369-375 Glasses. Differential scanning calorimetry studies of Se85Te15–Pb ( = 4, 6, 8 and 10) glasses · N B Maharajan N S Saxena Deepika Bhandari Mousa M Imran D D ...

Effect of natural irradiation in fluorites: possible implications for nuclear waste management?

Czech Academy of Sciences Publication Activity Database

Vlček, V.; Skála, Roman; Goliáš, V.; Drahokoupil, Jan; Čížek, J.; Strnad, L.; Ederová, J.

2012-01-01

Roč. 57, č. 1 (2012), s. 45-52 ISSN 1802-6222 R&D Projects: GA ČR GA106/07/0805; GA AV ČR KAN300100801 Institutional research plan: CEZ:AV0Z30130516 Keywords : fluorite * irradiation * X-ray diffraction * differential scanning calorimetry * defects * real structure Subject RIV: DB - Geology ; Mineralogy Impact factor: 0.804, year: 2012

Formulation Optimization and In-vitro Evaluation of Oral Floating ...

African Journals Online (AJOL)

The concentrations of HPMC K100M (X1) and xanthan gum (X2) were chosen as control variables. Conversely, the response variables selected were timed to release 50 % of the drug (t50%) at 6 h (Q6) and 12 h (Q12). Fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC) were used to ...

Stress corrosion crack growth rate in dissimilar metal welds; Evolucion microestructural de la ZAC en la union soldada con MIG sobre una aleacion del aluminio AA7020

Energy Technology Data Exchange (ETDEWEB)

Bloem, C. A.; Salvador, M. D.; Amigo, V.; Busquets, D.

2003-07-01

The aim of the present study is to evaluate the changes through the HAZ, analyzed under two different but complementary techniques. These are Transmission Electronic Microscopy (TEM) and Differential Scanning Calorimetry (DSC). The results shown that there are remarkable changes in size and morphology of the precipitates, being in accordance with the results obtained by DSC. (Author) 10 refs.

Stress corrosion crack growth rate in dissimilar metal welds

International Nuclear Information System (INIS)

Bloem, C. A.; Salvador, M. D.; Amigo, V.; Busquets, D.

2003-01-01

The aim of the present study is to evaluate the changes through the HAZ, analyzed under two different but complementary techniques. These are Transmission Electronic Microscopy (TEM) and Differential Scanning Calorimetry (DSC). The results shown that there are remarkable changes in size and morphology of the precipitates, being in accordance with the results obtained by DSC. (Author) 10 refs

Crystallization of Pd40CU30Ni10P20 bulk metallic glass with and without pressure

DEFF Research Database (Denmark)

Yang, B.; Jiang, Jianzhong; Zhuang, Yanxin

2007-01-01

The glass-transition behavior of Pd40Cu30Ni10P20 bulk metallic glass was investigated by differential scanning calorimetry (DSC) and X-ray powder diffraction (XRD). The effect of pressure on the crystallization behavior of Pd40Cu30Ni10P20 bulk glass was studied by in situ high-pressure and high...

Investigations on the optical, thermal and surface modifications of electron irradiated L-threonine single crystals

Energy Technology Data Exchange (ETDEWEB)

Ramesh Kumar, G.; Gokul Raj, S. [Department of Physics, Presidency College, Chepauk, Chennai 600005 (India); Bogle, K.A.; Dhole, S.D.; Bhoraskar, V.N. [Department of Physics, University of Pune, Pune 411007 (India); Mohan, R. [Department of Physics, Presidency College, Chepauk, Chennai 600005 (India)], E-mail: professormohan@yahoo.co.in

2008-06-15

L-Threonine single crystals have been irradiated by 6 MeV electrons. Irradiated crystals at various electron fluences were subjected to various techniques such as UV-vis-NIR, atomic force microscopy (AFM) and thermomechanical analyses. Thermal strength of the irradiated crystals has also been studied through differential scanning calorimetry (DSC) measurements. The results have been discussed in detail.

Influência de alguns parâmetros experimentais nos resultados de análises calorimétricas diferenciais - DSC

OpenAIRE

Bernal, Cláudia; Couto, Andréa Boldarini; Breviglieri, Susete Trazzi; Cavalheiro, Éder Tadeu Gomes

2002-01-01

A series of experiments were performed in order to demonstrate to undergraduate students or users of the differential scanning calorimetry (DSC), that several factors can influence the qualitative and quantitative aspects of DSC results. Saccharin, an artificial sweetner, was used as a probe and its thermal behavior is also discussed on the basis of thermogravimetric (TG) and DSC curves.