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Sample records for calorimetry dsc experimental

  1. Differential scanning calorimetry (DSC) of semicrystalline polymers.

    Science.gov (United States)

    Schick, C

    2009-11-01

    Differential scanning calorimetry (DSC) is an effective analytical tool to characterize the physical properties of a polymer. DSC enables determination of melting, crystallization, and mesomorphic transition temperatures, and the corresponding enthalpy and entropy changes, and characterization of glass transition and other effects that show either changes in heat capacity or a latent heat. Calorimetry takes a special place among other methods. In addition to its simplicity and universality, the energy characteristics (heat capacity C(P) and its integral over temperature T--enthalpy H), measured via calorimetry, have a clear physical meaning even though sometimes interpretation may be difficult. With introduction of differential scanning calorimeters (DSC) in the early 1960s calorimetry became a standard tool in polymer science. The advantage of DSC compared with other calorimetric techniques lies in the broad dynamic range regarding heating and cooling rates, including isothermal and temperature-modulated operation. Today 12 orders of magnitude in scanning rate can be covered by combining different types of DSCs. Rates as low as 1 microK s(-1) are possible and at the other extreme heating and cooling at 1 MK s(-1) and higher is possible. The broad dynamic range is especially of interest for semicrystalline polymers because they are commonly far from equilibrium and phase transitions are strongly time (rate) dependent. Nevertheless, there are still several unsolved problems regarding calorimetry of polymers. I try to address a few of these, for example determination of baseline heat capacity, which is related to the problem of crystallinity determination by DSC, or the occurrence of multiple melting peaks. Possible solutions by using advanced calorimetric techniques, for example fast scanning and high frequency AC (temperature-modulated) calorimetry are discussed.

  2. 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.

    Directory of Open Access Journals (Sweden)

    Cláudia Bernal

    2002-09-01

    Full Text Available 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.

  3. Determination of Purity by Differential Scanning Calorimetry (DSC).

    Science.gov (United States)

    Brown, M. E.

    1979-01-01

    An exercise is presented which demonstrates the determination of sample purity by differential scanning calorimetry. Data and references are provided to enable the exercise to be carried out as a dry-lab experiment. (BB)

  4. Nucleation and crystallisation kinetics of a Na-fluorrichterite based glass by differential scanning calorimetry (DSC)

    OpenAIRE

    Pérez, Juan M.; Casasola, Raquel; Rincón López, Jesús María; Romero, Maximina

    2012-01-01

    The present paper shows the results of a nucleation and crystallisation study of a Na-fluorrichterite glass carried out by dynamic scanning calorimetry (DSC). The kinetic study was performed using different procedures (Kissinger, Matusita–Sakka and Kissinger–Akahira–Sunose (KAS) methods), and the Avrami parameter was determined from the Ozawa and Malek approximations and the Malek equation. The results have indicated the coexistence of surface and bulk crystallisation in the devitrification p...

  5. 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. PMID:26721421

  6. Applications of differential scanning calorimetry for thermal stability analysis of proteins: qualification of DSC.

    Science.gov (United States)

    Wen, Jie; Arthur, Kelly; Chemmalil, Letha; Muzammil, Salman; Gabrielson, John; Jiang, Yijia

    2012-03-01

    Differential scanning calorimetry (DSC) has been used to characterize protein thermal stability, overall conformation, and domain folding integrity by the biopharmaceutical industry. Recently, there have been increased requests from regulatory agencies for the qualification of characterization methods including DSC. Understanding the method precision can help determine what differences between samples are significant and also establish the acceptance criteria for comparability and other characterization studies. In this study, we identify the parameters for the qualification of DSC for thermal stability analysis of proteins. We use these parameters to assess the precision and sensitivity of DSC and demonstrate that DSC is suitable for protein thermal stability analysis for these purposes. Several molecules from different structural families were studied. The experiments and data analyses were performed by different analysts using different instruments at different sites. The results show that the (apparent) thermal transition midpoint (T(m)) values obtained for the same protein by same and different instruments and/or analysts are quite reproducible, and the profile similarity values obtained for the same protein from the same instrument are also high. DSC is an appropriate method for assessing protein thermal stability and conformational changes.

  7. 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.

  8. Combustion calorimetry experimental chemical thermodynamics

    CERN Document Server

    Sunner, Stig

    1979-01-01

    Combustion Calorimetry deals with expertise knowledge concerning the calorimetry of combustion reactions of an element or compound. After defining the use of units and physical constants, the book discusses the basic principles of combustion calorimetry and the various instruments and calorimeters used in the experiments to measure operations concerning temperatures and its time variations. One paper discusses the theory and design criteria of combustion calorimeter calibration. Another paper discusses the results obtained from a combustion calorimeter after it has measured the energy or entha

  9. Monitoring of butter and animal fat oxidation stability by differential scanning calorimetry (DSC

    Directory of Open Access Journals (Sweden)

    Jasminka Sadadinović

    2005-07-01

    Full Text Available Oxidation of fat is one of the basic reactions which causes the depletion of butter and animal fat quality as well as other products containing them. Since the most of reaction products of fat oxidation are harmful for consumers' health, inadequate and scarce monitoring of edible fats and fat containing products quality, presents increased health risk as well as financial loss for the producers. In fat oxidation stability estimation, standard chemical methods were used (iodine number, acid number, peroxide number, anisidine number etc., which require time and chemical usage. Differential scanning calorimetry (DSC analysis presents the simple and efficient way for butter and animal fats oxidation stability estimation. Laboratory investigations were performed to monitor oxidation stability of butter and animal fat in fresh state, as well as in spent phase, used in frying process. The results obtained were compared to the results of standard chemical analysis, and they confirmed the reproducibility and applicability of differential scanning calorimetry in oxidation stability of butter and animal fats monitoring.

  10. Evaluation of peritoneal tissue by means of differential scanning calorimetry (DSC

    Directory of Open Access Journals (Sweden)

    Łukasz Pietrzyk

    2012-01-01

    Full Text Available Abdominal surgeries alter the integrity of the peritoneal layer and cause imbalances among immunological, inflammatory and angiogenic mechanisms within the tissue. During laparoscopic procedures a protective function of the peritoneal layer can be disturbed by the gas used to create a pneumoperitoneum. The aim of this study was to characterize peritoneal tissue by means of differential scanning calorimetry (DSC as a reference for future investigations on the influence of surgical procedures on the physicochemical state of the peritoneum. Thirty-seven patients participated in the study. Patients were divided into three groups according to the type of surgery: group H — patients who underwent hernia repair; group Ch — patients who underwent laparoscopic cholecystectomy; and group C — patients operated due to rectal cancer. It was observed that onset temperature (To, denaturation temperature (Tm and change of enthalpy (ΔH during thermal denaturation of peritoneal collagen in were significantly different for these three groups of patients. The mean values of onset temperature (To and denaturation temperature (Tm in group H were significantly lower, while DH in this group was significantly higher than in the two other groups (Ch and C. This preliminary study does not answer whether the differences in collagen denaturation found in peritoneal tissue from different groups of patients resulted from a different inherent state of the tissue, or from surgical procedures. However, the results suggest that DSC is an appropriate method to study subtle changes in the physicochemical condition of the peritoneum using small samples obtained during surgical procedures. (Folia Histochemica et Cytobiologica 2011; Vol. 49, No. 4, pp. 700–705

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

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    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.

  12. Effects of experimental variables in quantitative differential scanning calorimetry

    OpenAIRE

    Dooren, Adrianus August van

    1982-01-01

    Dit proefschriÍt beschrijft een onderzoek naar de effecten van experimentele omstandigheden op curve-karakteristieken en enige toepassingen van kwantitatieve Differentiele Scanning calorimetry (DSC). ... Zie: Samenvatting

  13. Determination of melting point of vegetable oils and fats by differential scanning calorimetry (DSC technique.

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    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.

  14. Characterization of a Friction Stir Weld in Aluminum Alloy 7055 Using Microhardness, Electrical Conductivity, and Differential Scanning Calorimetry (DSC)

    Science.gov (United States)

    Bush, Ralph; Kiyota, Michelle; Kiyota, Catherine

    2016-07-01

    Optical microscopy, microhardness, electrical conductivity, and differential scanning calorimetry (DSC) were used to characterize the microstructure, hardness, and precipitate structure as a function of position in a friction stir weld, naturally aged for 10 years, in aluminum alloy 7055. Results are shown for the as-welded/naturally aged condition and for a weld that was post-aged using a -T76 regimen. The grain structure and microhardness results reveal the expected central recrystallized region, a thermo-mechanical affected zone (TMAZ), and heat-affected zone (HAZ) with typical changes in microhardness. DSC scans for the as-welded/naturally aged condition indicate a precipitate structure similar to that of a naturally aged condition in the central recrystallized region. Maximum precipitate coarsening and overaging occurs near the TMAZ/HAZ boundary with reduced precipitate dissolution and coarsening as the distance from the weld increases. The post-weld aging resulted in the transformation of GP zones to more stable precipitates plus coarsening of the more stable η' and η precipitates. A combination of DSC testing and CALPHAD calculations allowed calculation of precipitate volume fraction in the HAZ. The precipitate volume fraction decreased monotonically from 0.052 in the baseline material to 0.044 at the TMAZ/HAZ interface.

  15. Differential scanning calorimetry (DSC) as a tool for probing the reactivity of polyynes relevant to hexadehydro-Diels-Alder (HDDA) cascades.

    Science.gov (United States)

    Woods, Brian P; Hoye, Thomas R

    2014-12-19

    The differential scanning calorimetry (DSC) behavior of a number of alkyne-rich compounds is described. The DSC trace for each compound exhibits an exothermic event at a characteristic onset temperature. For the tri- and tetraynes whose [4 + 2] HDDA reactivity in solution has been determined, these onset temperatures show a strong correlation with the cyclization activation energy. The studies reported here exemplify how the data available through this operationally simple analytical technique can give valuable insights into the thermal behavior of small molecules.

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

    Science.gov (United States)

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

    2015-11-01

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

  17. Estimation of hydrogen bondings in coal utilizing FTir and differential scanning calorimetry (DSC); FTir to DSC wo mochiita sekitannai suiso ketsugo no teiryoteki hyoka no kokoromi

    Energy Technology Data Exchange (ETDEWEB)

    Mae, K.; Miura, K. [Kyoto University, Kyoto (Japan). Faculty of Engineering

    1996-10-28

    With an objective to know coal condensation structure which has influence on coal conversion reaction, an attempt was made on quantitative evaluation of hydrogen bonding in coal. Using as test samples the VDC made from Taiheiyo coal swollen by tetralin and vacuum-dried, and its pyrolyzed char, DSC measurement and Fourier transform infrared spectroscopy (FT) were performed. An FT spectrum comparison revealed that the VDC swollen at 220{degree}C has the hydrogen bonding relaxed partly from the original coal. However, since the change is in a huge coal molecular structure restraining space, it has stopped at relaxation of the bonding energy without causing separation as far as free radicals. On the other hand, the DSC curve shows that the VDC has slower endothermic velocity than the original coal. In other words, the difference in heat absorption amounts in both materials is equivalent to the difference of enthalpy ({Delta} H) of both materials, which corresponds to the relaxation of the hydrogen bonding. Therefore, the {Delta} H was related to wavenumber shift of the FT spectra (which corresponds to change in the hydrogen bonding condition). By using this relationship, a method for evaluating hydrogen bonding distribution was proposed from an O-H contracting vibration change that can be measured by using the FT spectra and a thermal change that can be measured by using the DSC. 3 refs., 7 figs.

  18. Calorimetry

    International Nuclear Information System (INIS)

    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

  19. 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

  20. Can the thermodynamic melting temperature of sucrose, glucose, and fructose be measured using rapid-scanning differential scanning calorimetry (DSC)?

    Science.gov (United States)

    Lee, Joo Won; Thomas, Leonard C; Schmidt, Shelly J

    2011-04-13

    The loss of crystalline structure in sucrose, glucose, and fructose has been shown to be due to the kinetic process of thermal decomposition (termed apparent melting), rather than thermodynamic melting. The purpose of this research was to investigate whether or not it is possible to scan quickly enough to suppress the kinetic process of thermal decomposition and reach the thermodynamic melting temperature of these sugars using a new rapid-scanning DSC. Indium, a thermodynamic melting material, and sucrose, glucose, and fructose were analyzed at three heating rates from 1 to 25 °C/min using standard DSC and at seven heating rates from 50 to 2000 °C/min using rapid-scanning DSC. Thermodynamic melting was achieved when the onset temperature (T(m onset)) of the endothermic peak leveled off to a constant value independent of heating rate. The T(m onset) for indium was constant (156.74 ± 0.42 °C) at all heating rates. In the case of fructose, the T(m onset) increased considerably until a heating rate of approximately 698 °C/min, after which the average T(m onset) for the remaining three heating rates was constant at 135.83 ± 1.14 °C. Thus, 135.83 °C is proposed to be the thermodynamic melting temperature of fructose. It is important to note that the heating rate at which this thermodynamic melting temperature is achieved is most likely influenced by the type and amount of trace components (e.g., water and salts) contained in the fructose, which are known to vary widely in sugars. In the case of sucrose and glucose, thermodynamic melting temperatures were not able to be obtained, because the upper limit heating rate used was not fast enough to suppress thermal decomposition and achieve thermodynamic melting, perhaps due to the higher apparent T(m onset) for sucrose and glucose compared to that for fructose.

  1. Mikrokalorimetrinin Hububat Teknolojisinde Kullanım İmkanları I. Differential Scanning Calorimetry (DSC) ve Yöntemin Genel Karakteristikleri

    OpenAIRE

    Certel, Muharrem; Ertugay, Zeki

    1991-01-01

    Hububat teknolojisinde, özellikle hububat ve ürünlerinden kalite kontrollerinde, basit ve hızlı bir ölçüm tekniği ile elde edilen sonuçların çok yönlülüğü nedeniyle, mikrokalorimetri günden güne artan bir önem arz etmektedir. Differential Scanning Calorimetry (DSC), gıdalardaki karbonhidrat, protein ve yağ komponentlerinin fonksiyonel özelliklerinin karakterize edilmesi ve bunların gıda teknolojisinde, özellikle de gıda işlem mühendisliğinde amaca yönelik olarak kullanımına imkan tanıyacak gü...

  2. 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.

  3. Differential Scanning Calorimetry Techniques: Applications in Biology and Nanoscience

    OpenAIRE

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

    2010-01-01

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

  4. [Experimental high energy physics using electromagnetic energy calorimetry

    International Nuclear Information System (INIS)

    In the current year, the major part of the research on this contract was focussed on the construction of the DO detector, testing of production modules (as opposed to prototypes) and in actual coding of tracking software. We are contributing in two areas to the DO Project: the calorimetry, where we are involved in coordination, construction and testing of the central and end calorimeter modules, the test beam program and software development; and the central drift chamber being constructed at Stony Brook and for which we have developed the electronics, test facilities, tracking and general purpose software

  5. Evaluation of polymerization of an experimental bonding resin cured with light emitting diodes using Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    Jafarzadekashi T.

    2009-08-01

    Full Text Available "nBackground and Aim: Extent of polymerization (Ep is the rate at which methacrylate C=C bonds are converted to aliphatic C-C bonds. The higher the Ep value, the better the polymerization of the polymer. If the polymer dose not polymerize sufficiently, it could have destructive effects e.g. releasing monomer, initiator, free radical or insufficient polymerization of hybrid layer. Therefore, measuring the Ep value is very important. Light-emitting diodes (LEDs are becoming increasingly popular in dental practice as they have a long life expectancy. LEDs do not generate infrared wavelength, and have a constant light output. Therefore, comparison of LED and Quartz tungsten halogen (QTH from the point of Ep is important. Differential Scanning Calorimetry (DSC is a proper tool for determining the Ep value, monitoring the process of reaction and reaction kinetics. The aim of this study was to measure the Ep value of a dental bonding containing camphorquinone/amine photoinitiator which were cured by LED and QTH using DSC. "nMaterials and Methods: In this experimental study, 2.5 mg of bonding material were placed in DSC aluminum pans. Two different light cures, LED & QTH (Coltene Company Coltolux ®75 LED Curing Light, were used in this study. The light guide was positioned at a distance of 9mm from the base of the sample chamber. Each sample was photopolymerized for 30 seconds, and the DSC curves were obtained after 100 seconds from initiation of photopolimerization of each sample, at both 23oC and 37oC. The heat of photopolymerization (DH was calculated from the area under the peak of the differential temperature curve. Five samples were used for each condition. The data was analyzed by two-way ANOVA. "nResults: There was highly significant difference between two temperatures in the experimental bonding (pvalue<0.001. Representative DSC curves showed the same kinetic behavior for LED and QTH. "nConclusion: The results revealed that the Ep generated by

  6. Experimental high energy physics using electromagnetic energy calorimetry

    International Nuclear Information System (INIS)

    The major emphasis of the work reported has been on the construction of the DO Project for the Fermilab 2 TeV anti p p collider (TeV I). DO has three major hardware systems - calorimetry, muon and central tracking. In addition, the group is involved in the Brookhaven neutrino experiment E734. The past year has seen publication of precision measurements of sin2Θ/sub w/ from elastic scattering of neutrinos from both electrons and protons. This experiment has just concluded its final data run which is expected to increase the neutrino-electron sample to 180ν/sub μ/e and 90 anti ν/sub μ/e events

  7. Experimental determination of the nucleation rates of undercooled micron-sized liquid droplets based on fast chip calorimetry

    International Nuclear Information System (INIS)

    Highlights: • Fast scanning calorimeter calibration with position dependence. • Calibration of fast scanning calorimeter during cooling. • Quantitative determination of nucleation rates by treating the undercooling as stochastic parameter - Abstract: Accurate thermal analyzes and calorimetry measurements depend on careful calibration measurements. For conventional differential scanning calorimeters (DSC) the calibration procedure is well known. The melting point of different pure metals is measured and compared with literature data to adjust the temperature reading of the calorimeter. Likewise, the measured melting enthalpies of standard reference substances serve for enthalpy calibration. Yet for fast chip calorimetry, new procedures need to be established. For the medium-area and large-area calorimeter chips, this procedure needs to be modified, because the calibration behavior depends on the position of the sample on the measurement area. Additionally, a way to calibrate the calorimeter for measurements performed during cooling will also be shown. For this second aspect, the athermal and diffusionless martensitic phase transformation of Ni49.9–Ti50.1 at% was used. The well-calibrated sensor chips are ideally suited to perform nucleation rate density analyzes based on a statistical approach. Here, the nucleation rate densities of micron-sized pure Sn droplets that had been coated with a non-catalytic coating have been determined by experimental analysis of the statistical variance of the undercooling response

  8. Experimental determination of the nucleation rates of undercooled micron-sized liquid droplets based on fast chip calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Simon, Christian, E-mail: ch.simon@uni-muenster.de; Peterlechner, Martin; Wilde, Gerhard

    2015-03-10

    Highlights: • Fast scanning calorimeter calibration with position dependence. • Calibration of fast scanning calorimeter during cooling. • Quantitative determination of nucleation rates by treating the undercooling as stochastic parameter - Abstract: Accurate thermal analyzes and calorimetry measurements depend on careful calibration measurements. For conventional differential scanning calorimeters (DSC) the calibration procedure is well known. The melting point of different pure metals is measured and compared with literature data to adjust the temperature reading of the calorimeter. Likewise, the measured melting enthalpies of standard reference substances serve for enthalpy calibration. Yet for fast chip calorimetry, new procedures need to be established. For the medium-area and large-area calorimeter chips, this procedure needs to be modified, because the calibration behavior depends on the position of the sample on the measurement area. Additionally, a way to calibrate the calorimeter for measurements performed during cooling will also be shown. For this second aspect, the athermal and diffusionless martensitic phase transformation of Ni{sub 49.9}–Ti{sub 50.1} at% was used. The well-calibrated sensor chips are ideally suited to perform nucleation rate density analyzes based on a statistical approach. Here, the nucleation rate densities of micron-sized pure Sn droplets that had been coated with a non-catalytic coating have been determined by experimental analysis of the statistical variance of the undercooling response.

  9. Monitoring of Pentoxifylline Thermal Behavior by Novel Simultaneous Laboratory Small and Wide X-Ray Scattering (SWAXS) and Differential Scanning Calorimetry (DSC).

    Science.gov (United States)

    Hodzic, Aden; Kriechbaum, Manfred; Schrank, Simone; Reiter, Franz

    2016-01-01

    The thermal and structural evolutions associated to active pharmaceutical ingredient (API) purity are monitored using a laboratory instrument (S3-MicroCaliX) allowing simultaneous time-resolved X-ray scattering at both wide and small angles (SWAXS) as a function of temperature. This is performed simultaneously with differential scanning calorimetric (DSC) that is carried out in the same apparatus at scanning rate of 2 K/min on the same sample in the range from 20° to 200°C. We have studied simultaneous thermal and structural properties of pentoxifylline, as an active pharmaceutical ingredient (API), for its purity quality control. We have found a satisfying API purity, due to obtained melting temperature and enthalpy values, which are in a well agreement with literature. We have also found that the combination of these techniques allows the thermal monitoring of scanning rates of 2 K/min, continuously without the need for static thermal equilibration, particularly for X-ray spectra. Hence, DSC and SWAXS allowing better identification of the structural thermal events recorded by following of the phase transitions simultaneously. This interpretation is much better possible when X-ray scattering at small and wide angles is coupled with DSC from the same sample. Hence, as a laboratory tool, the method presents a reproducible thermal and crystallographic API purity quality control of non-complex samples, as crucial information for pharmaceutical technology. PMID:27467972

  10. Monitoring of Pentoxifylline Thermal Behavior by Novel Simultaneous Laboratory Small and Wide X-Ray Scattering (SWAXS) and Differential Scanning Calorimetry (DSC).

    Science.gov (United States)

    Hodzic, Aden; Kriechbaum, Manfred; Schrank, Simone; Reiter, Franz

    2016-01-01

    The thermal and structural evolutions associated to active pharmaceutical ingredient (API) purity are monitored using a laboratory instrument (S3-MicroCaliX) allowing simultaneous time-resolved X-ray scattering at both wide and small angles (SWAXS) as a function of temperature. This is performed simultaneously with differential scanning calorimetric (DSC) that is carried out in the same apparatus at scanning rate of 2 K/min on the same sample in the range from 20° to 200°C. We have studied simultaneous thermal and structural properties of pentoxifylline, as an active pharmaceutical ingredient (API), for its purity quality control. We have found a satisfying API purity, due to obtained melting temperature and enthalpy values, which are in a well agreement with literature. We have also found that the combination of these techniques allows the thermal monitoring of scanning rates of 2 K/min, continuously without the need for static thermal equilibration, particularly for X-ray spectra. Hence, DSC and SWAXS allowing better identification of the structural thermal events recorded by following of the phase transitions simultaneously. This interpretation is much better possible when X-ray scattering at small and wide angles is coupled with DSC from the same sample. Hence, as a laboratory tool, the method presents a reproducible thermal and crystallographic API purity quality control of non-complex samples, as crucial information for pharmaceutical technology.

  11. Monitoring of Pentoxifylline Thermal Behavior by Novel Simultaneous Laboratory Small and Wide X-Ray Scattering (SWAXS) and Differential Scanning Calorimetry (DSC)

    Science.gov (United States)

    Hodzic, Aden; Kriechbaum, Manfred; Schrank, Simone; Reiter, Franz

    2016-01-01

    The thermal and structural evolutions associated to active pharmaceutical ingredient (API) purity are monitored using a laboratory instrument (S3-MicroCaliX) allowing simultaneous time-resolved X-ray scattering at both wide and small angles (SWAXS) as a function of temperature. This is performed simultaneously with differential scanning calorimetric (DSC) that is carried out in the same apparatus at scanning rate of 2 K/min on the same sample in the range from 20° to 200°C. We have studied simultaneous thermal and structural properties of pentoxifylline, as an active pharmaceutical ingredient (API), for its purity quality control. We have found a satisfying API purity, due to obtained melting temperature and enthalpy values, which are in a well agreement with literature. We have also found that the combination of these techniques allows the thermal monitoring of scanning rates of 2 K/min, continuously without the need for static thermal equilibration, particularly for X-ray spectra. Hence, DSC and SWAXS allowing better identification of the structural thermal events recorded by following of the phase transitions simultaneously. This interpretation is much better possible when X-ray scattering at small and wide angles is coupled with DSC from the same sample. Hence, as a laboratory tool, the method presents a reproducible thermal and crystallographic API purity quality control of non-complex samples, as crucial information for pharmaceutical technology. PMID:27467972

  12. An experimental study of phase transformations in an Al-Zn-Mg-Zr alloy: DSC and hot microhardness and measurements

    International Nuclear Information System (INIS)

    Isothermal hot microhardness and multi-scan differential scanning calorimetry (DSC) experiments were carried out on an AlZnMgZr, 7000 series aluminum alloy to characterize the evolution and dissolution of GP zones and the formation of the η' phase. Three stages of hardness evolution with aging time were observed for aging in the 25-100 deg C temperature range corresponding to GP zone formation, simultaneous GP zone dissolution and η' formation, and η' formation and coarsening. The isothermal activation energy for the GP zone formation from hot microhardness measurements was about 0.35 eV per atom comparable with that from previous hardness measurements reported in the literature. From variable heating rate DSC scans, the activation energies for GP zone formation and dissolution were 0.75 and 0.92 eV per atom, respectively. The activation energy for η' phase formation and growth of the asquenched specimens as well as aged specimens was about 0.59 eV per atom, and the Avrami index for the transformation was inferred to be in the range 2.3-2.8 (±20%). The activation energies are discussed in terms of various diffusional processes in the Al matrix and are compared with values reported in the literature. (author). 37 refs., 3 tabs., 9 figs

  13. The use of Differential Scanning Calorimetry (DSC) to characterize phase diagrams of ionic mixtures of 1-n-butyl-3-methylimidazolium chloride and niobium chloride or zinc chloride

    International Nuclear Information System (INIS)

    The thermal behavior of the BMICl/NbCl5 and BMICl/ZnCl2 mixtures was investigated by DSC and correlated with previous studies using Raman spectroscopy. Combining both results, it was possible to built the phase diagram for these mixtures and suggest the formation of different compounds and the equilibria in the euthetic mixtures. The phase diagram of BMICl and NbCl5 mixture showed that probably only one compound is formed at XNbCl5 = 0.50 (BMINbCl6) and euthetic mixtures are present in the 0 ≤ XNbCl5 ≤ 0.50 composition range. For the BMICl and ZnCl2, four different compounds were detected: (BMI)2(ZnCl4) for XZnCl2 = 0.35; (BMI)2(Zn2Cl6); (BMI)2(Zn3Cl8) and (BMI)2(Zn4Cl10) for XZnCl2 = 0.70, and between these isoplets euthetic mixtures are formed.

  14. Effect of milling on DSC thermogram of excipient adipic acid.

    Science.gov (United States)

    Ng, Wai Kiong; Kwek, Jin Wang; Yuen, Aaron; Tan, Chin Lee; Tan, Reginald

    2010-03-01

    The purpose of this research was to investigate why and how mechanical milling results in an unexpected shift in differential scanning calorimetry (DSC) measured fusion enthalpy (Delta(fus)H) and melting point (T(m)) of adipic acid, a pharmaceutical excipient. Hyper differential scanning calorimetry (hyper-DSC) was used to characterize adipic acid before and after ball-milling. An experimental study was conducted to evaluate previous postulations such as electrostatic charging using the Faraday cage method, crystallinity loss using powder X-ray diffraction (PXRD), thermal annealing using DSC, impurities removal using thermal gravimetric analysis (TGA) and Karl Fischer titration. DSC thermograms showed that after milling, the values of Delta(fus)H and T(m) were increased by approximately 9% and 5 K, respectively. Previous suggestions of increased electrostatic attraction, change in particle size distribution, and thermal annealing during measurements did not explain the differences. Instead, theoretical analysis and experimental findings suggested that the residual solvent (water) plays a key role. Water entrapped as inclusions inside adipic acid during solution crystallization was partially evaporated by localized heating at the cleaved surfaces during milling. The correlation between the removal of water and melting properties measured was shown via drying and crystallization experiments. These findings show that milling can reduce residual solvent content and causes a shift in DSC results.

  15. Fast differential scanning calorimetry of liquid samples with chips

    DEFF Research Database (Denmark)

    Splinter, R.; van Herwaarden, A. W.; van Wetten, I. A.;

    2015-01-01

    Based on a modified version of standard chips for fast differential scanning calorimetry, DSC of liquid samples has been performed at temperature scan rates of up to 1000 °C/s. This paper describes experimental results with the protein lysozyme, bovine serum, and olive oil. The heating and cooling...

  16. Análise cinética da cura de adesivos de taninos das cascas de três espécies de Eucalyptus por calorimetria diferencial exploratória (DSC Kinetic analysis of bark tannin adhesives from three species of Eucalyptus by differential scanning calorimetry (DSC

    Directory of Open Access Journals (Sweden)

    Fábio Akira Mori

    2002-08-01

    Full Text Available O objetivo deste trabalho foi analisar a cinética de cura de adesivos à base de taninos de Eucalyptus grandis, Eucalyptus saligna e Eucalyptus urophylla por calorimetria diferencial exploratória (DSC, comparando-a com a cinética de cura de adesivos comerciais: fenol-formaldeído e de taninos de acácia-negra (Acacia mollissima D.Wild. Verificou-se que o adesivo de taninos de Eucalyptus urophylla apresentou os parâmetros cinéticos (energia de ativação, entalpia, temperatura de pico e ordem de reação mais próximos aos do adesivo comercial de taninos de acácia-negra, que foram totalmente diferentes do adesivo à base de fenol-formaldeído. Com base nestes parâmetros constatou-se que, em relação aos outros dois, o adesivo de taninos de Eucalyptus urophylla é o mais adequado para colagem, uma vez que em condições industriais ele necessitará de uso mínimo de energia e de tempo de prensagem durante o processo de colagem.This work aimed to analyze the cure kinetics of Eucalyptus grandis, Eucalyptus saligna and Eucalyptus urophylla tannins based adhesives by differential scanning calorimetry (DSC. Another objective was to compare cure kinetics of Eucalyptus tannin adhesives with the cure kinetics of phenol-formaldehyde and Wattle black (Acacia mollissima D. Wild tannin commercial adhesives. It was observed that the Eucalyptus urophylla tannin adhesives presented kinetic parameters (activation energy, entalpia, peak temperature and reaction order similar to the Wattle black commercial tannin adhesives but were different from the phenol-formaldehyde adhesives. Based on these parameters it was concluded that the Eucalyptus urophylla tannin adhesives are more adequate for wood bonding than the other two Eucalyptus tannin adhesives. Under industrial conditions, Eucalyptus urophylla tannin adhesive will need a minimum energy and pressing.

  17. Analysis of RNA folding and ligand binding by conventional and high-throughput calorimetry.

    Science.gov (United States)

    Sokoloski, Joshua E; Bevilacqua, Philip C

    2012-01-01

    Noncoding RNAs serve myriad functions in the cell, but their biophysical properties are not well understood. Calorimetry offers direct and label-free means for characterizing the ligand-binding and thermostability properties of these RNA. We apply two main types of calorimetry--isothermal titration calorimetry (ITC) and differential scanning calorimetry (DSC)--to the characterization of these functional RNA molecules. ITC can describe ligand binding in terms of stoichiometry, affinity, and heat (enthalpy), while DSC can provide RNA stability in terms of heat capacity, melting temperature, and folding enthalpy. Here, we offer detailed experimental protocols for studying such RNA systems with commercially available conventional and high-throughput ITC and DSC instruments.

  18. The Use of Differential Scanning Calorimetry in Studies of Wax Deposition: Measuring the Solid Formation and Binary Solid-Liquid Equilibrium Phase Diagrams La DSC (Differential Scanning Calorimetry appliquée à l'étude des dépôts de paraffines : mesure des quantités de dépôts et des diagrammes de phases (liquide-solide de mélange binaire

    Directory of Open Access Journals (Sweden)

    Coutinho J. A. P.

    2006-12-01

    Full Text Available The studies of wax formation in hydrocarbon mixtures, both crudes and refined products such as diesels and fuels, require measuring techniques able to deal with the solid phase behaviour. Experimental data on phase equilibria is important to understand the crystallisation of paraffins and for the development of thermodynamical models, that can describe it. It is here shown how the information obtained from Differential Scanning Calorimetry (DSC measurements can be used to assess the amount of solid forming when a fluid is cooled and also to make faster measurements of phase diagrams for binary systems where no solid solutions exist. The measurements performed with the proposed methods present a good agreement with literature data. L'étude de la cristallisation des paraffines dans les mélanges hydrocarbonés, qu'il s'agisse de pétroles bruts ou de produits raffinés tels que le Diesel ou le fioul, nécessite l'utilisation de techniques expérimentales permettant de déterminer le diagramme de phases. L'acquisition de ces données est primordiale, à la fois pour comprendre les mécanismes de la cristallisation et pour le développement des modèles thermodynamiques. Dans cet article, nous montrons comment l'analyse calorimétrique différentielle peut permettre d'estimer la quantité de solide déposée en fonction de la température et de mesurer les diagrammes de phases de mélanges binaires ne formant pas de solutions solides. Les résultats obtenus avec la méthode proposée s'accordent avec les données de la littérature.

  19. An experimental study of the (Ti-6Al-4V)-xH phase diagram using in situ synchrotron XRD and TGA/DSC techniques.

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Pei; Fang, Z. Zak; Koopman, Mark; Paramore, James D.; Chandran, K. S. Ravi; Ren, Yang; Lu, Jun

    2015-02-01

    Hydrogen has been investigated for decades as a temporary alloying element to refine the microstructure of Ti-6Al-4V, and is now being used in a novel powder metallurgy method known as "hydrogen sintering and phase transformation". Pseudo-binary phase diagrams of (Ti-6Al-4V)-xH have been studied and developed, but are not well established due to methodological limitations. In this paper, in situ studies of phase transformations during hydrogenation and dehydrogenation of (Ti-6Al-4V)-xH alloys were conducted using high-energy synchrotron X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The eutectoid phase transformation of β ↔ α + δ was observed in the (Ti-6Al-4V)-xH alloy via in situ synchrotron XRD at 211 °C with a hydrogen concentration of 37.5 at.% (measured using TGA-DSC). The relationships of hydrogen composition to partial pressure and temperature were investigated in the temperature range 450-900°C. Based on these results, a partial pseudo-binary phase diagram of (Ti-6Al-4V)-xH is proposed for hydrogen compositions up to 60 at.% in the temperature range 100-900°C. Using the data collected in real time under controlled parameters of temperature, composition and hydrogen partial pressure, this work characterizes relevant phase transformations and microstructural evolution for practical titanium-hydrogen technologies of Ti-6Al-4V.

  20. DSC Study of Collagen in Disc Disease

    OpenAIRE

    S. Skrzyński; Sionkowska, A.; A. Marciniak

    2010-01-01

    Differential scanning calorimetry (DSC) has been used to estimate the effect of disc disease on the collagen helix-coil transition and morphology for tissue extracted from patients during surgical operation. Forty discs were obtained from patients with degenerative disc disease undergoing surgery for low back pain. The patients were in the age between 20 and 70 years old. The specimens were kept wet during DSC experiment. The data allow the comparison between thermal stability of collagen ti...

  1. Modern Analysis of Protein Folding by Differential Scanning Calorimetry.

    Science.gov (United States)

    Ibarra-Molero, Beatriz; Naganathan, Athi N; Sanchez-Ruiz, Jose M; Muñoz, Victor

    2016-01-01

    Differential scanning calorimetry (DSC) is a very powerful tool for investigating protein folding and stability because its experimental output reflects the energetics of all conformations that become minimally populated during thermal unfolding. Accordingly, analysis of DSC experiments with simple thermodynamic models has been key for developing our understanding of protein stability during the past five decades. The discovery of ultrafast folding proteins, which have naturally broad conformational ensembles and minimally cooperative unfolding, opens the possibility of probing the complete folding free energy landscape, including those conformations at the top of the barrier to folding, via DSC. Exploiting this opportunity requires high-quality experiments and the implementation of novel analytical methods based on statistical mechanics. Here, we cover the recent exciting developments in this front, describing the new analytical procedures in detail as well as providing experimental guidelines for performing such analysis.

  2. Nucleic acid-lipid membrane interactions studied by DSC.

    Science.gov (United States)

    Giatrellis, Sarantis; Nounesis, George

    2011-01-01

    The interactions of nucleic acids with lipid membranes are of great importance for biological mechanisms as well as for biotechnological applications in gene delivery and drug carriers. The optimization of liposomal vectors for clinical use is absolutely dependent upon the formation mechanisms, the morphology, and the molecular organization of the lipoplexes, that is, the complexes of lipid membranes with DNA. Differential scanning calorimetry (DSC) has emerged as an efficient and relatively easy-to-operate experimental technique that can straightforwardly provide data related to the thermodynamics and the kinetics of the DNA-lipid complexation and especially to the lipid organization and phase transitions within the membrane. In this review, we summarize DSC studies considering nucleic acid-membrane systems, accentuating DSC capabilities, and data analysis. Published work involving cationic, anionic, and zwitterionic lipids as well as lipid mixtures interacting with RNA and DNA of different sizes and conformations are included. It is shown that despite limitations, issues such as DNA- or RNA-induced phase separation and microdomain lipid segregation, liposomal aggregation and fusion, alterations of the lipid long-range molecular order, as well as membrane-induced structural changes of the nucleic acids can be efficiently treated by systematic high-sensitivity DSC studies.

  3. Application and use of isothermal calorimetry in pharmaceutical development.

    Science.gov (United States)

    O'Neill, Michael A A; Gaisford, Simon

    2011-09-30

    There are many steps involved in developing a drug candidate into a formulated medicine and many involve analysis of chemical interaction or physical change. Calorimetry is particularly suited to such analyses as it offers the capacity to observe and quantify both chemical and physical changes in virtually any sample. Differential scanning calorimetry (DSC) is ubiquitous in pharmaceutical development, but the related technique of isothermal calorimetry (IC) is complementary and can be used to investigate a range of processes not amenable to analysis by DSC. Typically, IC is used for longer-term stability indicating or excipient compatibility assays because both the temperature and relative humidity (RH) in the sample ampoule can be controlled. However, instrument design and configuration, such as titration, gas perfusion or ampoule-breaking (solution) calorimetry, allow quantification of more specific values, such as binding enthalpies, heats of solution and quantification of amorphous content. As ever, instrument selection, experiment design and sample preparation are critical to ensuring the relevance of any data recorded. This article reviews the use of isothermal, titration, gas-perfusion and solution calorimetry in the context of pharmaceutical development, with a focus on instrument and experimental design factors, highlighted with examples from the recent literature.

  4. Electromagnetic calorimetry

    International Nuclear Information System (INIS)

    Electromagnetic calorimetry forms a key element of almost all current high energy particle physics detectors and has widespread application in related experimental fields such as nuclear physics and astro-particle physics. It will play a particularly important role in the latest generation of experiments at the CERN Large Hadron Collider (LHC), where it is expected that high energy electrons and photons will provide some of the clearest signatures for new discoveries. This article introduces the basic concepts underlying electromagnetic calorimetry and illustrates how these principles have been applied in recent and current detector designs, explaining the connection between technical choices and specific physics goals. Designs are described in sufficient detail to demonstrate the compromises that have to be made in achieving optimum performance within practical constraints. The main emphasis is on the LHC experiments, which provide outstanding examples of the state-of-the-art. Selected examples from other domains, such as nuclear physics and neutrino experiments are also considered and particular attention is given to calorimeter design studies for the proposed International Linear Collider (ILC) where the concept of Particle Flow Analysis is being used as a guiding influence in the overall detector optimization.

  5. Characterization of the Polycaprolactone Melt Crystallization: Complementary Optical Microscopy, DSC, and AFM Studies

    OpenAIRE

    Speranza, V; Sorrentino, A; F. De Santis; Pantani, R.

    2014-01-01

    The first stages of the crystallization of polycaprolactone (PCL) were studied using several techniques. The crystallization exotherms measured by differential scanning calorimetry (DSC) were analyzed and compared with results obtained by polarized optical microscopy (POM), rheology, and atomic force microscope (AFM). The experimental results suggest a strong influence of the observation scale. In particular, the AFM, even if limited on time scale, appears to be the most sensitive technique t...

  6. Análise cinética da cura de adesivos de taninos das cascas de três espécies de Eucalyptus por calorimetria diferencial exploratória (DSC) Kinetic analysis of bark tannin adhesives from three species of Eucalyptus by differential scanning calorimetry (DSC)

    OpenAIRE

    Fábio Akira Mori; Benedito Rocha Vital; Alexandre Santos Pimenta; Paulo Fernando Trugilho; Gulab Newandram Jahm; Ricardo Marius Della Lucia

    2002-01-01

    O objetivo deste trabalho foi analisar a cinética de cura de adesivos à base de taninos de Eucalyptus grandis, Eucalyptus saligna e Eucalyptus urophylla por calorimetria diferencial exploratória (DSC), comparando-a com a cinética de cura de adesivos comerciais: fenol-formaldeído e de taninos de acácia-negra (Acacia mollissima D.Wild). Verificou-se que o adesivo de taninos de Eucalyptus urophylla apresentou os parâmetros cinéticos (energia de ativação, entalpia, temperatura de pico e ordem de ...

  7. The analysis of Al-based alloys by calorimetry: quantitative analysis of reactions and reaction kinetics

    OpenAIRE

    Starink, M.J.

    2004-01-01

    Differential scanning calorimetry (DSC) and isothermal calorimetry have been applied extensively to the analysis of light metals, especially Al based alloys. Isothermal calorimetry and differential scanning calorimetry are used for analysis of solid state reactions, such as precipitation, homogenisation, devitrivication and recrystallisation; and solid–liquid reactions, such as incipient melting and solidification, are studied by differential scanning calorimetry. In producing repeatable calo...

  8. Comportamento de cura de adesivo epoxídico contendo grupo mercaptana avaliado por espectroscopia no infravermelho (MIR/NIR e calorimetria exploratória diferencial (DSC Cure behavior of epoxy adhesive containig mercaptan group evaluated by infrared spectroscopy (MIR/NIR and differential scanning calorimetry (DSC

    Directory of Open Access Journals (Sweden)

    Hilzette P. C. Andrade

    2008-01-01

    Full Text Available No presente trabalho, a flexibilidade de um adesivo epoxídico contendo diglicidiléter de bisfenol A (DGEBA e dietilenotriamina (DETA como agente de cura foi modificada pela adição de um segundo componente contendo grupos mercaptana (CAPCURE. A adição de amianto ao adesivo contendo CAPCURE também foi avaliada. As reações entre os grupos epoxídicos e os grupos amina, assim como entre os grupos epoxídicos e os grupos mercaptana, foram estudadas nas regiões espectrais do infravermelho médio (MIR e próximo (NIR. Observou-se que o amianto não interfere nas reações de cura e que a espectroscopia FT-NIR evidencia melhor as alterações espectrométricas ocorridas durante as reações em relação à análise FT-MIR. O tempo das reações de cura foi monitorado por calorimetria exploratória diferencial (DSC, observando-se que a introdução do CAPCURE acelerou a cura da resina. A energia de ativação (Ea das reações de cura foi obtida pelos métodos de Barrett e Borchardt-Daniels. Os adesivos contendo CAPCURE mostraram Ea em torno de 30 kJ.mol-1, enquanto o adesivo DGEBA/DETA apresentou Ea de 46 kJ.mol-1, ambas calculadas pelo método de Barrett.In the present work, the flexibility of an epoxy adhesive containing diglycidylether of bisphenol-A (DGEBA and diethylenetriamine (DETA as curing agent was changed by the addition of a second component containing mercaptan groups (CAPCURE. The addition of asbestos as a filler in the adhesive containing CAPCURE was also evaluated. Epoxy-amine and epoxy-mercaptan reactions were studied in NIR and MIR spectral regions. The filler addition did not cause influence on the cure reactions and spectrometric changes of cure reactions could be better observed by FT-NIR than FT-MIR analysis. The cure reaction time was monitored by DSC experiments and it was observed that the introduction of CAPCURE accelerated the cure reaction. The activation energies (Ea of curing reactions were obtained using Barrett

  9. Oil Analysis by Fast DSC

    OpenAIRE

    Wetten, I.A.; Van Herwaarden, A.W.; Splinter, R.; Ruth, van, S.M.

    2014-01-01

    Thermal analysis of Olive and Sunflower Oil is done by Fast DSC to evaluate its potential to replace DSC for adulteration detection. DSC measurements take hours, Fast DSC minutes. Peak temperatures of the crystallisation peak in cooling for different Olive and Sunflower Oils are both comparable to DSC, but not always distinguishable. The heating curves of Olive and Sunflower Oil show more differences. Compared to DSC, Fast DSC shows lower peak temperatures for heating curve peaks.

  10. Calorimetry of Nucleic Acids.

    Science.gov (United States)

    Rozners, Eriks; Pilch, Daniel S; Egli, Martin

    2015-12-01

    This unit describes the application of calorimetry to characterize the thermodynamics of nucleic acids, specifically, the two major calorimetric methodologies that are currently employed: differential scanning (DSC) and isothermal titration calorimetry (ITC). DSC is used to study thermally induced order-disorder transitions in nucleic acids. A DSC instrument measures, as a function of temperature (T), the excess heat capacity (C(p)(ex)) of a nucleic acid solution relative to the same amount of buffer solution. From a single curve of C(p)(ex) versus T, one can derive the following information: the transition enthalpy (ΔH), entropy (ΔS), free energy (ΔG), and heat capacity (ΔCp); the state of the transition (two-state versus multistate); and the average size of the molecule that melts as a single thermodynamic entity (e.g., the duplex). ITC is used to study the hybridization of nucleic acid molecules at constant temperature. In an ITC experiment, small aliquots of a titrant nucleic acid solution (strand 1) are added to an analyte nucleic acid solution (strand 2), and the released heat is monitored. ITC yields the stoichiometry of the association reaction (n), the enthalpy of association (ΔH), the equilibrium association constant (K), and thus the free energy of association (ΔG). Once ΔH and ΔG are known, ΔS can also be derived. Repetition of the ITC experiment at a number of different temperatures yields the ΔCp for the association reaction from the temperature dependence of ΔH.

  11. Application of experimental design in examination of the dissolution rate of carbamazepine from formulations: Characterization of the optimal formulation by DSC, TGA, FT-IR and PXRD analysis

    Directory of Open Access Journals (Sweden)

    Krstić Marko

    2015-01-01

    Full Text Available Poor solubility is one of the key reasons for the poor bioavailability of these drugs. This paper displays a formulation of a solid surfactant system with carbamazepine, in order to increase its dissolution rate. Solid state surfactant systems are formed by application of fractal experimental design. Poloxamer 237 and Poloxamer 338 were used as surfactants and Brij® 35 was used as the co-surfactant. The ratios of the excipients and carbamazepine were varied and their effects on the dissolution rate of carbamazepine were examined. Moreover, the effects of the addition of natural (diatomite and a synthetic adsorbent carrier (Neusiline UFL2 on the dissolution rate of carbamazepine were also tested. The prepared surfactant systems were characterized and the influence of the excipients on possible changes of the polymorphous form of carbamazepine examined by application of analytical techniques (DSC, TGA, FT-IR, PXRD. It was determined that an appropriate selection of the excipient type and ratio could provide a significant increase in the carbamazepine dissolution rate. By application of analytical techniques, it was found that that the employed excipients induce a transition of carbamazepine into the amorphous form and that the selected sample was stable for three months, when kept under ambient conditions. [Projekat Ministarstva nauke Republike Srbije, br. TR34007

  12. Melting of Single Lipid Components in Binary Lipid Mixtures: A Comparison between FTIR Spectroscopy, DSC and Monte Carlo Simulations

    CERN Document Server

    Fidorra, M; Seeger, H M

    2007-01-01

    Monte Carlo (MC) Simulations, Differential Scanning Calorimetry (DSC) and Fourier Transform InfraRed (FTIR) spectroscopy were used to study the melting behavior of single lipid components in two-component membranes of 1,2-Dimyristoyl-D54-sn-Glycero-3-Phosphocholine (DMPC-d54) and 1,2-Distearoyl-sn-Glycero-3-Phosphocholine (DSPC). Microscopic information on the temperature dependent melting of the single lipid species could be investigated using FTIR. The microscopic behavior measured could be well described by the results from the MC simulations. These simulations also allowed to calculate heat capacity profiles as determined with DSC. These ones provide macroscopic information about melting enthalpies and entropy changes which are not accessible with FTIR. Therefore, the MC simulations allowed us to link the two different experimental approaches of FTIR and DSC.

  13. Oil Analysis by Fast DSC

    NARCIS (Netherlands)

    Wetten, I.A.; Herwaarden, A.W.; Splinter, R.; Ruth, van S.M.

    2014-01-01

    Thermal analysis of Olive and Sunflower Oil is done by Fast DSC to evaluate its potential to replace DSC for adulteration detection. DSC measurements take hours, Fast DSC minutes. Peak temperatures of the crystallisation peak in cooling for different Olive and Sunflower Oils are both comparable to D

  14. Modern calorimetry: going beyond tradition

    OpenAIRE

    Jeong, Y. H.

    2001-01-01

    Calorimetry has been a traditional tool for obtaining invaluable thermodynamic information of matter, the free energy. We describe recent efforts to go beyond this traditional calorimetry: After introducing dynamic heat capacity, we present the various experimental methods to measure it. Applications and future prospects are also given.

  15. Hadron Calorimetry

    International Nuclear Information System (INIS)

    Hadron calorimetry has been a rapidly developing field in the past few decades. Perhaps not too far in the future, a realistic calorimeter will be capable of measuring the energies of all the fundamental particles with ∼1% precision. Currently, calorimeters with unprecedented complexity attest to the knowledge and experience that have been accumulated in high energy physics. In this review, we touch on fundamental concepts and explain new developments that we expect to be important in the future. In addition to describing applications in accelerator-based high energy physics, we briefly mention the use of hadron calorimeters in other fields.

  16. Characterization of the polycaprolactone melt crystallization: complementary optical microscopy, DSC, and AFM studies.

    Science.gov (United States)

    Speranza, V; Sorrentino, A; De Santis, F; Pantani, R

    2014-01-01

    The first stages of the crystallization of polycaprolactone (PCL) were studied using several techniques. The crystallization exotherms measured by differential scanning calorimetry (DSC) were analyzed and compared with results obtained by polarized optical microscopy (POM), rheology, and atomic force microscope (AFM). The experimental results suggest a strong influence of the observation scale. In particular, the AFM, even if limited on time scale, appears to be the most sensitive technique to detect the first stages of crystallization. On the contrary, at least in the case analysed in this work, rheology appears to be the least sensitive technique. DSC and POM provide closer results. This suggests that the definition of induction time in the polymer crystallization is a vague concept that, in any case, requires the definition of the technique used for its characterization.

  17. Quantum Calorimetry

    Science.gov (United States)

    Stahle, Caroline Kilbourne; McCammon, Dan; Irwin, Kent D.

    1999-01-01

    Your opponent's serve was almost perfect, but you vigorously returned it beyond his outstretched racquet to win the point. Now the tennis ball sits wedged in the chain-link fence around the court. What happened to the ball's kinetic energy? It has gone to heat the fence, of course, and you realize that if the fence were quite colder, you might be able to measure that heat and determine just how energetic your swing really was. Calorimetry has been a standard measurement technique since James Joule and Julius von Mayer independently concluded, about 150 years ago, that heat is a form of energy. But only in the past 15 years or so has calorimetry been applied, at millikelvin temperatures, to the measurement of the energy of individual photons and particles with exquisite sensitivity. In this article, we have tried to show that continuing research in low-temperature physics leads to a greater understanding of high-temperature astrophysics. Adaptations of the resulting spectrometers will be useful tool for fields of research beyond astrophysics.

  18. Characterisation of gas hydrates formation and dissociation using high pressure DSC

    Energy Technology Data Exchange (ETDEWEB)

    Le Parlouer, P. [Thermal Consulting, Caluire (France); Etherington, G. [Setaram Inc., Pennsauken, NJ (United States)

    2008-07-01

    This paper provided details of an innovative methodology that used a high pressure micro-scale differential scanning calorimetry (DSC) method to characterize the thermodynamic properties and kinetics of gas hydrate formation. The calorimeter was based on a symmetrical heat flux design that used a Peltier cooling and heating principle. No refrigerating fluids were required. The method described phase transitions in relation to time, temperature and pressure. The DSC method was designed for use with gas hydrates trapped in marine sediments; hydrate formation in drilling muds and annulars during offshore oil and gas extraction; the storage and transportation of natural gas; and gas hydrate formation and dissociation for cold storage and transportation. Tests demonstrated that the DSC accurately predicted the formation of gas hydrates under high pressure conditions. Experimental studies were conducted to investigate salt solutions under methane pressure; and hydrate dissociation in a sodium chloride (NaC1) and ethyleneglycol solution. Data obtained comparing the method with classical PVT techniques showed that the MicroDSC technique was less time-consuming and required smaller sample volumes. It was concluded that the method is suitable for use with various types of fluids. 13 refs., 7 figs.

  19. Vapor pressure data for fatty acids obtained using an adaptation of the DSC technique

    Energy Technology Data Exchange (ETDEWEB)

    Matricarde Falleiro, Rafael M. [LPT, Departamento de Processos Quimicos (DPQ), Faculdade de Engenharia Quimica, Universidade de Campinas (UNICAMP), 13083-852 Campinas - SP (Brazil); Akisawa Silva, Luciana Y. [Departamento de Ciencias Exatas e da Terra, Universidade Federal de Sao Paulo (UNIFESP), 09972-270 Diadema - SP (Brazil); Meirelles, Antonio J.A. [EXTRAE, Departamento de Engenharia de Alimentos (DEA), Faculdade de Engenharia de Alimentos, Universidade de Campinas (UNICAMP), 13083-862 Campinas - SP (Brazil); Kraehenbuehl, Maria A., E-mail: mak@feq.unicamp.br [LPT, Departamento de Processos Quimicos (DPQ), Faculdade de Engenharia Quimica, Universidade de Campinas (UNICAMP), 13083-852 Campinas - SP (Brazil)

    2012-11-10

    Highlights: Black-Right-Pointing-Pointer Vapor pressure data of fatty acids were measured by Differential Scanning Calorimetry. Black-Right-Pointing-Pointer The DSC technique is especially advantageous for expensive chemicals. Black-Right-Pointing-Pointer High heating rate was used for measuring the vapor pressure data. Black-Right-Pointing-Pointer Antoine constants were obtained for the selected fatty acids. - Abstract: The vapor pressure data for lauric (C{sub 12:0}), myristic (C{sub 14:0}), palmitic (C{sub 16:0}), stearic (C{sub 18:0}) and oleic (C{sub 18:1}) acids were obtained using Differential Scanning Calorimetry (DSC). The adjustments made in the experimental procedure included the use of a small sphere (tungsten carbide) placed over the pinhole of the crucible (diameter of 0.8 mm), making it possible to use a faster heating rate than that of the standard method and reducing the experimental time. The measurements were made in the pressure range from 1333 to 9333 Pa, using small sample quantities of fatty acids (3-5 mg) at a heating rate of 25 K min{sup -1}. The results showed the effectiveness of the technique under study, as evidenced by the low temperature deviations in relation to the data reported in the literature. The Antoine constants were fitted to the experimental data whose values are shown in Table 5.

  20. Physical ageing studies of poly(ethylene terephthalate) using SANS and DSC

    Energy Technology Data Exchange (ETDEWEB)

    Ellis, Andrew [Department of Metallurgy and Materials, University of Birmingham, Birmingham B15 2TT (United Kingdom); Gordon, Duncan [Department of Metallurgy and Materials, University of Birmingham, Birmingham B15 2TT (United Kingdom); King, Stephen [ISIS Spallation Neutron Source, Rutherford-Appleton Laboratory, Didcot, Oxfordshire OX11 0QX (United Kingdom); Jenkins, Mike [Department of Metallurgy and Materials, University of Birmingham, Birmingham B15 2TT (United Kingdom)]. E-mail: M.J.Jenkins@bham.ac.uk

    2006-11-15

    The process of physical ageing in a blend of deuterated and hydrogenated poly(ethylene terephalate) has been investigated using a combination of differential scanning calorimetry (DSC) and small-angle neutron scattering (SANS). The development of an endothermic peak on the glass transition has been shown using DSC. Furthermore, the radius of gyration was found to decrease during physical ageing.

  1. Performance Evaluation of DSC Windows for Buildings

    Directory of Open Access Journals (Sweden)

    Jun-Gu Kang

    2013-01-01

    Full Text Available Interest in BIPV systems with dye-sensitized solar cells (DSCs that can replace building windows has increased for zero energy buildings. Although DSCs have lower efficiency in terms of electricity generation than silicon solar cells, they allow light transmission and application of various colors; they also have low production costs, which make them especially suitable for BIPV systems. DSC research is interdisciplinary, involving electrical, chemical, material, and metal engineering. A considerable amount of research has been conducted on increasing the electrical efficiency of DSC and their modules. However, there has not been sufficient research on building applications of DSC systems. The aim of this study is to evaluate the optical performance and thermal performance of DSC windows in buildings. For this study, DSC experimental models with different thicknesses and dye colors were manufactured, and their optical properties, such as transmittance and reflectivity, were measured by a spectrometer. The thermal and optical characteristics of double-glazed windows with DSC were analyzed with a window performance analysis program, WINDOW 6.0.

  2. DSC Study on the Polyacrylonitrile Precursors for Carbon Fibers

    Institute of Scientific and Technical Information of China (English)

    Wangxi ZHANG; Musen LI

    2005-01-01

    Different polyacrylonitrile (PAN) precursor fibers that displayed various thermal properties were studied by using differential scanning calorimetry (DSC). Results showed that some commercial PAN precursor fibers displayed double separated peaks and these fibers were of high quality because of their process stability during their conversion to carbon fibers of high performance. Some fabrication processes, such as spinning, drawing, could not apparently change the DSC features of a PAN precursor fiber. It was concluded that the thermal properties of a PAN precursor fiber was mainly determined from its comonomer content type and compositions.

  3. Determination of the oxidative stability by DSC of vegetable oils from the Amazonian area.

    Science.gov (United States)

    Pardauil, Juliana J R; Souza, Luiz K C; Molfetta, Fábio A; Zamian, José R; Rocha Filho, Geraldo N; da Costa, C E F

    2011-05-01

    Differential scanning calorimetry (DSC) and a Rancimat method apparatus were applied to evaluate the oxidative stability of buriti pulp oil (Mauritia flexuosa Mart), rubber seed oil (Hevea brasiliensis), and passion fruit oil (Passiflora edulis). The Rancimat measurements taken for the oxidative induction times were performed under isothermal conditions at 100°C and in an air atmosphere. The DSC technique involved the oxidation of oil samples in an oxygen-flow DSC cell. The DSC cell temperature was set at five different isothermal temperatures: 100, 110, 120, 130 and 140°C. During the oxidation reaction, an increase in heat was observed as a sharp exothermic curve. The value T(0) represents the oxidative induction time, which is determined from the downward extrapolated DSC oxidative curve verses the time axis. These curves indicate a good correlation between the DSC T(0) and oxidative stability index (OSI) values. The DSC method is useful because it consumes less time and less sample.

  4. 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

  5. Thermal analysis and safety information for metal nanopowders by DSC

    International Nuclear Information System (INIS)

    Highlights: • Metal nanopowders are common and frequently employed in industry. • Nano iron powder experimental results of To were 140–150 °C. • Safety information can benefit relevant metal powders industries. - Abstract: Metal nanopowders are common and frequently employed in industry. Iron is mostly applied in high-performance magnetic materials and pollutants treatment for groundwater. Zinc is widely used in brass, bronze, die casting metal, alloys, rubber, and paints, etc. Nonetheless, some disasters induced by metal powders are due to the lack of related safety information. In this study, we applied differential scanning calorimetry (DSC) and used thermal analysis software to evaluate the related thermal safety information, such as exothermic onset temperature (To), peak of temperature (Tp), and heat of reaction (ΔH). The nano iron powder experimental results of To were 140–150 °C, 148–158 °C, and 141–149 °C for 15 nm, 35 nm, and 65 nm, respectively. The ΔH was larger than 3900 J/g, 5000 J/g, and 3900 J/g for 15 nm, 35 nm, and 65 nm, respectively. Safety information can benefit the relevant metal powders industries for preventing accidents from occurring

  6. The slow relaxation dynamics in active pharmaceutical ingredients studied by DSC and TSDC: Voriconazole, miconazole and itraconazole.

    Science.gov (United States)

    Ramos, Joaquim J Moura; Diogo, Hermínio P

    2016-03-30

    The slow molecular mobility of three active pharmaceutical drugs (voriconazole, miconazole and itraconazole) has been studied by differential scanning calorimetry (DSC) and thermally stimulated depolarization currents (TSDC). This study yielded the main kinetic features of the secondary relaxations and of the main (glass transition) relaxation, in particular their distribution of relaxation times. The dynamic fragility of the three glass formers was determined from DSC data (using two different procedures) and from TSDC data. According to our results voriconazole behaves as a relatively strong liquid, while miconazole is moderately fragile and itraconazole is a very fragile liquid. There are no studies in this area published in the literature relating to voriconazole. Also not available in the literature is a slow mobility study by dielectric relaxation spectroscopy in the amorphous miconazole. Apart from that, the results obtained are in reasonable agreement with published works using different experimental techniques.

  7. 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 DSC

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

    Science.gov (United States)

    Popescu, C; Gummer, C

    2016-10-01

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

  9. Differential scanning calorimetry predicts the critical quality attributes of amorphous glibenclamide

    DEFF Research Database (Denmark)

    Mah, Pei T; Laaksonen, Timo; Rades, Thomas;

    2015-01-01

    quality attributes (i.e. physical stability and dissolution behaviour) of amorphous material. Glibenclamide (model drug) was milled for various durations using a planetary mill and characterised using Raman spectroscopy and differential scanning calorimetry (DSC). Physical stability studies upon storage...

  10. Contactless Calorimetry for Levitated Samples

    Science.gov (United States)

    Lee, M. C.; Dokko, W.

    1986-01-01

    Temperature and specific heat of hot sample measured with pyrometer in proposed experimental technique. Technique intended expecially for contactless calorimetry of such materials as undercooled molten alloys, samples of which must be levitated to prevent contamination and premature crystallization. Contactless calorimetry technique enables data to be taken over entire undercooling temperature range with only one sample. Technique proves valuable in study of undercooling because difference in specific heat between undercooled-liquid and crystalline phases at same temperature provides driving force to convert metastable undercooled phase to stable crystalline phase.

  11. Some Remarks on the Degree of Crystallinity Measured on DSC

    Institute of Scientific and Technical Information of China (English)

    邱高; 唐志廉; 黄南薰

    2001-01-01

    A modified mathematical model based on the melting and recrystallization of an initial distribution of melting temperatures predicts the melting behavior of polymer in differential scanning calorimetry ( DSC ), taking into account of changes in heat of fusion with melting temperature of crystal and average heat capacity of sample. It has been used to analytically prove that the crystallinity measured on a DSC diagram could not be equal to the weight percentage of crystalline state in the initial specimen. The deviation of the measured crystallinity, as observed relevant to the melting and recrystallization processes, is caused by the changes of the heat of fusion with the melting temperature of crystals, as well as the difference of heat capacities of liquld and solid state polymer. Furthermore, upper and lower limits of the deviation have been discussed.

  12. Thermogravimetric and DSC testing of poly(lactic acid) nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Mróz, Patrycja; Białas, Sylwia [Faculty of Process and Environmental Engineering, Technical University of Łódź, Wólczańska 15 Street, 90-924 Łódź (Poland); Mucha, Maria, E-mail: muchama@wipos.p.lodz.pl [Faculty of Process and Environmental Engineering, Technical University of Łódź, Wólczańska 15 Street, 90-924 Łódź (Poland); Kaczmarek, Halina [Nicolaus Copernicus University, Faculty of Chemistry, Gagarin 7 Street, 87-100 Toruń (Poland)

    2013-12-10

    Highlights: • The presence of nanoadditivities in PLA matrix improves thermal stability of PLA. • Shielding effect main reason for PLA thermal stability by nanofillers. • Thermal degradation suppression in UV-irradiated PLA by the removing of unstable compounds. - Abstract: Polymer nanocomposites based on poly(lactic acid), PLA, and two types of nanofillers: nanosilver and nanoclay were obtained by casting method. The thermal properties of PLA and nanocomposites have been studied by thermogravimetric analysis (TA) and differential scanning calorimetry (DSC). All samples have been UV-irradiated and the effect of photoprocess on their thermal stability has been estimated. It was found that nanoadditives and UV irradiation causes an increase of the activation energy of PLA thermal decomposition. DSC result supplies information on glass transition and crystallization/melting processes in PLA in the presence of nanosilver or nanoclay, also after exposure to UV.

  13. The non-isothermal DSC kinetics of polyethylene tereftalate–epoxy compatible blends

    International Nuclear Information System (INIS)

    Highlights: ► The non-isothermal DSC kinetics of the reaction of DGEBA with DDS, in particular in the presence of phase separating PET, has been studied. ► The specific features in the kinetics of PET formulations in comparison to the pure system have been discussed. ► The fast pre-curing of the epoxy phase allows supposing sub-micro phase separation of PET and efficient toughening of the epoxy matrix. - Abstract: Polyethylene tereftalate has been dissolved in an epoxy resin based on diglycidyl ether of bisphenol-A, DGEBA, and the epoxy component has been cross-linked with the aid of two diamine hardeners. Two series of samples have been tested at the epoxy-amine stoichiometry applying the differential scanning calorimetry, DSC, in scanning mode. One of the series of samples was pre-cured at low temperatures with the aid of an aliphatic diamine hardener near the gel point and post-cured with diaminodiphenyl sulfone, DDS. The other series of samples contained the higher temperature hardener only. Consequently, the experimental data obtained in this study on both systems relate to the non-isothermal curing of DGEBA with DDS. The kinetics has been estimated applying preferably isoconversional (model free) methods. It has been established that the fast pre-curing allows performing a sub-micro phase separation and efficient toughening of the epoxy matrix

  14. The non-isothermal DSC kinetics of polyethylene tereftalate–epoxy compatible blends

    Energy Technology Data Exchange (ETDEWEB)

    Zvetkov, V.L., E-mail: zvetval@yahoo.com [Institute of Mechanics, Bulgarian Academy of Sciences, bl. I, Sofia 1113 (Bulgaria); Djoumaliisky, S.; Simeonova-Ivanova, E. [Institute of Mechanics, Bulgarian Academy of Sciences, bl. I, Sofia 1113 (Bulgaria)

    2013-02-10

    Highlights: ► The non-isothermal DSC kinetics of the reaction of DGEBA with DDS, in particular in the presence of phase separating PET, has been studied. ► The specific features in the kinetics of PET formulations in comparison to the pure system have been discussed. ► The fast pre-curing of the epoxy phase allows supposing sub-micro phase separation of PET and efficient toughening of the epoxy matrix. - Abstract: Polyethylene tereftalate has been dissolved in an epoxy resin based on diglycidyl ether of bisphenol-A, DGEBA, and the epoxy component has been cross-linked with the aid of two diamine hardeners. Two series of samples have been tested at the epoxy-amine stoichiometry applying the differential scanning calorimetry, DSC, in scanning mode. One of the series of samples was pre-cured at low temperatures with the aid of an aliphatic diamine hardener near the gel point and post-cured with diaminodiphenyl sulfone, DDS. The other series of samples contained the higher temperature hardener only. Consequently, the experimental data obtained in this study on both systems relate to the non-isothermal curing of DGEBA with DDS. The kinetics has been estimated applying preferably isoconversional (model free) methods. It has been established that the fast pre-curing allows performing a sub-micro phase separation and efficient toughening of the epoxy matrix.

  15. Analysis of crystallization kinetics of undercooled Fe-B hypereutectic alloy using DSC technique

    International Nuclear Information System (INIS)

    Highlights: ► Crystallization kinetics of undercooled Fe-B alloy was studied by DSC technique. ► Crystallization rate increased firstly and then was suppressed with increasing ΔT. ► Thermodynamic calculation was adopted to describe nucleation and growth rate. ► Temperature–time-transformation curve was constructed to explain experiment results. - Abstract: Crystallization kinetics of undercooled Fe-B hypereutectic alloy was researched using differential scanning calorimetry (DSC) technique. With the combination of melt-fluxing and high pure argon gas to purify and protect the melts, high undercooling up to 410 K was obtained successfully. The comparison of time dependent transformation fraction at different undercoolings has shown that the crystallization rate increased firstly with increasing ΔT until 354 K and then, the crystallization process was retarded with the further increase of ΔT. Applying quantitative thermodynamic calculation, the evolution of the nucleation and growth rates as a function of temperature was described. On this basis, the temperature–time-transformation (TTT) curve was thus constructed, which gives a reasonable explanation of the observed experimental results.

  16. Analysis of crystallization kinetics of undercooled Fe-B hypereutectic alloy using DSC technique

    Energy Technology Data Exchange (ETDEWEB)

    Yang, W., E-mail: weiyang@mail.nwpu.edu.cn [National Defence Key Discipline Laboratory of Light Alloy Processing Science and Technology, Nanchang Hangkong University, Nanchang 330063 (China); Liu, F.; Yang, G.C. [State Key Laboratory of Solidification Processing, Northwestern Polytechnical University, Xi' an, Shaanxi 710072 (China); Xu, Z.F.; Wang, J.H.; Wang, Z.T. [National Defence Key Discipline Laboratory of Light Alloy Processing Science and Technology, Nanchang Hangkong University, Nanchang 330063 (China)

    2012-01-10

    Highlights: Black-Right-Pointing-Pointer Crystallization kinetics of undercooled Fe-B alloy was studied by DSC technique. Black-Right-Pointing-Pointer Crystallization rate increased firstly and then was suppressed with increasing {Delta}T. Black-Right-Pointing-Pointer Thermodynamic calculation was adopted to describe nucleation and growth rate. Black-Right-Pointing-Pointer Temperature-time-transformation curve was constructed to explain experiment results. - Abstract: Crystallization kinetics of undercooled Fe-B hypereutectic alloy was researched using differential scanning calorimetry (DSC) technique. With the combination of melt-fluxing and high pure argon gas to purify and protect the melts, high undercooling up to 410 K was obtained successfully. The comparison of time dependent transformation fraction at different undercoolings has shown that the crystallization rate increased firstly with increasing {Delta}T until 354 K and then, the crystallization process was retarded with the further increase of {Delta}T. Applying quantitative thermodynamic calculation, the evolution of the nucleation and growth rates as a function of temperature was described. On this basis, the temperature-time-transformation (TTT) curve was thus constructed, which gives a reasonable explanation of the observed experimental results.

  17. Dynamic Calorimetry for Students

    Science.gov (United States)

    Kraftmakher, Yaakov

    2007-01-01

    A student experiment on dynamic calorimetry is described. Dynamic calorimetry is a powerful technique for calorimetric studies, especially at high temperatures and pressures. A low-power incandescent lamp serves as the sample. The ScienceWorkshop data-acquisition system with DataStudio software from PASCO Scientific displays the results of the…

  18. 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 correlati...

  19. DSC and NMR Study on the Inclusion Complex of Lappaconitine with β—Cyclodextrin

    Institute of Scientific and Technical Information of China (English)

    KaiJunLIAO; XiaoHuaYAN; 等

    2002-01-01

    The inclusion complex of lappaconitine(Lap) with β-cyclodextrin (β-CD) has been studied by the differential scanning calorimetry (DSC) and 1H-NMR,2D-NMR spectroscopy. The structure of the complex has been deduced.

  20. DSC and NMR Study on the Inclusion Complex of Lappaconitine with β-Cyclodextrin

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    The inclusion complex of lappaconitine (Lap) with β-cyclodextrin (β-CD) has been studied by the differential scanning calorimetry (DSC) and 1H-NMR, 2D-NMR spectroscopy.The structure of the complex has been deduced.``

  1. Rheological and DSC Studies on the Interaction between κ-Carrageenan and Cellulose Nanocrystals (CNC)

    Institute of Scientific and Technical Information of China (English)

    Rui GUO; En Yong DING

    2006-01-01

    Rheometer and differential scanning calorimetry (DSC) have been used to probe the mechanism of gelation in gels formed by mixture of κ-carrageenan and cellulose nanocrystals (CNC). The results indicated that an association occurred between CNC chains and aggregated κ-carrageenan helices.

  2. Thermal analysis of synthetic lubricating oils with DSC and TGA; Thermoanalyse synthetischer Schmieroele mit DSC und TGA

    Energy Technology Data Exchange (ETDEWEB)

    Fahl, J. [FUCHS DEA Schmierstoffe GmbH and Co. KG, Lab. Hamburg (Germany); Bruns, B. [DEA Mineraloel AG, Hamburg (Germany); Langenberg, E. [TA Instruments, Alzenau (Germany); Poetke, W. [Technische Univ. Bergakademie Freiberg (Germany)

    2001-07-01

    Thermal stability of selected lubricating oils was studied using thermoanalytical methods differential scanning calorimetry (DSC) and thermogravimetrical analysis (TGA). The ways worked out allow fast estimation of different base oils and additives especially under influence of CO{sub 2}. Based on heating curves thermal decomposition and evaporation reactions can be interpreted. Relations between chemical structure and thermal stability of synthetic lubricants result. (orig.) [German] Mit den thermoanalytischen Verfahren TGA und DSC wurden ausgewaehlte Schmieroele hinsichtlich ihrer thermischen Stabilitaet untersucht. Die erarbeiteten Methoden ermoeglichen eine schnelle Bewertung unterschiedlicher Grundoele und deren Additivierung insbesondere auch unter Einfluss von CO{sub 2}. Anhand der Aufheizkurven ist eine Interpretation thermischer Zersetzungs- und Verdampfungsreaktionen moeglich, und es ergeben sich somit Rueckschluesse der chemischen Struktur auf die thermische Stabilitaet. (orig.)

  3. 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.

  4. On the use of a reduced model for the simulation of melting of solutions in DSC experiments

    Energy Technology Data Exchange (ETDEWEB)

    Gibout, Stéphane, E-mail: stephane.gibout@univ-pau.fr [LaTEP-ENSGTI, Université de Pau et des Pays de l’Adour, Bâtiment d’Alembert, rue Jules Ferry, 64 075 Pau Cedex (France); Franquet, Erwin [LaTEP-ENSGTI, Université de Pau et des Pays de l’Adour, Bâtiment d’Alembert, rue Jules Ferry, 64 075 Pau Cedex (France); INRIA Bordeaux Sud Ouest, CAGIRE Team, 351 Cours de la Libération, 33 405 Talence Cedex (France); Maréchal, William; Dumas, Jean-Pierre [LaTEP-ENSGTI, Université de Pau et des Pays de l’Adour, Bâtiment d’Alembert, rue Jules Ferry, 64 075 Pau Cedex (France)

    2013-08-20

    Highlights: • Extension to binary solutions of a previous method developed for pure substances. • Thermal behavior of DSC sample can be obtained using a one-dimensional reduced model. • Thermodynamical parameters remain unchanged using this model. • In the perspective of future identification, this leads to a reduced computational time by 100 or even 1000. - Abstract: It is known that when studying the fusion of phase change materials (PCM) in differential scanning calorimetry (DSC) experiments, the geometry of the samples is not well known. Yet, some studies show that a numerical model, needing obviously to clearly define the shape of the sample, may reproduce the experimental DSC curve. In particular, such methods are currently applied to identification process based on inversion methods applied to the thermodynamical parameters governing the numerical model. Consequently, it means that if several numerical models are able to reproduce the thermal behavior of a PCM undergoing phase transition, the best one is the simplest one, that is to say the one which is the fastest to solve. Recently, we have thus shown that for pure substances PCM, a reduced model based on a spherical assumption for the shape of the sample leads to similar DSC curves that a more general model based on cylindrical shape. Clearly, if this result may be extended to other kinds of PCM, this will promote the capability of this method to be used in inversion process involved by identification process. The aim of the present paper is therefore to further study this method by considering non-pure materials, i.e. binary solution in the present case.

  5. Thermodynamic investigations of nitroxoline sublimation by simultaneous DSC-FTIR method and isothermal TG analysis.

    Science.gov (United States)

    Gao, Gau-Yi; Lin, Shan-Yang

    2010-01-01

    To investigate the physicochemical characteristics, thermodynamics, possible sublimation process and kinetics of nitroxoline, differential scanning calorimetry (DSC), isothermal thermogravimetry (TG), and Fourier transform infrared (FTIR) microspectroscopy equipped with a micro hot-stage of DSC microscopy assembly (simultaneous DSC-FTIR method) were used. The DSC result indicates that nitroxoline exhibited a sharp endothermic peak at 182 degrees C with enthalpy of 103.1 J/g due to the melting point of nitroxoline. A sublimation behavior of nitroxoline was found from 129 degrees C by gradual weight loss in TG curve. However, the nonisothermal DSC-FTIR method reveals that the temperature at 95 degrees C was the onset temperature of nitroxoline sublimation. A significant difference between DSC-FTIR method and TG analysis suggests that the simultaneous DSC-FTIR method was more sensitive than that of the TG analysis to detect the beginning temperature of nitroxoline sublimation. The sublimation kinetics of nitroxoline determined by isothermal TG analysis evidenced that the zero-order kinetics was followed over the sublimation time. The sublimation enthalpy correction was also carried out by a group additivity approach for the estimation of heat capacity. The enthalpy of nitroxoline sublimation estimated was 86.14 KJ/mol at 298.15 K.

  6. 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.

  7. One-step Real-time Food Quality Analysis by Simultaneous DSC-FTIR Microspectroscopy.

    Science.gov (United States)

    Lin, Shan-Yang; Lin, Chih-Cheng

    2016-01-01

    This review discusses an analytical technique that combines differential scanning calorimetry and Fourier-transform infrared (DSC-FTIR) microspectroscopy, which simulates the accelerated stability test and detects decomposition products simultaneously in real time. We show that the DSC-FTIR technique is a fast, simple and powerful analytical tool with applications in food sciences. This technique has been applied successfully to the simultaneous investigation of: encapsulated squid oil stability; the dehydration and intramolecular condensation of sweetener (aspartame); the dehydration, rehydration and solidification of trehalose; and online monitoring of the Maillard reaction for glucose (Glc)/asparagine (Asn) in the solid state. This technique delivers rapid and appropriate interpretations with food science applications.

  8. 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....... There was no correlation between the intrinsic stability, specified by the transition temperature in the DSC, and the long-term stability derived from the peak area. The results are discussed with respect to the role of enzyme denaturation for the ubiquitous slowdown observed in the enzymatic hydrolysis of cellulose....

  9. Calorimetry at the SSC

    International Nuclear Information System (INIS)

    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

  10. Solid state and sub-cooled liquid vapour pressures of substituted dicarboxylic acids using Knudsen Effusion Mass Spectrometry (KEMS and Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    A. M. Booth

    2010-02-01

    Full Text Available Solid state vapour pressures of a selection of substituted dicarboxylic acids have been measured using Knudsen Effusion Mass Spectrometry (KEMS. Enthalpies of fusion and melting points obtained using Differential Scanning Calorimetry (DSC were used to obtain sub-cooled liquid vapour pressures. They have been compared to estimation methods used on the E-AIM website. These methods are shown to poorly represent -OH groups in combination with COOH groups. Partitioning calculations have been performed to illustrate the impact of the different estimation methods on organic aerosol mass compared to the use of experimental data.

  11. Solid state and sub-cooled liquid vapour pressures of substituted dicarboxylic acids using Knudsen Effusion Mass Spectrometry (KEMS and Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    A. M. Booth

    2010-05-01

    Full Text Available Solid state vapour pressures of a selection of atmospherically important substituted dicarboxylic acids have been measured using Knudsen Effusion Mass Spectrometry (KEMS over a range of 20 K (298–318 K. Enthalpies of fusion and melting points obtained using Differential Scanning Calorimetry (DSC were used to obtain sub-cooled liquid vapour pressures. They have been compared to estimation methods used on the E-AIM website. These methods are shown to poorly represent – OH groups in combination with COOH groups. Partitioning calculations have been performed to illustrate the impact of the different estimation methods on organic aerosol mass compared to the use of experimental data.

  12. Calorimetry of dehydrogenation and dangling-bond recombination in several hydrogenated amorphous silicon materials

    OpenAIRE

    Roura Grabulosa, Pere; Farjas Silva, Jordi; Rath, Chandana; Serra-Miralles, J.; Bertrán Serra, Enric; Roca I Cabarrocas, Pere

    2006-01-01

    Differential scanning calorimetry (DSC) was used to study the dehydrogenation processes that take place in three hydrogenated amorphous silicon materials: nanoparticles, polymorphous silicon, and conventional device-quality amorphous silicon. Comparison of DSC thermograms with evolved gas analysis (EGA) has led to the identification of four dehydrogenation processes arising from polymeric chains (A), SiH groups at the surfaces of internal voids (A'), SiH groups at interfaces (B), and in the b...

  13. 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.

  14. 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 freque......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...

  15. Cure Kinetics of DGEBA with Hyperbranched Poly(3-hydroxyphenyl) Phosphate as Curing Agent Studied by Non-isothermal DSC

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    The cure kinetics of diglycidyl ether of bisphenol A(DGEBA) with hyperbranched poly(3-hydroxyphenyl) phosphate(HHPP) as the curing agent was investigated by means of non-isothermal differential scanning calorimetry(DSC) at various heating rates. The results were compared with the corresponding results by using 1,3-dihydroxybenzene(DHB) as a model compound. The results show that HHPP can enhance the cure reaction of DGEBA, resulting in the decrease of the peak temperature of the curing curve as well as the decrease of the activation energy because of the flexible -P-O- groups in the backbone of HHPP. However, both the activation energy of the cured polymer and the peak temperature of the curing curve are increased with DHB as a curing agent. The cure kinetics of the DGEBA/HHPP system was calculated by using the isoconversional method given by Málek. It was found that the two-parameter autocatalytic model(esták-Berggren equation) is the most adequate one to describe the cure kinetics of the studied system at various heating rates. The obtained non-isothermal DSC curves from the experimental data show the results being accordant with those theoretically calculated.

  16. Differential scanning calorimetry and fluorescence study of lactoperoxidase as a function of guanidinium-HCl, urea, and pH.

    Science.gov (United States)

    Zelent, Bogumil; Sharp, Kim A; Vanderkooi, Jane M

    2010-07-01

    The stability of bovine lactoperoxidase to denaturation by guanidinium-HCl, urea, or high temperature was examined by differential scanning calorimetry (DSC) and tryptophan fluorescence. The calorimetric scans were observed to be dependent on the heating scan rate, indicating that lactoperoxidase stability at temperatures near Tm is controlled by kinetics. The values for the thermal transition, Tm, at slow heating scan rate were 66.8, 61.1, and 47.2 degrees C in the presence of 0.5, 1, and 2 M guanidinium-HCl, respectively. The extrapolated value for Tm in the absence of guanidinium-HCl is 73.7 degrees C, compared with 70.2 degrees C obtained by experiment; a lower experimental value without a denaturant is consistent with distortion of the thermal profile due to aggregation or other irreversible phenomenon. Values for the heat capacity, Cp, at Tm and Ea for the thermal transition decrease under conditions where Tm is lowered. At a given concentration, urea is less effective than guanidinium-HCl in reducing Tm, but urea reduces Cp relatively more. Both fluorescence and DSC indicate that thermally denatured protein is not random coil. A change in fluorescence around 35 degrees C, which was previously reported for EPR and CD measurements (Boscolo et al. Biochim. Biophys. Acta 1774 (2007) 1164-1172), is not seen by calorimetry, suggesting that a local and not a global change in protein conformation produces this fluorescence change.

  17. Changes of multi-scale structure during mimicked DSC heating reveal the nature of starch gelatinization

    Science.gov (United States)

    Wang, Shujun; Zhang, Xiu; Wang, Shuo; Copeland, Les

    2016-06-01

    A thorough understanding of starch gelatinization is extremely important for precise control of starch functional properties for food processing and human nutrition. Here we reveal the molecular mechanism of starch gelatinization by differential scanning calorimetry (DSC) in conjunction with a protocol using the rapid viscosity analyzer (RVA) to generate material for analysis under conditions that simulated the DSC heating profiles. The results from DSC, FTIR, Raman, X-ray diffraction and small angle X-ray scattering (SAXS) analyses all showed that residual structural order remained in starch that was heated to the DSC endotherm end temperature in starch:water mixtures of 0.5 to 4:1 (v/w). We conclude from this study that the DSC endotherm of starch at a water:starch ratio of 2 to 4 (v/w) does not represent complete starch gelatinization. The DSC endotherm of starch involves not only the water uptake and swelling of amorphous regions, but also the melting of starch crystallites.

  18. Changes of multi-scale structure during mimicked DSC heating reveal the nature of starch gelatinization.

    Science.gov (United States)

    Wang, Shujun; Zhang, Xiu; Wang, Shuo; Copeland, Les

    2016-06-20

    A thorough understanding of starch gelatinization is extremely important for precise control of starch functional properties for food processing and human nutrition. Here we reveal the molecular mechanism of starch gelatinization by differential scanning calorimetry (DSC) in conjunction with a protocol using the rapid viscosity analyzer (RVA) to generate material for analysis under conditions that simulated the DSC heating profiles. The results from DSC, FTIR, Raman, X-ray diffraction and small angle X-ray scattering (SAXS) analyses all showed that residual structural order remained in starch that was heated to the DSC endotherm end temperature in starch:water mixtures of 0.5 to 4:1 (v/w). We conclude from this study that the DSC endotherm of starch at a water:starch ratio of 2 to 4 (v/w) does not represent complete starch gelatinization. The DSC endotherm of starch involves not only the water uptake and swelling of amorphous regions, but also the melting of starch crystallites.

  19. Water calorimetry: The heat defect

    International Nuclear Information System (INIS)

    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 H2O2. 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 H2 and of O2 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 H2-saturated water. The production of H2O2 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 H2 of 50% and of O2 of 50% is suitable for water calorimetry if the water is stirred and is in contact with a gas space of similar volume. H2-saturated water does not require a gas space but O2 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 O2-saturated water in water calorimeters are discussed

  20. 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…

  1. Differential scanning calorimetry: An invaluable tool for a detailed thermodynamic characterization of macromolecules and their interactions

    Directory of Open Access Journals (Sweden)

    Michael H Chiu

    2011-01-01

    Full Text Available Differential Scanning Calorimetry (DSC is a highly sensitive technique to study the thermotropic properties of many different biological macromolecules and extracts. Since its early development, DSC has been applied to the pharmaceutical field with excipient studies and DNA drugs. In recent times, more attention has been applied to lipid-based drug delivery systems and drug interactions with biomimetic membranes. Highly reproducible phase transitions have been used to determine values, such as, the type of binding interaction, purity, stability, and release from a drug delivery mechanism. This review focuses on the use of DSC for biochemical and pharmaceutical applications.

  2. 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

  3. Thermal Analysis of Whole Bacterial Cells Exposed to Potassium Permanganate Using Differential Scanning Calorimetry: a Biphasic Dose-Dependent Response to Stress

    OpenAIRE

    Marina K. Abuladze; Victor M. Sokhadze; Emma N. Namchevadze; Kiziria, E.; Leila V. Tabatadze; Lejava, Lia V.; Sh. Gogichaishvili; Bakradze, Nugzar B.

    2009-01-01

    Differential scanning calorimetry (DSC) was applied to estimate the impact of the toxic oxidant potassium permanganate (PM) on the intracellular structural and functional alterations at whole cell level using soil bacteria Arthrobacter oxydans as a model culture. Differential scanning calorimetry (DSC) was applied in order to estimate the impact of the toxic oxidant potassium permanganate (PM) on the intracellular structural and functional alterations at the whole cell level using the soil b...

  4. Calorimetry Task Force Report

    CERN Document Server

    Abdullin, Salavat; Banerjee, Sunanda; Beauceron, Stephanie; Beaudette, Florian; Bhatti, Anwar; Chlebana, Frank; Cossutti, Fabio; Hirschauer, James; Ivanchenko, V; Jang, Dong Wook; Jun, Soon Yung; Kunori, Shuichi; Kroeger, Rob; Liu, Yanwen; Moeller, Anthony; Paulini, Manfred; Piperov, Stefan; Rahmat, Rahmat; Rovelli, Chiara; Safronov, Grigory; Sharma, Seema; Spiropulu, Maria; Yetkin, Taylan

    2010-01-01

    In this note we summarize the progress made by the calorimeter simulation task force (CaloTF) over the past year. The CaloTF was established in February 2008 in order to understand and reconcile the discrepancies observed between the CMS calorimetry simulation and test beam data recorded during 2004 and 2006. The simulation has been significantly improved by using a newer version of Geant4 and an improved physics list for the full CMS detector simulation. Simulation times have been reduced by introducing flexible parameterizations to describe showering in the calorimeter (using a Gflash-like approach) which have been tuned to the test beam data.

  5. Scintillating-fibre calorimetry

    International Nuclear Information System (INIS)

    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.)

  6. Low-temperature phase behavior of fatty acid methyl esters by differential scanning calorimetry (DSC)

    Science.gov (United States)

    Fatty acid methyl ester (FAME) mixtures have many uses including biodiesel, lubricants, metal-working fluids, surfactants, polymers, coatings, green solvents and phase-change materials. The physical properties of a FAME mixture depends on the fatty acid concentration (FAC) profile. Some products hav...

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

    Energy Technology Data Exchange (ETDEWEB)

    Kestens, V., E-mail: vikram.KESTENS@ec.europa.eu [European Commission - Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, 2440 Geel (Belgium); Zeleny, R.; Auclair, G.; Held, A.; Roebben, G.; Linsinger, T.P.J. [European Commission - Joint Research Centre, Institute for Reference Materials and Measurements (IRMM), Retieseweg 111, 2440 Geel (Belgium)

    2011-09-20

    Highlights: {yields} Purity assessment of polycyclic aromatic hydrocarbons and chloramphenicol by DSC. {yields} DSC results compared with traditional purity methods. {yields} Different methods give different results, multiple method approach recommended. {yields} 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.

  8. Detection of sunflower oil in extra virgin olive oil by fast differential scanning calorimetry

    NARCIS (Netherlands)

    Wetten, I.A.; Herwaarden, A.W.; Splinter, R.; Boerrigter-Eenling, R.; Ruth, van S.M.

    2015-01-01

    Extra virgin olive oil (EVOO) is an economically valuable product, due to its high quality and premium price. Therefore it is vulnerable for adulteration by means of the addition of cheaper vegetable oils. Differential scanning calorimetry (DSC) has been suggested as a fast technique for the detecti

  9. 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...

  10. 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...

  11. Comparative study by TG and DSC Of membranes polyamide66/bentonite clay nanocomposite; Estudo comparativo por TG e DSC de membranas de nanocompositos poliamida66/argila bentonitica

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros, K.M. de; Kojuch, L.R.; Araujo, E.M.; Lira, H.L., E-mail: keilamm@ig.com.b [Universidade Federal de Campina Grande (UFCG), PB (Brazil). Unidade Academica de Engenharia de Materiais; Lima, F. [Universidade Estadual da Paraiba (UEPB), Campina Grande, PB (Brazil). Dept. de Quimica

    2010-07-01

    In this study, it was obtained membranes of nanocomposites polyamide66 with 3 and 5% bentonite clay consists of silicates in layers from the interior of Paraiba. The clay was treated with a quaternary ammonium salt in order to make it organophilic. The membranes were prepared by phase inversion technique from the nanocomposites in solution. The clays were characterized by X-ray diffraction (XRD) and thermogravimetry (TG). Also the membranes were characterized by differential scanning calorimetry (DSC) and TG. The XRD and TG confirmed the presence of salt in the clay and thermal stability of the treated clay. For DSC, it was observed that there was no change in melting temperature of the membranes of nanocomposites compared to membrane pure polyamide66. By TG, it was found that the decomposition of the membranes of polyamide66 with treated clay were higher compared with the untreated clay. (author)

  12. 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.

  13. Dual-readout Calorimetry

    CERN Document Server

    Akchurin, N; Cardini, A.; Cascella, M.; Cei, F.; De Pedis, D.; Fracchia, S.; Franchino, S.; Fraternali, M.; Gaudio, G.; Genova, P.; Hauptman, J.; La Rotonda, L.; Lee, S.; Livan, M.; Meoni, E.; Moggi, A.; Pinci, D.; Policicchio, A.; Saraiva, J.G.; Sill, A.; Venturelli, T.; Wigmans, R.

    2013-01-01

    The RD52 Project at CERN is a pure instrumentation experiment whose goal is to un- derstand the fundamental limitations to hadronic energy resolution, and other aspects of energy measurement, in high energy calorimeters. We have found that dual-readout calorimetry provides heretofore unprecedented information event-by-event for energy resolution, linearity of response, ease and robustness of calibration, fidelity of data, and particle identification, including energy lost to binding energy in nuclear break-up. We believe that hadronic energy resolutions of {\\sigma}/E $\\approx$ 1 - 2% are within reach for dual-readout calorimeters, enabling for the first time comparable measurement preci- sions on electrons, photons, muons, and quarks (jets). We briefly describe our current progress and near-term future plans. Complete information on all aspects of our work is available at the RD52 website http://highenergy.phys.ttu.edu/dream/.

  14. Evaluation of integrated Raman-DSC technology in early pharmaceutical development: characterization of polymorphic systems.

    Science.gov (United States)

    Huang, Jun; Dali, Manisha

    2013-12-01

    Differential Scanning Calorimetry and Raman spectroscopy are both powerful tools used heavily in pharmaceutical development. For many studies such as polymorph characterization these two techniques are complimentary and provide data on different yet important aspects of material properties when combined together. In this work we describe an integrated Raman-DSC technology that simultaneously generates both DSC thermogram and Raman spectra of the pharmaceutical material being studied. The integrated system consists of a DSC with a Raman fiber optic probe inserted right on top of the sample furnace. The technology integrates synchronized Raman acquisition into DSC scan, enabling collection of molecular and structural information coupled with observation of thermal events. We first establish the technology by optimizing the instrumental set-up that offers relatively high-quality results for simultaneous DSC and Raman data collection. We then demonstrate the application of the technology by studying the polymorphs of d-mannitol, a common pharmaceutical excipient and BMS-A, an investigational drug candidate that exhibits multiple coexisting polymorphs. In both cases, the Raman-DSC technology was able to provide valuable information on the process of phase change and polymorph identification. Although similar information may be obtained by using various characterization techniques together, the integrated Raman-DSC indicated special advantages for industrial development such as high efficiency, material sparing and comprehensive data analysis. Moreover the technology provides an alternative to better correlate real-time phase behavior to molecular understanding. The technology thus has the potential to be used for Process Analytical Technology (PAT) purpose.

  15. Cure kinetics of epoxy matrix resin by differential scanning calorimetry

    Science.gov (United States)

    Cizmecioglu, M.; Gupta, A.

    1982-01-01

    A study was made on the cure kinetics of an epoxy neat-resin (Narmco 5208) using Differential Scanning Calorimetry (DSC). Two interrelated analytical methods were applied to dynamic DSC data for evaluating the kinetic parameters, such as activation energy, E, the order of reaction, n, and the total heat of polymerization (or crosslinking), delta H sub t. The first method was proposed by Ellerstein (1968), and uses a thorough differential-integral analysis of a single DSC curve to evaluate the kinetic parameters. The second method was proposed by Kissinger (1957), and uses multiple DSC curves obtained at various heating rates to evaluate E regardless of n. Kinetic analysis of Narmco 5208 epoxy resin showed that the reaction order, n, is substantially affected by the rate of heating; i.e., n is approximately 2 at slow scan rates but is reduced to 1.5 at higher scan rates. The activation energy, E, is not affected by the scan rate, and the average value of E is 25.6 + or - 1.8 kcal/mole.

  16. DSC、MDSC测定物质比热容的比较%Comparison of differential scanning calorimetry and modulated differential scanning calorimetry in measurement of specific heat capacities

    Institute of Scientific and Technical Information of China (English)

    鲁红; 冯大春; 杨继佑

    2011-01-01

    实验用TA公司具有DSC、MDSC两种模式、具备先进Tzero技术的热流型DSCQ200热分析仪测定物质的比热容.对如何运用传统方法及调制方法测定物质的比热容进行了详细阐述;以氯化钾、苯甲酸、去离子水为测试样,对两种方法所得实验结果进行了分析比较.%The specific heat capacities of potassium choride, benzoic acid and deionized water samples were measured by DSCQ 200 tbermal analyzer in two different method (differential scanning calorimetry. DSC, and modulated differential scanning calorimetry. MDSC), The results obtained by two methods are compared.The questions in the application of DSC and MDSC are discussed in detail.

  17. Inhibitors of thermally induced burn incidents – characterization by microbiological procedure, electrophoresis, SEM, DSC and IR spectroscopy.

    Science.gov (United States)

    Pielesz, Anna; Machnicka, Alicja; Gawłowski, Andrzej; Fabia, Janusz; Sarna, Ewa; Biniaś, Włodzimierz

    2015-07-01

    Differential scanning calorimetry (DSC) and thermogravimetric (TGA) investigations, acetate electrophoresis (CAE), Fourier-transform infrared spectrometry (FTIR), scanning electron microscopy (SEM) analysis and microbiological procedures were all carried out after heating the samples to a temperature sufficient for simulating a burn incident. In particular, the purpose of the present study was to analyze the effect of antioxidants, such as fucoidan from brown seaweed and flame-retardant cyclic organophosphates and phosphonates, on an organic chicken skin that gets changed by a burn incident. DSC was considered to be a useful tool in assessing in vitro temperature-mediated cross-linking; an innovative analytical conclusion was obtained from the experimentation described in the paper. FTIR tests revealed that heating a dry organic chicken skin to the boiling point leads to the disappearance of a wide band in the 1650-1550 cm(-1) area or the conversion of a band, which may be attributed to the intermolecular β-sheet aggregates. Fucoidan from brown seaweed and flame-retardant cyclic organophosphates and phosphonates probably bind with the collagen that is changed by the burn (in addition to the influence of antioxidant solutions on samples of a blank or not boiled organic chicken skin) incident forming a polymer film with the collagen of the chicken skin surface (SEM analysis), decreasing the aggregation process and native collagen recovery. Good bacteriostatic properties were determined for fucoidan samples from brown seaweed and flame-retardant cyclic organophosphates and phosphonates against the pathogenic bacteria Escherichia coli and Staphylococcus aureus. Thus, it was observed that the fucoidan incorporated into collagen films can be used as a therapeutically active biomaterial that speeds up the wound-healing process.

  18. [DSC and FTIR study of adsorbed lysozyme on hydrophobic surface].

    Science.gov (United States)

    Lei, Zu-meng; Geng, Xin-peng; Dai, Li; Geng, Xin-du

    2008-09-01

    During a process of hen egg white lysozyme adsorption and folding on a moderately hydrophobic surface (PEG-600), the effects of salt((NH4)2SO4) concentrations, surface coverage and denaturant (guanidine hydrochloride, GuHCl) concentrations on thermal stability and the changes in the molecular conformation of adsorbed native and denatured lysozyme without aqueous solution were studied with a combination of differential scanning calorimetry (DSC) with FTIR spectroscopy. The results showed that temperature due to endothermic peaks was reduced and the disturbance increased at higher temperature with the increase in salt concentration and surface coverage of adsorbed protein. beta-Sheet and beta-Turn stucture increased while alpha-Helix structure decreased after the adsorption. The peaks corresponding to both C-C stretching frequency in 1400-1425 cm(-1) and amide I band frequency in 1650-1670 cm(-1) of adsorbed denatured lysozyme can be detected in FTIR spectra while that due to amide I band frequency of adsorbed native lysozyme almost can't be observed. Adsorption resulted in structural loss of adsorbed native lysozyme, whose performance was less stable. PMID:19093560

  19. Thermo-kinetic prediction of metastable and stable phase precipitation in Al–Zn–Mg series aluminium alloys during non-isothermal DSC analysis

    Energy Technology Data Exchange (ETDEWEB)

    Lang, Peter, E-mail: pl404@cam.ac.uk [Department of Materials Science and Metallurgy, University of Cambridge, Charles Babbage Road 27, Cambridge CB3 0FS (United Kingdom); Wojcik, Tomasz [Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria); Povoden-Karadeniz, Erwin [Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria); Christian Doppler Laboratory “Early Stages of Precipitation”, Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria); Falahati, Ahmad [Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria); Kozeschnik, Ernst [Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria); Christian Doppler Laboratory “Early Stages of Precipitation”, Institute of Materials Science and Technology, Vienna University of Technology, Favoritenstraße 9-11, Vienna 1040 (Austria)

    2014-10-01

    Highlights: • Comparison of laboratory Al–Zn–Mg alloy to industrial Al 7xxx series. • Heat flow evolution during non-isothermal DSC analysis is calculated. • TEM investigations of laboratory Al–Zn–Mg alloy at three pronounced temperatures. • Simulation and modelling of precipitation sequence. • Calculation and prediction of heat flow curves of Al 7xxx series. - Abstract: The technological properties of heat treatable Al–Zn–Mg alloys originate in the morphology and distribution of metastable particles. Starting from the solution-annealed condition, this paper describes the precipitate evolution during non-isothermal temperature changes, namely continuous heating differential scanning calorimetry (DSC) analysis. The distribution and the morphology of the metastable and stable precipitates and the heat flow accompanying the precipitation process is investigated experimentally and calculated by numerical thermo-kinetic simulations. The computer simulation results of the sizes and distributions are confirmed by transmission electron microscopy (TEM). The theoretical background and the results of the investigations are discussed.

  20. DSC analyses of static and dynamic precipitation of an Al–Mg–Si–Cu aluminum alloy

    OpenAIRE

    Manping Liu; Zhenjie Wu; Rui Yang; Jiangtao Wei; Yingda Yu; Pål C. Skaret; Hans J. Roven

    2015-01-01

    In the present investigation, both static and dynamic precipitations of an Al–Mg–Si–Cu aluminum alloy after solid-solution treatment (SST) were comparatively analyzed using differential scanning calorimetry (DSC). Dynamic aging was performed in the SST alloy through equal channel angular pressing (ECAP) at different temperatures of room temperature, 110, 170, 191 and 300 °C. For comparison, static artificial aging was conducted in the SST alloy at 191 °C with two aging times of 4 and 10 h. Th...

  1. Hydration characteristics of water in radiation polymerized hema-co- ionomeric controlled drug delivery matrices: a DSC study

    International Nuclear Information System (INIS)

    The changes in the bulk (freezable) and bound (non-freezable) water contents of radiation polymerized (2-hydroxy ethyl methacrylate) (PHEMA) containing two different types of ionomers have been studied by differential scanning calorimetry (DSC). It was found that introduction of 5-10% of acrylic acid into PHEMA matrix affects mainly the bulk water content whereas introduction of sodium para styrene sulphonate affects both types of water significantly. (author)

  2. Performance Evaluation of DSC Windows for Buildings

    OpenAIRE

    Jun-Gu Kang; Jin-Hee Kim; Jun-Tae Kim

    2013-01-01

    Interest in BIPV systems with dye-sensitized solar cells (DSCs) that can replace building windows has increased for zero energy buildings. Although DSCs have lower efficiency in terms of electricity generation than silicon solar cells, they allow light transmission and application of various colors; they also have low production costs, which make them especially suitable for BIPV systems. DSC research is interdisciplinary, involving electrical, chemical, material, and metal engineering. A con...

  3. Laser-high-speed-DSC: Process-oriented Thermal Analysis of PA 12 in Selective Laser Sintering

    Science.gov (United States)

    Lanzl, Lydia; Wudy, Katrin; Drexler, Maximilian; Drummer, Dietmar

    In the Selective Laser Sintering process very high heating rates occur due to the melting of the material by a laser. Extreme scanning rates could not be measured by conventional thermal analysis methods, since typical heating rates for DSC (differential scanning calorimetry) are between 5-20K min-1. By using a Laser-High-Speed-DSC, a self-developed combination of a Flash-DSC and a fitted laser head, the sample is directly heated by a CO2 laser like in the SLS process. These experiments allow a process-oriented thermal analyzation of the material. In this paper, the set-up and function of this new measuring method is introduced. Furthermore, the reliability of the measurements is evaluated by statistical design of experiment methods. By using this new measuring method, the time-dependent melting behavior of the polymer can be analyzed. Moreover, sample temperatures and heating rates dependent on laser exposure times can be quantified.

  4. 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

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

    International Nuclear Information System (INIS)

    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 (Cp) 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 Cp values are now reported for the wide 5–600 K range. The experimental Cp of solid sucrose at 5–300 K was used to calculate the vibrational, solid Cp based on the vibrational molecular motions. The calculated solid and liquid Cp together with the transition parameters for equilibrium conditions were used as references for detailed quantitative thermal analysis of crystalline and amorphous sucrose. Melting temperature (Tm) 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 Tm and heat of fusion of crystalline sucrose were estimated at zero heating rate as Tom = 424.4 K and ΔHof = 32 kJ/mol, respectively. The glass transition temperature (Tg) of amorphous sucrose was at 331 K with a change in Cp 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 Tm was 483 K and Tg was 364 K. Superheating effects were observed during the melting with

  6. 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...

  7. Experimental tests of particle flow calorimetry

    International Nuclear Information System (INIS)

    Precision physics at future colliders requires highly granular calorimeters to support the Particle Flow Approach for event reconstruction. This article presents a review of about 10-15 years of R and D, mainly conducted within the CALICE collaboration, for this novel type of detector. The performance of large scale prototypes in beam tests validate the technical concept of particle flow calorimeters. The comparison of test beam data with simulation, of e.g. hadronic showers, supports full detector studies and gives deeper insight into the structure of hadronic cascades than was possible previously.

  8. Experimental Tests of Particle Flow Calorimetry

    CERN Document Server

    Sefkow, Felix; Kawagoe, Kiyotomo; Pöschl, Roman; Repond, José

    2015-01-01

    Precision physics at future colliders requires highly granular calorimeters to support the Particle Flow Approach for event reconstruction. This article presents a review of about 10 - 15 years of R\\&D, mainly conducted within the CALICE collaboration, for this novel type of detector. The performance of large scale prototypes in beam tests validate the technical concept of particle flow calorimeters. The comparison of test beam data with simulation, of e.g.\\ hadronic showers, supports full detector studies and gives deeper insight into the structure of hadronic cascades than was possible previously.

  9. 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 ...

  10. 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...

  11. Development of Particle Flow Calorimetry

    OpenAIRE

    Repond, Jose

    2011-01-01

    This talk reviews the development of imaging calorimeters for the purpose of applying Particle Flow Algorithms (PFAs) to the measurement of hadronic jets at a future lepton collider. After a short introduction, the current status of PFA developments is presented, followed by a review of the major developments in electromagnetic and hadronic calorimetry.

  12. DSC analysis of EB-cured polyurethane-acrylate

    International Nuclear Information System (INIS)

    The gel films obtained by electron beam (EB) solid-state polymerization of urethane-acrylate prepolymers were characterized by differential scanning calorimetry (DSC). Two kinds of urethane-acrylates were synthesized by reaction of poly(butylene adipate)diol (PBAD), 4,4'-diphenylmethane diisocyanate (MDI) and 2-hydroxyethyl acrylate (HEA) for this purpose. One is a semicrystalline prepolymer (UA-251M) with a number average molecular weight (M-barn) of 3200, and the other is an amorphous one (UA-071M) with M-barn of 1450. The M-barn varied by changing M-barn of PBAD. UA-251M gel film decreased in glass transition temperature (Tg) and increased in heat capacity change (ΔCp) at Tg with increasing irradiation dose, while the Tg and ΔCp values of UA-071M gel film changed in the opposite way to those of UA-251M gel film. Above 5 Mrad, gel fraction reached more than 90 %, and the Tg and ΔCp values changed steeply for both prepolymers. This steep change in Tg and ΔCp was attributed to the crosslinking of PBAD chains as well as of terminal acryloyl groups. Since the Tg change of UA-071M gel film depends merely on the crosslinking, the crosslinking structure was evaluated using two equations which relate the shift in Tg to crosslinking. The molecular weight between crosslinking junctions was found to be larger than the M-barn of the prepolymer. The crosslinking by the EB polymerization restricted the mobility of the polymer chain less strongly than the crosslinking by the three-functional isocyanate and α,ω-dihydroxy(polypropylene oxide) with a molecular weight of 1000 did. (author)

  13. DSC analysis of EB-cured polyurethane-acrylate

    Energy Technology Data Exchange (ETDEWEB)

    Ando, Masayuki; Uryu, Toshiyuki

    1987-10-01

    The gel films obtained by electron beam (EB) solid-state polymerization of urethane-acrylate prepolymers were characterized by differential scanning calorimetry (DSC). Two kinds of urethane-acrylates were synthesized by reaction of poly(butylene adipate)diol (PBAD), 4,4'-diphenylmethane diisocyanate (MDI) and 2-hydroxyethyl acrylate (HEA) for this purpose. One is a semicrystalline prepolymer (UA-251M) with a number average molecular weight (M-bar/sub n/) of 3200, and the other is an amorphous one (UA-071M) with M-bar/sub n/ of 1450. The M-bar/sub n/ varied by changing M-bar/sub n/ of PBAD. UA-251M gel film decreased in glass transition temperature (T/sub g/) and increased in heat capacity change (..delta..C/sub p/) at T/sub g/ with increasing irradiation dose, while the T/sub g/ and ..delta..C/sub p/ values of UA-071M gel film changed in the opposite way to those of UA-251M gel film. Above 5 Mrad, gel fraction reached more than 90 %, and the T/sub g/ and ..delta..C/sub p/ values changed steeply for both prepolymers. This steep change in T/sub g/ and ..delta..C/sub p/ was attributed to the crosslinking of PBAD chains as well as of terminal acryloyl groups. Since the T/sub g/ change of UA-071M gel film depends merely on the crosslinking, the crosslinking structure was evaluated using two equations which relate the shift in T/sub g/ to crosslinking. The molecular weight between crosslinking junctions was found to be larger than the M-bar/sub n/ of the prepolymer. The crosslinking by the EB polymerization restricted the mobility of the polymer chain less strongly than the crosslinking by the three-functional isocyanate and ..cap alpha..,..omega..-dihydroxy(polypropylene oxide) with a molecular weight of 1000 did.

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

    International Nuclear Information System (INIS)

    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

  15. Thermodynamic Study of 8-Hydroxyquinoline by Adiabatic Calorimetry and Thermal Analysis

    Institute of Scientific and Technical Information of China (English)

    WANG Shao-Xu; TAN Zhi-Cheng; LI Yan-Sheng; TONG Bo; LI Ying; SHI Quan; ZHANG Jing-Nan

    2008-01-01

    A calorimetric study and thermal analysis for 8-hydroxyquinoline were performed.The low-temperature heat capacity of this compound was measured with a precise automated adiabatic calorimeter over the temperature range from 78 to 370 K.The melting point True,molar enthalpy △fusHm and molar entropy △fusSm of fusion of this sub-tively.The thermodynamic functions of the substance,such as molar enthalpy and entropy of fusion,and thermo-dynamic functions [Hr-H298.15] and [ST-S298.15] were derived from two polynomial equations of the experi-mental molar heat capacities against the reduced temperature fitted by the least square method.The melting tem-peratures for the sample and the absolutely pure compound have been obtained from fractional melting experiments to be 345.601 and 345.761 K,respectively,and the molar fraction purity of the sample was calculated to be 0.9978 according to the van't Hoff equation.The thermal stability of the compound was further investigated by differential scanning calorimetry(DSC).

  16. Differential scanning calorimetry of coal

    Science.gov (United States)

    Gold, P. I.

    1978-01-01

    Differential scanning calorimetry studies performed during the first year of this project demonstrated the occurrence of exothermic reactions associated with the production of volatile matter in or near the plastic region. The temperature and magnitude of the exothermic peak were observed to be strongly affected by the heating rate, sample mass and, to a lesser extent, by sample particle size. Thermal properties also were found to be influenced by oxidation of the coal sample due to weathering effects.

  17. Indirect calorimetry during incubation of hatching eggs

    NARCIS (Netherlands)

    Brand, van den H.; Heetkamp, M.J.W.; Kemp, B.

    2015-01-01

    Indirect calorimetry can be used during incubation of avian eggs to monitor the quality of the incubation process, the development of the embryo and the utilization of nutrients. Indirect calorimetry has several benefits above direct calorimetry, particularly in hatching eggs. However, to obtain rel

  18. DSC Analysis of LT-3 Aluminum Alloy Vacuum Brazing

    Institute of Scientific and Technical Information of China (English)

    FENG Tao; WU Lu-hai; LOU Song-nian; LI Ya-jiang

    2005-01-01

    LT-3 aluminum alloy is a kind of two-side cladding aluminum special used in vacuum brazing. Differential Scanning Calorimeter (DSC) was used to measure the exothermic and endothermic reaction during the brazing process that the cortex metal and the base metal are melted and re-crystal. The analysis results inidicate that eutectic reaction is the main reaction in the melted cortex metal crystallization process. But the main reaction in the melted base metal crystallization process is the reaction that a-A1 segregated out. According to the experimental details, the critical work of nucleation is 3.82 × 1017J, the critical radius of nucleation is 8.69 × 1010 m, the volume of critical crystal nucleus is 2.75× 10-27 m3 and the per unit cell in critical crystal nucleus is 43.

  19. The Heats of Dilution. Calorimetry and Van't-Hoff

    OpenAIRE

    Stepanov, I. A.

    2000-01-01

    Earlier it has been found that there is a big difference between heats of dilution measured by calorimetry and by the Van't-Hoff equation. In the present paper a reason for that is proposed. Experimental data for dilution of benzene and n-hexane in water were used.

  20. 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…

  1. The Heats of Dilution Calorimetry and Van't-Hoff

    CERN Document Server

    Stepanov, I A

    2000-01-01

    Earlier it has been found that there is a big difference between heats of dilution measured by calorimetry and by the Van't-Hoff equation. In the present paper a reason for that is proposed. Experimental data for dilution of benzene and n-hexane in water were used.

  2. A Guide to Differential Scanning Calorimetry of Membrane and Soluble Proteins in Detergents.

    Science.gov (United States)

    Yang, Zhengrong; Brouillette, Christie G

    2016-01-01

    Differential scanning calorimetry (DSC) detects protein thermal unfolding by directly measuring the heat absorbed. Simple DSC experiments that require relatively small amounts of pure material can provide a wealth of information related to structure, especially with respect to domain architecture, without the need for a complete thermodynamic analysis. Thus, DSC is an ideal additional tool for membrane protein characterization and also offers several advantages over indirect thermal unfolding methods. Integral membrane proteins (IMPs) that comprise both large multitopic transmembrane domains (TMDs) and extramembranous domains (EMDs) are differentially affected by detergent interactions with both domains. In fact, in some cases, destabilization of the EMD by detergent may dominate overall IMP stability. This chapter will (1) provide a perspective on the advantages of DSC for membrane protein characterization and stability measurements, including numerous examples spanning decades of research; (2) introduce models for the interaction and destabilization of IMPs by detergents; (3) discuss two case studies from the authors' lab; and (4) offer practical advice for performing DSC in the presence of detergents.

  3. 用差示扫描量热法测定金属Gd的比热容%Determination of Specific-heat Capacity of Gd by Differential Scanning Calorimetry Method

    Institute of Scientific and Technical Information of China (English)

    哈斯朝鲁; 石海荣; 宋志强; 刘雨江; 特古斯

    2011-01-01

    The specific-heat capacity of metal gadolinium was measured by using the differential scanning calorimetry (DSC) method. The results obtained from DSC method are in good agreement with the results reported in the literatures. On the basis of the Debye model.the lattice heat capacity of Gd is determined by fitting the experimental result,then the magnetic heat capacity is separated. The relationship between the relative magnetic entropy and temperature was obtained from the magnetic part of specific heat near the phase transformation point. The maximal magnetic entropy change of Gd is 4. 7J ? Mol-1 ? K-1 near room temperature.%采用差示扫描量热(DSC)法测定了金属Gd的比热容,测量结果与已有文献的结果基本一致.根据德拜理论拟合比热容实验曲线确定Gd的晶格比热容,从而分离出Gd的磁比热容,得到相变点附近相对磁熵随温度的变化关系.室温附近Gd的最大磁熵变为4.7J·mol-1·K-1.

  4. 更加完美索尼DSC-TX9C/DSC-WX5C魅力出击

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    DSC-TX9C和DSC-WX5C分别为一代经典大热机型DSC-TXTC和DSC—WX1的后继产品。延续Exmor RCMOS影像传感器所带来的强大功能,在设计细节和功能应用上均有大幅提升。

  5. FTIR and DSC studies of the thermal and photochemical stability of Balanites aegyptiaca oil (Toogga oil).

    Science.gov (United States)

    Gardette, Jean-Luc; Baba, Mohamed

    2013-01-01

    The oil extracted from the bean of Balanites aegyptiaca was characterized, and its photochemical and thermal stabilization were evaluated. The chemical composition was determined using gas chromatography (GC), revealing that the oil is very rich in unsaturated fatty acids (72% omega-6 and omega-9). The photochemical stability was assessed by subjecting it to artificially accelerated photo-aging and then examining the changes using infrared spectroscopy. The thermal stability was studied at six different temperatures ranging from 130 to 200°C and monitored in situ by differential scanning calorimetry (DSC). The kinetic parameters (EA and k) describing the thermal degradation of this oil were calculated. It has been shown that the antioxidants present in the oil delay the oxidation process (induction period). The degradation of the Toogga oil was compared with that of oleic and linoleic fatty acids. In addition, the degradation of the Toogga oil extracted with hexane was compared to that of the neat oil.

  6. Crystallization Kinetics of Lithium Aluminum Germanium Phosphate Glass by DSC Technique

    Institute of Scientific and Technical Information of China (English)

    HE Kun; WANG Yanhang; ZU Chengkui; LIU Yonghua; ZHAO Huifeng; HAN Bin; CHENG Jiang

    2012-01-01

    The crystallization kinetics of Li2O-Al2O3-GeO2-P2O5 (LAGP) glass fabricated via the conventional melt-quenching method was studied by differential scanning calorimetry (DSC) under nonisothermal condition at different heating rates.The activation energy of glass transition Eg is 634.4 kJ/mol,indicating that LAGP glass is easy to crystallize at an elevated temperature.The activation energy of crystallization Ec and Avrami index n obtained from Matusita's model are 442.01 kJ/mol and 1.7,respectively.The value of n reveals that bulk crystallization predominates slightly over surface crystallization during crystallization process.LAGP glass-ceramics after different heat treatments have the same crystalline phases determined as major phase LiGe2(PO4)3,with AlPO4 and GeO2 as their impurity phases.

  7. Application of rigorous nonlinear regression for the analysis of complex isothermal DSC reactivity curves

    Energy Technology Data Exchange (ETDEWEB)

    Pickard, J.M.

    1988-01-01

    Differential scanning calorimetry (DSC) provides a convenient technique for monitoring the global reactivity in real time for decomposition of a variety of secondary explosives. Thermograms for decomposition of explosives are frequently characterized by nonzero initial rates followed by additional transitions involving autocatalysis. An example of this phenomenon is illustrated for decomposition of 2,2',4,4',6,6'-hexanitroazobenzene (HNAB) at temperatures of 590 and 600K. Thermograms exhibit nonzero initial rates followed by autocatalytic transitions exhibiting maxima in the range of 250--500 s. In view of the complexity and frequency of occurrence of these types of thermograms, a computer program was devised to evaluate global rate parameters using nonlinear regression. 7 refs., 5 figs., 1 tab.

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

    Science.gov (United States)

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

    2016-07-01

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

  9. Assessment of interactions between four proteins and benzothiazole derivatives by DSC and CD

    Energy Technology Data Exchange (ETDEWEB)

    Hassan, Natalia [Soft Matter and Molecular Biophysics Group, Department of Applied Physics, Faculty of Physics, Campus Vida, University of Santiago de Compostela, E-15782 Santiago de Compostela (Spain); Verdes, Pedro V., E-mail: pedro.vazquez@usc.e [Soft Matter and Molecular Biophysics Group, Department of Applied Physics, Faculty of Physics, Campus Vida, University of Santiago de Compostela, E-15782 Santiago de Compostela (Spain); Ruso, Juan M. [Soft Matter and Molecular Biophysics Group, Department of Applied Physics, Faculty of Physics, Campus Vida, University of Santiago de Compostela, E-15782 Santiago de Compostela (Spain)

    2011-03-15

    The thermal denaturation of ovalbumin, lysozyme, myoglobin and fibrinogen at different BTS concentrations have been investigated using differential scanning calorimetry (DSC) and circular dichroism (CD) spectroscopy. Thermodynamic parameters: melting temperatures (T{sub m}), calorimetric enthalpy ({Delta}H), van't Hoff enthalpy ({Delta}H{sub v}) were obtained for all the systems under study. Thermal denaturation of the four proteins was completely irreversible. Changes in the protein conformation due to the adsorption of BTS molecules have been monitored by using UV-CD spectra. Greater changes in {alpha}-helical contents correspond with the BTS higher concentrations. The lysozyme denaturation temperature increases at low concentrations BTS indicating that BTS acts as a structure stabilizer; meanwhile it acts as a destabilizer at higher concentrations in all the proteins studied. The major effect is observed in the case of myoglobin, the protein with the highest {alpha}-helical secondary structure (75%).

  10. Simultaneous Thermodynamic and Kinetic Parameters Determination Using Differential Scanning Calorimetry

    Directory of Open Access Journals (Sweden)

    Nader Frikha

    2011-01-01

    Full Text Available Problem statement: The determination of reaction kinetics is of major importance, as for industrial reactors optimization as for environmental reasons or energy limitations. Although calorimetry is often used for the determination of thermodynamic parameters alone, the question that arises is: how can we apply the Differential Scanning Calorimetry for the determination of kinetic parameters. The objective of this study consists to proposing an original methodology for the simultaneous determination of thermodynamic and kinetic parameters, using a laboratory scale Differential Scanning Calorimeter (DSC. The method is applied to the dichromate-catalysed hydrogen peroxide decomposition. Approach: The methodology is based on operating of experiments carried out with a Differential Scanning Calorimeter. The interest of this approach proposed is that it requires very small quantities of reactants (about a few grams to be implemented. The difficulty lies in the fact that, using such microcalorimeters, the reactants temperature cannot directly be measured and a particular calibration procedure has thus to be developed, to determine the media temperature in an indirect way. The proposed methodology for determination of kinetics parameters is based on resolution of the coupled heat and mass balances. Results: A complete kinetic law is proposed. The Arrhenius parameters are determined as frequency factor k0 = 1.39×109 s−1 and activation energy E = 54.9 kJ mol−1. The measured enthalpy of reaction is ΔrH=−94 kJ mol−1. Conclusion: The comparison of the results obtained by such an original methodology with those obtained using a conventional laboratory scale reactor calorimetry, for the kinetics determination of, shows that this new approach is very relevant.

  11. DSC and universal bit-level combining for HARQ systems

    Directory of Open Access Journals (Sweden)

    Lv Tiejun

    2011-01-01

    Full Text Available Abstract This paper proposes a Dempster -Shafer theory based combining scheme for single-input single-output (SISO systems with hybrid automatic retransmission request (HARQ, referred to as DSC, in which two methods for soft information calculations are developed for equiprobable (EP and non-equiprobable (NEP sources, respectively. One is based on the distance from the received signal to the decision candidate set consisting of adjacent constellation points when the source bits are equiprobable, and the corresponding DSC is regarded as DSC-D. The other is based on the posterior probability of the transmitted signals when the priori probability for the NEP source bits is available, and the corresponding DSC is regarded as DSC-APP. For the diverse EP and NEP source cases, both DSCD and DSC-APP are superior to maximal ratio combining, the so-called optimal combining scheme for SISO systems. Moreover, the robustness of the proposed DSC is illustrated by the simulations performed in Rayleigh channel and AWGN channel, respectively. The results show that the proposed DSC is insensitive to and especially applicable to the fading channels. In addition, a DS detection-aided bit-level DS combining scheme is proposed for multiple-input multiple-output--HARQ systems. The bit-level DS combining is deduced to be a universal scheme, and the traditional log-likelihood-ratio combining is a special case when the likelihood probability is used as bit-level soft information.

  12. Vesicle-cholesterol interactions : Effects of added cholesterol on gel-to-liquid crystal transitions in a phospholipid membrane and five dialkyl-based vesicles as monitored using DSC

    NARCIS (Netherlands)

    Blandamer, MJ; Briggs, B; Cullis, PM; Rawlings, BJ; Engberts, JBFN; Cullis, Paul M.; Rawlings, Bernard J.

    2003-01-01

    Differential scanning calorimetry (DSC) results are reported characterising the effects of added cholesterol (CHOL) on vesicle bilayer systems formed in aqueous systems by three sodium dialkylphosphates, (RO)(2)PO2--Na+ where R = dodecyl (DDP), tetradecyl (DTP) and octadecyl (DOP), (ii) two dialkyld

  13. Vapour liquid equilibria of monocaprylin plus palmitic acid or methyl stearate at P=(1.20 and 2.50) kPa by using DSC technique

    DEFF Research Database (Denmark)

    Cunico, Larissa P.; Damaceno, Daniela S.; Matricarde Falleiro, Rafael M.;

    2015-01-01

    The Differential Scanning Calorimetry (DSC) technique is used for measuring isobaric (vapour+liquid) equilibria for two binary mixtures: {monocaprylin+palmitic acid (system 1) or methyl stearate (system 2)} at two different pressures P=(1.20 and 2.50) kPa. The obtained PTx data are correlated by ...

  14. Direct animal calorimetry, the underused gold standard for quantifying the fire of life.

    Science.gov (United States)

    Kaiyala, Karl J; Ramsay, Douglas S

    2011-03-01

    Direct animal calorimetry, the gold standard method for quantifying animal heat production (HP), has been largely supplanted by respirometric indirect calorimetry owing to the relative ease and ready commercial availability of the latter technique. Direct calorimetry, however, can accurately quantify HP and thus metabolic rate (MR) in both metabolically normal and abnormal states, whereas respirometric indirect calorimetry relies on important assumptions that apparently have never been tested in animals with genetic or pharmacologically-induced alterations that dysregulate metabolic fuel partitioning and storage so as to promote obesity and/or diabetes. Contemporary obesity and diabetes research relies heavily on metabolically abnormal animals. Recent data implicating individual and group variation in the gut microbiome in obesity and diabetes raise important questions about transforming aerobic gas exchange into HP because 99% of gut bacteria are anaerobic and they outnumber eukaryotic cells in the body by ∼10-fold. Recent credible work in non-standard laboratory animals documents substantial errors in respirometry-based estimates of HP. Accordingly, it seems obvious that new research employing simultaneous direct and indirect calorimetry (total calorimetry) will be essential to validate respirometric MR phenotyping in existing and future pharmacological and genetic models of obesity and diabetes. We also detail the use of total calorimetry with simultaneous core temperature assessment as a model for studying homeostatic control in a variety of experimental situations, including acute and chronic drug administration. Finally, we offer some tips on performing direct calorimetry, both singly and in combination with indirect calorimetry and core temperature assessment.

  15. 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, J.; 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...

  16. DSC analyses of static and dynamic precipitation of an Al–Mg–Si–Cu aluminum alloy

    Directory of Open Access Journals (Sweden)

    Manping Liu

    2015-04-01

    Full Text Available In the present investigation, both static and dynamic precipitations of an Al–Mg–Si–Cu aluminum alloy after solid-solution treatment (SST were comparatively analyzed using differential scanning calorimetry (DSC. Dynamic aging was performed in the SST alloy through equal channel angular pressing (ECAP at different temperatures of room temperature, 110, 170, 191 and 300 °C. For comparison, static artificial aging was conducted in the SST alloy at 191 °C with two aging times of 4 and 10 h. The DSC analyses reveal that the dynamic precipitation has occurred in the ECAPed samples, while the activation energies associated with the strengthening precipitates in the dynamic samples are considerably higher than the energies in the SST and static aged samples. The higher activation energies are probably attributed to the smaller grains and higher dislocation density developed after ECAP. The results in the present investigation allow the prediction of the type of the dynamic precipitates to influence the strength of the ultrafine grained alloy during ECAP at various temperatures.

  17. Thermal properties of poly(ethylene oxide)/lauric acid blends. A SSA-DSC study

    Energy Technology Data Exchange (ETDEWEB)

    Pielichowski, Krzysztof; Flejtuch, Kinga [Department of Chemistry and Technology of Polymers, Cracow University of Technology, ul. Warszawska 24, 31-155 Krakow (Poland)

    2006-03-15

    A series of poly(ethylene oxide) (PEO)/lauric acid blends with different compositions has been prepared and characterised by differential scanning calorimetry (DSC) in dynamic mode. It has been found that the enthalpy of melting and crystallisation reaches its highest value for PEO/lauric acid blend (1:1, w/w) which makes this system a promising candidate for thermal energy storage applications. Further studies by step-scan alternating (SSA)-DSC revealed that an increase of the temperature step causes that the average total heating rate is also increasing and the heat flow is characterised by higher values. Reversing component of the heat flow during melting reaches lowest values at highest step (step=1{sup o}) when the re-crystallisation of PEO is hindered. An increase of step generally leads to an increase of the number of non-equilibrium effects and facilitates the activation of kinetic non-reversing processes, hindering the overall crystallisation of PEO. For lauric acid, due to facile crystallisation and self-association, formation of ordered regular structures takes place faster and is influenced by non-reversing processes in higher proportion. (author)

  18. Application of chemometric methods to differential scanning calorimeter (DSC) to estimate nimodipine polymorphs from cosolvent system.

    Science.gov (United States)

    Siddiqui, Akhtar; Rahman, Ziyaur; Khan, Mansoor A

    2015-06-01

    The focus of this study was to evaluate the applicability of chemometrics to differential scanning calorimetry data (DSC) to evaluate nimodipine polymorphs. Multivariate calibration models were built using DSC data from known mixtures of the nimodipine modification. The linear baseline correction treatment of data was used to reduce dispersion in thermograms. Principal component analysis of the treated and untreated data explained 96% and 89% of the data variability, respectively. Score and loading plots correlated variability between samples with change in proportion of nimodipine modifications. The R(2) for principal component regression (PCR) and partial lease square regression (PLS) were found to be 0.91 and 0.92. The root mean square of standard error of the treated samples for calibration and validation in PCR and PLS was found to be lower than the untreated sample. These models were applied to samples recrystallized from a cosolvent system, which indicated different proportion of modifications in the mixtures than those obtained by placing samples under different storage conditions. The model was able to predict the nimodipine modifications with known margin of error. Therefore, these models can be used as a quality control tool to expediently determine the nimodipine modification in an unknown mixture.

  19. Multivariate statistical analysis treatment of DSC thermal properties for animal fat adulteration.

    Science.gov (United States)

    Dahimi, Omar; Rahim, Alina Abdul; Abdulkarim, S M; Hassan, Mohd Sukri; Hashari, Shazamawati B T Zam; Mashitoh, A Siti; Saadi, Sami

    2014-09-01

    The adulteration of edible fats is a kind of fraud that impairs the physical and chemical features of the original lipid materials. It has been detected in various food, pharmaceutical and cosmeceutical products. Differential scanning calorimetry (DSC) is the robust thermo-analytical machine that permits to fingerprint the primary crystallisation of triacylglycerols (TAGs) molecules and their transition behaviours. The aims of this study was to assess the cross-contamination caused by lard concentration of 0.5-5% in the mixture systems containing beef tallow (BT) and chicken fat (CF) separately. TAGs species of pure and adulterated lipids in relation to their crystallisation and melting parameters were studied using principal components analysis (PCA). The results showed that by using the heating profiles the discrimination of LD from BT and CF was very clear even at low dose of less than 1%. Same observation was depicted from the crystallisation profiles of BT adulterated by LD doses ranging from 0.1% to 1% and from 2% to 5%, respectively. Furthermore, CF adulterated with LD did not exhibit clear changes on its crystallisation profiles. Consequently, DSC coupled with PCA is one of the techniques that might use to monitor and differentiate the minimum adulteration levels caused by LD in different animal fats.

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

    Science.gov (United States)

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

    2014-09-15

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

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

    Science.gov (United States)

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

    2014-09-01

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

  2. Recent development of material calorimetry%材料量热学的发展现状

    Institute of Scientific and Technical Information of China (English)

    孙玉霞; 李荣德

    2000-01-01

    材料量热学是测量材料变化过程中与热有关的各种物理量(如热焓、熵值等)变化规律的一门学科,分析了国内外材料量热学的发展状况,尤其是对材料量热学中的热分析技术进行了论述,对热分析方法中的差热分析方法(DTA)和差示扫描量热法(DSC)的应用情况做了分析和展望.%Material calorimetry is a subject that measures the changing laws of physical quantities such as enthalpy and entropy that are related to thermal. Recent development of material calorimetry at home and abroad has been reviewed and especially Thermal Analysis (fA) in calorimetric methods has been discussed in the paper. Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC) in thermal analysis have been analyzed in derail. Moreover, several suggestions have been put forward in the end.

  3. Raman and DSC studies of fragility in tellurium-zinc oxide glass formers

    Energy Technology Data Exchange (ETDEWEB)

    Stavrou, Elissaios [Department of Physics, National Technical University of Athens (Greece); Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany); Kripotou, Sotiria; Raptis, Constantine [Department of Physics, National Technical University of Athens (Greece); Turrell, Sylvia [Laboratoire de Spectrochimie Infrarouge et Raman (CNRS 8516), Centre d' Etudes et de Recherches Lasers et Applications (CERLA-FR CNRS 2416), Universite de Sciences et Technologies de Lille, Villeneuve d' Ascq cedex (France); Syassen, Karl [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

    2011-11-15

    Raman scattering and differential scanning calorimetry (DSC) measurements have been carried out in four mixed (TeO{sub 2}){sub 1-x}(ZnO){sub x} (x = 0.1, 0.2, 0.3, 0.4) glasses at high temperatures (Raman and DSC through the glass transition) and high pressures (Raman) with the aim of determining the fragility of these glass forming oxides. Four different criteria, corresponding to four parameters, were applied to assess the fragility of the glasses. From the DSC studies, we have obtained the fragility parameter m which corresponds to the slopes of Arrhenius (lnQ vs. 1/T{sub g}, were Q is the heating rate) plots, and the glass transition width {delta}T{sub g}. Also, from the low-frequency Raman scattering, and in particular the boson peak intensity of the glasses at T{sub g}, we have estimated the fragility ratio r{sub R} (T{sub g}) = I{sub min}/I{sub max} whose value serves as another (empirical) fragility criterion. Finally, from high pressure Raman measurements on the glasses, we have estimated the Grueneisen parameter {gamma}{sub T} for each glass, which constitutes the fourth fragility parameter adopted in this work. Considering the four parameters {delta}T{sub g}, m, r (T{sub g}) and {gamma}{sub T} and the generally accepted (empirical) fragility criteria, we conclude that the mixed tellurium-zinc oxides constitute strong-to-intermediate glass formers (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

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

    Science.gov (United States)

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

    2016-06-01

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

  5. Micromegas for imaging hadronic calorimetry

    CERN Document Server

    Adloff, C; Cap, S; Chefdeville, M; Dalmaz, A; Drancourt, C; Espargiliere, A; Gaglione, R; Gallet, R; Geffroy, N; Jacquemier, J; Karyotakis, Y; Peltier, F; Prast, J; Vouters, G

    2011-01-01

    The recent progress in R&D of the Micromegas detectors for hadronic calorimetry including new engineering-technical solutions, electronics development, and accompanying simulation studies with emphasis on the comparison of the physics performance of the analog and digital readout is described. The developed prototypes are with 2 bit digital readout to exploit the Micromegas proportional mode and thus improve the calorimeter linearity. In addition, measurements of detection efficiency, hit multiplicity, and energy shower profiles obtained during the exposure of small size prototypes to radioactive source quanta, cosmic particles and accelerator beams are reported. Eventually, the status of a large scale chamber (1{\\times}1 m2) are also presented with prospective towards the construction of a 1 m3 digital calorimeter consisting of 40 such chambers.

  6. Development of Quartz Fiber Calorimetry

    CERN Multimedia

    2002-01-01

    % RD40 \\\\ \\\\ Very Forward Calorimeters (VFCs) in LHC detectors should cover the pseudorapidity range from $\\eta$~=~2.5 to at least $\\eta$~=~5 in order to compute missing transverse energy and for jet tagging. Operation at such high rapidity requires the use of a calorimetry technique that is very radiation resistant, fast and insensitive to radioactivity (especially to neutrons). This can be accomplished through the Quartz-Calorimeter~(Q-Cal) concept of embedding silica core fibers, that resist to the Gigarad radiation level, into an absorber. In this calorimeter the shower particles produce light through the Cherenkov effect generating a signal less than 10~ns in duration. Unique to this new technology the visible energy of hadronic showers has a transverse dimension nearly an order of magnitude smaller than that in conventional calorimeters, enabling precise spatial resolution, sharper isolation cuts and better jet recognition against the minimum bias events background. Last but not least, most radioactive ...

  7. STRUCTURAL CHARACTERIZATION OF POLYETHYLENES BY DSC ANALYSIS AFTER CRYSTALLIZATION SEGREGATION

    Institute of Scientific and Technical Information of China (English)

    Yu Ma; Mao Xu

    2000-01-01

    The molecular structure of polyethylene (PE) samples with various comonomers including propylene, 1-butene and 1-hexene was investigated by DSC and 13C-NMR techniques. The density of the samples varies from 0.948 g/cm3 to 0.917 g/cm3, and the molecular weight determined by the GPC method is in the range of 1~2 × 105. The branch point content of the samples was determined by 13C-NMR measurements and was found to be less than 20 per 1000 C atoms along the main chain. Crystallization segregation DSC technique (CSDSC) was used to characterize the branch point distribution or the segment length distribution of PEs. The crystallization segregation was performed in a successive annealing process at decreasing temperatures. The interval of two successive annealing temperatures was 6 K, and the time length of each annealing step was 2.5 h. The CSDSC results clearly indicate that all the PE samples used, including some metallocene PEs,more or less exhibit their non-uniformity in segment length distribution, and bimodal or multimodal CSDSC curves were usually observed. For quantitative characterization of the CSDSC curves and the segment length distribution two parameters,the average melting point, TmAV, and the root-mean-square deviation of melting temperature, (ATm2AV)1/2, were proposed.TmAV is corresponding to the average segment length due to branching and (ATm2AV)1/2 gives information about the width of the segment length distribution. Experimental results show that both the degree of average melting temperature depression and the width of the distribution seem to increase with increasing the branching content and are dependent on the type of comonomers. Very good reproducibility and additivity of the CSDSC method were evidenced experimentally. It was concluded that the CSDSC technique is a sensitive and convenient method for characterizing the segment length distribution of branched polyethylenes and will be of great interest in structure-property relationship

  8. DMSO-Induced Dehydration of DPPC Membranes Studied by X-ray Diffraction, Small-Angle Neutron Scattering, and Calorimetry

    OpenAIRE

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

    2001-01-01

    The influence of dimethyl sulfoxide (DMSO) on membrane thickness, multilamellar repeat distance, and phase transitions of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC) was investigated by X-ray diffraction and small-angle neutron scattering (SANS). The differential scanning calorimetry (DSC) study of water freezing and ice melting was performed in the ternary DPPC /DMSO /water and binary DMSO /water systems. The methods applied demonstrated the differences in membrane structure in t...

  9. Pcm inclusion in gypsum boards for thermal energy storage through latent heat: thermal characterization with DSC; Incorporacion de materiales de cambio de fase en placas de yeso para almacenamiento de energia termica mediante calor latente: caracterizacion termica del material mediante la tecnica DSC

    Energy Technology Data Exchange (ETDEWEB)

    Oliver, A.; Neila, F. J.; Garcia, A.

    2011-07-01

    Differential Scanning Calorimetry (DSC) is a thermal analysis technique which has been used for more than three decades to measure the temperatures and heat flows associated with transitions in materials as a function of time. Other techniques, are Differential Thermal Analysis DTA and Conventional Calorimetry. There is great uncertainty in the values supplied by the manufacturers (because they are referred to pure substances) and the DSC should be used to get more accurate values. It will be analyzed the thermal storage capacity depending on temperature for several compound materials formed by some aggregates, mainly gypsum and phase change materials, in various proportions. The results have been compared with other building materials such as gypsum boards and brick layer. The suitability of the new construction material for thermal energy storage will be assessed in comparison with other materials traditionally used for this purpose. (Author) 21 refs.

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

    Science.gov (United States)

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

    2014-01-01

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

  11. Dijet mass resolution and compensating calorimetry

    International Nuclear Information System (INIS)

    The calorimetry for SSC detectors has as its role the detection of the basic particles of the Standard Model. Those germane to calorimetry are quarks, photons, electrons, and gluons. Note that all the hadronic entities appear in the calorimetry as jets. The detection of single hadrons belongs to a past era when ''quark molecules'' were the focus of intense study. Thus, the goal of calorimetry at the SSC must be the study of jets. In particular, one must understand what defines the limits of accuracy of the jets. If there are intrinsic physical processes which limit the precision of jet measurements, then calorimetry which is more accurate is unnecessary if not wasteful. 5 refs., 5 figs

  12. 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. PMID:10333299

  13. 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.

  14. First application of simultaneous SANS and differential scanning calorimetry: Microphase separated alkane blends

    International Nuclear Information System (INIS)

    For almost 30 years, it has been possible at synchrotron facilities to perform small-angle x-ray scattering experiments whilst simultaneously measuring phase transitions using differential scanning calorimetry (DSC). However, a range of challenges exist to enable the collection of simultaneous small-angle neutron scattering (SANS) and DSC data associated not only with intrinsic flux limitations but also scattering geometry and thermal control. The development of a DSC (temperature range ca. −150 C to 500 C) suitable for SANS is detailed here which, to our knowledge, is the first and only one of its kind. An example study is presented from the 40 m SANS instrument, QUOKKA, at the OPAL reactor at ANSTO (Figure 1), concerned with phase transitions in a binary blend of normal alkanes in which one component has been deuterium labelled[1]. The ability to conduct simultaneous DSC and neutron scattering studies allows investigators to use these two complementary techniques to provide insight into structural and thermal changes and opens up the opportunity for SANS to make significant new contributions to a range of systems in which either scattering contrast is insufficient for SAXS studies or where neutron scattering is essential or inherently desirable (e.g. isotope effects).

  15. WA80 BGO calorimetry electronics

    International Nuclear Information System (INIS)

    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-cm2 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

  16. DSC modelling for predicting resilient modulus of crushed rock base as a road base material for Western Australia roads

    Institute of Scientific and Technical Information of China (English)

    KHOBKLANG Pakdee; VIMONSATIT Vanissorn; JITSANGIAM Peerapong; NIKRAZ Hamid

    2013-01-01

    In order to increase the applied efficiency of crushed rock base (CRB) in pavement structure design for Western Australia roads,the material modelling based on the experimental results was investigated,and the disturbed state concept (DSC) was used to predict the resilient modulus of CRB because of its simplicity and strong ability in capturing the elastic and inelastic responses of materials to loads.The actual deformation of DSC,at any loading state,was determined from its assumed relative intact (RI) state.The DSC equation of CRB was constructed by using a set of experimental results of resilient modulus tests,and an idealized material model,namely the linear elastic model,of relative intact (RI) part was considered.Analysis results reveal that the resilient modulus-applied stress relationships back-predicted by using the DSC modelling are consistent with the experimental results,so,the DSC equation is suited for predicting the resilient modulus of CRB specimen.However,the model and the equation coming from the test results are conducted in accordance with the Austroads standard,so further investigation and validation with respect to the field behaviours of pavement structure should be performed.7 figs,11 refs.

  17. Advances in simultaneous DSC-FTIR microspectroscopy for rapid solid-state chemical stability studies: some dipeptide drugs as examples.

    Science.gov (United States)

    Lin, Shan-Yang; Wang, Shun-Li

    2012-04-01

    The solid-state chemistry of drugs has seen growing importance in the pharmaceutical industry for the development of useful API (active pharmaceutical ingredients) of drugs and stable dosage forms. The stability of drugs in various solid dosage forms is an important issue because solid dosage forms are the most common pharmaceutical formulation in clinical use. In solid-state stability studies of drugs, an ideal accelerated method must not only be selected by different complicated methods, but must also detect the formation of degraded product. In this review article, an analytical technique combining differential scanning calorimetry and Fourier-transform infrared (DSC-FTIR) microspectroscopy simulates the accelerated stability test, and simultaneously detects the decomposed products in real time. The pharmaceutical dipeptides aspartame hemihydrate, lisinopril dihydrate, and enalapril maleate either with or without Eudragit E were used as testing examples. This one-step simultaneous DSC-FTIR technique for real-time detection of diketopiperazine (DKP) directly evidenced the dehydration process and DKP formation as an impurity common in pharmaceutical dipeptides. DKP formation in various dipeptides determined by different analytical methods had been collected and compiled. Although many analytical methods have been applied, the combined DSC-FTIR technique is an easy and fast analytical method which not only can simulate the accelerated drug stability testing but also at the same time enable to explore phase transformation as well as degradation due to thermal-related reactions. This technique offers quick and proper interpretations.

  18. Process induced transformations during tablet manufacturing: phase transition analysis of caffeine using DSC and low frequency micro-Raman spectroscopy.

    Science.gov (United States)

    Hubert, Sébastien; Briancon, Stéphanie; Hedoux, Alain; Guinet, Yannick; Paccou, Laurent; Fessi, Hatem; Puel, François

    2011-11-25

    The phase transition of a model API, caffeine Form I, was studied during tableting process monitored with an instrumented press. The formulation used had a plastic flow behavior according to the Heckel model in the compression pressure range of 70-170 MPa. The quantitative methods of analysis used were Differential Scanning Calorimetry (DSC) and low frequency Micro Raman Spectroscopy (MRS) which was used for the first time for the mapping of polymorphs in tablets. They brought complementary contributions since MRS is a microscopic spectral analysis with a spatial resolution of 5 μm(3) and DSC takes into account a macroscopic fraction (10mg) of the tablet. Phase transitions were present at the surfaces, borders and center of the tablets. Whatever the pressure applied during the compression process, the transition degree of caffeine Form I toward Form II was almost constant. MRS provided higher transition degrees (50-60%) than DSC (20-35%). MRS revealed that caffeine Form I particles were partially transformed in all parts of the tablets at a microscopic scale. Moreover, tablet surfaces showed local higher transition degree compared to the other parts.

  19. The application of differential scanning calorimetry as a mean to determine the oxidative stability of vegetable oils and its comparison with Rancimat

    Directory of Open Access Journals (Sweden)

    Yousef Ramezan

    2015-09-01

    Full Text Available Differential scanning calorimetry (DSC and Rancimat apparatus have been used to evaluate the oxidative stability of eight different edible vegetable oils. Rancimat apparatus was operated at 110 ⁰C with an air flow of 18-20 L/hand measures the induction period (IP of the selected samples. The DSC technique involved the oxidation of the samples in an oxygen flow DSC cell when the cell temperature was set at isothermal temperatures of 100, 110, 120 and 130 ⁰C. Oxidative induction time (T0 determined by the time, where a rapid exothermic reaction were occurred between oil and oxygen. The results showed that unsaturated edible oils are more susceptible to oxidation in short time, than saturated one. Furthermore, the results indicated that there is a good correlation (p<0.0001 between DSC T0 and the Rancimat values.

  20. Radiation Induced Aging Effects in Polymeric Cable Insulators at CERN. Compilation of the DSC and ATR-FTIR data on irradiated CERN cables.

    CERN Document Server

    Sorin, I

    2009-01-01

    This second part of the Report on Radiation Induced Aging Effects in Polymeric Cable Insulators at CERN [1] summarizes in a tabulated form all the experimental DSC results obtained in this work, concerning the life-time evaluation of the selected CERN cables irradiated in different conditions. Several examples of DSC curves and ATR-FTIR spectra were included to support the future polymeric materials analysis. Information on the experimental conditions, the instruments, the basic concept of life-time evaluation using the DSC data, as well as the examples of data processing and interpretation are presented and discussed in reference [1].

  1. Kinetics Characteristics of Nitrogen Hydrates Respond to Differential Scanning Calorimetry

    Science.gov (United States)

    Chen, Q.; Liu, C.; Ye, Y.; Gong, J.

    2012-12-01

    In this study, a high pressure differential scanning calorimetry (HP DSC) based on thermo-analytical technique was applied to investigate the kinetics and thermodynamics characteristics of nitrogen hydrates. Nitrogen hydrates was synthesized in the sample vessel under different pressures as temperature decreased from 293 to 233 K with a constant cooling rate of 0.2 K/min controlled by the DSC. To measure the hydrates dissociation enthalpies , the temperature was slowly raised up from 233 to 293 K at a constant rate ranging of 0.05 K/min. 1. Peak area on the heat flow curves represents the amount of heat during phase transition. In these experiments, the total water added to the sample vessel (mt) is already known. By integrating the peak areas of ice and hydrate, we know the total heats of ice (Qi) and hydrate (Qh), respectively. As the heat of ice per gram can be measured easily (336.366 J/g), the mass of ice (mi) can be obtain. Then, the dissociation heat of nitrogen hydrate per gram (Hh ) can be calculated by the equation: H(J/g)=Qh/(mt-mi) It is shown that the dissociation heats of nitrogen hydrates are a little larger than ice, but do not change a lot with different pressures. The average value of dissociation heat is 369.158 J/g. 2. During the DSC cooling stage, hydrate formed at temperature much lower than equilibrium. The biggest sub-cooling is about 291 K, while the smallest one is about 279 K. However, during these experiments, the pressure did not show obvious relationship with sub-cooling. It confirmed that even the proper conditions were achieved, formation was still a stochastic process. For one thing, due to the random distribution of dissolved gas in water, the interfacial tension and the water activity were not equal in the whole system. And if there was a free gas phase, which leads to different fugacity on water-gas interface, the stochastic behavior would be more significant in the sample vessel. 3. The energy released from hydrates formation as

  2. Automatic calorimetry system monitors RF power

    Science.gov (United States)

    Harness, B. W.; Heiberger, E. C.

    1969-01-01

    Calorimetry system monitors the average power dissipated in a high power RF transmitter. Sensors measure the change in temperature and the flow rate of the coolant, while a multiplier computes the power dissipated in the RF load.

  3. Thermodynamic properties of isomeric iso-butoxybenzoic acids: Experimental and theoretical study

    International Nuclear Information System (INIS)

    Highlights: • Vapor pressures of butoxy benzoic acid derivatives were measured. • Vaporization, sublimation and fusion enthalpies were derived. • Molar enthalpies of formation were measured by calorimetry. • Thermochemical data tested for consistency using additivity rules and computations. • Simple additivity method suggested for prediction thermochemical properties. - Abstract: Standard (p° = 0.1 MPa) molar enthalpies of formation at the temperature T = 298.15 K of the 2-, 3-, and 4-iso-butoxybenzoic acids were measured using the combustion calorimetry. Standard molar enthalpies of vaporization and sublimation were derived from the vapor pressure temperature dependencies measured by the transpiration method. Molar enthalpies of the solid state phase transitions were measured by the DSC. Thermodynamic data on alkoxy substituted benzoic acids available in the literature were collected and combined with own experimental results. This data set on alkoxybenzoic acids was evaluated by using quantum-chemical and group-additivity methods

  4. Thermodynamic properties of isomeric iso-butoxybenzoic acids: Experimental and theoretical study

    Energy Technology Data Exchange (ETDEWEB)

    Jakubczyk, Michał; Sporzyński, Andrzej [Faculty of Chemistry, Warsaw University of Technology, 00-664 Warszawa (Poland); Emel’yanenko, Vladimir N.; Varfolomeev, Mikhail A. [Department of Physical Chemistry, Kazan Federal University, 420008 Kazan (Russian Federation); Verevkin, Sergey P., E-mail: sergey.verevkin@uni-rostock.de [Department of Physical Chemistry, Kazan Federal University, 420008 Kazan (Russian Federation); Department of Physical Chemistry and Department, Science and Technology of Life, Light and Matter, University of Rostock, D-18059 Rostock (Germany)

    2015-09-10

    Highlights: • Vapor pressures of butoxy benzoic acid derivatives were measured. • Vaporization, sublimation and fusion enthalpies were derived. • Molar enthalpies of formation were measured by calorimetry. • Thermochemical data tested for consistency using additivity rules and computations. • Simple additivity method suggested for prediction thermochemical properties. - Abstract: Standard (p° = 0.1 MPa) molar enthalpies of formation at the temperature T = 298.15 K of the 2-, 3-, and 4-iso-butoxybenzoic acids were measured using the combustion calorimetry. Standard molar enthalpies of vaporization and sublimation were derived from the vapor pressure temperature dependencies measured by the transpiration method. Molar enthalpies of the solid state phase transitions were measured by the DSC. Thermodynamic data on alkoxy substituted benzoic acids available in the literature were collected and combined with own experimental results. This data set on alkoxybenzoic acids was evaluated by using quantum-chemical and group-additivity methods.

  5. Entropy production in ac-calorimetry

    OpenAIRE

    Garden, Jean-Luc; Richard, Jacques

    2007-01-01

    In calorimetry and particularly in heat capacity measurements, different characteristic relaxation time constants may perturb the experiment which cannot be considered at thermodynamic equilibrium. In this case, thermodynamics of irreversible processes has to be taken into account and the calorimetric measurements must be considered as dynamic. In a temperature modulated experiment, such as ac-calorimetry, these non-equilibrium experiments give rise to the notion of frequency dependent comple...

  6. Kinetics of the thermal degradation of Erica arborea by DSC: Hybrid kinetic method

    CERN Document Server

    Cancellieri, Dominique; Rossi, Jean Louis; 10.1016/j.tca.2005.07.013

    2008-01-01

    The scope of this work was the determination of kinetic parameters of the thermal oxidative degradation of a Mediterranean scrub using a hybrid method developed at the laboratory. DSC and TGA were used in this study under air sweeping to record oxidative reactions. Two dominating and overlapped exothermic peaks were recorded in DSC and individualized using an experimental and numerical separation. This first stage allowed obtaining the enthalpy variation of each exothermic phenomenon. In a second time, a model free method was applied on each isolated curve to determine the apparent activation energies. A reactional kinetic scheme was proposed for the global exotherm composed of two independent and consecutive reactions. In fine mean values of enthalpy variation and apparent activation energy previously determined were injected in a model fitting method to obtain the reaction order and the preexponential factor of each oxidative reaction. We plan to use these data in a sub-model to be integrated in a wildland ...

  7. Thermal degradation of ligno-cellulosic fuels. DSC and TGA studies

    Energy Technology Data Exchange (ETDEWEB)

    Leroy, V.; Cancellieri, D.; Leoni, E. [SPE-CNRS UMR 6134, University of Corsica, Campus Grossetti, BP 52, 20250 Corti (France)

    2006-12-01

    The scope of this work was to show the utility of thermal analysis and calorimetric experiments to study the thermal oxidative degradation of Mediterranean scrubs. We investigated the thermal degradation of four species; DSC and TGA were used under air sweeping to record oxidative reactions in dynamic conditions. Heat released and mass loss are important data to be measured for wildland fires modelling purpose and fire hazard studies on ligno-cellulosic fuels. Around 638 and 778K, two dominating and overlapped exothermic peaks were recorded in DSC and individualized using a experimental and numerical separation. This stage allowed obtaining the enthalpy variation of each exothermic phenomenon. As an application, we propose to classify the fuels according to the heat released and the rate constant of each reaction. TGA experiments showed under air two successive mass loss around 638 and 778K. Both techniques are useful in order to measure ignitability, combustibility and sustainability of forest fuels. (author)

  8. Thermal degradation of ligno-cellulosic fuels: DSC and TGA studies

    CERN Document Server

    Leroy, Valérie; Leoni, Eric; 10.1016/j.tca.2006.09.017

    2008-01-01

    The scope of this work was to show the utility of thermal analysis and calorimetric experiments to study the thermal oxidative degradation of Mediterranean scrubs. We investigated the thermal degradation of four species; DSC and TGA were used under air sweeping to record oxidative reactions in dynamic conditions. Heat released and mass loss are important data to be measured for wildland fires modelling purpose and fire hazard studies on ligno-cellulosic fuels. Around 638 and 778 K, two dominating and overlapped exothermic peaks were recorded in DSC and individualized using a experimental and numerical separation. This stage allowed obtaining the enthalpy variation of each exothermic phenomenon. As an application, we propose to classify the fuels according to the heat released and the rate constant of each reaction. TGA experiments showed under air two successive mass loss around 638 and 778 K. Both techniques are useful in order to measure ignitability, combustibility and sustainability of forest fuels.

  9. Differential scanning calorimetry predicts the critical quality attributes of amorphous glibenclamide.

    Science.gov (United States)

    Mah, Pei T; Laaksonen, Timo; Rades, Thomas; Peltonen, Leena; Strachan, Clare J

    2015-12-01

    Selection of a crystallinity detection tool that is able to predict the critical quality attributes of amorphous formulations is imperative for the development of process control strategies. The main aim of this study was to determine the crystallinity detection tool that best predicts the critical quality attributes (i.e. physical stability and dissolution behaviour) of amorphous material. Glibenclamide (model drug) was milled for various durations using a planetary mill and characterised using Raman spectroscopy and differential scanning calorimetry (DSC). Physical stability studies upon storage at 60°C/0% RH and dissolution studies (non-sink conditions) were performed on the milled glibenclamide samples. Different milling durations were needed to render glibenclamide fully amorphous according to Raman spectroscopy (60min) and onset of crystallisation using DSC (150min). This could be due to the superiority of DSC (onset of crystallisation) in detecting residual crystallinity in the samples milled for between 60 and 120min, which were not detectable with Raman spectroscopy. The physical stability upon storage and dissolution behaviour of the milled samples improved with increased milling duration and plateaus were reached after milling for certain periods of time (physical stability - 150min; dissolution - 120min). The residual crystallinity which was detectable with DSC (onset of crystallisation), but not with Raman spectroscopy, adversely affected the critical quality attributes of milled glibenclamide samples. In addition, mathematical simulations were performed on the dissolution data to determine the solubility advantages of the milled glibenclamide samples and to describe the crystallisation process that occurred during dissolution in pH7.4 phosphate buffer. In conclusion, the onset of crystallisation obtained from DSC measurements best predicts the critical quality attributes of milled glibenclamide samples and mathematical simulations based on the

  10. Combination of TREF, high-temperature HPLC, FTIR and HPer DSC for the comprehensive analysis of complex polypropylene copolymers.

    Science.gov (United States)

    Cheruthazhekatt, Sadiqali; Pijpers, Thijs F J; Mathot, Vincent B F; Pasch, Harald

    2013-11-01

    A novel, powerful analytical technique, preparative temperature rising elution fractionation (prep TREF)/high-temperature (HT)-HPLC/Fourier transform infrared spectroscopy (FTIR)/high-performance differential scanning calorimetry (HPer DSC)), has been introduced to study the correlation between the polymer chain microstructure and the thermal behaviour of various components in a complex impact polypropylene copolymer (IPC). For the comprehensive analysis of this complex material, in a first step, prep TREF is used to produce less complex but still heterogeneous fractions. These chemically heterogeneous fractions are completely separated by using a highly selective chromatographic separation method--high-temperature solvent gradient HPLC. The detailed structural and thermal analysis of the HPLC fractions was conducted by offline coupling of HT-HPLC with FTIR spectroscopy and a novel DSC method--HPer DSC. Three chemically different components were identified in the mid-elution temperature TREF fractions. For the first component, identified as isotactic polypropylene homopolymer by FTIR, the macromolecular chain length is found to be an important factor affecting the melting and crystallisation behaviour. The second component relates to ethylene-propylene copolymer molecules with varying ethylene monomer distributions and propylene tacticity distributions. For the polyethylene component (last eluting component in all semi-crystalline TREF fractions), it was found that branching produced defects in the long crystallisable ethylene sequences that affected the thermal properties. The different species exhibit distinctively different melting and crystallisation behaviour, as documented by HPer DSC. Using this novel approach of hyphenated techniques, the chain structure and melting and crystallisation behaviour of different components in a complex copolymer were investigated systematically.

  11. Isothermal Titration Calorimetry: Assisted Crystallization of RNA-Ligand Complexes.

    Science.gov (United States)

    Da Veiga, Cyrielle; Mezher, Joelle; Dumas, Philippe; Ennifar, Eric

    2016-01-01

    The success rate of nucleic acids/ligands co-crystallization can be significantly improved by performing preliminary biophysical analyses. Among suitable biophysical approaches, isothermal titration calorimetry (ITC) is certainly a method of choice. ITC can be used in a wide range of experimental conditions to monitor in real time the formation of the RNA- or DNA-ligand complex, with the advantage of providing in addition the complete binding profile of the interaction. Following the ITC experiment, the complex is ready to be concentrated for crystallization trials. This chapter describes a detailed experimental protocol for using ITC as a tool for monitoring RNA/small molecule binding, followed by co-crystallization.

  12. Thermal Properties of Silk Fibroin Using Fast Scanning Calorimetry

    Science.gov (United States)

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

    We performed fast scanning chip-based calorimetry of silk protein using the Mettler Flash DSC1. We suggest the methodology by which to obtain quantitative information on the very first scan to high temperature, including the melting endotherm of the beta pleated sheets. For proteins, this first scan is the most important one, because the crystalline secondary structural features, the beta pleated sheets, melt after the first heating and cannot be thermally reintroduced. To obtain high quality data, the samples must be treated to drying and enthalpy relaxation sequences. The heat flow rates in heating and cooling must be corrected for asymmetric heat loses. We evaluate methods to obtain an estimate of the sample mass, finally choosing internal calibration using the known heat capacity increment at the glass transition. We report that even heating at rates of 2000 K/s, thermal degradation of silk cannot be totally avoided, though it can be minimized. Using a set of nineteen samples, we successfully determine the liquid state heat capacity of silk as: Cpliquid (T) = (1.98 +0.06) J/gK + T (6.82 +1.4) x10-4 J/gK2. Methods for estimation of the sample mass will be presented and compared. National Science Foundation, Polymers Program DMR-1206010; DAAD; Tufts Faculty Supported Leave.

  13. DSC and TMA studies on freezing and thawing gelation of galactomannan polysaccharide

    Energy Technology Data Exchange (ETDEWEB)

    Iijima, Mika, E-mail: m-iijima@nagasaki-u.ac.jp [Faculty of Education, Nagasaki University, 1-14, Bunkyo-machi, Nagasaki 852-8521 (Japan); Hatakeyama, Tatsuko [Lignocell Research, 73-8 Yatsumata, Fukui 910-3558 (Japan); Hatakeyama, Hyoe [Department of Environment and Biotechnology, Faculty of Engineering, Fukui University of Technology, 3-6-1, Gakuen, Fukui 910-8505 (Japan)

    2012-03-20

    Research highlights: Black-Right-Pointing-Pointer Locust bean gum forms hydrogels by freezing and thawing. Black-Right-Pointing-Pointer Syneresis was observed when freezing and thawing cycle (n) increased. Black-Right-Pointing-Pointer Dynamic Young's modulus increased with increasing n. Black-Right-Pointing-Pointer Non-freezing water content restrained by hydrogels decreased with increasing n. Black-Right-Pointing-Pointer Strong gel with densely packed network structure formed with increasing n. - Abstract: Among various kinds of polysaccharides known to form hydrogels, locust bean gum (LBG) consisting of a mannose backbone and galactose side chains has unique characteristics, since LBG forms hydrogels by freezing and thawing. In this study, effect of thermal history on gelation was investigated by differential scanning calorimetry (DSC) and thermomechanical analysis (TMA). Gel/sol ratio calculated by weighing method was found to be affected by sol concentration, freezing rate and the number of freezing and thawing cycle (n). Once LBG hydrogels are formed, they are thermally stable, although syneresis was observed when n increased. Dynamic Young's modulus (E Prime ) of hydrogels measured by TMA in water increased with increasing n and decreasing freezing rate. Non-freezing water calculated from DSC melting peak of ice in the gel decreased with increasing n and decreasing freezing rate. Morphological observation of freeze-dried gels was carried out by scanning electron microscopy (SEM). The above results indicate that weak hydrogel having large molecular network structure transformed into strong gel with densely packed network structure by increasing n and decreasing freezing rate.

  14. Cryomilled Aluminum with Diamantane: Thermal Characterization by DSC and Effects of Magnesium

    Science.gov (United States)

    Arnold, Michael Colin

    Many structural applications require a material that is both lightweight and corrosion resistant, for which aluminum and its alloys may be considered for use if not for their relatively low strength. By improving strength of aluminum through the Hall-Petch mechanism, it could become a more suitable choice for many structural applications. Cryomilling is used as a production technique to strengthen aluminum by reduction of grain size to the 20-50 nm range. Although the powders produced by cryomilling are well within the nanocrystalline regime, the powders experience significant grain growth during consolidation to a solid body. Cryomilled powders have been shown to remain nanocrystalline by introducing a nano-diamond, diamantane to the grain boundaries. To better characterize the thermal stability of the cryomilled powder with diamantane, Differential Scanning Calorimetry (DSC) was used to measure the isothermal heat flow in the 0.6Tm to 0.9Tm range. A model was developed to correlate the isothermal DSC signal to a grain growth curve and grain growth parameters were elucidated by assuming variable boundary mobility with a sigmoidal form. The model revealed a tendency for boundary mobility to transition from an athermal grain growth mechanism to standard thermally activated grain growth. Grain growth parameters were compared to shed light on possible mechanisms of aluminum-diamantane involvement during grain growth. Powders and consolidated samples with very low concentrations of diamantane and with magnesium were observed by TEM, SEM and XRD, and compared both separately and together to characterize the how thermal stability is affected by diamantane concentration and the presence of magnesium.

  15. In situ stability of substrate-associated cellulases studied by DSC.

    Science.gov (United States)

    Alasepp, Kadri; Borch, Kim; Cruys-Bagger, Nicolaj; Badino, Silke; Jensen, Kenneth; Sørensen, Trine H; Windahl, Michael S; Westh, Peter

    2014-06-24

    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 of the transition peak was used as a gauge of the population of native enzyme. Analogous measurements were made for enzymes in pure buffer. Investigations of two cellobiohydrolases, Cel6A and Cel7A, from Trichoderma reesei, which is an anamorph of the fungus Hypocrea jerorina, showed that these enzymes were essentially stable at 25 °C. Thus, over a 53 h experiment, Cel6A lost less than 15% of the native population and Cel7A showed no detectable loss for either the free or substrate-adsorbed state. At higher temperatures we found significant losses in the native populations, and at the highest tested temperature (49 °C) about 80% Cel6A and 35% of Cel7A was lost after 53 h of hydrolysis. The data consistently showed that Cel7A was more long-term stable than Cel6A and that substrate-associated enzyme was less long-term stable than enzyme in pure buffer stored under otherwise equal conditions. There was no correlation between the intrinsic stability, specified by the transition temperature in the DSC, and the long-term stability derived from the peak area. The results are discussed with respect to the role of enzyme denaturation for the ubiquitous slowdown observed in the enzymatic hydrolysis of cellulose.

  16. Thermodynamic properties of methylquinolines: Experimental results for 2,6-dimethylquinoline and mutual validation between experiments and computational methods for methylquinolines

    Energy Technology Data Exchange (ETDEWEB)

    Chirico, Robert D. [Physical and Chemical Properties Division, National Institute of Standards and Technology (NIST), Boulder, CO 80305-3328 (United States)]. E-mail: chirico@boulder.nist.gov; Johnson, Russell D. [Physical and Chemical Properties Division, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899-8380 (United States)]. E-mail: rjohnson@nist.gov; Steele, William V. [Physical Properties Research Facility, Chemical Engineering Department, 327 Dougherty Engineering Building, 1512 Middle Drive, University of Tennessee, Knoxville, TN 37996-2200 (United States) and Nuclear Science and Technology Division, Oak Ridge National Laboratory (ORNL), Oak Ridge, TN 37831-6273 (United States)]. E-mail: steelewv@ornl.gov

    2007-05-15

    Measurements leading to the calculation of the standard thermodynamic properties for gaseous 2,6-dimethylquinoline (Chemical Abstracts registry number [877-43-0]) are reported. Experimental methods included adiabatic heat-capacity calorimetry, vibrating-tube densimetry, comparative ebulliometry, inclined-piston gauge manometry, differential-scanning calorimetry (d.s.c.), and combustion calorimetry. The critical temperature was measured with d.s.c. The critical pressure and critical density were estimated. Molar entropies, molar enthalpies, and molar Gibbs free energies of formation for the ideal gas state were derived at selected temperatures between 298.15 K and 700 K. Results are compared with experimental property values reported previously in the literature. Independent calculations of the ideal gas entropies were performed at the B3LYP/6-31+G(d,p) model chemistry for 2,6-dimethylquinoline and other methylquinolines (including hindered internal rotations) and are shown to be in excellent accord with the calorimetric results. Implications of these results are discussed.

  17. Evaluation of the modified nanoclay effect on the vulcanization of SBR through rheometric curve and DSC;Avaliacao do efeito de nanoargila modificada na vulcanizacao de SBR atraves da curva reometrica e DSC

    Energy Technology Data Exchange (ETDEWEB)

    Forte, Maria Madalena C.; Brito, Karin J.S., E-mail: mmcforte@ufrgs.b [Universidade Federal do Rio Grande do Sul (PPGEM/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia Mecanica; Gheller Junior, Jordao [SENAI, Sao Leopoldo, RS (Brazil). Centro Tecnologico de Polimeros

    2009-07-01

    Rubber nanocomposites with nanoclays organically modified by quaternary ammonium salts may have the curing features modified significantly, since the salts may act on the rubber cure system. The aim of this work is to evaluate the influences of an organically modified montmorillonite (OMMT) on the curing reaction of an SBR (styrene butadiene rubber) with sulfur. The SBR/OMMT nanocomposites were prepared by co-coagulating SBR latex and Cloisite{sup R} 20A aqueous suspension at different nanoclay concentrations. The OMMT effect on the sulfur curing reaction was evaluated by the rheometric curve using a rheometer type RPA (Rubber Process Analyzer) and the heat of vulcanization (DELTAH{sub v}) using Differential Scanning Calorimetry (DSC). The evaluation of the clay nanolayers dispersion in the SBR matrix was accomplished by x-ray diffraction (XRD) analysis. (author)

  18. DSC Study on the Thermal Hysteresis Activity of Plant Antifreeze Proteins%沙冬青抗冻蛋白热滞活性的DSC研究

    Institute of Scientific and Technical Information of China (English)

    周晓蕾; 陈滔滔; 王保怀; 李芝芬; 费云标; 魏令波; 高素琴

    2001-01-01

    Differential scanning calorimetry (DSC) was used to measure thethermal hysteresis activity(THA) of plant antifreeze proteins(AFPs). The results reveal that DSC is a good method to screen and study AFPs. In the sixteen components extracted from Ammopipanthus mongolicus leaves, one(P3S1) was found to have apparent thermal hysteresis activity by DSC. As the amount of ice nuclei in the sample decreased, the THA of P3S1 increased from 0.01 ℃ to 0.65 ℃ . It is notable that the two-peak thermal hysteresis effect was observed. Two endothermic peaks appeared in the melting process of P3S1, while the freezing peak also consisted of two peaks. The peaks appeared antecedently showed larger thermal effect. This phenomenon shows P3S1 has two different kinds of interaction with water and ice crystal. It is probably an important property of a class of AFPs.

  19. Study of the developed precipitates in Al-0.63Mg-0.37Si-0.5Cu (wt.%) alloy by using DSC and TEM techniques

    Energy Technology Data Exchange (ETDEWEB)

    Gaber, A. [Physics Department, Faculty of Science, Assiut University (Egypt)]. E-mail: gaberaf@acc.aun.edu.eg; Ali, A. Mossad [Physics Department, Faculty of Science, Assiut University (Egypt); Matsuda, K. [Faculty of Engineering, University of Toyama (Japan); Kawabata, T. [Faculty of Engineering, University of Toyama (Japan); Yamazaki, T. [Faculty of Engineering, University of Toyama (Japan); Ikeno, S. [Faculty of Engineering, University of Toyama (Japan)

    2007-04-25

    Heat treatable Al-Mg-Si containing Cu alloys can be strengthened by the precipitation of the nano-scale metastable precipitates. In order to follow the precipitation sequence in balanced Al-1 mass%Mg{sub 2}Si containing 0.5 mass%Cu during continuous heating, differential scanning calorimetry (DSC) was performed. Analysis of non-isothermal DSC scans at various heating rates were carried out to evaluate the overall activation energies associated with the precipitation processes and, therefore, the mechanism of the developed precipitates has been characterized. The most important developed precipitates that assist the strength of the alloy are random, Q' and {beta}' precipitates. According to the obtained activation energies, the kinetics of the evolved Q'-precipitates could be controlled by the diffusion of Mg, Si and Cu in the crystal lattice of the alloy. Both conventional and high resolution transmission electron microscopy (HRTEM) were utilized to confirm the obtained results.

  20. Study of polymer film formation and their characterization using NMR, XRD and DSC

    Energy Technology Data Exchange (ETDEWEB)

    Ghoshal, Sushanta

    2012-07-01

    Film formation and their characterization of three eco-friendly polymers, namely gelatin, starch and poly(vinyl alcohol) (PVOH) were studied using nuclear magnetic resonance (NMR), wide-angle X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) techniques. Polymer solutions were prepared using water as a solvent followed by casting. The drying process of the cast sample was monitored at room temperature with a single-sided NMR scanner until complete solidification occurred. Depth-dependent NMR profiles with microscopic resolution were acquired at different stages of sample drying. Each profile point was accumulated from the echo decay. Spin-spin relaxation times (T{sub 2}) were measured from the echo decays at different layers and were correlated with the drying process during film formation. Additionally, spin-lattice relaxation times (T{sub 1}) were determined. Depending on the polymer studied and the initial concentration of each polymer, different types of molecular dynamics were observed at different heights during evaporation of the solvent. The study indicates that each polymer shows a spatial heterogeneity in the molecular dynamics during drying. In the advanced stage of drying process, the microscopic arrangement of the polymer chains during their solidification is influenced by this dynamic heterogeneity and determines the final structure of the film. XRD of the film in its final state confirmed the structural heterogeneity identified by the NMR.

  1. Qualitative and kinetic analysis of torrefaction of lignocellulosic biomass using DSC-TGA-FTIR

    Directory of Open Access Journals (Sweden)

    Bimal Acharya

    2015-11-01

    Full Text Available Torrefaction is a thermochemical conversion technique to improve the fuel properties of lignocellulosic biomass by treating at temperature 200 ℃-300 ℃ in the minimum oxygen environment for a reasonable residence time. In this study, thermal decomposition and thermal activities of miscanthus and wheat straw during the torrefaction at 200 ℃, 275 ℃, and 300 ℃ in a nitrogen environment for 45 minutes of residence time are analyzed in a simultaneous thermogravimetric analyzer (micro TGA with a differential scanning calorimetry (DSC, and a macro-TGA. The output of the micro TGA is fed into the Fourier transform infrared spectrometry (FTIR and qualitative analysis of the gaseous product is carried out. The composition of different gas products during the torrefaction of biomass are compared critically and kinetics were analyzed. It is found that the weight loss due to degradation of initial biomass in second stage (torrefaction process is a much faster conversion process than the weight loss process in the first stage (drying process. The weight loss of biomass increases with increase in the residence time and torrefaction treatment temperatures. The yield after torrefaction is a solid bio-coal product. The torrefied product were less reactive and has nearly 25% better heating value than the raw biomass. Between the two feedstocks studied, torrefied miscanthus proved to be a more stable fuel than the torrefied wheat straw. The major gaseous components observed during torrefaction are water, carbon dioxide, carbon monoxide, 1,2-Dibromethylene.

  2. Effect of hydrate formation-dissociation on emulsion stability using DSC and visual techniques

    Energy Technology Data Exchange (ETDEWEB)

    Lachance, J.W.; Dendy Sloan, E.; Koh, C.A. [Colorado School of Mines, Golden, CO (United States). Center for Hydrates Research

    2008-07-01

    Many flow assurance operators are now focusing on preventing hydrates from agglomerating and forming plugs within pipelines. A key factor in reducing plug formation in oil-dominated systems is the stability of emulsified water in gas hydrate formation. In this study, differential scanning calorimetry (DSC) studies were used to show that gas hydrate formation has a destabilizing effect on water and oil emulsions, and can result in a free water phase through the coalescence and agglomeration of dissociated hydrate particles. The study focused on investigating the ability of the hydrates to stay segregated with hydrate formation. The stability of water-in-oil emulsions with hydrate formation was investigated with a range of different crude oils with varying emulsion stability levels. Thermal properties were measured at both atmospheric and pressurized conditions. Thermocouples in the calorimetric furnace were used to measure the temperature difference between reference and sample cells. Emulsion stability was measured over a 1-month time period. Results of the study showed that hydrate formation and dissociation destabilizes emulsions. However, the asphaltene fraction in crude oils resists hydrate-induced destabilization. The stability of the emulsion increased when asphaltene content increased. It was concluded that emulsion stability is a key factor in preventing agglomeration in flow lines. 14 refs., 3 tabs., 8 figs.

  3. Thermal characterization and model free kinetics of aged epoxies and foams using TGA and DSC methods.

    Energy Technology Data Exchange (ETDEWEB)

    Cordaro, Joseph Gabriel; Kruizenga, Alan Michael; Nissen, April

    2013-10-01

    Two classes of materials, poly(methylene diphenyl diisocyanate) or PMDI foam, and cross-linked epoxy resins, were characterized using thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC), to help understand the effects of aging and %E2%80%9Cbake-out%E2%80%9D. The materials were evaluated for mass loss and the onset of decomposition. In some experiments, volatile materials released during heating were analyzed via mass spectroscopy. In all, over twenty materials were evaluated to compare the mass loss and onset temperature for decomposition. Model free kinetic (MFK) measurements, acquired using variable heating rate TGA experiments, were used to calculate the apparent activation energy of thermal decomposition. From these compiled data the effects of aging, bake-out, and sample history on the thermal stability of materials were compared. No significant differences between aged and unaged materials were detected. Bake-out did slightly affect the onset temperature of decomposition but only at the highest bake-out temperatures. Finally, some recommendations for future handling are made.

  4. COMPARATIVE KINETICS STUDY OF THE THERMAL AND THERMO-OXIDATIVE DEGRADATION OF A POLYSTYRENE-CLAY NANOCOMPOZITE BY TGA AND DSC

    Directory of Open Access Journals (Sweden)

    Ion Dranca

    2010-12-01

    Full Text Available The methods of thermogravimetry (TGA and differential scanning calorimetry (DSC have been used to study the thermal and thermo-oxidative degradation of polystyrene (PS and a PS-clay nanocomposite. An advanced isoconversional method has been applied for kinertic analysis. Introduction of the clay phase increasers the activation energy and affects the total heat of degradation, which suggests a change in the reaction mechanism. The obtained kinetic data permit a comparative assessment of the fire resistance of the studied materials

  5. Vesicle-cholesterol interactions: Effects of added cholesterol on gel-to-liquid crystal transitions in a phospholipid membrane and five dialkyl-based vesicles as monitored using DSC

    OpenAIRE

    Blandamer, MJ; Briggs, B.; Cullis, PM; Rawlings, BJ; Engberts, JBFN; Paul M. Cullis; Rawlings, Bernard J.

    2003-01-01

    Differential scanning calorimetry (DSC) results are reported characterising the effects of added cholesterol (CHOL) on vesicle bilayer systems formed in aqueous systems by three sodium dialkylphosphates, (RO)(2)PO2--Na+ where R = dodecyl (DDP), tetradecyl (DTP) and octadecyl (DOP), (ii) two dialkyldimethylammonium bromides R2N+Me2Br- where R = hexadecyl (DHAB) and octadecyl (DOAB) and (iii) dimyristoylphosphatidylcholine (DMPC). The results are examined in terms of the effects of added CHOL o...

  6. Use of the DSC technique to characterize water-in-crude oil emulsions stability; Utilisation de la DSC pour la caracterisation de la stabilite des emulsions eau dans petrole

    Energy Technology Data Exchange (ETDEWEB)

    Dalmazzone, C.; Seris, H. [Institut Francais du Petrole (IFP), 92 - Rueil-Malmaison (France)

    1998-07-01

    The DSC technique (Differential Scanning Calorimetry) was applied to the study of water-in-crude oil emulsions, which naturally form after an oil spill. The resulting emulsions contain between 50 and 80 % seawater and they are often heavy materials, hard recover mechanically, treat or burn. It is therefore important to assess their stability in order to optimize their treatments. A great variety of techniques are available for the assessment of emulsions stability. They are generally based on the analysis of the droplets size distribution. Unfortunately, most of the usual techniques can not be applied to opaque water-in-oil emulsions. The most useful method to characterize the stability of emulsions is of course the `bottle test`. It consists in monitoring the extent of phase separation with time. This type of test provides a significant amount of information relating to both the stability of the emulsion phase and the clarity of he separated water, but it is very empirical. The DSC technique is generally used to determine the composition of water-in-oil emulsions. It is the only technique capable of distinguishing free water from emulsified water. It was shown in this study that it is a very useful technique, which allows the study of the evolution of the droplet size distribution as well as a precise determination of the water content. (authors) 15 refs.

  7. Calculation of Temperature Rise in Calorimetry.

    Science.gov (United States)

    Canagaratna, Sebastian G.; Witt, Jerry

    1988-01-01

    Gives a simple but fuller account of the basis for accurately calculating temperature rise in calorimetry. Points out some misconceptions regarding these calculations. Describes two basic methods, the extrapolation to zero time and the equal area method. Discusses the theoretical basis of each and their underlying assumptions. (CW)

  8. Final Technical Report CMS fast optical calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Winn, David R. [Fairfield Univ., CT (United States)

    2012-07-12

    This is the final report of CMS FAST OPTICAL CALORIMETRY, a grant to Fairfield University for development, construction, installation and operation of the forward calorimeter on CMS, and for upgrades of the forward and endcap calorimeters for higher luminosity and radiation damage amelioration.

  9. Study of asphaltene precipitation by Calorimetry

    DEFF Research Database (Denmark)

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

    2007-01-01

    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...

  10. HDTHe calorimetry v.1.0

    Energy Technology Data Exchange (ETDEWEB)

    2016-01-12

    The software generates predicted results of differential scanning calorimetry experiments for samples of palladium in a perforated capsule in an atmosphere containing a mixture of hydrogen isotopologues and helium. It can also be used to predict the results of absorption-desorption experiments at constant temperature and solid-phase isotopic ratio.

  11. 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

  12. TOPEM DSC study of glass transition region of polyurethane cationomers

    International Nuclear Information System (INIS)

    Highlights: ► TOPEM DSC method was employed to investigate the glass transition (Tg) region of fluorinated polyurethane cationomers. ► Introduction of fluorine compounds significantly changes thermal behaviour of cationomers in the Tg region of hard segments. ► Introduction of fluorine compound leads to changes of the slope in activation diagram of glass transition. - Abstract: In this paper TOPEM DSC method was employed to investigate the glass transition region of fluorinated polyurethane cationomers. Fluorinated polyurethane cationomers have been synthesised in the reaction of MDI with poly(ethylene glycol) (600) and butane1,4-diol or N-methyl- or N-butyldiethanolamine and 2,2,3,3-tetrafluoro-1,4-butanediol. Better rigidity was found for generally amorphous cationomer coats. It was found that introduction of fluorine compound changes thermal behaviour of polyurethane cationomers as well as leads to changes in the slope in activation diagram profiles of glass transition in comparison to polyuretahene cationomer without fluorine compound. Application of TOPEM DSC allows to obtain more information concerning frequency dependence of glass transition region and thermodynamical stability of polyurethane structures.

  13. DSC and X-ray diffraction studies on the physicochemical changes occurring in polyester films exposed to heavy ion irradiation

    International Nuclear Information System (INIS)

    Poly(ethylene terephthalate) (PET) (commercial biaxially oriented Mylar and Hostaphan, 23 and 19 μm thick) and poly(butylene terephthalate) (PBT) (80μm thick) films were exposed to heavy ion irradiation and the resulting structural transformations were studied by differential scanning calorimetry (Perkin-Elmer DSC-7, heating rate in nitrogen flow , 2 or 3 K/min, open pans; heating cooling-heating cycles run at rates of 10-10-10 K/min, and 2-20-2 K/min, closed pans), wide-angle and small angle X-ray scattering (WAXS and SAXS), Fourier transform infrared spectroscopy (FTIR), gel permeation chromatography (GPC), and density measurements. The PBT film was prepared from the molten phase and then heated at 150oC. They were irradiated with Ar ions (5.5 MeV/amu, 1011 ions /cm2), Dy ions (13 MeV/amu, 1-5x1010 and 1011 ions/cm2), and Pb ions (11.4 MeV/amu, 1010 ions/cm2). The calculated radiation doses were found to be contained with the range of (1.1-22.0)x105 Gy. The irradiation-effected different film melting and crystallization courses detected by DSC and the changes in reflection intensities in WAXS diffractograms indicated to a reduced crystal phase content in the irradiated polyester films. The amorphization of the PET film was confirmed by SAXS and FTIR spectra and also by density measurements. As found by GPC, the molecular weight of the soluble fraction in PET decreases on irradiation and the accompanying increase in the content of the insoluble phase indicates that cross-linking process occur. The DSC and X-ray techniques proved to be helpful in following the structural changes induced in polymer films by irradiation with heavy ions. (author)

  14. DIFFERENTIAL SCANNING CALORIMETRY AND X-RAY DIFFRACTION STUDIES ON AGING BEHAVIOR OF Zn-Al ALLOYS

    Institute of Scientific and Technical Information of China (English)

    X.L. Xu; Z.W. Yu; S.J. Ji; J.C. Sun; Z.K. Hei

    2001-01-01

    Decomposition processes of the quenched Zn-Al alloys were studied by differentiai scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the stabilities of supersaturated solid solution (SSS) of Zn-Al alloy and c' phase formed by quenching would reduce with increasing Zn content and precipitating η-Zn phases even when aging at ambient temperature,so that exothermic precipitation peak in DSC curve would disappear. The activation energy of the η-Zn precipitation and their reaction enthalpy were calculated and measured. The kinetics of α' decomposition or η-Zn formation was determined by XRD.The microstructure change during aging was observed by TEM.

  15. Evaluation of the Ignition Temperature in Thermal Explosion Synthesis of TiAl3 by Differential Scanning Calorimetry

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    Application of the Semenov theory of spontaneous ignition to evaluation of the critical temperature (Tc′) in thermal explosion (TE) synthesis was conducted with the Ti-75at pct Al binary system using nonisothermal differential scanning calorimetry (DSC) at different heating rates. And the critical temperature for isothermal TE is predicted to be 728.9°C by the multiple linear regression of Tc′s evaluated according to Semenov theory, which is close to the range of 740~745°C obtained from the isothermal DSC observation. This result proves that Semenov theory of spontaneous ignition is also feasible for TE synthesis in binary metallic systems like Ti-75 at. pct Al system.

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

    Energy Technology Data Exchange (ETDEWEB)

    Stavrou, E; Tsiantos, C; Tsopouridou, R D; Kripotou, S; Kontos, A G; Raptis, C [Department of Physics, National Technical University of Athens, GR-15780 Athens (Greece); Capoen, B; Bouazaoui, M [Laboratoire de Physique des Lasers, Atomes et Molecules (CNRS, UMR 8523), Batiment P-5, Centre d' Etudes et de Recherches Lasers et Applications (CERLA-FR CNRS 2416), Universite de Sciences et Technologies de Lille, F-59655 Villeneuve d' Ascq Cedex (France); Turrell, S; Khatir, S, E-mail: craptis@central.ntua.g [Laboratoire de Spectrochimie Infrarouge et Raman (CNRS 8516), Batiment C-5, Centre d' Etudes et de Recherches Lasers et Applications (CERLA-FR CNRS 2416), Universite de Sciences et Technologies de Lille, F-59655 Villeneuve d' Ascq Cedex (France)

    2010-05-19

    Raman scattering and differential scanning calorimetry (DSC) measurements have been carried out on four mixed tellurium-zinc oxide (TeO{sub 2}){sub 1-x}(ZnO){sub 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{sub g} has been determined for each glass, showing a monotonous decrease of T{sub 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{sub d} very close to the respective T{sub 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{sub 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{sub g} and confirms the correlation between the BP and the MRO of glasses.

  17. 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.

  18. Cerium fluoride crystals for calorimetry at LHC

    International Nuclear Information System (INIS)

    High-resolution homogeneous calorimetry is fully justified for part of the physics program at the Large Hadron Collider (LHC). The main design features of proposed CeF3 crystals for calorimetry for LHC are discussed. The severe constraints LHC imposes on detectors make the use of 'classical' crystals impossible. Therefore, a large R and D effort has been undertaken by the 'Crystal Clear' collaboration in order to find new, dense, fast and radiation hard crystals. A good candidate, cerium fluoride, has been identified and studied. It is interesting at this stage to review the specifications of scintillators for LHC and to see how well available data on CeF3 luminescence, decay time, light yield, optical transmission and resistance to radiation meet them. Milestones to reach before starting a large scale crystal production in view of the eventual construction of a calorimeter, are also discussed. (author) 15 refs., 15 figs., 1 tab

  19. Neutrino mass and low-temperature calorimetry

    CERN Document Server

    Wang Shui Cai; Redi, O; Stroke, Hinko Henry; Coron, N; Leblanc, J W

    1998-01-01

    We describe how the problem of measuring the neutrino mass led us to the development of low-temperature calorimetry. The search for a "17-keV neutrino" concluded with a negative result, but a wide range of applications are now carried on by us and by other groups in the fields of x-ray astronomy, recoil measurements of dark matter particles, high precision particle spectrometry, specific heat determinations, neutron detection, rare decay studies. The masses of the bolometers (calorimeters) extend from 1 mg to 1 Kg, nearly as large as for quantum detectors. By lowering the temperature into the 10-20 mK range, calorimetry is on the way to surpass substantially the high precision of particle metrology obtainable with the quantum detectors. Calorimeter developments and perspectives are discussed.

  20. Calibration and monitoring for crystal calorimetry

    CERN Document Server

    Zhu, Ren Yuan

    2005-01-01

    Crystal calorimetry provides excellent energy resolution in high energy and nuclear physics. The light output of heavy crystal scintillators, however, suffers from not negligible damage in radiation environment. A precision calibration and monitoring thus is crucial for maintaining crystal precision in situ. The performance of calibration and monitoring approaches used by BaBar, CLEO and L3 experiments are presented. The design and construction of a laser- based light monitoring system for CMS PWO calorimeter is also discussed.

  1. Analysis of Cooperativity by Isothermal Titration Calorimetry

    OpenAIRE

    Alan Brown

    2009-01-01

    Cooperative binding pervades Nature. This review discusses the use of isothermal titration calorimetry (ITC) in the identification and characterisation of cooperativity in biological interactions. ITC has broad scope in the analysis of cooperativity as it determines binding stiochiometries, affinities and thermodynamic parameters, including enthalpy and entropy in a single experiment. Examples from the literature are used to demonstrate the applicability of ITC in the characterisation of coop...

  2. Calorimetry and thermodynamics of living systems

    International Nuclear Information System (INIS)

    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

  3. Missing energy induced by thin hadron calorimetry

    International Nuclear Information System (INIS)

    It is relatively straightforward to estimate the total, unsegmented, depth required in SSC experiments. Typically depths in the range of 9--11 absorption lengths were specified by the SDC and GEM experiments. With these depths, the induced missing energy signal due to calorimeter leakage was found to be well below the signals caused by light gluinos, and the exterior muon systems were well protected from punch through backgrounds. In certain applications, where calorimetry is inscribed inside the magnetic field producing coils, that depth of calorimetry becomes exceedingly expensive. Examples are the ZEUS barrel and the proposed CMS barrel calorimeters. The problems can be alleviated by placing a ''tailcatcher'' of active elements outside the coil, but the problem of inert material placed within the active volume of the calorimetry remains. This inert material can potentially induce missing transverse energy signals which are large with respect to real physics signatures. The purpose of this note is to explore schemes to minimize the measured leakage energy

  4. 索尼DSC-P200数码相机

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    作为面向普通家用的时尚主打机型,索尼DSC-P系列一直保持着相当高的市场份额,在DSC-P150把家用数码相机带到700万像素级后,索尼继续推出了DSC-P150的升级机型DSC-P200。

  5. A DSC STUDY OF PHOTOPOLYMERIZATION OF POLYESTERS CONTAINING CONJUGATED DIACETYLENES

    Institute of Scientific and Technical Information of China (English)

    Yao-wen Bai; Xiao-fang Chen; Dong Zhang; Xin-hua Wan; Qi-feng Zhou

    2000-01-01

    The photopolymerization of two kinds of prepolyesters containing conjugated diacetylene (PDA-6 and PDA-12)was investigated using DSC. By measuring the endothermic enthalpy of the prepolymers after different UV-irradiation times,the polymerizations were found to follow the first-order rate law which agreed with the results of other investigators using a different method. The endothermic enthalpy measurements of PDA-6 and PDA-12 before UV-irradiation precluded the possibility that the decrease of endothermic enthalpy was caused by thermal polymerization.

  6. 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.

  7. Laboratory Annealing Experiments Of Refractory Silicate Grain Analogs Using Differential Scanning Calorimetry

    Science.gov (United States)

    Kimura, Yuki; Nuth, Joseph A., III; Tsukamota, Katsuo; Kaito, Chihiro

    2010-01-01

    Exothermic reactions during the annealing of laboratory synthesized amorphous magnesium-bearing silicate particles used as grain analogs of cosmic dust were detected by differential scanning calorimetry (DSC) in air. With infrared spectroscopy and transmission electron microscopy, we show that cosmic dust could possibly undergo fusion to larger particles, with oxidation of magnesium silicide and crystallization of forsterite as exothermic reactions in the early solar system. The reactions begin at approximately 425, approximately 625, and approximately 1000 K, respectively, and the reaction energies (enthalpies) are at least 727, 4151, and 160.22 J per gram, respectively. During the crystallization of forsterite particles, the spectral evolution of the 10 micrometer feature from amorphous to crystalline was observed to begin at lower temperature than the crystallization temperature of 1003 K. During spectral evolution at lower temperature, nucleation and/or the formation of nanocrystallites of forsterite at the surface of the grain analogs was observed.

  8. The oxidation of aluminum at high temperature studied by Thermogravimetric Analysis and Differential Scanning Calorimetry.

    Energy Technology Data Exchange (ETDEWEB)

    Coker, Eric Nicholas

    2013-10-01

    The oxidation in air of high-purity Al foil was studied as a function of temperature using Thermogravimetric Analysis with Differential Scanning Calorimetry (TGA/DSC). The rate and/or extent of oxidation was found to be a non-linear function of the temperature. Between 650 and 750 ÀC very little oxidation took place; at 850 ÀC oxidation occurred after an induction period, while at 950 ÀC oxidation occurred without an induction period. At oxidation temperatures between 1050 and 1150 ÀC rapid passivation of the surface of the aluminum foil occurred, while at 1250 ÀC and above, an initial rapid mass increase was observed, followed by a more gradual increase in mass. The initial rapid increase was accompanied by a significant exotherm. Cross-sections of oxidized specimens were characterized by scanning electron microscopy (SEM); the observed alumina skin thicknesses correlated qualitatively with the observed mass increases.

  9. Differential scanning calorimetry and reaction kinetics studies of {gamma} + {alpha}{sub 2} Ti aluminide

    Energy Technology Data Exchange (ETDEWEB)

    Gupta, R.K., E-mail: rohitkumar_gupta@vssc.gov.in [Vikram Sarabhai Space Centre, ISRO, Trivandrum 695 022 (India); Pant, Bhanu [Vikram Sarabhai Space Centre, ISRO, Trivandrum 695 022 (India); Agarwala, Vijaya [Indian Institute of Technology Roorkee, Roorkee 247 667 (India); Sinha, P.P. [Vikram Sarabhai Space Centre, ISRO, Trivandrum 695 022 (India)

    2012-12-14

    Reaction synthesis method for titanium aluminide processing consists of an exothermic reaction among alloying elements present and primarily between titanium and aluminium particles at specific temperature range. Study of this reaction helps in understanding the process of aluminide formation. Differential scanning calorimetry (DSC) study is the suitable method to study such reactions. In the present work, five different alloy mixtures based on Ti48Al2Cr2Nb0.1B are prepared and DSC study is carried out. Onset temperature, peak temperature and completion temperature of the major exothermic reaction is analyzed at different heating rates. Further, kinetics of the reaction is studied using Johnson-Mehl-Avrami equation. Activation energy and Avrami parameter are calculated and compared with the reported works on binary alloy. It has been observed that exothermic reaction is triggered by melting of aluminium. Boron assists in increasing the enthalpy of reaction by boride formation. Primary reaction product is found to be TiAl{sub 3}. Activation energy as well as Avrami parameter is found to have marginal variation due to small change in alloying elements in different alloys and due to heating rates in the same alloy. -- Highlights: Black-Right-Pointing-Pointer Reaction kinetics studies of Ti-aluminide alloy powder mixtures carried out. Black-Right-Pointing-Pointer Five compositions studied through non-isothermal differential scanning calorimetry. Black-Right-Pointing-Pointer Effect of minor boron addition and role of Ti particle size is noted. Black-Right-Pointing-Pointer Activation energies using JMA equations are between 169.5 and 192.49 kJ mol{sup -1}.

  10. Unspecific membrane protein-lipid recognition: combination of AFM imaging, force spectroscopy, DSC and FRET measurements.

    Science.gov (United States)

    Borrell, Jordi H; Montero, M Teresa; Morros, Antoni; Domènech, Òscar

    2015-11-01

    In this work, we will describe in quantitative terms the unspecific recognition between lactose permease (LacY) of Escherichia coli, a polytopic model membrane protein, and one of the main components of the inner membrane of this bacterium. Supported lipid bilayers of 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphoethanolamine (POPE) and 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphoglycerol (POPG) (3:1, mol/mol) in the presence of Ca(2+) display lateral phase segregation that can be distinguished by atomic force microscopy (AFM) as well as force spectroscopy. LacY shows preference for fluid (Lα) phases when it is reconstituted in POPE : POPG (3:1, mol/mol) proteoliposomes at a lipid-to-protein ratio of 40. When the lipid-to-protein ratio is decreased down to 0.5, two domains can be distinguished by AFM. While the upper domain is formed by self-segregated units of LacY, the lower domain is constituted only by phospholipids in gel (Lβ) phase. On the one hand, classical differential scanning calorimetry (DSC) measurements evidenced the segregation of a population of phospholipids and point to the existence of a boundary region at the lipid-protein interface. On the other hand, Förster Resonance Energy Transfer (FRET) measurements in solution evidenced that POPE is selectively recognized by LacY. A binary pseudophase diagram of POPE : POPG built from AFM observations enables to calculate the composition of the fluid phase where LacY is inserted. These results are consistent with a model where POPE constitutes the main component of the lipid-LacY interface segregated from the fluid bulk phase where POPG predominates.

  11. Profiles in Leadership: Clifton J. Latiolais, MSc, DSc.

    Science.gov (United States)

    White, Sara; Godwin, Harold N; Weber, Robert J

    2013-09-01

    The Director's Forum series is designed to guide pharmacy leaders in establishing patient-centered services in hospitals and health systems. August 2013 marks the 50th anniversary of the publication of the Mirror to Hospital Pharmacy, which was a comprehensive study of pharmacy services in the United States. The late Clifton J. Latiolais, MS, DSc, served as the assistant program director for the study and was a co-author of the Mirror. The late Don E. Francke, MS, DSc, was the lead author of the Mirror and the principal investigator of the federally funded study that reviewed hospital pharmacy services across the United States. The next 2 articles in Director's Forum profile the leadership of Drs. Latiolais and Francke. This article highlights Dr. Latiolais ("Clif") by briefly reviewing his biography and key career accomplishments, describing his leadership philosophy, and translating that philosophy to today's health care challenges. Clif's influence on health system pharmacy serves as an example of effective leadership. This historical perspective on Clif's leadership, as seen through the eyes of those who knew him, provides directors of pharmacy a valuable leadership viewpoint as they develop strategies to enhance patient-centered pharmacy services.

  12. Study on biodegradation process of lignin by FTIR and DSC.

    Science.gov (United States)

    Liu, Yang; Hu, Tianjue; Wu, Zhengping; Zeng, Guangming; Huang, Danlian; Shen, Ying; He, Xiaoxiao; Lai, Mingyong; He, Yibin

    2014-12-01

    The biodegradation process of lignin by Penicillium simplicissimum was studied to reveal the lignin biodegradation mechanisms. The biodegradation products of lignin were detected using Fourier transform infrared spectroscopy (FTIR), UV-Vis spectrophotometer, different scanning calorimeter (DSC), and stereoscopic microscope. The analysis of FTIR spectrum showed the cleavage of various ether linkages (1,365 and 1,110 cm(-1)), oxidation, and demethylation (2,847 cm(-1)) by comparing the different peak values in the corresponding curve of each sample. Moreover, the differences (Tm and ΔHm values) between the DSC curves indirectly verified the FTIR analysis of biodegradation process. In addition, the effects of adding hydrogen peroxide (H2O2) to lignin biodegradation process were analyzed, which indicated that H2O2 could accelerate the secretion of the MnP and LiP and improve the enzymes activity. What is more, lignin peroxidase and manganese peroxidase catalyzed the lignin degradation effectively only when H2O2 was presented.

  13. Reticulation of Aqueous Polyurethane Systems Controlled by DSC Method

    Directory of Open Access Journals (Sweden)

    Jakov Stamenkovic

    2006-06-01

    Full Text Available The DSC method has been employed to monitor the kinetics of reticulation ofaqueous polyurethane systems without catalysts, and with the commercial catalyst of zirconium(CAT®XC-6212 and the highly selective manganese catalyst, the complex Mn(III-diacetylacetonemaleinate (MAM. Among the polyol components, the acrylic emulsions wereused for reticulation in this research, and as suitable reticulation agents the water emulsiblealiphatic polyisocyanates based on hexamethylendoisocyanate with the different contents ofNCO-groups were employed. On the basis of DSC analysis, applying the methods of Kissinger,Freeman-Carroll and Crane-Ellerstein the pseudo kinetic parameters of the reticulation reactionof aqueous systems were determined. The temperature of the examination ranged from 50oC to450oC with the heat rate of 0.5oC/min. The reduction of the activation energy and the increaseof the standard deviation indicate the catalytic action of the selective catalysts of zirconium andmanganese. The impact of the catalysts on the reduction of the activation energy is thestrongest when using the catalysts of manganese and applying all the three afore-said methods.The least aberrations among the stated methods in defining the kinetic parameters wereobtained by using the manganese catalyst.

  14. Black carbon quantification in charcoal-enriched soils by differential scanning calorimetry

    Science.gov (United States)

    Hardy, Brieuc; Cornelis, Jean-Thomas; Leifeld, Jens

    2015-04-01

    Black carbon (BC), the solid residue of the incomplete combustion of biomass and fossil fuels, is ubiquitous in soil and sediments, fulfilling several environmental services such as long-term carbon storage. BC is a particularly important terrestrial carbon pool due to its large residence time compared to thermally unaltered organic matter, which is largely attributed to its aromatic structure. However, BC refers to a wide range of pyrogenic products from partly charred biomass to highly condensed soot, with a degree of aromaticity and aromatic condensation varying to a large extend across the BC continuum. As a result, BC quantification largely depends on operational definitions, with the extraction efficiency of each method varying across the entire BC range. In our study, we investigated the adequacy of differential scanning calorimetry (DSC) for the quantification of BC in charcoal-enriched soils collected in the topsoil of pre-industrial charcoal kilns in forest and cropland of Wallonia, Belgium, where charcoal residues are mixed to uncharred soil organic matter (SOM). We compared the results to the fraction of the total organic carbon (TOC) resisting to K2Cr2O7 oxidation, another simple method often used for BC measurement. In our soils, DSC clearly discriminates SOM from chars. SOM is less thermally stable than charcoal and shows a peak maximum around 295°C. In forest and agricultural charcoal-enriched soils, three peaks were attributed to the thermal degradation of BC at 395, 458 and 523°C and 367, 420 and 502 °C, respectively. In cropland, the amount of BC calculated from the DSC peaks is closely related (slope of the linear regression = 0.985, R²=0.914) to the extra organic carbon content measured at charcoal kiln sites relative to the charcoal-unaffected adjacent soils, which is a positive indicator of the suitability of DSC for charcoal quantification in soil. The first BC peak, which may correspond to highly degraded charcoal, contributes to a

  15. An evaluation tool for FKBP12-dependent and -independent mTOR inhibitors using a combination of FKBP-mTOR fusion protein, DSC and NMR.

    Science.gov (United States)

    Sekiguchi, Mitsuhiro; Kobashigawa, Yoshihiro; Kawasaki, Masashi; Yokochi, Masashi; Kiso, Tetsuo; Suzumura, Ken-ichi; Mori, Keitaro; Teramura, Toshio; Inagaki, Fuyuhiko

    2011-11-01

    Mammalian target of rapamycin (mTOR), a large multidomain protein kinase, regulates cell growth and metabolism in response to environmental signals. The FKBP rapamycin-binding (FRB) domain of mTOR is a validated therapeutic target for the development of immunosuppressant and anticancer drugs but is labile and insoluble. Here we designed a fusion protein between FKBP12 and the FRB domain of mTOR. The fusion protein was successfully expressed in Escherichia coli as a soluble form, and was purified by a simple two-step chromatographic procedure. The fusion protein exhibited increased solubility and stability compared with the isolated FRB domain, and facilitated the analysis of rapamycin and FK506 binding using differential scanning calorimetry (DSC) and solution nuclear magnetic resonance (NMR). DSC enabled the rapid observation of protein-drug interactions at the domain level, while NMR gave insights into the protein-drug interactions at the residue level. The use of the FKBP12-FRB fusion protein combined with DSC and NMR provides a useful tool for the efficient screening of FKBP12-dependent as well as -independent inhibitors of the mTOR FRB domain.

  16. Probing lipid-cholesterol interactions in DOPC/eSM/Chol and DOPC/DPPC/Chol model lipid rafts with DSC and (13)C solid-state NMR.

    Science.gov (United States)

    Fritzsching, Keith J; Kim, Jihyun; Holland, Gregory P

    2013-08-01

    The interaction between cholesterol (Chol) and phospholipids in bilayers was investigated for the ternary model lipid rafts, DOPC/eSM/Chol and DOPC/DPPC/Chol, with differential scanning calorimetry (DSC) and (13)C cross polarization magic angle spinning (CP-MAS) solid-state NMR. The enthalpy and transition temperature (Tm) of the Lα liquid crystalline phase transition from DSC was used to probe the thermodynamics of the different lipids in the two systems as a function of Chol content. The main chain (13)C (CH2)n resonance is resolved in the (13)C CP-MAS NMR spectra for the unsaturated (DOPC) and saturated (eSM or DPPC) chain lipid in the ternary lipid raft mixtures. The (13)C chemical shift of this resonance can be used to detect differences in chain ordering and overall interactions with Chol for the different lipid constituents in the ternary systems. The combination of DSC and (13)C CP-MAS NMR results indicate that there is a preferential interaction between SM and Chol below Tm for the DOPC/eSM/Chol system when the Chol content is ≤20mol%. In contrast, no preferential interaction between Chol and DPPC is observed in the DOPC/DPPC/Chol system above or below Tm. Finally, (13)C CP-MAS NMR resolves two Chol environments in the DOPC/eSM/Chol system below Tm at Chol contents >20mol% while, a single Chol environment is observed for DOPC/DPPC/Chol at all compositions.

  17. Determination of the thermo-mechanical properties in starch and starch/gluten systems at low moisture content - a comparison of DSC and TMA.

    Science.gov (United States)

    Homer, Stephen; Kelly, Michael; Day, Li

    2014-08-01

    The impact of heating rate on the glass transition (Tg) and melting transitions observed by differential scanning calorimetry (DSC) on starch and a starch/gluten blend (80:20 ratio) at low moisture content was examined. The results were compared to those determined by thermo-mechanical analysis (TMA). Comparison with dynamic mechanical thermal analysis (DMTA) and phase transition analysis (PTA) is also discussed. Higher heating rates increased the determined Tg as well as the melting peak temperatures in both starch and the starch/gluten blend. A heating rate of 5°C/min gave the most precise value of Tg while still being clearly observed above the baseline. Tg values determined from the first and second DSC scans were found to differ significantly and retrogradation of starch biopolymers may be responsible. Tg values of starch determined by TMA showed good agreement with DSC results where the Tg was below 80°C. However, moisture loss led to inaccurate Tg determination for TMA analyses at temperatures above 80°C.

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

    International Nuclear Information System (INIS)

    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

  19. 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.

  20. Overriding "doing wrong" and "not doing right": validation of the Dispositional Self-Control Scale (DSC).

    Science.gov (United States)

    Ein-Gar, Danit; Sagiv, Lilach

    2014-01-01

    We present the Dispositional Self-Control (DSC) Scale, which reflects individuals' tendency to override 2 types of temptations, termed doing wrong and not doing right. We report a series of 5 studies designed to test the reliability and validity of the scale. As hypothesized, high DSC predicts distant future orientation and low DSC predicts deviant behaviors such as aggression, alcohol misuse, and aberrant driving. DSC also predicts task performance among resource-depleted participants. Taken together, these findings suggest that the DSC Scale could be a useful tool toward further understanding the role of personality in overcoming self-control challenges.

  1. 自我增值这选:Sony DSC-F717

    Institute of Scientific and Technical Information of China (English)

    高飞

    2002-01-01

    近年的10月都是Sony推出旗舰级数码相机的日子,2000年的DSC-505v、2001年的DSC-F707,2002年有这部终极强化版的DSC-F717。改用回DSC-F505银色机身的F717,外形与DSC-F707无甚分别。不过,在机能上则作出了自我增值!

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

    Science.gov (United States)

    Zeng, Xiangkai; Zhu, Zhixiong; Chen, Yang

    2016-04-25

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

  3. Thermal Analysis of Whole Bacterial Cells Exposed to Potassium Permanganate Using Differential Scanning Calorimetry: a Biphasic Dose-Dependent Response to Stress

    Directory of Open Access Journals (Sweden)

    Marina K. Abuladze

    2009-01-01

    Full Text Available Differential scanning calorimetry (DSC was applied to estimate the impact of the toxic oxidant potassium permanganate (PM on the intracellular structural and functional alterations at whole cell level using soil bacteria Arthrobacter oxydans as a model culture. Differential scanning calorimetry (DSC was applied in order to estimate the impact of the toxic oxidant potassium permanganate (PM on the intracellular structural and functional alterations at the whole cell level using the soil bacteria Arthrobacter oxydans as a model culture. We compared the total melting heat and the temperature of DNA-protein complex (DNP melting at the PM application prior to the calorimetry measurement and after 24-h exposure at the concentration range 0.02–1.4 mM. The initial oxidative effect caused changes in the pattern of the whole cell melting spectra (mainly at the temperature range 56–78°C, the decrease of Tmax °C DNP melting, and did not influence significantly the total heat of bacterial melting at different concentrations of PM. The prolonged effect of permanganate up to 24 h was characterized by a biphasic dose-dependent response to stress estimated by the DSC technique and the colony-forming assay. The low doses of PM (0.02 and 0.2 mM stimulated cell proliferation, and increased the total whole cell melting heat and the temperature of DNP melting. The toxic effect of PM up to 0.04 mM reduced cell viability, changed the character of multipeaked thermograms, and lowered the total melting heat and the temperature of DNP melting in a concentration-dependent manner. This study presents the DSC method for evaluating and monitoring the effects of exposure to potential human and environmental toxicants.

  4. 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.

  5. Protein Unfolding Coupled to Ligand Binding: Differential Scanning Calorimetry Simulation Approach

    Science.gov (United States)

    Soledad Celej, María; Fidelio, Gerardo Daniel; Dassie, Sergio Alberto

    2005-01-01

    The aim of this work is to present the physicochemical basis underlying the changes in protein thermostability upon ligand binding. The article is addressed to advanced undergraduate and postgraduate chemistry students with an interest in protein biophysics. In addition, this article provides a useful tool for both learning and teaching biophysics because it links fundamental concepts: thermodynamics, chemical equilibrium, and protein stability. The influence of protein ligand interactions on thermally-induced protein denaturation was monitored by differential scanning calorimetry (DSC). The changes in DSC output (thermogram) emerge by linking binding equilibrium with reversible protein unfolding thermodynamics. We derive the formalism for the description of protein unfolding in the presence of ligand that can bind to a single site on either native, unfolded, or both protein states. In addition to a rigorous mathematical description of the involved equilibria, the model provides the general formulation for simulating thermograms and calculating the changes in protein species during heating. First, we describe ligand interaction and emphasize the relationship between protein stability parameters and redistribution of species in equilibrium. After that, we describe the origin of bimodal thermograms, and finally, the effect on thermogram shape of protein concentration at constant ligand/protein mole ratio.

  6. Thermal stability of Phaseolus vulgaris leucoagglutinin: a differential scanning calorimetry study.

    Science.gov (United States)

    Biswas, Shyamasri; Kayastha, Arvind M

    2002-09-30

    Phaseolus vulgaris phytohemagglutinin L is a homotetrameric-leucoagglutinating seed lectin. Its three-dimensional structure shows similarity with other members of the legume lectin family. The tetrameric form of this lectin is pH dependent. Gel filtration results showed that the protein exists in its dimeric state at pH 2.5 and as a tetramer at pH 7.2. Contrary to earlier reports on legume lectins that possess canonical dimers, thermal denaturation studies show that the refolding of phytohemagglutinin L at neutral pH is irreversible. Differential scanning calorimetry (DSC) was used to study the denaturation of this lectin as a function of pH that ranged from 2.0 to 3.0. The lectin was found to be extremely thermostable with a transition temperature around 82 degrees C and above 100 degrees C at pH 2.5 and 7.2, respectively. The ratio of calorimetric to vant Hoff enthalpy could not be calculated because of its irreversible-folding behavior. However, from the DSC data, it was discovered that the protein remains in its compact-folded state, even at pH 2.3, with the onset of denaturation occurring at 60 degrees C. PMID:12359088

  7. Assessment of fluidity of different invasomes by electron spin resonance and differential scanning calorimetry.

    Science.gov (United States)

    Dragicevic-Curic, Nina; Friedrich, Manfred; Petersen, Silvia; Scheglmann, Dietrich; Douroumis, Dennis; Plass, Winfried; Fahr, Alfred

    2011-06-30

    The aim of this study was to investigate the influence of membrane-softening components (terpenes/terpene mixtures, ethanol) on fluidity of phospholipid membranes in invasomes, which contain besides phosphatidylcholine and water, also ethanol and terpenes. Also mTHPC was incorporated into invasomes in order to study its molecular interaction with phospholipids in vesicular membranes. Fluidity of bilayers was investigated by electron spin resonance (ESR) using spin labels 5- and 16-doxyl stearic acid and by differential scanning calorimetry (DSC). Addition of 1% of a single terpene/terpene mixture led to significant fluidity increase around the C16 atom of phospholipid acyl chains comprising the vesicles. However, it was not possible to differentiate between the influences of single terpenes or terpene mixtures. Incorporation of mTHPC into the bilayer of vesicles decreased fluidity near the C16 atom of acyl chains, indicating its localization in the inner hydrophobic zone of bilayers. These results are in agreement with DSC measurements, which showed that terpenes increased fluidity of bilayers, while mTHPC decreased fluidity. Thus, invasomes represent vesicles with very high membrane fluidity. However, no direct correlation between fluidity of invasomes and their penetration enhancing ability was found, indicating that besides fluidity also other phenomena might be responsible for improved skin delivery of mTHPC.

  8. Experimental investigation and modelling of heat capacity, heat of fusion and melting interval of rocks

    Energy Technology Data Exchange (ETDEWEB)

    Leth-Miller, R.; Jensen, A.D.; Glarborg, P.; Jensen, L.M.; Hansen, P.B.; Joergensen, S.B

    2003-11-28

    The heat capacity and heat of fusion were measured for a number of minerals using differential scanning calorimetry (DSC). The DSC measurements showed that the heat of fusion for the minerals is very low compared to the heat of fusion for pure crystalline phases reported elsewhere. A model for the melting behaviour of mineral materials in terms of melting interval, heat capacities and heat of fusion has been developed. The only model input is the chemical composition of the mineral material. The model was developed to be implemented in a detailed model of a cupola furnace, thus the focus for the development was not only precision but also to obtain a model that was continuous and differentiable. The model is based on several different submodels that each covers a part of the heating and melting of rocks. Each submodel is based on large amounts of empirical data. Comparison of the model and the DSC measurements showed reasonable agreement for the model to be used when a fast estimate is needed and experimental data is not available.

  9. An isothermal titration and differential scanning calorimetry study of the G-quadruplex DNA-insulin interaction.

    Science.gov (United States)

    Timmer, Christine M; Michmerhuizen, Nicole L; Witte, Amanda B; Van Winkle, Margaret; Zhou, Dejian; Sinniah, Kumar

    2014-02-20

    The binding of insulin to the G-quadruplexes formed by the consensus sequence of the insulin-linked polymorphic region (ILPR) was investigated with differential scanning calorimetry (DSC) and isothermal titration calorimetry (ITC). The thermal denaturation temperature of insulin was increased by almost 4 °C upon binding to ILPR G-quadruplex DNA as determined by DSC. The thermodynamic parameters (K(D), ΔH, ΔG, and ΔS) of the insulin-G-quadruplex complex were further investigated by temperature-dependent ITC measurement over the range of 10-37 °C. The binding of insulin to the ILPR consensus sequence displays micromolar affinity in phosphate buffer at pH 7.4, which is mainly driven by entropic factors below 25 °C but by enthalpic terms above 30 °C. The interaction was also examined in several different buffers, and results showed that the observed ΔH is dependent on the ionization enthalpy of the buffer used. This indicates proton release upon the binding of G-quadruplex DNA to insulin. Additionally, the large negative change in heat capacity for this interaction may be associated with the dominant hydrophobicity of the amino acid sequence of insulin's β subunit, which is known to bind to the ILPR G-quadruplex DNA.

  10. Calorimetry of the CMD-3 detector

    Science.gov (United States)

    Shebalin, V. E.; Akhmetshin, R. R.; Anisenkov, A. V.; Aulchenko, V. M.; Bashtovoy, N. S.; Epifanov, D. A.; Epshteyn, L. B.; Erofeev, A. L.; Grebenuk, A. A.; Grigoriev, D. N.; Ignatov, F. V.; Kazanin, V. F.; Kovalenko, O. A.; Kozyrev, A. N.; Kuzmenko, A. E.; Kuzmin, A. S.; Logashenko, I. B.; Mikhailov, K. Yu.; Okhapkin, V. S.; Razuvaev, G. P.; Ruban, A. A.; Shwartz, B. A.; Titov, V. M.; Talyshev, A. A.; Yudin, Yu. V.

    2016-07-01

    CMD-3 is a general purpose detector designed to study e+e- annihilation into hadrons. It is mounted at VEPP-2000 collider which operates in the wide energy range, E c . m . s = 0.32 - 2 GeV. The calorimetry at the detector is based on three subsystems: closest to the beam pipe barrel Liquid Xenon calorimeter, outer barrel calorimeter based on CsI scintillation crystals and the endcap calorimeter made of BGO scintillation crystals. We describe the structure of the calorimeters, their electronics and the energy calibration procedures.

  11. 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.....

  12. 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....

  13. Utilisation de la DSC pour la caractérisation de la stabilité des émulsions eau dans pétrole Use of the Dsc Technique to Characterize Water-In-Crude Oil Emulsions Stability

    Directory of Open Access Journals (Sweden)

    Dalmazzone C.

    2006-12-01

    Full Text Available La technique DSC (Differential Scanning Calorimetry a été appliquée à l'étude des émulsions eau dans pétrole, qui se forment naturellement après un déversement de pétrole en mer. Ces émulsions, également appelées mousses au chocolat , peuvent contenir de 50 à 80% d'eau et se présentent souvent sous la forme d'un produit visqueux, difficile à récupérer mécaniquement, à traiter ou à brûler. Il est par conséquent important de pouvoir estimer leur stabilité pour optimiser le choix du traitement. Un grand nombre de techniques, généralement fondées sur l'analyse de la distribution de tailles de gouttes, peuvent être utilisées pour estimer la stabilité d'une émulsion. Malheureusement, la plupart ne sont pas adaptées à l'étude des émulsions eau dans huile opaques. La méthode la plus utilisée pour caractériser la stabilité de ce type d'émulsions est le bottle test. Elle consiste à mesurer la séparation de phases en fonction du temps. Ce test est la source d'une quantité d'informations appréciables quant à la stabilité de l'émulsion et à la qualité de la phase aqueuse séparée, mais il reste très empirique. La technique DSC est généralement utilisée pour déterminer la composition des émulsions eau dans huile, car elle permet de distinguer l'eau libre de l'eau émulsifiée. Cette étude a montré qu'il s'agit d'une technique très utile qui permet à la fois l'étude de l'évolution de la taille des gouttes dans l'émulsion, et une détermination précise de la quantité d'eau. The DSC technique (Differential Scanning Calorimetry was applied to the study of water-in-crude oil emulsions, which naturally form after an oil spill. The resulting emulsions contain between 50 and 80% seawater and they are often heavy materials, hard to recover mechanically, treat or burn. It is therefore important to assess their stability in order to optimize their treatments. A great variety of techniques are available for

  14. Adsorption calorimetry of conjugated organic molecules on metal surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Lytken, Ole; Drescher, Hans-Joerg; Bebensee, Fabian; Steinrueck, Hans-Peter; Gottfried, J. Michael [Universitaet Erlangen-Nuernberg, Lehrstuhl fuer Physikalische Chemie II (Germany)

    2011-07-01

    Traditional experimental methods for determining adsorption energies, such as temperature programmed desorption (TPD) and equilibrium adsorption isotherms, rely on desorption. However, on many metal surfaces large conjugated organic molecules, such as PTCDA and pentacene, decompose at elevated temperatures before or simultaneously with desorption. Discussions about relative bond strengths are, therefore, typically based on indirect arguments, such as the height of the adsorbed species above the surface as measured with normal incidence X-ray standing waves (NIXSW) or chemical shifts in spectroscopic techniques such as X-ray photoelectron spectroscopy (XPS). Unlike the more traditional methods, nanojoule adsorption calorimetry does not require desorption of the molecules; instead, the heat of adsorption is measured directly as an adsorption-induced temperature change of the sample. We will describe the construction of such a calorimeter at the Universitaet Erlangen-Nuernberg.

  15. DSC melting behavior of irradiated low density polyethylenes containing antioxidants

    International Nuclear Information System (INIS)

    The effect of antioxidants (0.5 wt% content) on the melting behaviour of low density polyethylenes, one branched and one linear, was examined with data obtained by DSC. The two polyethylenes exhibit noticeable differences in pure form: LLDPE has a higher melting point, lower heat of fusion and a more complex fusion endotherm than LDPE. The addition of antioxidants has a scarcely noticeable influence on the melting behaviour of LDPE whether irradiated or not, while in the case of LLDPE the effect is more visible. However, a careful analysis of the observed characteristics, peak temperatures and lamellae thickness distribution as well as heat of fusion, show that the observed effects are appearing as the consequence of chemical processes, scission and crosslinking, which occur in PE under either thermomechanical action (mixing in the course of the sample preparation), or radiation. (author)

  16. INVESTIGATION OF THE TRANSITIONS OF OLIGO-POLYSULFONES BY DSC

    Institute of Scientific and Technical Information of China (English)

    DONG Lisong; ZHENG Guodong; FENG Zhiliu

    1987-01-01

    The transitions of bisphenol A and phenolphthalein oligopolysulfones were investigated by DSC. It is found that both the oligomers have three transitions within the temperature range (230-550K) studied.Considering the strong dependence of the appearance of the two transitions, lower and higher than Tg, on the specimens' thermal history, i.e., temperature and time of heat-treatment, and their particular molecular structure, it is proposed that these two transitions are morphological in origin and are due to the disordering of relatively short range order of very small regions, and to the disordering of relatively well-ordered intraor/and intermolecular segments, respectively. Equations for linear relationship between Tg and 1/(M)(n)for both the oligomers are given in the paper.

  17. CRYSTALLIZATION SEGREGATION DSC STUDIES OF PP/PE COPOLYMERS

    Institute of Scientific and Technical Information of China (English)

    Yu Ma; Ying Wang; Shan-nong Zhu; Mao Xu

    2001-01-01

    The structural analysis of two PP/PE copolymer samples, I and 2, was conducted by using 13C-NMR, GPC and crystallization segregation DSC (CSDSC) techniques. A pure polypropylene sample was also used for comparison. It was found that the two copolymer samples are very close in composition (the ethylene mol content is 4.3% and 4.5%,respectively), stereoregularity (96% and 97%) and molecular weight (Mw, = 7.0 x 104 and 7.3x104; Mw/Mn = 5.0 and 6.1,respectively). While the CSDSC thermograms of the two samples are quite different from each other. Sample 1 shows a higher average melting temperature and a broader distribution of its thermogram. These phenomena were explained as an indication of a less uniform distribution of ethylene units along the PP chains for sample 1. It was noted that CSDSC is a very sensitive and convenient technique for structural studies of copolymers.

  18. DSC study and calculation of metronidazole and clarithromycin thermodynamic melting parameters for individual substances and for eutectic mixture

    International Nuclear Information System (INIS)

    Highlights: • The system clarithromycin–metronidazole is a system with a simple eutectic. • The eutectic melting temperature for the system clarithromycin–metronidazole is 155.2 ± 0.5 °C and it is not changed by varying the composition of the system. • The DSC curve for the composition of 89:11 mol or 64.9:35.1 wt% corresponds to the eutectic (or the invariant) composition for the system clarithromycin–metronidazole. - Abstract: In this study melting thermodynamic characteristics of clarithromycin and metronidazole as individual substances were investigated by DSC method. It was found that the binary system of clarithromycin and metronidazole is a system with simple eutectic. Composition, melting temperature and the heat of fusion of the eutectic were determined by calculation and experimental methods

  19. DSC study and calculation of metronidazole and clarithromycin thermodynamic melting parameters for individual substances and for eutectic mixture

    Energy Technology Data Exchange (ETDEWEB)

    Agafonova, Evgeniia V., E-mail: agafonova.ev@samgtu.ru [Samara State Technical University, Molodogvardeyskaya 244, 443100 Samara (Russian Federation); Moshchenskiy, Yuriy V. [Samara State Technical University, Molodogvardeyskaya 244, 443100 Samara (Russian Federation); Tkachenko, Mikhail L., E-mail: tka-mikhail@yandex.ru [Samara State Medical University, Chapaevskaya 89, 443099 Samara (Russian Federation)

    2014-03-01

    Highlights: • The system clarithromycin–metronidazole is a system with a simple eutectic. • The eutectic melting temperature for the system clarithromycin–metronidazole is 155.2 ± 0.5 °C and it is not changed by varying the composition of the system. • The DSC curve for the composition of 89:11 mol or 64.9:35.1 wt% corresponds to the eutectic (or the invariant) composition for the system clarithromycin–metronidazole. - Abstract: In this study melting thermodynamic characteristics of clarithromycin and metronidazole as individual substances were investigated by DSC method. It was found that the binary system of clarithromycin and metronidazole is a system with simple eutectic. Composition, melting temperature and the heat of fusion of the eutectic were determined by calculation and experimental methods.

  20. The glass transition process in humid biopolymers. DSC study

    Energy Technology Data Exchange (ETDEWEB)

    Grunina, N A; Belopolskaya, T V; Tsereteli, G I [V.A. Fock Research Institute for Physics of Saint-Petersburg State University, 198504, Petrodvorets (Russian Federation)

    2006-05-15

    Thermal properties of native and denatured biopolymers with quite different chemical and steric structure (globular and fibrillar proteins, DNA, starches) were studied by means of differential scanning calorimetry in a wide range of temperatures and concentrations of water. It was shown that both native and denatured humid biopolymers are glassy systems. The glass transition temperature of these systems strongly depends on percentage of water, with water being simultaneously an intrinsic element of systems' ordered structure and a plasticizer of its amorphous state. On the base of the absolute values of heat capacities for biopolymer-water systems as a whole, heat capacities for biopolymers themselves were calculated as functions on water concentration at fixed temperatures. The S-shaped change of heat capacity observed on diagrams of state both for native and denatured biopolymers is the manifestation of biopolymers' passing through the vitrification region, as it occurs for denatured samples at heating.

  1. Synergistic antioxidation of organic molybdenum complex with dithiocarbamate antioxidant evaluated by differential scanning calorimetry and thin film micro oxidation test

    International Nuclear Information System (INIS)

    An oil-soluble sulfur- and phosphorus-free organic molybdenum complex (MC) was synthesized. The antioxidation properties of MC- and methylene bis(di-n-butyldithiocarbamate) (V 7723)-containing poly-α-olefin (PAO)-derived lubricants were evaluated by differential scanning calorimetry (DSC) and modified penn state micro-oxidation test (PMOT). DSC test measures incipient oxidation temperature (OT) and oxidation induction time (IT) of the lubricant at high temperatures and the oxidation stability of oil weight loss is measured by PMOT test. DSC test shows that OT and IT of V 7723-containing PAO were improved significantly by MC addition. PMOT test indicates that when combining with V 7723 antioxidants, MC can also effectively reduce the increase in weight loss of PAO. These results suggest that the MC shows a good oxidative synergism with V 7723 antioxidant. In addition, FTIR results from PMOT test confirm that addition of MC can significantly enhance the oxidation induction time of oils and inhibit formation of oxidation products containing carbonyl bonds or hydroxyl group. The proposed mechanism of the inhibition involves a synergy between MC and V 7723

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

    International Nuclear Information System (INIS)

    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

  3. Thermooxidative stability of poppy seeds studied by non-isothermal DSC measurements.

    Science.gov (United States)

    Cibulková, Zuzana; Čertík, Milan; Dubaj, Tibor

    2014-05-01

    Papaver somniferum L. is an important crop cultivated mostly for seed production. Poppy seeds have a high nutritive value and are used as a food and as a source of edible oil. This oil is a rich source of polyunsaturated fatty acids. It is well known that the unsaturated fatty acids easily undergo oxidation reactions, which lead to the reduction of shelf life, nutritional quality, development of unpleasant tastes and odors. The goal of this study was to develop the methodology for testing the stability of poppy seeds using non-isothermal DSC. For the treatment of the experimental data a method based on non-Arrhenian temperature function has been applied and the values the kinetic parameters have been obtained. In order to assess the durability of the commercial poppy seeds, the lengths of induction periods have been calculated.

  4. Characterizing crystal disorder of trospium chloride: a comprehensive,(13) C CP/MAS NMR, DSC, FTIR, and XRPD study.

    Science.gov (United States)

    Urbanova, Martina; Sturcova, Adriana; Brus, Jiri; Benes, Hynek; Skorepova, Eliska; Kratochvil, Bohumil; Cejka, Jan; Sedenkova, Ivana; Kobera, Libor; Policianova, Olivia; Sturc, Antonin

    2013-04-01

    Analysis of C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray powder diffraction data of trospium chloride (TCl) products crystallized from different mixtures of water-ethanol [φ(EtOH) = 0.5-1.0] at various temperatures (0°C, 20°C) and initial concentrations (saturated solution, 30%-50% excess of solvent) revealed extensive structural variability of TCl. Although (13) C CP/MAS NMR spectra indicated broad variety of structural phases arising from molecular disorder, temperature-modulated DSC identified presence of two distinct components in the products. FTIR spectra revealed alterations in the hydrogen bonding network (ionic hydrogen bond formation), whereas the X-ray diffraction reflected unchanged unit cell parameters. These results were explained by a two-component character of TCl products in which a dominant polymorphic form is accompanied by partly separated nanocrystalline domains of a secondary phase that does not provide clear Bragg reflections. These phases slightly differ in the degree of molecular disorder, in the quality of crystal lattice and hydrogen bonding network. It is also demonstrated that, for the quality control of such complex products, (13) C CP/MAS NMR spectroscopy combined with factor analysis (FA) can satisfactorily be used for categorizing the individual samples: FA of (13) C CP/MAS NMR spectra found clear relationships between the extent of molecular disorder and crystallization conditions. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1235-1248, 2013.

  5. Silicon calorimetry for the SSC[ Superconducting Supercollider

    International Nuclear Information System (INIS)

    SSC experiments will rely heavily on their calorimeters. Silicon calorimetry, which has been introduced in recent years as a useful technology, has many attractive characteristics which may make it a viable option for consideration. The many attractive properties of silicon detectors are reviewed. The relevant present day applications of large areas of silicon detectors are summarize to illustrate the emerging use. The troublesome issue of radiation damage in a high luminosity environment like the SSC is considered with a summary of much of the recent new measurements which help clarify this situation. A discussion of the electronics and a possible mechanical configuration is presented, followed by a summary of the outstanding R and D issues. 31 refs., 11 figs., 3 tabs

  6. Bipolar monolithic preamplifiers for SSC silicon calorimetry

    International Nuclear Information System (INIS)

    This paper describes preamplifiers designed specifically to address the requirements of silicon calorimetry for the Superconducting Super Collider (SSC). Eight different preamplifiers designed for detector capacitances ranging from 20 pF to 500 pF and operating temperatures from 25 degree C to -20 degree C are discussed. The preamplifiers were fabricated with two different high-frequency processes (one with the VTC, Inc. VJ900 process, seven with the Harris Semiconductor VHF Process). The different topologies and their features are discussed in addition to the design methodologies employed. The results for noise, power consumption, speed, and radiation damage effects as well as data for post-damage annealing are presented for the VTC process preamplifier. Simulations for the VHF Process circuits are presented. This work was funded through SSC Generic Detector funding, SSC Detector Subsystem funding, and the Oak Ridge National Laboratory (ORNL) Detector Center

  7. Isothermal Titration Calorimetry to Characterize Enzymatic Reactions.

    Science.gov (United States)

    Mazzei, Luca; Ciurli, Stefano; Zambelli, Barbara

    2016-01-01

    Isothermal titration calorimetry (ITC) is a technique that measures the heat released or absorbed during a chemical reaction as an intrinsic probe to characterize any chemical process that involves heat changes spontaneously occurring during the reaction. The general features of this method to determine the kinetic and thermodynamic parameters of enzymatic reactions (kcat, KM, ΔH) are described and discussed here together with some detailed applications to specific cases. ITC does not require any modification or labeling of the system under analysis, can be performed in solution, and needs only small amounts of enzyme. These properties make ITC an invaluable, powerful, and unique tool to extend the knowledge of enzyme kinetics to drug discovery.

  8. Isothermal Titration Calorimetry of Chiral Polymeric Nanoparticles.

    Science.gov (United States)

    Werber, Liora; Preiss, Laura C; Landfester, Katharina; Muñoz-Espí, Rafael; Mastai, Yitzhak

    2015-09-01

    Chiral polymeric nanoparticles are of prime importance, mainly due to their enantioselective potential, for many applications such as catalysis and chiral separation in chromatography. In this article we report on the preparation of chiral polymeric nanoparticles by miniemulsion polymerization. In addition, we describe the use of isothermal titration calorimetry (ITC) to measure the chiral interactions and the energetics of the adsorption of enantiomers from aqueous solutions onto chiral polymeric nanoparticles. The characterization of chirality in nano-systems is a very challenging task; here, we demonstrate that ITC can be used to accurately determine the thermodynamic parameters associated with the chiral interactions of nanoparticles. The use of ITC to measure the energetics of chiral interactions and recognition at the surfaces of chiral nanoparticles can be applied to other nanoscale chiral systems and can provide further insight into the chiral discrimination processes of nanomaterials.

  9. Calorimetry studies on U-Cr alloys

    International Nuclear Information System (INIS)

    A calorimetric study of Uranium-Chromium system is of interest on both basic and applied fronts. With the advent of U-Pu-Zr alloy as the fuel, in combination with ferritic-martensitic steel as the cladding material, the metal fuelled fast reactors constitute the second major step in Indian nuclear power program. In such a context, a fundamental investigation on the high temperature phase stability of U-Cr alloys is of particular relevance in getting further insight in to the complex issue of the metallurgical compatibility of ferritic steels with metallic Uranium-Zirconium fuel. It may be added that following U-Fe, and U-Zr binaries, the U-Cr constitutes one of the important subsystems of the complex U-Zr-Pu-Fe- Cr-Mn-Si-V-Nb-C-N multinary system. In the current study, the results of calorimetry investigations on U, U-2, 3, 7, 15wt. % Cr alloys are presented

  10. Calorimetry for Fast Authentication of Edible Oils

    Science.gov (United States)

    Angiuli, Marco; Bussolino, Gian Carlo; Ferrari, Carlo; Matteoli, Enrico; Righetti, Maria Cristina; Salvetti, Giuseppe; Tombari, Elpidio

    2009-06-01

    There are little data in the literature on how to authenticate edible oils through calorimetry techniques. However, oil melting curves can be used to represent correlations between calorimetric results and oil quality. A calorimetric method has been developed for studying the solid-liquid phase transitions of olive oil and seed oils, in which melting peak behavior is correlated to the type, quality, and composition of the oil. Good reproducible thermograms were obtained by defining precise protocols for use in testing, which take into account the specific characteristics of a particular oil. This approach does not replace classical analytical methods; nevertheless, it is believed that calorimetric tests could be a useful preliminary stage for quality testing. The calorimetric technique allows the detection of the adulterant (seed oils or refined olive oil), oil origin, and possible photo-oxidation degradation processes, before more complex and expensive procedures and analyses are applied.

  11. Isothermal calorimetry on enzymatic biodiesel production

    DEFF Research Database (Denmark)

    Fjerbæk, Lene

    2008-01-01

    information about effects taking place when using lipases immobilized on an inert carrier for transesterification of a triglyceride and an alcohol as for biodiesel production. The biodiesel is produced by rapeseed oil and methanol as well as ethanol and a commercial biocatalyst Novozym 435 from Novozymes...... containing a Candida Antarctica B lipase immobilized on an acrylic resin. The reaction investigated is characterized by immiscible liquids (oil, methanol, glycerol and biodiesel) and enzymes imm. on an inert carrier during reaction, which allows several effects to take place that during normal reaction...... conditions can not be elucidated. These effects have been observed with isothermal calorimetry bringing forth new information about the reaction of enzymes catalyzing transesterification. Enzymatic biodiesel production has until now not been investigated with isothermal microcalorimetry, but the results...

  12. Fast Scanning Calorimetry Studies of Supercooled Liquids and Glasses

    Science.gov (United States)

    Bhattacharya, Deepanjan

    This dissertation is a compilation of research results of extensive Fast Scanning Calorimetry studies of two non-crystalline materials: Toluene and Water. Motivation for fundamental studies of non-crystalline phases, a brief overview of glassy materials and concepts and definitions related to them is provided in Chapter 1. Chapter 2 provides fundamentals and details of experimental apparata, experimental protocol and calibration procedure. Chapter 3 & 4 provides extensive studies of stable non-crystalline toluene films of micrometer and nanometer thicknesses grown by vapor deposition at distinct deposition rates and temperatures and probed by Fast Scanning Calorimetry. Fast scanning calorimetry is shown to be extremely sensitive to the structure of the vapor-deposited phase and was used to characterize simultaneously its kinetic stability and its thermodynamic properties. According to our analysis, transformation of vapor -deposited samples of toluene during heating with rates in excess 100,000 K/s follows the zero-order kinetics. The transformation rate correlates strongly with the initial enthalpy of the sample, which increases with the deposition rate according to sub-linear law. Analysis of the transformation kinetics of vapor deposited toluene films of various thicknesses reveal a sudden increase in the transformation rate for films thinner than 250 nm. The change in kinetics correlates with the surface roughness scale of the substrate, which is interpreted as evidence for kinetic anisotropy of the samples. We also show that out-of-equilibrium relaxation kinetics and possibly the enthalpy of vapor-deposited (VD) films of toluene are distinct from those of ordinary supercooled (OS) phase even when the deposition takes place at temperatures above the glass softening (Tg). The implications of these findings for the formation mechanism and structure of vapor deposited stable glasses are discussed. Chapter 5 and 6 provide detailed Fast Scanning Calorimetry studies

  13. [Study on the Effects of Ginsenoside Rb1 on DPPC Bilayers by Using Thermo-Raman Spectrum and DSC].

    Science.gov (United States)

    Hui, Ge; Liu, Wei; Zhang, Jing-zhou; Zhou, Tie-li; Wang, Si-ming; Zhao, Yu; Zhao, Bing

    2015-08-01

    The research on the interactions between Ginsenosides and biomembranes plays a crucial role in thorough understanding the pharmacological activity and biologyical effect of Chinese medicine Panax ginseng. With the bilayer structure, DPPC often serves as an simulation model of the cell membrane to study the role of drug molecules and cell membranes. Ginsenoside Rb1, one of the most important components of Panaxginseng, playing the significant roles of pharmacological effects and biological properties. Raman and differential scanning calorimetry (DSC) are respectively a powerful tool for discussing the molecular interaction, and a kind of general technology by which researching the bilayer monomer structures and its interactions with drug molecules. However, rarely research reports on the interactions between drug molecules and biomembranes by means of both technologies above. In this paper, the influence of ginsenoside monomer Rb1 on DPPC membrane bilayers was investigated by thermo-Raman and DSC. In Raman spectra, the changes of DPPC molecule have been observed before and after interacted with ginsenoside Rb1, the data analysis indicates three aspects: the O-C-C-N+ polar head group skeleton, C-C stretching vibration area, and the C-H bond stretching vibrarion in terminated methyl group of alkyl chains. The results showed that ginsenoside Rb1 molecule with certain concentration has not changed the gauche conformation of the polar head backbone group in DPPC bilayers, the order of the internal molecular chain and the lateral chain-chain packing have been decreased as the temperature increased, the lateral disposed disorder has been increased. The changes of some thermodynamic constants obtained by DSC experiment such as phase transition temperature (Tm), the temperature at which the transition is half completed (ΔT1/2), and the transition enthalpy normalized per mol of DPPC (AH) have been showed further results of the thermo Raman experiments, with increasing the

  14. Profiles in Leadership: Donald E. Francke, MSc, DSc (Hon).

    Science.gov (United States)

    Stevenson, James G; Beham, Rachel E; Weber, Robert J

    2013-10-01

    The Director's Forum series is designed to guide pharmacy leaders in establishing patient-centered services in hospitals and health systems. August 2013 marked the 50th anniversary of the publication of the Mirror to Hospital Pharmacy, the results of a federally funded comprehensive study of pharmacy services in the United States. The late Don E. Francke, MS, DSc, was the lead author of the Mirror and the principal investigator for the US Public Health Service grant W-45. To celebrate the anniversary of the Mirror, the Director's Forum is profiling the leadership styles of Drs. Latiolais and Francke. September's article highlighted Dr. Clifton J. Latiolais; this month's Director's Forum reviews Dr. Francke's biography and key career accomplishments, describes his leadership philosophy, and translates that philosophy to today's health care challenges. Don's influence on health system pharmacy serves as an example of effective leadership. This historical perspective provides directors of pharmacy a valuable leadership view as they develop strategies to enhance patient-centered pharmacy services. PMID:24421553

  15. Hydrogen determinations in a zirconium based alloy with a DSC

    International Nuclear Information System (INIS)

    In the present work a method to measure hydrogen concentrations in zirconium-based alloys was developed measuring simultaneously both, the temperature of terminal solid solubility, TTSSd, and the hydride dissolution heat, Qδ->α, using a differential scanning calorimeter (DSC). The hydrogen concentration measured with that technique, [H]Q, and the values obtained with a standard hydrogen gas meter, [H]HGM, shows a linear relation: [H]Q=(1.00+/-0.03)[H]HGM|+(9.2+/-8.0) with a correlation factor of 0.99 in the entire solubility interval in the αZr phase, from 15 to 650wt.ppm-H. The mean enthalpy value determined with two different criteria for TTSSd and Qδ->α measurements is ΔHδ->α(Q)=39.3+/-1.5kJ/mol H. The present method is specially appropriate for alloys where a partition of the overall hydrogen concentration in two phases exists. It is applicable to all hydride forming metals which ideally follows the van't Hoff law

  16. Titration Calorimetry Standards and the Precision of Isothermal Titration Calorimetry Data

    OpenAIRE

    Daumantas Matulis; Jurgita Matulienė; Vilma Petrikaitė; Lina Baranauskienė

    2009-01-01

    Current Isothermal Titration Calorimetry (ITC) data in the literature have relatively high errors in the measured enthalpies of protein-ligand binding reactions. There is a need for universal validation standards for titration calorimeters. Several inorganic salt co-precipitation and buffer protonation reactions have been suggested as possible enthalpy standards. The performances of several commercial calorimeters, including the VP-ITC, ITC200, and Nano ITC-III, were validated using these sug...

  17. DSC study of denaturation of β-lactoglobulin B

    Institute of Scientific and Technical Information of China (English)

    王邦宁; 谈夫

    1995-01-01

    The denaturation of bovine β-lactoglobulin B (β-Lg B) has been studied in phosphate solutions with various concentrations of GuHCl with differential scanning calorimetry The experiments demonstrated that the presence of GuHCl made the β-Lg B undergo both cold denaturation and heat denaturation under the condition of a high concentration of the protein. The enthalpy changes of both kinds of denaturation exhibit opposite signs. Both the cold denaturation and the renaturation of the protein are reproducible, but its heat denaturation is irreversible. The cooperation among monomer molecules of the protein is involved in its heat denaturation The heat denaturation of the protein can be represented by the thermodynamic model Nc D→F. The activation energy of heat denaturation is 285 kJ/mol, which imples that the depression of temperature and enthalpy of heat denaturation of the P-Lg B does not result from decreasing considerably the activation energy by GuHCl As for the cold denaturation of the protein, es

  18. Surfactant softening of plant leaf cuticle model wax--a Differential Scanning Calorimetry (DSC) and Quartz Crystal Microbalance with Dissipation (QCM-D) study.

    Science.gov (United States)

    Fagerström, Anton; Kocherbitov, Vitaly; Westbye, Peter; Bergström, Karin; Arnebrant, Thomas; Engblom, Johan

    2014-07-15

    The aim was to quantify the softening effect that two surfactants (C10EO7 and C8G1.6) have on a plant leaf cuticle model wax. Effects on the thermotropic phase behavior and fluidity of the wax (C22H45OH/C32H66/H2O) were determined. The model wax is crystalline at ambient conditions, yet it is clearly softened by the surfactants. Both surfactants decreased the transition temperatures in the wax and the G″/G' ratio of the wax film increased in irreversible steps following surfactant exposure. C10EO7 has a stronger fluidizing effect than C8G1.6 due to stronger interaction with the hydrophobic waxes. Intracuticular waxes (IW) comprise both crystalline and amorphous domains and it has previously been proposed that the fluidizing effects of surfactants are due to interactions with the amorphous parts. New data suggests that this may be a simplification. Surfactants may also absorb in crevices between crystalline domains. This causes an irreversible effect and a softer cuticle wax.

  19. Calorimetry for ILC Experiments: CALICE Collaboration R&D

    OpenAIRE

    Bailey, D.S.; Collaboration, for the CALICE

    2008-01-01

    The CALICE Collaboration is carrying out research and development into calorimetry for a detector at the International Linear Collider (ILC). CALICE is investigating a range of technologies for both electromagnetic and hadronic calorimetry. An overview of the prototypes and selected test-beam results are presented.

  20. Microwave curing of initially compatible epoxy–poly(ethylene terephthalate) blends: DSC kinetic study and nano-structure analysis☆

    International Nuclear Information System (INIS)

    Graphical abstract: The curves proposed to tabulate the curing regime in microwave field. - Highlights: • The monitoring of the curing process in microwave field is the aim of the study. • We consider an approach to estimate the curing regime in microwave field. • We present physical evidences for obtaining nano-modified epoxy composites. - Abstract: Poly(ethylene terephthalate), PET, dissolved in diglycidyl ether of bisphenol-A epoxy resins, DGEBA, is used as a toughening modifier. Two DGEBA resins in the presence of PET have been cured with the aid of diaminodiphenyl sulfone, DDS, in stoichiometric proportion. The curing process of the system DGEBA with DDS, in the presence of PET in particular, is monitored applying differential scanning calorimetry, DSC, in isothermal mode. The curing data are used to estimate the temperature regime in a microwave, MW, cavity. Physical confirmations for obtaining sub-micro phase separated DGEBA–DDS–PET composites and, in turn, for efficient modifying of the epoxy phase, have been discussed

  1. Thermal Hazard Evaluation of Cumene Hydroperoxide-Metal Ion Mixture Using DSC, TAM III, and GC/MS.

    Science.gov (United States)

    You, Mei-Li

    2016-01-01

    Cumene hydroperoxide (CHP) is widely used in chemical processes, mainly as an initiator for the polymerization of acrylonitrile-butadiene-styrene. It is a typical organic peroxide and an explosive substance. It is susceptible to thermal decomposition and is readily affected by contamination; moreover, it has high thermal sensitivity. The reactor tank, transit storage vessel, and pipeline used for manufacturing and transporting this substance are made of metal. Metal containers used in chemical processes can be damaged through aging, wear, erosion, and corrosion; furthermore, the containers might release metal ions. In a metal pipeline, CHP may cause incompatibility reactions because of catalyzed exothermic reactions. This paper discusses and elucidates the potential thermal hazard of a mixture of CHP and an incompatible material's metal ions. Differential scanning calorimetry (DSC) and thermal activity monitor III (TAM III) were employed to preliminarily explore and narrate the thermal hazard at the constant temperature environment. The substance was diluted and analyzed by using a gas chromatography spectrometer (GC) and gas chromatography/mass spectrometer (GC/MS) to determine the effect of thermal cracking and metal ions of CHP. The thermokinetic parameter values obtained from the experiments are discussed; the results can be used for designing an inherently safer process. As a result, the paper finds that the most hazards are in the reaction of CHP with Fe(2+). When the metal release is exothermic in advance, the system temperature increases, even leading to uncontrollable levels, and the process may slip out of control. PMID:27136518

  2. Evaluation of mechanical properties and DSC study of commercial multilayer PA/PE film treated with E-beam radiation

    International Nuclear Information System (INIS)

    Packaging materials have been widely processed by ionizing radiation in order to improve their chemical and physical properties and also for sterilization purposes. Basically, flexible packaging manufacturers apply specific radiation doses to promote cross-linking and scission of the polymeric chains and thus obtain alterations in certain properties of the material. While enhancing a specific property, significant losses may result in others. In this study, we examined the effects of E-beam radiation on a commercial multilayer PA6/LDPE based film, irradiated with doses up to 127 kGy. Food producers mostly use this structure as a thermoforming bottom web for processed meat products. Two weeks after irradiation, tensile strength and elongation of the film were analyzed. Both mechanical properties were again analyzed 18 months after irradiation took place. Significant changes of mechanical properties were observed specially 18 months after irradiation. Once cross-linking and scission are able to affect the material crystalline arrangement and consequently cause properties changes, a DSC ( Differential Scanning Calorimetry) study was carried out for doses up to 130 kGy in order to verify such changes. (author)

  3. Thermal Hazard Evaluation of Cumene Hydroperoxide-Metal Ion Mixture Using DSC, TAM III, and GC/MS.

    Science.gov (United States)

    You, Mei-Li

    2016-04-28

    Cumene hydroperoxide (CHP) is widely used in chemical processes, mainly as an initiator for the polymerization of acrylonitrile-butadiene-styrene. It is a typical organic peroxide and an explosive substance. It is susceptible to thermal decomposition and is readily affected by contamination; moreover, it has high thermal sensitivity. The reactor tank, transit storage vessel, and pipeline used for manufacturing and transporting this substance are made of metal. Metal containers used in chemical processes can be damaged through aging, wear, erosion, and corrosion; furthermore, the containers might release metal ions. In a metal pipeline, CHP may cause incompatibility reactions because of catalyzed exothermic reactions. This paper discusses and elucidates the potential thermal hazard of a mixture of CHP and an incompatible material's metal ions. Differential scanning calorimetry (DSC) and thermal activity monitor III (TAM III) were employed to preliminarily explore and narrate the thermal hazard at the constant temperature environment. The substance was diluted and analyzed by using a gas chromatography spectrometer (GC) and gas chromatography/mass spectrometer (GC/MS) to determine the effect of thermal cracking and metal ions of CHP. The thermokinetic parameter values obtained from the experiments are discussed; the results can be used for designing an inherently safer process. As a result, the paper finds that the most hazards are in the reaction of CHP with Fe(2+). When the metal release is exothermic in advance, the system temperature increases, even leading to uncontrollable levels, and the process may slip out of control.

  4. Examination of fluorination effect on physical properties of saturated long-chain alcohols by DSC and Langmuir monolayer.

    Science.gov (United States)

    Nakahara, Hiromichi; Nakamura, Shohei; Okahashi, Yoshinori; Kitaguchi, Daisuke; Kawabata, Noritake; Sakamoto, Seiichi; Shibata, Osamu

    2013-02-01

    Partially fluorinated long-chain alcohols have been newly synthesized from a radical reaction, which is followed by a reductive reaction. The fluorinated alcohols have been investigated by differential scanning calorimetry (DSC) and compression isotherms in a Langmuir monolayer state. Their melting points increase with an increase in chain length due to elongation of methylene groups. However, the melting points for the alcohols containing shorter fluorinated moieties are lower than those for the typical hydrogenated fatty alcohols. Using the Langmuir monolayer technique, surface pressure (π)-molecular area (A) and surface potential (ΔV)-A isotherms of monolayers of the fluorinated alcohols have been measured in the temperature range from 281.2 to 303.2K. In addition, a compressibility modulus (Cs(-1)) is calculated from the π-A isotherms. Four kinds of the alcohol monolayers show a phase transition (π(eq)) from a disordered to an ordered state upon lateral compression. The π(eq) values increase linearly with increasing temperatures. A slope of π(eq) against temperature for the alcohols with shorter fluorocarbons is unexpectedly larger than that for the corresponding fatty alcohols. Generally, fluorinated amphiphiles have a greater thermal stability (or resistance), which is a characteristic of highly fluorinated or perfluorinated compounds. Herein, however, the alcohols containing perfluorobutylated and perfluorohexylated chains show the irregular thermal behavior in both the solid and monolayer states.

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

    International Nuclear Information System (INIS)

    Highlights: • The heat capacity of the (Li1−xCax)F1+x liquid solution was measured. • A procedure for DSC was developed to measure heat capacity of encapsulated samples. • A significant excess heat capacity of (Li1−xCax)F1+x liquid solution was observed. - Abstract: 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 modifications were introduced in the standard configuration of the instrument and they are described in this work as well. For comparison one of the analysed composition (xCaF2 = 0.5) was also measured using drop calorimetry, which has been previously used for similar studies. The reliability of the results obtained was confirmed by the good agreement between the two techniques. Moreover, the excess heat capacity of the (Li1−xCax)F1+x liquid solution was derived and a strong deviation from the ideal behaviour was observed

  6. Thermodynamic optimization of individual steel database by means of systematic DSC measurements according the CALPHAD approach

    Science.gov (United States)

    Presoly, P.; Six, J.; Bernhard, C.

    2016-03-01

    Reliable thermodynamic data are essential information required for the design of new steel types and are a prerequisite to effective process optimization and simulation. Moreover, it is important to know the exact temperatures at which the high-temperature phase transformations (TLiquid, TSolid, TPerit, Tγ→δ) occur in order to describe the solidification sequence and to describe further processing parameters. By utilizing DTA/DSC measurements, our earlier experimental studies of selected commercial DP, TRIP and high-Mn TWIP steels, have indicated that currently commercially available databases can often not be utilised to reliably describe the behaviour and microstructural development in such complex alloy systems. Because of these ostensible deficiencies, an experimental study was undertaken in an attempt to determine the pertaining thermodynamic data to analyse the behaviour of the important five- component Fe-C-Si-Mn-Al alloy system. High purity model alloys with systematic alloy variations were prepared and utilized in order to determine the influence of individual alloying elements in this complex, but industrially important alloy system. The present study provides new validated experimental thermodynamic data and analysis of the five-component Fe-C-Si- Mn-Al system, which will allow the construction of new phase diagrams, prediction of solidification sequences and the assessment of micro-segregation.

  7. 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.

  8. Kinetic analysis by DSC of the cationic curing of mixtures of DGEBA and 6,6-dimethyl (4,8-dioxaspiro[2.5]octane-5,7-dione)

    Energy Technology Data Exchange (ETDEWEB)

    Gonzalez, Lidia [Departament de Quimica Analitica i Quimica Organica, Universitat Rovira i Virgili, C/Marcelli Domingo s/n, 43007 Tarragona (Spain); Ramis, Xavier [Laboratori de Termodinamica, ETSEIB, Universitat Politecnica de Catalunya, Av. Diagonal 647, 08028 Barcelona (Spain); Salla, Josep Maria [Laboratori de Termodinamica, ETSEIB, Universitat Politecnica de Catalunya, Av. Diagonal 647, 08028 Barcelona (Spain)], E-mail: salla@mmt.upc.edu; Mantecon, Ana; Serra, Angels [Departament de Quimica Analitica i Quimica Organica, Universitat Rovira i Virgili, C/Marcelli Domingo s/n, 43007 Tarragona (Spain)

    2007-11-25

    The kinetics of the thermal cationic cure reaction of mixtures in different proportions of diglycidylether of bisphenol A (DGEBA) with 6,6-dimethyl (4,8-dioxaspiro[2.5]octane-5,7-dione) (MCP) initiated by ytterbium or lanthanum triflates or using a conventional initiator, BF{sub 3}.MEA was investigated. The non-isothermal differential scanning calorimetry (DSC) experiments at a controlled heating rate was used for obtaining the kinetic parameters of the reactive systems. BF{sub 3}.MEA and lanthanide triflates initiated curing systems follow a complete different kinetic model. Among lanthanide triflates, ytterbium is the most active initiator.

  9. 47 CFR 80.359 - Frequencies for digital selective calling (DSC).

    Science.gov (United States)

    2010-10-01

    ... this incorporation by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of this... 47 Telecommunication 5 2010-10-01 2010-10-01 false Frequencies for digital selective calling (DSC... for digital selective calling (DSC). (a) General purpose calling. The following table describes...

  10. 7 CFR 1710.114 - TIER, DSC, OTIER and ODSC requirements.

    Science.gov (United States)

    2010-01-01

    ... substantially in their entirety are in 7 CFR 1717.155. (4) If a distribution borrower has in service or under... 7 Agriculture 11 2010-01-01 2010-01-01 false TIER, DSC, OTIER and ODSC requirements. 1710.114... AND GUARANTEES Loan Purposes and Basic Policies § 1710.114 TIER, DSC, OTIER and ODSC requirements....

  11. 47 CFR 80.103 - Digital selective calling (DSC) operating procedures.

    Science.gov (United States)

    2010-10-01

    ... accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies of this standard can be inspected at the Federal... 47 Telecommunication 5 2010-10-01 2010-10-01 false Digital selective calling (DSC) operating... Procedures-General § 80.103 Digital selective calling (DSC) operating procedures. (a) Operating...

  12. Homogeneous and isotropic calorimetry for space experiments

    Energy Technology Data Exchange (ETDEWEB)

    Mori, N., E-mail: mori@fi.infn.it [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); Adriani, O. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); University of Florence, Department of Physics and Astronomy, via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Basti, A. [INFN sezione di Pisa, Largo B. Pontecorvo 3, 56127 Pisa (Italy); Bigongiari, G. [University of Siena, Department of Physics, Earth and Environmental Sciences, Via Laterina 8, 53100 Siena (Italy); Bonechi, L. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); Bonechi, S. [INFN sezione di Pisa, Largo B. Pontecorvo 3, 56127 Pisa (Italy); University of Siena, Department of Physics, Earth and Environmental Sciences, Via Laterina 8, 53100 Siena (Italy); Bongi, M. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); University of Florence, Department of Physics and Astronomy, via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Bottai, S. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); Brogi, P. [INFN sezione di Pisa, Largo B. Pontecorvo 3, 56127 Pisa (Italy); University of Siena, Department of Physics, Earth and Environmental Sciences, Via Laterina 8, 53100 Siena (Italy); D' Alessandro, R. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); University of Florence, Department of Physics and Astronomy, via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Detti, S.; Lenzi, P. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); Maestro, P.; Marrocchesi, P.S. [INFN sezione di Pisa, Largo B. Pontecorvo 3, 56127 Pisa (Italy); University of Siena, Department of Physics, Earth and Environmental Sciences, Via Laterina 8, 53100 Siena (Italy); Papini, P. [INFN sezione di Firenze, via B. Rossi 1, 50019 Sesto Fiorentino (Italy); and others

    2013-12-21

    Calorimetry plays an essential role in experiments observing high energy gamma and cosmic rays in space. The observational capabilities are mainly limited by the geometrical dimensions and the mass of the calorimeter. Since deployable mass depends on the design of the detector and the total mass of the payload, it is important to optimize the geometrical acceptance of the calorimeter for rare events, its granularity for particle identification, and its absorption depth for the measurement of the particle energy. A design of a calorimeter that could simultaneously optimize these characteristics assuming a mass limit of about 1.6 t has been studied. As a result, a homogeneous calorimeter instrumented with cesium iodide (CsI) crystals was chosen as the best compromise given the total mass constraint. The most suitable geometry found is cubic and isotropic, so as to detect particles arriving from every direction in space, thus maximizing the acceptance; granularity is obtained by filling the cubic volume with small cubic CsI crystals. The total radiation length in any direction is very large, and allows for optimal electromagnetic particle identification and energy measurement, while the interaction length is at least sufficient to allow a precise reconstruction of hadronic showers. Optimal values for the size of the crystals and spacing among them have been studied. Two prototypes have been constructed and preliminary tests with high energy ion and muon beams are reported.

  13. Current status of tritium calorimetry at TLK

    International Nuclear Information System (INIS)

    Inside a tritium facility, calorimetry is an important analytical method as it is the only reference method for accountancy (it is based on the measurement of the heat generated by the radioactive decay). Presently, at Tritium Laboratory Karlsruhe (TLK), 4 calorimeters are in operation, one of isothermal type and three of inertial guidance control type (IGC). The volume of the calorimeters varies between 0.5 and 20.6 liters. About two years ago we started an extensive work to improve our calorimeters with regard to reliability and precision. We were forced to upgrade 3 of our 4 calorimeters due to the outdated interfaces and software. This work involved creating new LabView programs driving the devices, re-tuning control loops and replacing obsolete hardware components. In this paper we give a review on the current performance of our calorimeters, comparing it to recently available devices from the market and in the literature. We also show some ideas for a next generation calorimeter based on experiences with our IGC calorimeters and other devices reported in the literature. (authors)

  14. Current status of tritium calorimetry at TLK

    Energy Technology Data Exchange (ETDEWEB)

    Buekki-Deme, A.; Alecu, C.G.; Kloppe, B.; Bornschein, B. [Institute of Technical Physics, Tritium Laboratory Karsruhe - TLK, Karlsruhe Institute of Technology - KIT, Karlsruhe (Germany)

    2015-03-15

    Inside a tritium facility, calorimetry is an important analytical method as it is the only reference method for accountancy (it is based on the measurement of the heat generated by the radioactive decay). Presently, at Tritium Laboratory Karlsruhe (TLK), 4 calorimeters are in operation, one of isothermal type and three of inertial guidance control type (IGC). The volume of the calorimeters varies between 0.5 and 20.6 liters. About two years ago we started an extensive work to improve our calorimeters with regard to reliability and precision. We were forced to upgrade 3 of our 4 calorimeters due to the outdated interfaces and software. This work involved creating new LabView programs driving the devices, re-tuning control loops and replacing obsolete hardware components. In this paper we give a review on the current performance of our calorimeters, comparing it to recently available devices from the market and in the literature. We also show some ideas for a next generation calorimeter based on experiences with our IGC calorimeters and other devices reported in the literature. (authors)

  15. Small-angle x-ray scattering and differential scanning calorimetry studies of DPPC multilamellar structures containing membranotropic agents of different chemical nature

    International Nuclear Information System (INIS)

    Multilamellar structures formed in DPPC/water/glycerol and DPPC/water/oxyethylated glycerol systems are studied by small-angle X-ray scattering (SAXS) and differential scanning calorimetry (DSC) methods. The effects of glycerol, oxyethylated glycerol, and other membranotropic agents (MTAs) on the lamellar repeat distance D are compared in gel, ripple, and high-temperature (Lα) liquid crystal phases of the hydrated phospholipids. It is noted that the introduction of MTAs could lead to different types of 'D vs. temperature' behavior in the Lα phase, which is correlated with changes in D caused by the introduction of these substances to the DPPC/water reference system

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

    Science.gov (United States)

    Shao, Changming; Desai, Chandra S.

    2000-05-01

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

  17. Comparative study of DSC-PWI and 3D-ASL in ischemic stroke patients.

    Science.gov (United States)

    Zhang, Shui-xia; Yao, Yi-hao; Zhang, Shun; Zhu, Wen-jie; Tang, Xiang-yu; Qin, Yuan-yuan; Zhao, Ling-yun; Liu, Cheng-xia; Zhu, Wen-zhen

    2015-12-01

    The purpose of this study was to quantitatively analyze the relationship between three dimensional arterial spin labeling (3D-ASL) and dynamic susceptibility contrast-enhanced perfusion weighted imaging (DSC-PWI) in ischemic stroke patients. Thirty patients with ischemic stroke were included in this study. All subjects underwent routine magnetic resonance imaging scanning, diffusion weighted imaging (DWI), magnetic resonance angiography (MRA), 3D-ASL and DSC-PWI on a 3.0T MR scanner. Regions of interest (ROIs) were drawn on the cerebral blood flow (CBF) maps (derived from ASL) and multi-parametric DSC perfusion maps, and then, the absolute and relative values of ASL-CBF, DSC-derived CBF, and DSC-derived mean transit time (MTT) were calculated. The relationships between ASL and DSC parameters were analyzed using Pearson's correlation analysis. Receiver operative characteristic (ROC) curves were performed to define the thresholds of relative value of ASL-CBF (rASL) that could best predict DSC-CBF reduction and MTT prolongation. Relative ASL better correlated with CBF and MTT in the anterior circulation with the Pearson correlation coefficients (R) values being 0.611 (P1.0 were 75.7%, 89.2% and 87.8% respectively. ASL-CBF map has better linear correlations with DSC-derived parameters (DSC-CBF and MTT) in anterior circulation in ischemic stroke patients. Additionally, when rASL is lower than 0.585, it could predict DSC-CBF decrease with moderate accuracy. If rASL values range from 0.585 to 0.952, we just speculate the prolonged MTT.

  18. Experimental study of the ternary Ag-Cu-In phase diagram

    Energy Technology Data Exchange (ETDEWEB)

    Bahari, Zahra [Laboratoire de chimie physique et minerale, Faculte des sciences pharmaceutiques et biologiques, Universite Paris Descartes, avenue de l' Observatoire, 75006 Paris (France); Laboratoire de chimie du solide mineral (LCSM), Faculte des sciences, Universite Mohamed 1er, Route Sidi Maafa, B.P. 524, Oujda, Maroc (Morocco); Elgadi, Mohamed [Laboratoire de chimie du solide mineral (LCSM), Faculte des sciences, Universite Mohamed 1er, Route Sidi Maafa, B.P. 524, Oujda, Maroc (Morocco); Rivet, Jacques [Laboratoire de chimie physique et minerale, Faculte des sciences pharmaceutiques et biologiques, Universite Paris Descartes, avenue de l' Observatoire, 75006 Paris (France); Dugue, Jerome [Laboratoire de chimie physique et minerale, Faculte des sciences pharmaceutiques et biologiques, Universite Paris Descartes, avenue de l' Observatoire, 75006 Paris (France)], E-mail: jerome.dugue@univ-paris5.fr

    2009-05-27

    The phase diagram of the Ag-Cu-In system was investigated using powder X-ray diffraction (XRD), differential scanning calorimetry (DSC) and electron probe microanalysis (EPMA). Two isothermal sections (at 510 and 607 deg. C) and 15 isopletic sections were studied. The results showed seven ternary peritectics, one ternary eutectic and one ternary metatectic. A complete reaction scheme was constructed, the valleys were drawn and the liquidus surfaces were derived from DSC data in the entire composition range.

  19. Synthesis kinetics of Mg_2Sn in Mg-Sn powder mixture using non-isothermal differential scanning calorimetry

    Institute of Scientific and Technical Information of China (English)

    WU Yu-feng; DU Wen-bo; ZUO Tie-yong

    2009-01-01

    The non-isothermal heating process of Mg-Sn powder mixture was studied by differential scanning calorimetry(DSC) technique and the synthesis kinetics of Mg_2Sn was evaluated by the model-free and model-fitting methods. The activation energy and conversion function of Mg_2Sn synthesis reaction are calculated to be 281.7 kJ/mol and g(α)=[-ln(1-α)]~(1/4), respectively. The reaction mechanism of 2Mg+Sn→Mg_2Sn under non-isothermal condition is regarded as "nucleation and growth". During the non-isothermal heating process, the phase transformation occurred in the Mg-Sn powder mixture was analyzed by XRD and the microstructure evolution of Mg_2Sn was observed by optical microscopy, which is in good agreement with the reaction mechanism of 2Mg+Sn→Mg_2Sn deduced from the kinetic evaluation.

  20. Calorimetry and Langmuir-Blodgett studies on the interaction of a lipophilic prodrug of LHRH with biomembrane models.

    Science.gov (United States)

    Sarpietro, Maria G; Accolla, Maria L; Santoro, Nancy; Mansfeld, Friederike M; Pignatello, Rosario; Toth, Istvan; Castelli, Francesco

    2014-05-01

    The interaction between an amphiphilic luteinizing hormone-releasing hormone (LHRH) prodrug that incorporated a lipoamino acid moiety (C12-LAA) with biological membrane models that consisted of multilamellar liposomes (MLVs) and phospholipid monolayers, was studied using Differential Scanning Calorimetry (DSC) and Langmuir-Blodgett film techniques. The effect of the prodrug C12[Q1]LHRH on the lipid layers was compared with the results obtained with the pure precursors, LHRH and C12-LAA. Conjugation of LHRH with a LAA promoiety showed to improve the peptide interaction with biomembrane models. Basing on the calorimetric findings, the LAA moiety aided the transfer of the prodrug from an aqueous solution to the biomembrane model.

  1. Characterization of membrane protein interactions by isothermal titration calorimetry.

    Science.gov (United States)

    Situ, Alan J; Schmidt, Thomas; Mazumder, Parichita; Ulmer, Tobias S

    2014-10-23

    Understanding the structure, folding, and interaction of membrane proteins requires experimental tools to quantify the association of transmembrane (TM) helices. Here, we introduce isothermal titration calorimetry (ITC) to measure integrin αIIbβ3 TM complex affinity, to study the consequences of helix-helix preorientation in lipid bilayers, and to examine protein-induced lipid reorganization. Phospholipid bicelles served as membrane mimics. The association of αIIbβ3 proceeded with a free energy change of -4.61±0.04kcal/mol at bicelle conditions where the sampling of random helix-helix orientations leads to complex formation. At bicelle conditions that approach a true bilayer structure in effect, an entropy saving of >1kcal/mol was obtained from helix-helix preorientation. The magnitudes of enthalpy and entropy changes increased distinctly with bicelle dimensions, indicating long-range changes in bicelle lipid properties upon αIIbβ3 TM association. NMR spectroscopy confirmed ITC affinity measurements and revealed αIIbβ3 association and dissociation rates of 4500±100s(-1) and 2.1±0.1s(-1), respectively. Thus, ITC is able to provide comprehensive insight into the interaction of membrane proteins.

  2. Study of Liquid Argon Dopants for LHC Hadron Calorimetry

    CERN Multimedia

    2002-01-01

    Hadron calorimetry based on the Liquid Argon Ionisation Chamber technique is one of the choice techniques for LHC-experimentation. A systematic study of the effect of selected dopants on Liquid Argon (LAr) will be carried out with the aim to achieve an improvement on: \\item (i)~``Fast Liquid Argon'' search and study of dopants to increase the drift velocity. It has been already shown that CH&sub4. added at a fraction of one percent increases the drift velocity by a factor of two or more. \\item (ii)~``Compensated Liquid Argon'' search and study of dopants to increase the response to densely ionising particles, resulting in improved compensation, such as photosensitive dopants. \\end{enumerate}\\\\ \\\\ Monitoring of the parameters involved in understanding the response of a calorimeter is essential. In case of doped LAr, the charge yield, the non-saturated drift velocity and the electron lifetime in the liquid should be precisely and simultaneously monitored as they all vary with the level of dopant concentrati...

  3. IATC, DSC, and PPC Analysis of Reversible and Multistate Structural Transition of Cytochrome c.

    Science.gov (United States)

    Kidokoro, Shun-ichi; Nakamura, Shigeyoshi

    2016-01-01

    Development of precise calorimeters has enabled us to monitor the structural transition of biomolecules by calorimetry to characterize the thermodynamic property changes accompanying three-dimensional structure change. We developed isothermal acid-titration calorimetry to evaluate the pH dependence of protein enthalpy, and demonstrated the thermodynamic transition between the native and molten globule (MG) states of cytochrome c with very small enthalpy change (~20 kJ/mol) by this method. The double deconvolution method with precise differential scanning calorimetry has revealed the MG state as an equilibrium intermediate state of the reversible thermal transition of the protein, and pressure perturbation calorimetry has succeeded in determining its volumetric properties. These examples strongly indicate the importance of a precise calorimetry and analysis model in the field of protein research.

  4. Summary session of the Gas Sampling Calorimetry Workshop

    International Nuclear Information System (INIS)

    The summary session of the Gas Sampling Calorimetry Workshop was a review and discussion session. A number of questions were raised and briefly discussed. More extensive discussions of energy resolution formed the heart of the final session

  5. Application of adiabatic calorimetry to metal systems. Final report

    International Nuclear Information System (INIS)

    Research on the application of adiabatic calorimetry to metal systems is described. Investigations into formation of pearlite in steels, ferromagnetic effects, cold working and annealing, solid solution alloys, pure solid metals, and pure liquid metals, are briefly described

  6. Thermal characterization of starch-water system by photopyroelectric technique and adiabatic scanning calorimetry

    Science.gov (United States)

    Cruz-Orea, A.; Bentefour, E. H.; Jamée, P.; Chirtoc, M.; Glorieux, C.; Pitsi, G.; Thoen, J.

    2003-01-01

    Starch is one of the most important carbohydrate sources in human nutrition. For the thermal analysis of starch, techniques such as differential scanning calorimetry have been extensively used. As an alternative, we have applied a photopyroelectric (PPE) configuration and adiabatic scanning calorimetry (ASC) to study the thermal properties of starch-water systems. For this study we used nixtamalized corn flour and potato starch with different quantities of distilled water, in order to obtain samples with different moisture content. By using PPE and ASC methods we have measured, for each technique separately, the heat capacity by unit volume (ρcp) at room temperature for a corn flour sample at 90% moisture. The obtained values agree within experimental uncertainty. By using these techniques we also studied the thermal behavior of potato starch, at 80% moisture, in the temperature range where phase transitions occur. In this case the PPE signal phase could be used as a sensitive and versatile monitor for phase transitions.

  7. Isothermal Calorimetry for Biological Applications in Food Science and Technology

    OpenAIRE

    Wadsö, Lars; Gomez, Federico

    2009-01-01

    All physical, chemical and biological processes produce heat and isothermal calorimetry is a general measurement technique to study all kinds of processes by the heat they produce. This paper gives several examples of studies of biological processes in the food area using isothermal calorimetry. It is for example shown how different unit operations influence respiration of vegetable tissue, how the kinetics of a fermentation process can be studied, and how spoilage processes can be followed f...

  8. Particle Flow Calorimetry and the PandoraPFA Algorithm

    OpenAIRE

    Thomson, M. A.

    2009-01-01

    The Particle Flow (PFlow) approach to calorimetry promises to deliver unprecedented jet energy resolution for experiments at future high energy colliders such as the proposed International Linear Collider (ILC). This paper describes the PandoraPFA particle flow algorithm which is then used to perform the first systematic study of the potential of high granularity PFlow calorimetry. For simulated events in the ILD detector concept, a jet energy resolution of sigma_E/E < 3.8 % is achieved for 4...

  9. Differential scanning calorimetry of superelastic Nitinol for tunable cymbal transducers

    OpenAIRE

    Feeney, Andrew; Lucas, Margaret

    2015-01-01

    Recent research has shown that estimations of the transformation temperatures of superelastic Nitinol using differential scanning calorimetry can be inaccurate, in part, due to the residual stress in the material. Superelastic Nitinol is selected as the end-cap material in a tunable cymbal transducer. The differential scanning calorimetry accuracy is initially probed by comparing transformation temperature measurements of cold-worked superelastic Nitinol with the same material after an anneal...

  10. 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.

  11. A DSC study on the effect of marination on the stability of skin collagen from chicken wings

    Directory of Open Access Journals (Sweden)

    Jolanta Tomaszewska-Gras

    2010-12-01

    Full Text Available   Background. Marination is a good method to enhance attractiveness of chicken wings, which are considered by consumers as least attractive. Sensory value of marinated wings is dependent largely on the flavour of skin, because they contain proportionally more skin than other carcass elements. Moreover, skin constitutes a natural barrier, which may facilitate or hinder the penetration of marinade components, depending on the conformation state of proteins it is composed of primarily collagen. The aim of the study was to investigate the effect of specific marinades on thermal stability of collagen – the main component of skin proteins using differential scanning calorimetry (DSC. Material and methods. Chicken wings were marinated using model marinades, marinades prepared according to original recipes and ready-to-use marinades used in industrial practice. Marinated skin samples were weighted (approx. 10 mg and analyzed by DSC. Heating rate was 5°C/min, within the range from 20 to 100°C. Results. In analyses using model marinades denaturation temperature (Tmax of collagen was reduced by approx. 3°C and enthalpy (ΔH was lowered by approx. 40%. An even bigger reduction of collagen denaturation temperature (by approx. 7°C and enthalpy ΔH (by approx. 48% was found after the application of marinades prepared following original recipes (W1, W2, W3. In turn, the application of model marinades containing NaCl and organic acids (acetic or citric resulted in stabilization of collagen, which was manifested by an increase of enthalpy (ΔH by approx. 50% (for marinade containing 2% citric acid. Conclusions. Temperature and enthalpy of collagen denaturation was dependent on type of marinade. The extent of collagen denaturation affects nutritional and sensory value. Considering that time and temperature of intensive heat treatment are important factors in the formation process of carcinogenic compounds i.e. heterocyclic aromatic amines, it bis

  12. DSC study of cold and heat denaturation processes of β-lactoglobulin A with guanidine hydrochloride

    Institute of Scientific and Technical Information of China (English)

    王邦宁; 谈夫

    1997-01-01

    The cold and heat denaturations of bovine β-lactoglobuhn A (β-lg A) has been studied in solutions of guanidine hydrochloride (GuHCl) by differential scanning calorimelry (DSC) The experimental results are presented and discussed.It is shown that the number of protons bound by the monomeric molecules of β-lg A was unchanged before and after its heat denaturation below pH 3,and that the activation energy of the heat denaturation was depressed owing to the presence of GuHCl.In the solutions with 2.50 and 3.06 mol/L of GuHCl,both the cold and heat denat-urations of β-lg A were observed.In comparison with the heat denaturation,the activation energy of cold denaturation was far lower and the number of GuHCl molecules bound by the unfolded polypeptide chains after cold denaturation increased a lot.The absolute value of the enthalpy of cold denaturation was larger than that of heat denaturation It was found by the analysis that the contribution to the total denaturational enthalpy of conformational change i

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

    International Nuclear Information System (INIS)

    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 (XDMSO) 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 ≤ XDMSO ≤ 0.3 can be explained in the framework of DMSO-induced dehydration of intermembrane space

  14. Thermal and structural behavior of dioctadecyldimethylammonium bromide dispersions studied by differential scanning calorimetry and X-ray scattering.

    Directory of Open Access Journals (Sweden)

    Eloi Feitosa

    Full Text Available Dioctadecyldimethylammonium bromide (DODAB is a double chain cationic lipid, which assembles as bilayer structures in aqueous solution. The precise structures formed depend on, e.g., lipid concentration and temperature. We here combine differential scanning calorimetry (DSC and X-ray scattering (SAXS and WAXS to investigate the thermal and structural behavior of up to 120 mM DODAB in water within the temperature range 1-70 °C. Below 1 mM, this system is dominated by unilamellar vesicles (ULVs. Between 1 and 65 mM, ULVs and multilamellar structures (MLSs co-exist, while above 65 mM, the MLSs are the preferred structure. Depending on temperature, DSC and X-ray data show that the vesicles can be either in the subgel (SG, gel, or liquid crystalline (LC state, while the MLSs (with lattice distance d = 36.7 Å consist of interdigitated lamellae in the SG state, and ULVs in the LC state (no Bragg peak. Critical temperatures related to the thermal transitions of these bilayer structures obtained in the heating and cooling modes are reported, together with the corresponding transition enthalpies.

  15. Study of temperature dependent zirconium silicide phases in Zr/Si structure by differential scanning calorimetry

    International Nuclear Information System (INIS)

    The differential scanning calorimetry (DSC) technique is employed to study the formation of different silicide compounds of Zr thin-film deposited on a 100 μm-thick Si (1 0 0) substrate by dc sputtering. A detailed analysis shows that silicide layers start growing at  ∼246 °C that changes to stable ZrSi2 at 627 °C via some compounds with different stoichiometric ratios of Zr and Si. It is further observed that oxygen starts reacting with Zr at  ∼540 °C but a stoichiometric ZrO2 film is formed after complete consumption of Zr metal at 857 °C. A further rise in temperature changes a part of ZrSi2 to Zr-Silicate. The synchrotron radiation-based grazing incidence x-ray diffraction and x-ray photoelectron spectroscopy studies also corroborate the above findings. Atomic force microscopy is also carried out on the samples. It is evident from the observations that an intermixing and nucleation of Zr and Si occur at lower temperature prior to the formation of the interfacial silicate layer. Zr-Silicate formation takes place only at a higher temperature. (paper)

  16. Energy expenditure in critically ill patients estimated by population-based equations, indirect calorimetry and CO2-based indirect calorimetry

    OpenAIRE

    Rousing, Mark Lillelund; Hahn-Pedersen, Mie Hviid; Andreassen, Steen; Pielmeier, Ulrike; Preiser, Jean-Charles

    2016-01-01

    Background Indirect calorimetry (IC) is the reference method for measurement of energy expenditure (EE) in mechanically ventilated critically ill patients. When IC is unavailable, EE can be calculated by predictive equations or by VCO2-based calorimetry. This study compares the bias, quality and accuracy of these methods. Methods EE was determined by IC over a 30-min period in patients from a mixed medical/postsurgical intensive care unit and compared to seven predictive equations and to VCO2...

  17. Identification of the thermal transitions in potato starch at a low water content as studied by preparative DSC

    NARCIS (Netherlands)

    Steeneken, P.A.M.; Woortman, A.J.J.

    2009-01-01

    The aim of this work was to identify the transitions in the complex DSC profiles of potato starch at a low water content. Preparative DSC involves the thermal processing of samples in stainless steel DSC pans in a way that allows their subsequent structural characterization. The low temperature (LT)

  18. Effects of pH and buffer concentration on the thermal stability of etanercept using DSC and DLS.

    Science.gov (United States)

    Kim, Nam Ah; An, In Bok; Lim, Dae Gon; Lim, Jun Yeul; Lee, Sang Yeol; Shim, Woo Sun; Kang, Nae-Gyu; Jeong, Seong Hoon

    2014-01-01

    The protein size, electrical interaction, and conformational stability of etanercept (marketed as Enbrel®) were examined by thermodynamic and light scattering methods with changing pH and buffer concentration. As pH of etanercept increased from pH 6.6 to 8.6, electrical repulsion in the solution increased, inducing a decrease in protein size. However, the size changed less in high buffer concentration and irreversible aggregation issues were not observed; in contrast, aggregates of about 1000 nm were observed in low buffer concentration at the pH range. Three significant unfolding transitions (Tm) were observed by differential scanning calorimetry (DSC). Unlikely to Tm1, Tm2 and Tm3 were increased as the pH increased. Higher Tm at high buffer concentration was observed, indicating increased conformational stability. The apparent activation energy of unfolding was further investigated since continuous increase of Tm2 and Tm3 was not sufficient to determine optimal conditions. A higher energy barrier was calculated at Tm2 than at Tm3. In addition, the energy barriers were the highest at pH from 7.4 to 7.8 where higher Tm1 was also observed. Therefore, the conformational stability of protein solution significantly changed with pH dependent steric repulsion of neighboring protein molecules. An optimized pH range was obtained that satisfied the stability of all three domains. Electrostatic circumstances and structural interactions resulted in irreversible aggregation at low buffer concentrations and were suppressed by increasing the concentration. Therefore, increased buffer concentration is recommended during protein formulation development, even in the earlier stages of investigation, to avoid protein instability issues.

  19. Mathematical model of cycad cones' thermogenic temperature responses: inverse calorimetry to estimate metabolic heating rates.

    Science.gov (United States)

    Roemer, R B; Booth, D; Bhavsar, A A; Walter, G H; Terry, L I

    2012-12-21

    A mathematical model based on conservation of energy has been developed and used to simulate the temperature responses of cones of the Australian cycads Macrozamia lucida and Macrozamia. macleayi during their daily thermogenic cycle. These cones generate diel midday thermogenic temperature increases as large as 12 °C above ambient during their approximately two week pollination period. The cone temperature response model is shown to accurately predict the cones' temperatures over multiple days as based on simulations of experimental results from 28 thermogenic events from 3 different cones, each simulated for either 9 or 10 sequential days. The verified model is then used as the foundation of a new, parameter estimation based technique (termed inverse calorimetry) that estimates the cones' daily metabolic heating rates from temperature measurements alone. The inverse calorimetry technique's predictions of the major features of the cones' thermogenic metabolism compare favorably with the estimates from conventional respirometry (indirect calorimetry). Because the new technique uses only temperature measurements, and does not require measurements of oxygen consumption, it provides a simple, inexpensive and portable complement to conventional respirometry for estimating metabolic heating rates. It thus provides an additional tool to facilitate field and laboratory investigations of the bio-physics of thermogenic plants.

  20. Perfusion calorimetry in the characterization of solvates forming isomorphic desolvates.

    Science.gov (United States)

    Baronsky, Julia; Preu, Martina; Traeubel, Michael; Urbanetz, Nora Anne

    2011-09-18

    In this study, the potential of perfusion calorimetry in the characterization of solvates forming isomorphic desolvates was investigated. Perfusion calorimetry was used to expose different hydrates forming isomorphic desolvates (emodepside hydrates II-IV, erythromycin A dihydrate and spirapril hydrochloride monohydrate) to stepwise increasing relative vapour pressures (RVP) of water and methanol, respectively, while measuring thermal activity. Furthermore, the suitability of perfusion calorimetry to distinguish the transformation of a desolvate into an isomorphic solvate from the adsorption of solvent molecules to crystal surfaces as well as from solvate formation that is accompanied by structural rearrangement was investigated. Changes in the samples were confirmed using FT-Raman and FT-IR spectroscopy. Perfusion calorimetry indicates the transformation of a desolvate into an isomorphic solvate by a substantial exothermic, peak-shaped heat flow curve at low RVP which reflects the rapid incorporation of solvent molecules by the desolvate to fill the structural voids in the lattice. In contrast, adsorption of solvent molecules to crystal surfaces is associated with distinctly smaller heat changes whereas solvate formation accompanied by structural changes is characterized by an elongated heat flow. Hence, perfusion calorimetry is a valuable tool in the characterization of solvates forming isomorphic desolvates which represents a new field of application for the method.

  1. Combined experimental and density functional theory studies of an organic-inorganic hybrid perovskite.

    Science.gov (United States)

    Kassou, S; El-Mrabet, R; Kaiba, A; Guionneau, P; Belaaraj, A

    2016-04-14

    Single crystals of [C6H5-C2H4-NH3]2ZnCl4 were obtained by slow evaporation at room temperature. Single-Crystal X-Ray Diffraction (SCXRD), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and UV-Visible spectroscopy were used to characterize the crystal structure, and thermal and optical properties, respectively. At 293 K, PEA-ZnCl4 crystallizes in a monoclinic unit-cell in the P21/c space group a = 7.449(2) Å, b = 24.670(3) Å, c = 11.187(2) Å and β = 91.762(5)°, V = 2054.8(2) Å(3) and Z = 4. The DSC and TGA analyses show respectively the presence of two first order reversible phase transitions and a sample thermal stability below 541 K. The optical study reveals that the compound undergoes a direct optical transition and an energy gap about of Eg = 4.46 eV. In parallel, ab initio DFT calculations are performed to study the electronic band structure, to examine electronic density and to calculate the gap energy value. The calculated values are in good agreement with the experimental data.

  2. An investigation into the subambient behavior of aqueous mannitol solutions using differential scanning calorimetry, cold stage microscopy, and X-ray diffractometry.

    Science.gov (United States)

    Kett, Vicky L; Fitzpatrick, Shaun; Cooper, Brett; Craig, Duncan Q M

    2003-09-01

    The subambient behavior of aqueous mannitol solutions is of considerable relevance to the preparation of freeze dried formulations. In this investigation the properties of 3% w/v mannitol solutions were investigated using differential scanning calorimetry (DSC), cold stage microscopy (CSM), and X-ray diffraction (XRD) to identify the thermal transitions and structural transformations undergone by this system. It was found that on cooling from ambient the system formed ice at circa -20 degrees C while a further exotherm was seen at approximately -30 degrees C. Upon reheating an endotherm was seen at circa -30 degrees C followed immediately by an exotherm at circa -25 degrees C. Temperature cycling indicated that the thermal transitions observed upon reheating were not reversible. Modulated temperature DSC (MTDSC) indicated that the transitions observed upon reheating corresponded to a glass transition immediately followed by recrystallization, XRD data showed that recrystallization was into the beta form. Annealing at -35 degrees C for 40 min prior to cooling and reheating resulted in a maximum enthalpy being observed for the reheating exotherm. It is concluded that on cooling 3% w/v aqueous mannitol solutions an amorphous phase is formed that subsequently recrystallises into the beta form. The study has also shown that DSC, CSM, and XRD are useful complementary techniques for the study of frozen systems.

  3. Water absorption of freeze-dried meat at different water activities: a multianalytical approach using sorption isotherm, differential scanning calorimetry, and nuclear magnetic resonance.

    Science.gov (United States)

    Venturi, Luca; Rocculi, Pietro; Cavani, Claudio; Placucci, Giuseppe; Dalla Rosa, Marco; Cremonini, Mauro A

    2007-12-26

    Hydration of freeze-dried chicken breast meat was followed in the water activity range of aw=0.12-0.99 by a multianalytical approach comprising of sorption isotherm, differential scanning calorimetry (DSC), and nuclear magnetic resonance (NMR). The amount of frozen water and the shape of the T2-relaxogram were evaluated at each water content by DSC and NMR, respectively. Data revealed an agreement between sorption isotherm and DSC experiments about the onset of bulk water (aw=0.83-0.86), and NMR detected mobile water starting at aw=0.75. The origin of the short-transverse relaxation time part of the meat NMR signal was also reinvestigated through deuteration experiments and proposed to arise from protons belonging to plasticized matrix structures. It is proved both by D2O experiments and by gravimetry that the extra protons not contributing to the water content in the NMR experiments are about 6.4% of the total proton NMR CPMG signal of meat.

  4. Endoplasmic Reticulum Exit of Golgi-resident Defective for SREBP Cleavage (Dsc) E3 Ligase Complex Requires Its Activity.

    Science.gov (United States)

    Raychaudhuri, Sumana; Espenshade, Peter J

    2015-06-01

    Layers of quality control ensure proper protein folding and complex formation prior to exit from the endoplasmic reticulum. The fission yeast Dsc E3 ligase is a Golgi-localized complex required for sterol regulatory element-binding protein (SREBP) transcription factor activation that shows architectural similarity to endoplasmic reticulum-associated degradation E3 ligases. The Dsc E3 ligase consists of five integral membrane proteins (Dsc1-Dsc5) and functionally interacts with the conserved AAA-ATPase Cdc48. Utilizing an in vitro ubiquitination assay, we demonstrated that Dsc1 has ubiquitin E3 ligase activity that requires the E2 ubiquitin-conjugating enzyme Ubc4. Mutations that specifically block Dsc1-Ubc4 interaction prevent SREBP cleavage, indicating that SREBP activation requires Dsc E3 ligase activity. Surprisingly, Golgi localization of the Dsc E3 ligase complex also requires Dsc1 E3 ligase activity. Analysis of Dsc E3 ligase complex formation, glycosylation, and localization indicated that Dsc1 E3 ligase activity is specifically required for endoplasmic reticulum exit of the complex. These results define enzyme activity-dependent sorting as an autoregulatory mechanism for protein trafficking.

  5. 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. ...

  6. Interlayer thermal conductivity of rubrene measured by ac-calorimetry

    Science.gov (United States)

    Zhang, H.; Brill, J. W.

    2013-07-01

    We have measured the interlayer thermal conductivity of crystals of the organic semiconductor rubrene, using ac-calorimetry. Since ac-calorimetry is most commonly used for measurements of the heat capacity, we include a discussion of its extension for measurements of the transverse thermal conductivity of thin crystals of poor thermal conductors, including the limitations of the technique. For rubrene, we find that the interlayer thermal conductivity, ≈0.7 mW/cm . K, is several times smaller than the (previously measured) in-layer value, but its temperature dependence indicates that the interlayer mean free path is at least a few layers.

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

    Science.gov (United States)

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

    2011-01-01

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

  8. Yeast SREBP cleavage activation requires the Golgi Dsc E3 ligase complex.

    Science.gov (United States)

    Stewart, Emerson V; Nwosu, Christine C; Tong, Zongtian; Roguev, Assen; Cummins, Timothy D; Kim, Dong-Uk; Hayles, Jacqueline; Park, Han-Oh; Hoe, Kwang-Lae; Powell, David W; Krogan, Nevan J; Espenshade, Peter J

    2011-04-22

    Mammalian lipid homeostasis requires proteolytic activation of membrane-bound sterol regulatory element binding protein (SREBP) transcription factors through sequential action of the Golgi Site-1 and Site-2 proteases. Here we report that while SREBP function is conserved in fungi, fission yeast employs a different mechanism for SREBP cleavage. Using genetics and biochemistry, we identified four genes defective for SREBP cleavage, dsc1-4, encoding components of a transmembrane Golgi E3 ligase complex with structural homology to the Hrd1 E3 ligase complex involved in endoplasmic reticulum-associated degradation. The Dsc complex binds SREBP and cleavage requires components of the ubiquitin-proteasome pathway: the E2-conjugating enzyme Ubc4, the Dsc1 RING E3 ligase, and the proteasome. dsc mutants display conserved aggravating genetic interactions with components of the multivesicular body pathway in fission yeast and budding yeast, which lacks SREBP. Together, these data suggest that the Golgi Dsc E3 ligase complex functions in a post-ER pathway for protein degradation.

  9. Comparative SAXS and DSC study on stratum corneum structural organization in an epidermal cell culture model (ROC): impact of cultivation time.

    Science.gov (United States)

    Kuntsche, Judith; Herre, Angela; Fahr, Alfred; Funari, Sérgio S; Garidel, Patrick

    2013-12-18

    Cell cultured skin equivalents present an alternative for dermatological in vitro evaluations of drugs and excipients as they provide the advantage of availability, lower variability and higher assay robustness compared to native skin. For penetration/permeation studies, an adequate stratum corneum barrier similar to that of human stratum corneum is, however, a prerequisite. In this study, the stratum corneum lipid organization in an epidermal cell culture model based on rat epidermal keratinocytes (REK organotypic culture, ROC) was investigated by small-angle X-ray scattering (SAXS) in dependence on ROC cultivation time and in comparison to native human and rat stratum cornea. In addition, the thermal phase behavior was studied by differential scanning calorimetry (DSC) and barrier properties were checked by measurements of the permeability of tritiated water. The development of the barrier of ROC SC obtained at different cultivation times (7, 14 and 21 days at the air-liquid interface) was connected with an increase in structural order of the SC lipids in SAXS measurements: Already cultivation for 14 days at the air-liquid interface resulted overall in a competent SC permeability barrier and SC lipid organization. Cultivation for 21 days resulted in further minor changes in the structural organization of ROC SC. The SAXS patterns of ROC SC had overall large similarities with that of human SC and point to the presence of a long periodicity phase with a repeat distance of about 122Å, e.g. slightly smaller than that determined for human SC in the present study (127Å). Moreover, SAXS results also indicate the presence of covalently bound ceramides, which are crucial for a proper SC barrier, although the corresponding thermal transitions were not clearly detectable by DSC. Due to the competent SC barrier properties and high structural and organizational similarity to that of native human SC, ROC presents a promising alternative for in vitro studies, particularly as

  10. A study of ultra-strength polymer fibers via calorimetry

    Science.gov (United States)

    Egorov, V. M.; Boiko, Yu. M.; Marikhin, V. A.; Myasnikova, L. P.; Radovanova, E. I.

    2016-08-01

    Xerogel reactor powders and supramolecular polyethylene fibers with various degrees of hood have been studied via differential scanning calorimetry. A higher strength of laboratory fibers in comparison with industrial ones is found to be achieved due to a multistage band high-temperature hood that causes the thermodynamic parameters of supramolecular polymer structure.

  11. Warm-up calorimetry of Dewar-Detector Assemblies

    Science.gov (United States)

    Veprik, A.; Shlomovich, B.; Tuito, A.

    2015-12-01

    Boil-off isothermal calorimetry of Dewar-Detector Assemblies (DDA) is a routine part of their Acceptance Testing Procedure. In this approach, the cryogenic liquid coolant (typically LN2) is allowed to naturally boil-off from the Dewar well to the atmosphere through a mass flow meter; the parasitic heat load is then evaluated as the product of the latent heat of vaporization and the "last drop" boil-off rate. An inherent major limitation of this technique is that it may be performed only at the fixed boiling temperature of the chosen liquid coolant. A further drawback is related to the explosive nature of "last drop" boiling, manifesting itself as an uneven flow rate. This especially holds true for advanced High Operational Temperature Dewar-Detector Assemblies, typically featuring short cold fingers and working at 150 K and above. In this work, we adapt the well-known technique of dual-slope calorimetry and show how accurate heat load evaluation may be performed by comparing the slopes of the warm-up thermal transients under different trial added heat loads. Because of the simplicity, accuracy and ability to perform calorimetry literally at any temperature of interest, this technique shows good potential for replacing traditional boil-off calorimetry.

  12. Preparation of Solid Derivatives by Differential Scanning Calorimetry.

    Science.gov (United States)

    Crandall, E. W.; Pennington, Maxine

    1980-01-01

    Describes the preparation of selected aldehydes and ketones, alcohols, amines, phenols, haloalkanes, and tertiaryamines by differential scanning calorimetry. Technique is advantageous because formation of the reaction product occurs and the melting point of the product is obtained on the same sample in a short time with no additional purification…

  13. On the Interpretation of Low Temperature Calorimetry Data

    DEFF Research Database (Denmark)

    Kjeldsen, Ane Mette; Geiker, Mette Rica

    2008-01-01

    The effect of selected factors and phenomena on Low Temperature Calorimetry (LTC) results has been investigated, in order to determine the possibilities and limitations of using LTC for characterisation of the porosity of cement-based materials. LTC was carried out on a model material with mono...

  14. 更胜一筹:Sony DSC-H20

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Sony DSC-H20是H10的后续版本,相比之下新款相机的像素值提高至1010万像素,具备720P、1280×720、30fps高画质录像能力.搭载3英寸、23万像素LCD屏幕。DSC-H20支持双重防抖功能,相机采用10倍光学变焦镜头.

  15. 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.

  16. 触,爱 SONY DSC-T2索尼数码相机

    Institute of Scientific and Technical Information of China (English)

    邢瑜

    2007-01-01

    索尼DSC-T2数码相机是DSC-T1的升级产品.与DSC-T1相比.要小巧秀气了许多.在没有打开镜头的时候,很多人都会误以为它是一个播放器或是小首饰盒之类的物件,无意中DSC-T2迷惑了众人的眼睛。

  17. Differential scanning calorimetry study of glass transition in frozen starch gels.

    Science.gov (United States)

    Tananuwong, Kanitha; Reid, David S

    2004-06-30

    The effects of initial water content, maximum heating temperature, amylopectin crystallinity type, and annealing on the glass transition of starch gels were studied by differential scanning calorimetry (DSC). The glass transition temperatures of the frozen gels measured as the onset (T(g,onset)) or midpoint temperature (T(g,midpoint)), heat capacity change during the glass transition (deltaC(p)), unfrozen water of starch gels, and additional unfrozen water (AUW) arising from gelatinization were reported. The results show that T(g,onset) and T(g,midpoint) of the partially gelatinized gels are independent of the initial water content, while both of the T(g) values of the fully gelatinized gel increase as the initial water content increases. These observations might result from the difference in the level of structural disruption associated with different heating conditions, resulting in different gel structures as well as different concentrations of the sub-T(g) unfrozen matrix. The amylopectin crystallinity type does not greatly affect T(g,onset) and T(g,midpoint) of the gels. Annealing at a temperature near T(g,onset) increases both T(g,onset) and T(g,midpoint) of the gels, possibly due to an increase in the extent of the freeze concentration as evidenced by a decrease in AUW. Annealing results in an increase in the deltaC(p) value of the gels, presumably due to structural relaxation. A devitrification exotherm may be related to AUW. The annealing process decreases AUW, thus also decreasing the size of the exotherm.

  18. Brain Metastases from Different Primary Carcinomas: an Evaluation of DSC MRI Measurements.

    Science.gov (United States)

    Zhang, H; Zhang, G; Oudkerk, M

    2012-03-01

    This study evaluated the roles of different dynamic susceptibility contrast magnetic imaging (DSC MRI) measurements in discriminating between brain metastases derived from four common primary carcinomas. Thirty-seven patients with brain metastases were enrolled. Relative cerebral blood volume (rCBV), cerebral blood flow (rCBF) and relative mean transit time (rMTT) in both tumor and peritumoral edema were measured. Metastases were grouped by their primary tumor (lung, gastrointestinal, breast and renal cell carcinoma). DSC MRI measurements were compared between groups. Mean rCBV, rCBF, rMTT in tumor and peritumoral edema of all brain metastases (n=37) were 2.79 ± 1.73, 2.56 ± 2.11, 1.21 ± 0.48 and 1.05 ± 0.53, 0.86 ± 0.40, 1.99 ± 0.41, respectively. The tumoral rCBV (5.26 ± 1.89) and rCBF (5.32 ± 3.28) of renal metastases were greater than those of the other three metastases (P0.05). Evaluating various DSC MRI measurements can provide complementary hemodynamic information on brain metastases. The tumoral rCBV, rCBF and likely rMTT can help discriminate between brain metastases originating from different primary carcinomas. The peritumoral DSC MRI measurements had limited value in discriminating between brain metastases.

  19. Rapid examination of the kinetic process of intramolecular lactamization of gabapentin using DSC-FTIR

    Energy Technology Data Exchange (ETDEWEB)

    Hsu, C.-H. [Lab. Pharm. Biopharm., Department of Biotechnology, Yuanpei University, Hsin Chu, Taiwan (China); Lin, S.-Y. [Lab. Pharm. Biopharm., Department of Biotechnology, Yuanpei University, Hsin Chu, Taiwan (China)], E-mail: sylin@mail.ypu.edu.tw

    2009-03-20

    The thermal stability and thermodynamics of gabapentin (GBP) in the solid state were investigated by DSC and TG techniques, and FTIR microspectroscopy. The detailed intramolecular lactamization process of GBP to form gabapentin-lactam (GBP-L) was also determined by thermal FTIR microspectroscopy. GBP exhibited a DSC endothermic peak at 169 deg. C. The weight loss in TG curve of GBP suggested that the evaporation process of water liberated via intramolecular lactamization was simultaneously combined with the evaporation process of GBP-L having a DSC endothermic peak at 91 deg. C. A thermal FTIR microspectroscopy clearly evidenced the IR spectra at 3350 cm{sup -1} for water liberated and at 1701 cm{sup -1} for lactam structure formed due to the lactam formation of GBP. This study indicates that the activation energy for combined processes of intramolecular lactamization of GBP and evaporation of GBP-L was about 114.3 {+-} 23.3 kJ/mol, but for the evaporation of GBP-L alone was 76.2 {+-} 1.5 kJ/mol. A powerful simultaneous DSC-FTIR combined technique was easily used to quickly examine the detailed kinetic processes of intramolecular cyclization of GPB and evaporation of GBP-L in the solid state.

  20. Direct Animal Calorimetry, the Underused Gold Standard for Quantifying the Fire of Life*

    OpenAIRE

    Kaiyala, Karl J.; Ramsay, Douglas S.

    2010-01-01

    Direct animal calorimetry, the gold standard method for quantifying animal heat production (HP), has been largely supplanted by respirometric indirect calorimetry owing to the relative ease and ready commercial availability of the latter technique. Direct calorimetry, however, can accurately quantify HP and thus metabolic rate (MR) in both metabolically normal and abnormal states, whereas respirometric indirect calorimetry relies on important assumptions that apparently have never been tested...

  1. Microwave curing of initially compatible epoxy–poly(ethylene terephthalate) blends: DSC kinetic study and nano-structure analysis{sup ☆}

    Energy Technology Data Exchange (ETDEWEB)

    Zvetkov, V.L., E-mail: zvetval@yahoo.com; Simeonova-Ivanova, E.; Djoumaliisky, S.

    2014-11-10

    Graphical abstract: The curves proposed to tabulate the curing regime in microwave field. - Highlights: • The monitoring of the curing process in microwave field is the aim of the study. • We consider an approach to estimate the curing regime in microwave field. • We present physical evidences for obtaining nano-modified epoxy composites. - Abstract: Poly(ethylene terephthalate), PET, dissolved in diglycidyl ether of bisphenol-A epoxy resins, DGEBA, is used as a toughening modifier. Two DGEBA resins in the presence of PET have been cured with the aid of diaminodiphenyl sulfone, DDS, in stoichiometric proportion. The curing process of the system DGEBA with DDS, in the presence of PET in particular, is monitored applying differential scanning calorimetry, DSC, in isothermal mode. The curing data are used to estimate the temperature regime in a microwave, MW, cavity. Physical confirmations for obtaining sub-micro phase separated DGEBA–DDS–PET composites and, in turn, for efficient modifying of the epoxy phase, have been discussed.

  2. The Simulation of the ATLAS Liquid Argon Calorimetry

    CERN Document Server

    Archambault, J P; Carli, T; Costanzo, D; Dell'Acqua, A; Djama, F; Gallas, M; Fincke-Keeler, M; Khakzad, M; Kiryunin, A; Krieger, P; Leltchouk, M; Loch, P; Ma, H; Menke, S; Monnier, E; Nairz, A; Niess, V; Oakham, G; Oram, C; Pospelov, G; Rajagopalan, S; Rimoldi, A; Rousseau, D; Rutherfoord, J; Seligman, W; Soukharev, A; Strízenec, P; Tóth, J; Tsukerman, I; Tsulaia, V; Unal, G; Grahn, K J

    2008-01-01

    In ATLAS, all of the electromagnetic calorimetry and part of the hadronic calorimetry is performed by a calorimeter system using liquid argon as the active material, together with various types of absorbers. The liquid argon calorimeter consists of four subsystems: the electromagnetic barrel and endcap accordion calorimeters; the hadronic endcap calorimeters, and the forward calorimeters. A very accurate geometrical description of these calorimeters is used as input to the Geant 4-based ATLAS simulation, and a careful modelling of the signal development is applied in the generation of hits. Certain types of Monte Carlo truth information ("Calibration Hits") may, additionally, be recorded for calorimeter cells as well as for dead material. This note is a comprehensive reference describing the simulation of the four liquid argon calorimeteter components.

  3. Monitoring assembly of ribonucleoprotein complexes by isothermal titration calorimetry

    OpenAIRE

    Recht, Michael I.; Ryder, Sean P.; Williamson, James R.

    2008-01-01

    Isothermal titration calorimetry (ITC) is a useful technique to study RNA-protein interactions, as it provides the only method by which the thermodynamic parameters of free energy, enthalpy, and entropy can be directly determined. This chapter presents a general procedure for studying RNA-protein interactions using ITC, and gives specific examples for monitoring the binding of Caenorhabditis elegans GLD-1 STAR domain to TGE RNA and the binding of Aquifex aeolicus S6:S18 ribosomal protein hete...

  4. The upgraded CDF front end electronics for calorimetry

    International Nuclear Information System (INIS)

    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

  5. Accurate Measurement of Heat Capacity by Differential Scanning Calorimetry

    Science.gov (United States)

    1984-01-01

    Experience with high quality heat capacity measurement by differential scanning calorimetry is summarized and illustrated, pointing out three major causes of error: (1) incompatible thermal histories of the sample, reference and blank runs; (2) unstable initial and final isotherms; (3) incompatible differences between initial and final isotherm amplitudes for sample, reference and blank runs. Considering these problems, it is shown for the case of polyoxymethylene that accuracies in heat capacity of 0.1 percent may be possible.

  6. Application of kinetic inductance thermometers to x-ray calorimetry

    International Nuclear Information System (INIS)

    A kinetic inductance thermometer is applied to x-ray calorimetry, and its operation over a wide range of frequencies and geometries is discussed. Three amplifier configurations are described, one using a superconducting quantum interference device (SQUID) amplifier, another incorporating an FET amplifier in an amplitude modulated system, and the third, using a tunnel diode frequency modulated oscillator circuit. The predicted performance of each configuration is presented. 13 refs., 6 figs., 1 tab

  7. Depth of calorimetry for SSC [Superconducting Super Collider] experiments

    International Nuclear Information System (INIS)

    The depth of calorimetry required for SSC experiments is investigated using data of hadronic shower development in neutrino detectors and a parameterization of average hadronic shower shapes. The effect of hadronic shower fluctuations is included. A depth of nine to ten proton absorption lengths in iron is found to be sufficient to contain at least 95% of the energy of 95% of 1-TeV jets. 6 refs., 5 figs

  8. Benchmark Thermochemistry for Biologically Relevant Adenine and Cytosine. A Combined Experimental and Theoretical Study.

    Science.gov (United States)

    Emel'yanenko, Vladimir N; Zaitsau, Dzmitry H; Shoifet, Evgeni; Meurer, Florian; Verevkin, Sergey P; Schick, Christoph; Held, Christoph

    2015-09-17

    The thermochemical properties available in the literature for adenine and cytosine are in disarray. A new condensed phase standard (p° = 0.1 MPa) molar enthalpy of formation at T = 298.15 K was measured by using combustion calorimetry. New molar enthalpies of sublimation were derived from the temperature dependence of vapor pressure measured by transpiration and by the quarz-crystal microbalance technique. The heat capacities of crystalline adenine and cytosine were measured by temperature-modulated DSC. Thermodynamic data on adenine and cytosine available in the literature were collected, evaluated, and combined with our experimental results. Thus, the evaluated collection of data together with the new experimental results reported here has helped to resolve contradictions in the available enthalpies of formation. A set of reliable thermochemical data is recommended for adenine and cytosine for further thermochemical calculations. Quantum-chemical calculations of the gas phase molar enthalpies of formation of adenine and cytosine have been performed by using the G4 method and results were in excellent agreement with the recommended experimental data. The standard molar entropies of formation and the standard molar Gibbs functions of formation in crystal and gas state have been calculated. Experimental vapor-pressure data measured in this work were used to estimate pure-component PC-SAFT parameters. This allowed modeling solubility of adenine and cytosine in water over the temperature interval 278-310 K.

  9. 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. PMID:26041218

  10. Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Gordon Center for Integrated Science, 929 E. 57th Street, Chicago, Illinois 60637 (United States); Nash, P. [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Chen, X.Q.; Wei, P. [Materials processing Modeling Division, Shenyang National Laboratory for Materials Science, Institute of Metals Research, 72 Wenhua Road, Shenyang City (China)

    2015-06-05

    Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb{sub 3}Sc{sub 5}(−61.3 ± 2.9); PbTi{sub 4}(−16.6 ± 2.4); Pb{sub 3}Y{sub 5}(−64.8 ± 3.6); Pb{sub 3}Zr{sub 5}(−50.6 ± 3.1); PbNb{sub 3}(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd{sub 3}(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available.

  11. Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

    International Nuclear Information System (INIS)

    Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb3Sc5(−61.3 ± 2.9); PbTi4(−16.6 ± 2.4); Pb3Y5(−64.8 ± 3.6); Pb3Zr5(−50.6 ± 3.1); PbNb3(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd3(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available

  12. Thermal expansivities of peptides, polypeptides and proteins as measured by pressure perturbation calorimetry.

    Science.gov (United States)

    Pandharipande, Pranav P; Makhatadze, George I

    2015-04-01

    The main goal of this work was to provide direct experimental evidence that the expansivity of peptides, polypeptides and proteins as measured by pressure perturbation calorimetry (PPC), can serve as a proxy to characterize relative compactness of proteins, especially the denatured state ensemble. This is very important as currently only small angle X-ray scattering (SAXS), intrinsic viscosity and, to a lesser degree, fluorescence resonance transfer (FRET) experiments are capable of reporting on the compactness of denatured state ensembles. We combined the expansivity measurements with other biophysical methods (far-UV circular dichroism spectroscopy, differential scanning calorimetry, and small angle X-ray scattering). Three case studies of the effects of conformational changes on the expansivity of polypeptides in solution are presented. We have shown that expansivity appears to be insensitive to the helix-coil transition, and appears to reflect the changes in hydration of the side-chains. We also observed that the expansivity is sensitive to the global conformation of the polypeptide chain and thus can be potentially used to probe hydration of different collapsed states of denatured or even intrinsically disordered proteins.

  13. A High-Throughput Biological Calorimetry Core: Steps to Startup, Run, and Maintain a Multiuser Facility.

    Science.gov (United States)

    Yennawar, Neela H; Fecko, Julia A; Showalter, Scott A; Bevilacqua, Philip C

    2016-01-01

    Many labs have conventional calorimeters where denaturation and binding experiments are setup and run one at a time. While these systems are highly informative to biopolymer folding and ligand interaction, they require considerable manual intervention for cleaning and setup. As such, the throughput for such setups is limited typically to a few runs a day. With a large number of experimental parameters to explore including different buffers, macromolecule concentrations, temperatures, ligands, mutants, controls, replicates, and instrument tests, the need for high-throughput automated calorimeters is on the rise. Lower sample volume requirements and reduced user intervention time compared to the manual instruments have improved turnover of calorimetry experiments in a high-throughput format where 25 or more runs can be conducted per day. The cost and efforts to maintain high-throughput equipment typically demands that these instruments be housed in a multiuser core facility. We describe here the steps taken to successfully start and run an automated biological calorimetry facility at Pennsylvania State University. Scientists from various departments at Penn State including Chemistry, Biochemistry and Molecular Biology, Bioengineering, Biology, Food Science, and Chemical Engineering are benefiting from this core facility. Samples studied include proteins, nucleic acids, sugars, lipids, synthetic polymers, small molecules, natural products, and virus capsids. This facility has led to higher throughput of data, which has been leveraged into grant support, attracting new faculty hire and has led to some exciting publications.

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

    Science.gov (United States)

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

    2014-10-01

    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.

  15. Energy dispersive x-ray diffractometry as a tool alternative to differential scanning calorimetry for investigating polymer phase transitions

    International Nuclear Information System (INIS)

    Recently, a technique based on energy dispersive x-ray diffraction has been proposed to follow the polymer phase transitions. However, the potentialities of this method were not clear, as well as the experimental conditions in which it is more convenient than differential scanning calorimetry, generally used for the same purpose. In the present letter, the answer to this question is provided. It is shown that the two methods are complementary, rather than equivalent, the heating rate being the relevant parameter to establish which is preferable. The demonstration of this statement is given through the observation of the complex thermal properties of a reference sample studied in both ways at progressively lower heating rates. The connection between such unusual application of x-ray diffraction and the differential scanning calorimetry is discussed in terms of the two possible definitions of entropy

  16. Thermal degradation of ligno-cellulosic fuels: DSC and TGA studies

    OpenAIRE

    Leroy, Valérie; Cancellieri, Dominique; Leoni, Eric

    2008-01-01

    International audience The scope of this work was to show the utility of thermal analysis and calorimetric experiments to study the thermal oxidative degradation of Mediterranean scrubs. We investigated the thermal degradation of four species; DSC and TGA were used under air sweeping to record oxidative reactions in dynamic conditions. Heat released and mass loss are important data to be measured for wildland fires modelling purpose and fire hazard studies on ligno-cellulosic fuels. Around...

  17. 索尼DSC-S85数码相机试用记

    Institute of Scientific and Technical Information of China (English)

    杨明

    2003-01-01

    @@ Cyber-shot DSC-S85是索尼公司于2001年推出的第一款410万像素Super HAD CCD的数码照相机,但其太传统化的外形设计,几度要毁掉我购买它的信心,不过最终还是把它抱回家,因为是它的品质打动我.

  18. 红外光谱法/差示扫描量热法鉴别氯醚橡胶类型%Analysis of Epichlorohydrin Rubber Type by FTIR and DSC

    Institute of Scientific and Technical Information of China (English)

    姚玉红; 许耀东; 田友峰; 杨登基; 何广德; 陈晋阳

    2014-01-01

    用红外光谱法(FTIR)和差示扫描量热法(DSC)对氯醚橡胶生胶和硫化胶进行表征。结果表明,采用FTIR法,根据Beer-Lambert定律,可以准确鉴别氯醚橡胶生胶类型;采用DSC法测定的氯醚橡胶生胶和硫化胶Tg基本相同,可以以此作为鉴别氯醚橡胶的依据。%The raw rubber and vulcanizate of epichlorohydrin rubber (ECO) were characterized by infrared spectroscopy (FTIR) and differential scanning calorimetry (DSC). The results showed that FTIR could be used for accurate identiifcation of ECO type based on the Beer-Lambert law. DSC results showed that the Tg of raw ECO rubber and vulcanized ECO rubber were basically the same, which could also be used for identiifcation of epichlorohydrin rubber.

  19. Estimation of the nucleation rate by differential scanning calorimetry

    Science.gov (United States)

    Kelton, Kenneth F.

    1992-01-01

    A realistic computer model is presented for calculating the time-dependent volume fraction transformed during the devitrification of glasses, assuming the classical theory of nucleation and continuous growth. Time- and cluster-dependent nucleation rates are calculated by modeling directly the evolving cluster distribution. Statistical overlap in the volume fraction transformed is taken into account using the standard Johnson-Mehl-Avrami formalism. Devitrification behavior under isothermal and nonisothermal conditions is described. The model is used to demonstrate that the recent suggestion by Ray and Day (1990) that nonisothermal DSC studies can be used to determine the temperature for the peak nucleation rate, is qualitatively correct for lithium disilicate, the glass investigated.

  20. Subunit architecture of the Golgi Dsc E3 ligase required for sterol regulatory element-binding protein (SREBP) cleavage in fission yeast.

    Science.gov (United States)

    Lloyd, S Julie-Ann; Raychaudhuri, Sumana; Espenshade, Peter J

    2013-07-19

    The membrane-bound sterol regulatory element-binding protein (SREBP) transcription factors regulate lipogenesis in mammalian cells and are activated through sequential cleavage by the Golgi-localized Site-1 and Site-2 proteases. The mechanism of fission yeast SREBP cleavage is less well defined and, in contrast, requires the Golgi-localized Dsc E3 ligase complex. The Dsc E3 ligase consists of five integral membrane subunits, Dsc1 through Dsc5, and resembles membrane E3 ligases that function in endoplasmic reticulum-associated degradation. Using immunoprecipitation assays and blue native electrophoresis, we determined the subunit architecture for the complex of Dsc1 through Dsc5, showing that the Dsc proteins form subcomplexes and display defined connectivity. Dsc2 is a rhomboid pseudoprotease family member homologous to mammalian UBAC2 and a central component of the Dsc E3 ligase. We identified conservation in the architecture of the Dsc E3 ligase and the multisubunit E3 ligase gp78 in mammals. Specifically, Dsc1-Dsc2-Dsc5 forms a complex resembling gp78-UBAC2-UBXD8. Further characterization of Dsc2 revealed that its C-terminal UBA domain can bind to ubiquitin chains but that the Dsc2 UBA domain is not essential for yeast SREBP cleavage. Based on the ability of rhomboid superfamily members to bind transmembrane proteins, we speculate that Dsc2 functions in SREBP recognition and binding. Homologs of Dsc1 through Dsc4 are required for SREBP cleavage and virulence in the human opportunistic pathogen Aspergillus fumigatus. Thus, these studies advance our organizational understanding of multisubunit E3 ligases involved in endoplasmic reticulum-associated degradation and fungal pathogenesis.

  1. Classification of tumor area using combined DCE and DSC MRI in patients with glioblastoma.

    Science.gov (United States)

    Artzi, Moran; Blumenthal, Deborah T; Bokstein, Felix; Nadav, Guy; Liberman, Gilad; Aizenstein, Orna; Ben Bashat, Dafna

    2015-01-01

    This study proposes an automatic method for identification and quantification of different tissue components: the non-enhanced infiltrative tumor, vasogenic edema and enhanced tumor areas, at the subject level, in patients with glioblastoma (GB) based on dynamic contrast enhancement (DCE) and dynamic susceptibility contrast (DSC) MRI. Nineteen MR data sets, obtained from 12 patients with GB, were included. Seven patients were scanned before and 8 weeks following bevacizumab initiation. Segmentation of the tumor area was performed based on the temporal data of DCE and DSC at the group-level using k-means algorithm, and further at the subject-level using support vector machines algorithm. The obtained components were associated to different tissues types based on their temporal characteristics, calculated perfusion and permeability values and MR-spectroscopy. The method enabled the segmentation of the tumor area into the enhancing permeable component; the non-enhancing hypoperfused component, associated with vasogenic edema; and the non-enhancing hyperperfused component, associated with infiltrative tumor. Good agreement was obtained between the group-level, unsupervised and subject-level, supervised classification results, with significant correlation (r = 0.93, p DSC can be used to differentiate between vasogenic edema and infiltrative tumors in patients with GB, which is of major clinical importance in therapy response assessment.

  2. Yeast sterol regulatory element-binding protein (SREBP) cleavage requires Cdc48 and Dsc5, a ubiquitin regulatory X domain-containing subunit of the Golgi Dsc E3 ligase.

    Science.gov (United States)

    Stewart, Emerson V; Lloyd, S Julie-Ann; Burg, John S; Nwosu, Christine C; Lintner, Robert E; Daza, Riza; Russ, Carsten; Ponchner, Karen; Nusbaum, Chad; Espenshade, Peter J

    2012-01-01

    Schizosaccharomyces pombe Sre1 is a membrane-bound transcription factor that controls adaptation to hypoxia. Like its mammalian homolog, sterol regulatory element-binding protein (SREBP), Sre1 activation requires release from the membrane. However, in fission yeast, this release occurs through a strikingly different mechanism that requires the Golgi Dsc E3 ubiquitin ligase complex and the proteasome. The mechanistic details of Sre1 cleavage, including the link between the Dsc E3 ligase complex and proteasome, are not well understood. Here, we present results of a genetic selection designed to identify additional components required for Sre1 cleavage. From the selection, we identified two new components of the fission yeast SREBP pathway: Dsc5 and Cdc48. The AAA (ATPase associated with diverse cellular activities) ATPase Cdc48 and Dsc5, a ubiquitin regulatory X domain-containing protein, interact with known Dsc complex components and are required for SREBP cleavage. These findings provide a mechanistic link between the Dsc E3 ligase complex and the proteasome in SREBP cleavage and add to a growing list of similarities between the Dsc E3 ligase and membrane E3 ligases involved in endoplasmic reticulum-associated degradation.

  3. Effect of polyglycerol esters additive on palm oil crystallization using focused beam reflectance measurement and differential scanning calorimetry.

    Science.gov (United States)

    Saw, M H; Hishamuddin, E; Chong, C L; Yeoh, C B; Lim, W H

    2017-01-01

    The effect of 0.1-0.7% (w/w) of polyglycerol esters (PGEmix-8) on palm oil crystallization was studied using focused beam reflectance measurement (FBRM) to analyze the in-line changes of crystal size distribution during the crystallization. FBRM results show that 0.1-0.5% (w/w) of PGEmix-8 did not significantly affect nucleation but slightly retarded crystal growth. The use of 0.7% (w/w) additive showed greater heterogeneous nucleation compared to those with lower dosages of additive. Crystal growth was also greatly reduced when using 0.7% (w/w) dosage. The morphological study indicated that the palm oil crystals were smaller and more even in size than when more additive was added. Isothermal crystallization studies using differential scanning calorimetry (DSC) showed increased inhibitory effects on palm oil crystal growth with increasing concentration of PGEmix-8. These results imply that PGEmix-8 is a nucleation enhancing and crystal growth retarding additive in palm oil crystallization at 0.7% (w/w) dosage. PMID:27507476

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

    International Nuclear Information System (INIS)

    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.

  5. 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.

  6. Effect of polyglycerol esters additive on palm oil crystallization using focused beam reflectance measurement and differential scanning calorimetry.

    Science.gov (United States)

    Saw, M H; Hishamuddin, E; Chong, C L; Yeoh, C B; Lim, W H

    2017-01-01

    The effect of 0.1-0.7% (w/w) of polyglycerol esters (PGEmix-8) on palm oil crystallization was studied using focused beam reflectance measurement (FBRM) to analyze the in-line changes of crystal size distribution during the crystallization. FBRM results show that 0.1-0.5% (w/w) of PGEmix-8 did not significantly affect nucleation but slightly retarded crystal growth. The use of 0.7% (w/w) additive showed greater heterogeneous nucleation compared to those with lower dosages of additive. Crystal growth was also greatly reduced when using 0.7% (w/w) dosage. The morphological study indicated that the palm oil crystals were smaller and more even in size than when more additive was added. Isothermal crystallization studies using differential scanning calorimetry (DSC) showed increased inhibitory effects on palm oil crystal growth with increasing concentration of PGEmix-8. These results imply that PGEmix-8 is a nucleation enhancing and crystal growth retarding additive in palm oil crystallization at 0.7% (w/w) dosage.

  7. Differential scanning calorimetry studies of Se85Te15-xPbx (x 4,6,8 and 10) glasses

    International Nuclear Information System (INIS)

    Results of differential scanning calorimetry (DSC) studies of Se85Te15-xPbx (x = 4, 6, 8 and 10) glasses have been reported and discussed in this paper. The results have been analyzed on the basis of structural relaxation equation, Matusita's equation and modified Kissinger's equation. The activation energies of structural relaxation lie in between 226 and 593 kJ/mol. The crystallization growth is found to be one-dimensional for all compositions. The activation energies of crystallization are found to be 100-136 kJ/mol by Matusita's equation while 102-139 kJ/mol by modified Kissinger's equation. The Hruby number (indicator of ease of glass forming and higher stability) is the highest for Se85Te9Pb6 glass while S factor (indicator of resistance to devitrification) is highest for Se85Te7Pb8 glass at all heating rates in our experiment. Further the highest resistance to devitrification has the highest value of structural activation energy and the activation energy of crystallization is maximum for the most stable glass by both Matusita's equation and the modified Kissinger's equation. (author)

  8. Influence of rare earth elements on solidification behavior of a high speed steel for roll using differential scanning calorimetry

    Institute of Scientific and Technical Information of China (English)

    WANG Mingjia; CHEN Lei; WANG Zixi; BAO Er

    2011-01-01

    The influence of rare earths (RE) on solidification behavior of a high speed steel for roll was investigated by using differential scanning calorimetry (DSC) in combination of microstructure analysis.It was found that the sequence of solidification was L→γ,L→γ+MC,L→γ+M2C,L→γ+M6C,respectively.The start temperature and the latent heat liberated by unit mass of L→γ and L→γ+MC increased with increase of RE addition,indicating that RE could trigger the crystallization of the primary γ and the MC carbide more effectively.The promoting effect of RE on the heterogeneous nucleation was believed to be an important cause of this effect.Grain refinement,discontinuous network of eutectic carbides and disperse and finer MC were observed in the samples with RE addition,moreover,RES could act as the heterogeneous nucleus of the MC.RE addition was favorable for stable M6C at the expense of the metastable M2C.

  9. DMSO-Induced Dehydration of DPPC Membranes Studied by X-ray Diffraction, Small-Angle Neutron Scattering, and Calorimetry

    CERN Document Server

    Kiselev, M A; Kisselev, A M; Grabielle-Madelmond, C; Ollivon, M

    1999-01-01

    The influence of dimethyl sulfoxide (DMSO) on membrane thickness, multilamellar repeat distance, and phase transitions of 1,2-dipalmitoyl-sn-glycero-3-phosphatidylcholine (DPPC) was investigated by X-ray diffraction and small-angle neutron scattering (SANS). The differential scanning calorimetry (DSC) study of water freezing and ice melting was performed in the ternary DPPC /DMSO /water and binary DMSO /water systems. The methods applied demonstrated the differences in membrane structure in three sub-regions of the DMSO mole fraction (X_dmso): from 0.0 to 0.3 for the first, from 0.3 to 0.8 for the second, and from 0.9 to 1.0 for the third sub-region. The thickness of the intermembrane solvent at T =20C decreases from 14.4 +/- 1.8 A at X_dmso =0.0 to 7.8 +/- 1.8 A at X_dmso =0.1. The data were used to determine the number of free water molecules in the intermembrane space in the presence of DMSO. The results for 0.0 < X_dmso < 0.3 were explained in the framework of DMSO-induced dehydration of the interme...

  10. Differential scanning calorimetry studies of Se85Te15–Pb ( = 4, 6, 8 and 10) glasses

    Indian Academy of Sciences (India)

    N B Maharajan; N S Saxena; Deepika Bhandari; Mousa M Imran; D D Paudyal

    2000-10-01

    Results of differential scanning calorimetry (DSC) studies of Se85Te15–Pb ( = 4, 6, 8 and 10) glasses have been reported and discussed in this paper. The results have been analyzed on the basis of structural relaxation equation, Matusita’s equation and modified Kissinger’s equation. The activation energies of structural relaxation lie in between 226 and 593 kJ/mol. The crystallization growth is found to be onedimensional for all compositions. The activation energies of crystallization are found to be 100–136 kJ/mol by Matusita’s equation while 102–139 kJ/mol by modified Kissinger’s equation. The Hruby number (indicator of ease of glass forming and higher stability) is the highest for Se85Te9Pb6 glass while S factor (indicator of resistance to devitrification) is highest for Se85Te7Pb8 glass at all heating rates in our experiment. Further the highest resistance to devitrification has the highest value of structural activation energy and the activation energy of crystallization is maximum for the most stable glass by both Matusita’s equation and the modified Kissinger’s equation.

  11. Fabrication of 12% {sup 240}Pu calorimetry standards

    Energy Technology Data Exchange (ETDEWEB)

    Long, S.M.; Hildner, S.; Gutierrez, D.; Mills, C.; Garcia, W.; Gurule, C.

    1995-08-01

    Throughout the DOE complex, laboratories are performing calorimetric assays on items containing high burnup plutonium. These materials contain higher isotopic range and higher wattages than materials previously encountered in vault holdings. Currently, measurement control standards have been limited to utilizing 6% {sup 240}Pu standards. The lower isotopic and wattage value standards do not complement the measurement of the higher burnup material. Participants of the Calorimetry Exchange (CALEX) Program have identified the need for new calorimetric assay standards with a higher wattage and isotopic range. This paper describes the fabrication and verification measurements of the new CALEX standard containing 12% {sup 240}Pu oxide with a wattage of about 6 to 8 watts.

  12. A custom floating point format ADC for LHC calorimetry

    International Nuclear Information System (INIS)

    Due to their large dynamic range (in excess of 16 bits) signals from LHC calorimetry poses severe problems to the shaping and digitizing circuits. We are investigating a solution for an ADC based on a custom floating point format. Since the calorimeter precision is limited, the full dynamic range can be split into 8 positive sub-ranges and 5 negative ones, each with an 8 bits dynamic. The reduced number of bits (8 for the mantissa, 4 for the exponent and 1 for the sign) translates itself into a reduction of the power consumption both of the ADC and of the following digital filtering stages. (authors)

  13. Application of pressure perturbation calorimetry to lipid bilayers.

    OpenAIRE

    Heerklotz, Heiko; Seelig, Joachim

    2002-01-01

    Pressure perturbation calorimetry (PPC) is a new method that measures the heat consumed or released by a sample after a sudden pressure jump. The heat change can be used to derive the thermal volume expansion coefficient, alpha(V), as a function of temperature and, in the case of phase transitions, the volume change, DeltaV, occurring at the phase transition. Here we present the first report on the application of PPC to determine these quantities for lipid bilayers. We measure the volume chan...

  14. Fragment-Based Screening for Enzyme Inhibitors Using Calorimetry.

    Science.gov (United States)

    Recht, Michael I; Nienaber, Vicki; Torres, Francisco E

    2016-01-01

    Isothermal titration calorimetry (ITC) provides a sensitive and accurate means by which to study the thermodynamics of binding reactions. In addition, it enables label-free measurement of enzymatic reactions. The advent of extremely sensitive microcalorimeters have made it increasingly valuable as a tool for hit validation and characterization, but its use in primary screening is hampered by requiring large quantities of reagents and long measurement times. Nanocalorimeters can overcome these limitations of conventional ITC, particularly for screening libraries of 500-1000 compounds such as those encountered in fragment-based lead discovery. This chapter describes how nanocalorimetry and conventional microcalorimetry can be used to screen compound libraries for enzyme inhibitors.

  15. Performance of superconducting transition edge bolometers for infrared photometry and X-ray micro-calorimetry

    CERN Document Server

    Hoevers, H F C; Bruijn, M P; Frericks, M; Kiewiet, F B; Mels, W A; Korte, P D

    1999-01-01

    The performance of voltage biased superconducting transition edge bolometers for infrared photometry and X-ray micro-calorimetry is described. Experimental results for the resistance-temperature curve of the superconducting phase thermometer, the current-voltage characteristic of the bolometer, and its current noise are presented and evaluated. Excess current noise turns out to be present when the bolometers are biased in the superconducting transition. The possible origin of this excess noise is shortly discussed. For the infrared bolometer an NEP of 2 x10 sup - sup 1 sup 7 W/sq root Hz at 270 mK is obtained. The X-ray micro-calorimeter resolution is 60 eV sub F sub W sub H sub M at 155 mK for 5.9 keV X-rays, a factor 2.6 above the thermodynamical limit.

  16. Energetics of methanol and formic acid oxidation on Pt(111): Mechanistic insights from adsorption calorimetry

    Science.gov (United States)

    Silbaugh, Trent L.; Karp, Eric M.; Campbell, Charles T.

    2016-08-01

    The catalytic and electrocatalytic oxidation and reforming of methanol and formic acid have received intense interest due to potential use in direct fuel cells and as prototype models for understanding electrocatalysis. Consequently, the reaction energy diagram (energies of all the adsorbed intermediates and activation energies of all the elementary steps) have been estimated for these reactions on Pt(111) by density functional theory (DFT) in several studies. However, no experimental measurement of these energy diagrams have been reported, nor is there a consensus on the mechanisms. Here, we use energies of key intermediates on Pt(111) from single crystal adsorption calorimetry (SCAC) and temperature programmed desorption (TPD) to build a combined energy diagram for these reactions. It suggests a new pathway involving monodentate formate as a key intermediate, with bidentate formate only being a spectator species that slows the rate. This helps reconcile conflicting proposed mechanisms.

  17. A unified framework based on the binding polynomial for characterizing biological systems by isothermal titration calorimetry.

    Science.gov (United States)

    Vega, Sonia; Abian, Olga; Velazquez-Campoy, Adrian

    2015-04-01

    Isothermal titration calorimetry (ITC) has become the gold-standard technique for studying binding processes due to its high precision and sensitivity, as well as its capability for the simultaneous determination of the association equilibrium constant, the binding enthalpy and the binding stoichiometry. The current widespread use of ITC for biological systems has been facilitated by technical advances and the availability of commercial calorimeters. However, the complexity of data analysis for non-standard models is one of the most significant drawbacks in ITC. Many models for studying macromolecular interactions can be found in the literature, but it looks like each biological system requires specific modeling and data analysis approaches. The aim of this article is to solve this lack of unity and provide a unified methodological framework for studying binding interactions by ITC that can be applied to any experimental system. The apparent complexity of this methodology, based on the binding polynomial, is overcome by its easy generalization to complex systems.

  18. Evaluation of aluminosilicate glass sintering during differential scanning calorimetry

    International Nuclear Information System (INIS)

    In this work a difference in the baseline in differential scanning calorimetry analyses, observed in a work where aluminosilicate glasses microspheres containing Ho were studied for application in selective internal radiotherapy as hepatocellular carcinoma treatment, was studied. The glasses with nominal composition 53,7 SiO2 .10,5 Al2O3 . 35,8 MgO in %mol were produced from traditional melting. The first obtained were milled and sieved in the range of 45 a 63 μm. The material was used to produce glass microspheres by the gravitational fall method. The glass powder and the microspheres were characterized by X ray fluorescence spectrometry, laser diffraction, X ray diffraction, differential scanning calorimetry, differential thermal analysis, thermogravimetry, mass spectrometry, and scanning electron microscopy. After the thermal analyses, pellets were formed in the crucibles and were analyzed by scanning electron microscopy, X ray diffraction, and He pycnometry. The difference in the baseline was associated to the viscous flow sintering process and happens because of the decrease in the detected heat flow due to the sample shrinkage. Other events as concurrent crystallization with the sintering process were also studied. (author)

  19. Entalpia reticular, entalpia de fusão e temperatura de fusão de adutos: algumas correlações empíricas utilizando DSC

    OpenAIRE

    Farias Robson Fernandes de

    1999-01-01

    By using DSC data is shown that there are empirical correlations between lattice enthalpy, melting enthalpy and the temperature of melting for adducts, and that is possible, using only a single DSC curve, estimate the value of DM Hmq.

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

    Science.gov (United States)

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

    2012-01-01

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

  1. 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)

    Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C xH(2x+1)OSO3Li (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 xH(2x+1)OSO3Na and n-C xH(2x+1)OSO3K (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 18H37OSO3Li and n-C 20H41OSO3Li salts, each melting point produced a small ΔSmp value compared with the total entropy change in the solid phases (ΔStr1+ΔStr2). 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 18H37OSO3Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals

  2. DTA and DSC study on the effect of mechanical dispersion on poly(tetrafluorethylene properties

    Directory of Open Access Journals (Sweden)

    Dumitraşa Mihai

    2014-12-01

    Full Text Available Poly(tetrafluorethylene particles were obtained by mechanical processing of the formed polymer (Teflon bar. In order to assess the effect of mechanical wear on polymer properties, their melting and crystallization behaviour was investigated by DSC and DTA, and the results were compared to the ones obtained for the native polymer. An increase of the crystallinity degree and an accentuated decrease of the average molecular weight were found for the samples submitted to mechanical wear, as a result of mechanical degradation of the polymer

  3. DSC study on temperature memory effect of NiTi shape memory alloy

    Institute of Scientific and Technical Information of China (English)

    N. LIU; W. M. HUANG

    2006-01-01

    A systematic study on the temperature memory effect (TME) in a polycrystalline NiTi shape memory alloy was presented. The investigation was carried out through a series of differential scanning calorimeter (DSC) tests. Two types of tests were conducted,namely single-step test and multi-step test. The influence of the step temperature on the peak/trough temperatures in the subsequent heating process and the associated energy absorption/release in the phase transformations was investigated. Using a simple theoretical model,the exact mechanism behind TME was studied.

  4. XRD and TG-DSC analysis of the silicon carbide-palladium reaction

    OpenAIRE

    2014-01-01

    The attack of palladium on silicon carbide was investigated using high purity powders of α-SiC and palladium blended to produce a mixture with composition of 95 at.% SiC and 5 at.% Pd and cold pressed to pellets. The palladium silicon carbide reaction was studied by thermogravimetry (TG) and differential scanning calorimentry (DSC), whereas the phase composition of the specimens was studied using X-ray diffractometry (XRD) before and after thermoscans. X-ray powder analysis (XRD) was employed...

  5. 轻薄易用动你心——索尼DSC-T5

    Institute of Scientific and Technical Information of China (English)

    赵欣

    2005-01-01

    作为拥有目前世界轻薄机身记录的DSC—T7的下一代机型,DSC—T5并不刻意再在“薄”字上做文章,却走一条更时尚.更易用的道路。从名字上也可以看出.DSC-T5并没有要超越DSC—T7的意思.DSC—T5将以更适合大众使用的形象出现。

  6. DSC method: Determination of amorphous fraction in solid dosage and fragility

    Science.gov (United States)

    Saini, Manoj K.

    2015-06-01

    We have used Differential Scanning Calorimeter (DSC) method to quantifying the amorphous content in solid dosage of a commonly used drugs namely mephenesin. The glass transition temperature (Tg) of supercooled liquid sample and melting temperature (Tm) of as received sample are found to be 232.2 K and 343.1 K respectively. The "fragility index" of mephenesin has been discussed in detail using the coupling model (m = 250(± 30) - 320βKWW) and compared with acetaminophen and methocarbamol. The sample studied here is found to be kinetically strong in comparison.

  7. STUDY ON THE SHOCK WAVE CRYSTALLIZATION OF AMORPHOUS ALLOYS BY DSC

    Institute of Scientific and Technical Information of China (English)

    H.Y. Zhao; H. Wang; Q.J. Liu; J.D. Kan; Z.Q. Liu

    2002-01-01

    Shock wave and annealing crystallization of amorphous alloys FeSiB, FeMoSiB andFeCuNbSiB were studied by isothermal and non-isothermal DSC technique. It wasfound that the shock wave crystallization is very perfect, the fraction crystallized isvery close to 100%, though the period of crystallization is very short, only about10-4-10-6 s. Their produced phases differ from the parent phase in structure andcomposition. The high velocity of the transformation is very difficult to explain by thediffusion theory of solid state phase transition.

  8. A scanning AC calorimetry technique for the analysis of nano-scale quantities of materials

    OpenAIRE

    Vlassak, Joost J.; Xiao, Kechao; John M. Gregoire; McCluskey, Patrick J.

    2012-01-01

    We present a scanning AC nanocalorimetry method that enables calorimetry measurements at heating and cooling rates that vary from isothermal to \\(2×10^3 K/s\\), thus bridging the gap between traditional scanning calorimetry of bulk materials and nanocalorimetry. The method relies on a micromachined nanocalorimetry sensor with a serpentine heating element that is sensitive enough to make measurements on thin-film samples and composition libraries. The ability to perform calorimetry over such a ...

  9. Application of an open circuit indirect calorimetry system for gaseous exchange measurements in small ruminant nutrition

    OpenAIRE

    CRISCIONI FERREIRA, PATRICIA FABIOLA

    2016-01-01

    [EN] The main objective of this Thesis was to study the energy metabolism in small ruminants under different nutrition sceneries. As methodology we utilized indirect calorimetry instead of direct calorimetry or feeding trials. Within indirect calorimetry we worked with a portable open circuit gas exchange system with a head hood. This open circuit respiration system permitted completed the whole energy balance and evaluate the efficiency of utilization of the energy of the diet for different ...

  10. Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime Using Controlled Calorimetry

    International Nuclear Information System (INIS)

    A comprehensive description of the accomplishments of the DOE grant titled, ''Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime using Controlled Calorimetry''

  11. A novel photomultiplier tube for calorimetry at the SSC

    International Nuclear Information System (INIS)

    A silicon target photomultiplier tube with an anode consisting of a large area Avalanche Photodiode (APD) has been developed. The tube combines the advantages of an avalanche photodiode, excellent linearity and large dynamic range, with the properties of a phototube. The tube structure is proximity focussing, which is not affected by high magnetic fields approximately aligned with the axis. The high linearity makes this device attractive for calorimetry at the SSC. The extension of this concept to an APD array will provide a cost effective fiber readout for both digital (tracking) and analogue applications. A tube equipped with an APD array is being developed currently as a readout option for the SDC Shower Maximum Detector

  12. DETECTION OF Tg BY MODULATED DIFFERENTIAL SCANNING CALORIMETRY

    Institute of Scientific and Technical Information of China (English)

    1998-01-01

    The glassy transition of the polyethylene terephthalate (PET) samples which have been subjected to solvent induced crystallization (SINC) was investigated by modulated differential scanning calorimetry (MDSC) and density measurement. The differential of heat capacity signal, d Cp/dT from MDSC, was used to monitor the SINC process. It reveals that the Tg temperature shifts to higher value with the advancement of SINC. When the toluene-immersing time was longer (168h), the detection of Tg become more difficult, because some smaller peaks emerged at the lower temperatures and these are explained as the movement of small segments in the amorphous region. These observed results are due to the morphology and structure introduced by the SINC process.

  13. Isothermal titration calorimetry of ion-coupled membrane transporters.

    Science.gov (United States)

    Boudker, Olga; Oh, SeCheol

    2015-04-01

    Binding of ligands, ranging from proteins to ions, to membrane proteins is associated with absorption or release of heat that can be detected by isothermal titration calorimetry (ITC). Such measurements not only provide binding affinities but also afford direct access to thermodynamic parameters of binding--enthalpy, entropy and heat capacity. These parameters can be interpreted in a structural context, allow discrimination between different binding mechanisms and guide drug design. In this review, we introduce advantages and limitations of ITC as a methodology to study molecular interactions of membrane proteins. We further describe case studies where ITC was used to analyze thermodynamic linkage between ions and substrates in ion-coupled transporters. Similar type of linkage analysis will likely be applicable to a wide range of transporters, channels, and receptors.

  14. Applications of isothermal titration calorimetry in protein science

    Institute of Scientific and Technical Information of China (English)

    Yi Liang

    2008-01-01

    During the past decade,isothermal titration calorimetry (ITC)has developed from a specialist method for understanding molecular interactions and other biological processes within cells to a more robust,widely used method.Nowadays,ITC is used to investigate all types of protein interactions,including protein-protein interactions,protein-DNA/RNA interactions,protein-small molecule interactions and enzyme kinetics;it provides a direct route to the complete thermodynamic characterization of protein interactions.This review concentrates on the new applications of ITC in protein folding and misfolding,its traditional application in protein interactions,and an overview of what can be achieved in the field of protein science using this method and what developments are likely to occur in the near future.Also,this review discusses some new developments of ITC method in protein science,such as the reverse titration of ITC and the displacement method of ITC.

  15. Isothermal titration calorimetry of membrane proteins - progress and challenges.

    Science.gov (United States)

    Rajarathnam, Krishna; Rösgen, Jörg

    2014-01-01

    Integral membrane proteins, including G protein-coupled receptors (GPCR) and ion channels, mediate diverse biological functions that are crucial to all aspects of life. The knowledge of the molecular mechanisms, and in particular, the thermodynamic basis of the binding interactions of the extracellular ligands and intracellular effector proteins is essential to understand the workings of these remarkable nanomachines. In this review, we describe how isothermal titration calorimetry (ITC) can be effectively used to gain valuable insights into the thermodynamic signatures (enthalpy, entropy, affinity, and stoichiometry), which would be most useful for drug discovery studies, considering that more than 30% of the current drugs target membrane proteins. This article is part of a Special Issue entitled: Structural and biophysical characterisation of membrane protein-ligand binding.

  16. Hydroxylamine nitrate self-catalytic kinetics study with adiabatic calorimetry.

    Science.gov (United States)

    Liu, Lijun; Wei, Chunyang; Guo, Yuyan; Rogers, William J; Sam Mannan, M

    2009-03-15

    Hydroxylamine nitrate (HAN) is an important member of the hydroxylamine compound family with applications that include equipment decontamination in the nuclear industry and aqueous or solid propellants. Due to its instability and autocatalytic behavior, HAN has been involved in several incidents at the Hanford and Savannah River Site (SRS) [Technical Report on Hydroxylamine Nitrate, US Department of Energy, 1998]. Much research has been conducted on HAN in different areas, such as combustion mechanism, decomposition mechanism, and runaway behavior. However, the autocatalytic decomposition behavior of HAN at runaway stage has not been fully addressed due to its highly exothermic and rapid decomposition behavior. This work is focused on extracting HAN autocatalytic kinetics and analyzing HAN critical behavior from adiabatic calorimetry measurements. A lumped autocatalytic kinetic model for HAN and associated model parameters are determined. Also the storage and handling critical conditions of diluted HAN solution without metal presence are quantified.

  17. Particle flow calorimetry at the international linear collider

    Indian Academy of Sciences (India)

    Mark A Thomson

    2007-12-01

    One of the most important requirements for a detector at the ILC is good jet energy resolution. It is widely believed that the particle flow approach to calorimetry is the key to achieving the goal of $0.3/\\sqrt{E(GeV)}$. This paper describes the current performance of the PandoraPFA particle flow algorithm. For 45 GeV jets in the Tesla TDR detector concept, the ILC jet energy resolution goal is reached. At higher energies the jet energy resolution becomes worse and can be described by the empirical expression: $_{E}/E ≈ 0.265/\\sqrt{E(GeV)} + 1.2 times 10^{-4} E(GeV)$.

  18. NEUTRON-ENHANCED CALORIMETRY FOR HADRONS (NECH): FINAL REPORT

    Energy Technology Data Exchange (ETDEWEB)

    Andrew Stroud, Lee Sawyer

    2012-08-31

    We present the results of a project to apply scintillator technology recently developed at Louisiana Tech University to hadronic calorimetry. In particular, we developed a prototype calorimeter module incorporating scintillator embedded with metal oxide nanoparticles as the active layers. These metal oxide nanoparticles of gadolinium oxide, have high cross-sections for interactions with slow neutrons. As a part fo this research project, we have developed a novel method for producing plastic scintillators with metal oxide nanoparticles evenly distributed through the plastic without aggregation.We will test the performance of the calorimeter module in test beam and with a neutron source, in order to measure the response to the neutron component of hadronic showers. We will supplement our detector prototyping activities with detailed studies of the effect of neutron component on the resolution of hadronic energy measurements, particular in the next generation of particle flow calorimeters.

  19. Novel investigation of enzymatic biodiesel reaction by isothermal calorimetry

    DEFF Research Database (Denmark)

    Søtoft, Lene Fjerbaek; Westh, Peter; Christensen, Knud V.;

    2010-01-01

    Isothermal calorimetry (ITC) was used to investigate solvent-free enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by immobilized lipase Novozym 435 at 40 °C. The aim of the study was to determine reaction enthalpy for the enzymatic...... transesterification and to elucidate the mass transfer and energetic processes taking place. Based on the measured enthalpy and composition change in the system, the heat of reaction at 40 °C for the two systems was determined as −9.8 ± 0.9 kJ/mole biodiesel formed from rapeseed oil and methanol, and −9.3 ± 0.7 k...

  20. Thermal stability of the DSC ruthenium dye C106 in robust electrolytes

    DEFF Research Database (Denmark)

    Lund, Torben; Phuong, Nguyen Tuyet; Pechy, Peter;

    2014-01-01

    the dye from the TiO2 particles and analyzed its by HPLC coupled to UV/Vis and electro spray mass spectrometry. Samples prepared in the glove box gave the highest stability with a steady state photo anode surface concentration of 80% C106 intact and the remaining ∼20% being the N-butylbenzimidazole (NBB......) substitution products 3 and 4 formed by replacement of the thiocyanate ligand by NBB after 1500 h of heating at 80 °C. Samples prepared under ambient conditions gave a steady state C106 concentration of 60% of the initial value and 40% substitution products. The C106 degradation was found to be independent...... of the degree of dye loading of the TiO2 particles and the ratio between the amount of dyed TiO2 particles and electrolyte volume. Assuming that this substitution is the predominant loss mechanism in a DSC during thermal stress, we estimate the reduction in the DSC efficiency after long term heat to be 12...

  1. Interaction of formin FH2 with skeletal muscle actin. EPR and DSC studies.

    Science.gov (United States)

    Kupi, Tünde; Gróf, Pál; Nyitrai, Miklós; Belágyi, József

    2013-10-01

    Formins are highly conserved proteins that are essential in the formation and regulation of the actin cytoskeleton. The formin homology 2 (FH2) domain is responsible for actin binding and acts as an important nucleating factor in eukaryotic cells. In this work EPR and DSC were used to investigate the properties of the mDia1-FH2 formin fragment and its interaction with actin. MDia1-FH2 was labeled with a maleimide spin probe (MSL). EPR results suggested that the MSL was attached to a single SH group in the FH2. In DSC and temperature-dependent EPR experiments we observed that mDia1-FH2 has a flexible structure and observed a major temperature-induced conformational change at 41 °C. The results also confirmed the previous observation obtained by fluorescence methods that formin binding can destabilize the structure of actin filaments. In the EPR experiments the intermolecular connection between the monomers of formin dimers proved to be flexible. Considering the complex molecular mechanisms underlying the cellular roles of formins this internal flexibility of the dimers is probably important for manifestation of their biological functions.

  2. Efficient Isothermal Titration Calorimetry Technique Identifies Direct Interaction of Small Molecule Inhibitors with the Target Protein.

    Science.gov (United States)

    Gal, Maayan; Bloch, Itai; Shechter, Nelia; Romanenko, Olga; Shir, Ofer M

    2016-01-01

    Protein-protein interactions (PPI) play a critical role in regulating many cellular processes. Finding novel PPI inhibitors that interfere with specific binding of two proteins is considered a great challenge, mainly due to the complexity involved in characterizing multi-molecular systems and limited understanding of the physical principles governing PPIs. Here we show that the combination of virtual screening techniques, which are capable of filtering a large library of potential small molecule inhibitors, and a unique secondary screening by isothermal titration calorimetry, a label-free method capable of observing direct interactions, is an efficient tool for finding such an inhibitor. In this study we applied this strategy in a search for a small molecule capable of interfering with the interaction of the tumor-suppressor p53 and the E3-ligase MDM2. We virtually screened a library of 15 million small molecules that were filtered to a final set of 80 virtual hits. Our in vitro experimental assay, designed to validate the activity of mixtures of compounds by isothermal titration calorimetry, was used to identify an active molecule against MDM2. At the end of the process the small molecule (4S,7R)-4-(4-chlorophenyl)-5-hydroxy-2,7-dimethyl-N-(6-methylpyridin-2-yl)-4,6,7,8 tetrahydrIoquinoline-3-carboxamide was found to bind MDM2 with a dissociation constant of ~2 µM. Following the identification of this single bioactive compound, spectroscopic measurements were used to further characterize the interaction of the small molecule with the target protein. 2D NMR spectroscopy was used to map the binding region of the small molecule, and fluorescence polarization measurement confirmed that it indeed competes with p53.

  3. Applications of Immersion Calorimetry in Dubinin’s Theory and Electrochemistry

    OpenAIRE

    Stoeckli, Fritz; Centeno, Teresa A.

    2008-01-01

    This study shows that immersion calorimetry is a useful technique which simplifies considerably the analysis of porosity and chemical nature of activated carbons. The characterization of activated carbons in the general theoretical framework of Dubinin's theory with its extensions to calorimetry and adsorption from solutions allows the identification of some key parameters for the performance of these materials in electrochemical capacitors.

  4. DSC and conductivity studies on PVA based proton conducting gel electrolytes

    Indian Academy of Sciences (India)

    S L Agrawal; Arvind Awadhia

    2004-12-01

    An attempt has been made in the present work to prepare polyvinyl alcohol (PVA) based proton conducting gel electrolytes in ammonium thiocyanate (NH4SCN) solution and characterize them. DSC studies affirm the formation of gels along with the presence of partial complexes. The cole–cole plots exhibit maximum ionic conductivity (2.58 × 10-3 S cm-1) for gel samples containing 6 wt% of PVA. The conductivity of gel electrolytes exhibit liquid like nature at low polymer concentrations while the behaviour is seen to be affected by the formation of PVA–NH4SCN complexes upon increase in polymer content beyond 5 wt%. Temperature dependence of ionic conductivity exhibits VTF behaviour.

  5. Comparison of dual-echo DSC-MRI- and DCE-MRI-derived contrast agent kinetic parameters.

    Science.gov (United States)

    Quarles, C Chad; Gore, John C; Xu, Lei; Yankeelov, Thomas E

    2012-09-01

    The application of dynamic susceptibility contrast (DSC) MRI methods to assess brain tumors is often confounded by the extravasation of contrast agent (CA). Disruption of the blood-brain barrier allows CA to leak out of the vasculature leading to additional T(1), T(2) and T(2) relaxation effects in the extravascular space, thereby affecting the signal intensity time course in a complex manner. The goal of this study was to validate a dual-echo DSC-MRI approach that separates and quantifies the T(1) and T(2) contributions to the acquired signal and enables the estimation of the volume transfer constant, K(trans), and the volume fraction of the extravascular extracellular space, v(e). To test the validity of this approach, DSC-MRI- and dynamic contrast enhanced (DCE) MRI-derived K(trans) and v(e) estimates were spatially compared in both 9L and C6 rat brain tumor models. A high degree of correlation (concordance correlation coefficients >0.83, Pearson's r>0.84) and agreement was found between the DSC-MRI- and DCE-MRI-derived measurements. These results indicate that dual-echo DSC-MRI can be used to simultaneously extract reliable DCE-MRI kinetic parameters in brain tumors in addition to conventional blood volume and blood flow metrics.

  6. Front-End Electronics in calorimetry: from LHC to ILC

    Energy Technology Data Exchange (ETDEWEB)

    De La Taille, Ch.

    2009-09-15

    This report summarizes the electronics developments for liquid argon calorimeter read-out at LHC and the development carried out in the framework of the CALICE collaboration for those of the future linear collider (ILC). It also includes chips designed for multi-anode photomultipliers (MaPMT) used in the OPERA experiment or on ATLAS luminometer, which also find applications in medical imaging. Started in the early 90's, the development for ATLAS calorimetry was extremely challenging in terms of readout speed, radiation tolerance and measurement accuracy. The high speed has required a new approach using current-sensitive preamplifiers instead of charge sensitive ones and the redefinition of noise performance in terms of ENI. The preamplifiers developed at Orsay and the monolithic shapers are described in Chapter 1, including considerations of digital filtering, which was a new technique in our field. Chapter 2 is dedicated to the calibration system, designed and built by Orsay, for which the high performance and accuracy necessitated in-depth studies. The 3. chapter closes the studies for ATLAS with a summary of the detector measurements which had to be carried out on the 200 000 channels in order to understand and model the detector and achieve everywhere the accuracy and uniformity at per-cent level. These developments for ATLAS ended in 2004, although parallel work was also carried out for the NA48 and DO calorimeters which are not detailed here. The next generation of collider will require a new generation of calorimeters, much more granular, referred to as 'imaging calorimetry' with embedded read-out electronics. The ASICs developed for this purpose in the framework of the CALICE collaboration are described in Chapter 4. They integrate all the functionalities of amplification, digitization and read-out making them complex 'System-On-Chip' circuits extremely efficient that find many other applications. A family of 3 chips reads out the

  7. Estimation of Critical Temperature of Thermal Explosion for Nitrosubstituted Azetidines Using Non-isothermal DSC

    Institute of Scientific and Technical Information of China (English)

    HU, Rongzu; ZHAO, Fengqi; GAO, Hongxu; ZHANG, Jiaoqiang; ZHANG, Hai; MA, Haixia

    2009-01-01

    Based on reasonable hypothesis, two general expressions and their six derived formulae for estimating the critical temperature (T_b) of thermal explosion for energetic materials (EM) were derived from the Semenov's thermal explosion theory and eight non-isothermal kinetic equations. We can easily obtain the values of the initial temperature (T_(0i)) at which DSC curve deviates from the baseline of the non-isothermal DSC curve of EM, the onset temperature (T_(ei)), the exothermic decomposition reaction kinetic parameters and the values of T_(00) and T_(e0) from the equation T_(0i or ei)=T_(00 or e0)+α_1β_i+α_2β_i~2+…+α_(L-2)β_i~(L-2), i=1,2,…,L and then calculate the values of T_b by the six derived formulae. The T_b values for seven nitrosubstituted azetidines, 3,3-dinitroazetidinium nitrate (1), 3,3-dinitroazetidinium picrate (2), 3,3-dinitroazetidinium-3-nitro-1,2,4-triazol-5-onate (3), 1,3-bis(3',3'-dinitro-azetidine group)-2,2-dinitropropane (4), 1-(2',2',2'-trinitroethyi)-3,3-dinitroazetidine (5), 3,3-dinitroazetidinium perchiorate (6) and 1-(3',Y-dinitroazetidineyl)-2,2-dinitropropane (7), obtained with the six derived formulae are agreeable to each other, whose differences are within 1.5%. The results indicate that the heat-resistance stability of the seven nitrosubstituted azetidines decreases in the order 6>7>5>4>3>2>1.

  8. 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.

  9. 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.

  10. Isothermal titration calorimetry: A thermodynamic interpretation of measurements

    International Nuclear Information System (INIS)

    Highlights: ► Literature review shows that many ITC utilizations are based on empirical rules. ► A proper and rigorous thermodynamic interpretation of heats of titration is proposed. ► Heats of titration are independent of the cell type using infinitesimal titrations. ► Heats of interaction between solutes require only two different titration runs. - Abstract: Isothermal titration calorimeters have been developed and in use since the 1960s and the number of applications based on empirical rules to use them steadily increases. In this paper a rigorous study of the physical interpretation of the titration heat and the thermodynamic framework underlying isothermal titration calorimetry are proposed. For infinitesimal titrations, the titration heat is independent of the cell type employed, and the interpretation of the titration heat depends on the titrant composition and on the experiment type. Moreover, for the study of the interaction between two solutes in solution, only a combination of two experiments is necessary, and the result is interpreted as the partial enthalpy of interaction at infinite dilution of the solute contained in the titrant solution.

  11. Combined Forward Calorimetry Option for Phase II CMS Endcap Upgrade

    International Nuclear Information System (INIS)

    Traditionally, EM and HAD compartments are thought to be separate and are often optimized individually. However, it is possible to optimize a robust and economical combined calorimeter system for myriad physics objectives. By employing event-by-event compensation afforded by the dual-readout technique, we have shown that excellent jet performance can be attained with a longitudinally un-segmented calorimeter that is calibrated only with electrons. In addition, the linear hadronic energy scale renders complex off-line correction schemes unnecessary. The proposed replacement of the CMS EE and HE calorimeters with a single Combined Forward Calorimeter (CFC) shows excellent jet performance complemented by good EM object detection. In this paper, we give brief snapshots on basic design criteria, timing characteristics of Cherenkov and scintillation pulses, trigger generation criteria and performance under high radiation fields. Although CMS has recently chosen different technologies for its endcap calorimetry in Phase II, the concepts developed here are likely to remain valuable for some time to come

  12. Applying fast calorimetry on a spent nuclear fuel calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Liljenfeldt, Henrik [Swedish Nuclear Fuel and Waste Management (Sweden); Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Uppsala Univ. (Sweden)

    2015-04-15

    Recently at Los Alamos National Laboratory, sophisticated prediction algorithms have been considered for the use of calorimetry for treaty verification. These algorithms aim to predict the equilibrium temperature based on early data and therefore be able to shorten the measurement time while maintaining good accuracy. The algorithms have been implemented in MATLAB and applied on existing equilibrium measurements from a spent nuclear fuel calorimeter located at the Swedish nuclear fuel interim storage facility. The results show significant improvements in measurement time in the order of 15 to 50 compared to equilibrium measurements, but cannot predict the heat accurately in less time than the currently used temperature increase method can. This Is both due to uncertainties in the calibration of the method as well as identified design features of the calorimeter that limits the usefulness of equilibrium type measurements. The conclusions of these findings are discussed, and suggestions of both improvements of the current calorimeter as well as what to keep in mind in a new design are given.

  13. Characterization of protein-protein interactions by isothermal titration calorimetry.

    Science.gov (United States)

    Velazquez-Campoy, Adrian; Leavitt, Stephanie A; Freire, Ernesto

    2015-01-01

    The analysis of protein-protein interactions has attracted the attention of many researchers from both a fundamental point of view and a practical point of view. From a fundamental point of view, the development of an understanding of the signaling events triggered by the interaction of two or more proteins provides key information to elucidate the functioning of many cell processes. From a practical point of view, understanding protein-protein interactions at a quantitative level provides the foundation for the development of antagonists or agonists of those interactions. Isothermal Titration Calorimetry (ITC) is the only technique with the capability of measuring not only binding affinity but the enthalpic and entropic components that define affinity. Over the years, isothermal titration calorimeters have evolved in sensitivity and accuracy. Today, TA Instruments and MicroCal market instruments with the performance required to evaluate protein-protein interactions. In this methods paper, we describe general procedures to analyze heterodimeric (porcine pancreatic trypsin binding to soybean trypsin inhibitor) and homodimeric (bovine pancreatic α-chymotrypsin) protein associations by ITC.

  14. ANALYSIS OF BRANCHING DISTRIBUTION IN POLYETHYLENES BY DIFFERENTIAL SCANNING CALORIMETRY

    Institute of Scientific and Technical Information of China (English)

    Robert Shanks; Fei Chen; Gandara Amarasinghe

    2003-01-01

    Short chain branching has been characterized using thermal fractionation, a stepwise isothermal crystallization technique, followed by a melting analysis scan using differential scanning calorimetry. Short chain branching distribution was also characterized by a continuous slow cooling crystallization, followed by a melting analysis scan. Four different polyethylenes were studied: Ziegler-Natta gas phase, Ziegler-Natta solution, metallocene, constrained-geometry single site catalyzed polyethylenes. The branching distribution was calculated from a calibration of branch content with melting temperature. The lamellar thickness was calculated based on the thermodynamic melting temperature of each polyethylene and the surface free energy of the crystal face. The branching distribution and lamellar thickness distribution were used to calculate weight average branch content, mean lamellar thickness, and a branch dispersity index. The results for the branch content were in good agreement with the known comonomer content of the polyethylenes. A limitation was that high branch content polyethylenes did not reach their potential crystallization at ambient temperatures. Cooling to sub-ambient was necessary to equilibrate the crystallization, but melting temperature versus branch content was not applicable after cooling to below ambient because the calibration data were not performed in this way.

  15. Measuring the Kinetics of Molecular Association by Isothermal Titration Calorimetry.

    Science.gov (United States)

    Vander Meulen, Kirk A; Horowitz, Scott; Trievel, Raymond C; Butcher, Samuel E

    2016-01-01

    The real-time power response inherent in an isothermal titration calorimetry (ITC) experiment provides an opportunity to directly analyze association kinetics, which, together with the conventional measurement of thermodynamic quantities, can provide an incredibly rich description of molecular binding in a single experiment. Here, we detail our application of this method, in which interactions occurring with relaxation times ranging from slightly below the instrument response time constant (12.5 s in this case) to as large as 600 s can be fully detailed in terms of both the thermodynamics and kinetics. In a binding titration scenario, in the most general case an injection can reveal an association rate constant (kon). Under more restrictive conditions, the instrument time constant-corrected power decay following each injection is simply an exponential decay described by a composite rate constant (kobs), from which both kon and the dissociation rate constant (koff) can be extracted. The data also support the viability of this exponential approach, for kon only, for a slightly larger set of conditions. Using a bimolecular RNA folding model and a protein-ligand interaction, we demonstrate and have internally validated this approach to experiment design, data processing, and error analysis. An updated guide to thermodynamic and kinetic regimes accessible by ITC is provided.

  16. Measuring Multivalent Binding Interactions by Isothermal Titration Calorimetry.

    Science.gov (United States)

    Dam, Tarun K; Talaga, Melanie L; Fan, Ni; Brewer, Curtis F

    2016-01-01

    Multivalent glycoconjugate-protein interactions are central to many important biological processes. Isothermal titration calorimetry (ITC) can potentially reveal the molecular and thermodynamic basis of such interactions. However, calorimetric investigation of multivalency is challenging. Binding of multivalent glycoconjugates to proteins (lectins) often leads to a stoichiometry-dependent precipitation process due to noncovalent cross-linking between the reactants. Precipitation during ITC titration severely affects the quality of the baseline as well as the signals. Hence, the resulting thermodynamic data are not dependable. We have made some modifications to address this problem and successfully studied multivalent glycoconjugate binding to lectins. We have also modified the Hill plot equation to analyze high quality ITC raw data obtained from multivalent binding. As described in this chapter, ITC-driven thermodynamic parameters and Hill plot analysis of ITC raw data can provide valuable information about the molecular mechanism of multivalent lectin-glycoconjugate interactions. The methods described herein revealed (i) the importance of functional valence of multivalent glycoconjugates, (ii) that favorable entropic effects contribute to the enhanced affinities associated with multivalent binding, (iii) that with the progression of lectin binding, the microscopic affinities of the glycan epitopes of a multivalent glycoconjugate decrease (negative cooperativity), (iv) that lectin binding to multivalent glycoconjugates, especially to mucins, involves internal diffusion jumps, (bind and jump) and (v) that scaffolds of glycoconjugates influence their entropy of binding.

  17. A microfabrication-based approach to quantitative isothermal titration calorimetry.

    Science.gov (United States)

    Wang, Bin; Jia, Yuan; Lin, Qiao

    2016-04-15

    Isothermal titration calorimetry (ITC) directly measures heat evolved in a chemical reaction to determine equilibrium binding properties of biomolecular systems. Conventional ITC instruments are expensive, use complicated design and construction, and require long analysis times. Microfabricated calorimetric devices are promising, although they have yet to allow accurate, quantitative ITC measurements of biochemical reactions. This paper presents a microfabrication-based approach to integrated, quantitative ITC characterization of biomolecular interactions. The approach integrates microfabricated differential calorimetric sensors with microfluidic titration. Biomolecules and reagents are introduced at each of a series of molar ratios, mixed, and allowed to react. The reaction thermal power is differentially measured, and used to determine the thermodynamic profile of the biomolecular interactions. Implemented in a microdevice featuring thermally isolated, well-defined reaction volumes with minimized fluid evaporation as well as highly sensitive thermoelectric sensing, the approach enables accurate and quantitative ITC measurements of protein-ligand interactions under different isothermal conditions. Using the approach, we demonstrate ITC characterization of the binding of 18-Crown-6 with barium chloride, and the binding of ribonuclease A with cytidine 2'-monophosphate within reaction volumes of approximately 0.7 µL and at concentrations down to 2mM. For each binding system, the ITC measurements were completed with considerably reduced analysis times and material consumption, and yielded a complete thermodynamic profile of the molecular interaction in agreement with published data. This demonstrates the potential usefulness of our approach for biomolecular characterization in biomedical applications.

  18. Novel investigation of enzymatic biodiesel reaction by isothermal calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Sotoft, Lene Fjerbaek, E-mail: lfj@kbm.sdu.dk [Institute of Chemical Engineering, Biotechnology and Environmental Technology, University of Southern Denmark, Campusvej 55, DK-5230 Odense M (Denmark); Westh, Peter [Department of Life Science and Chemistry, Roskilde University, PO Box 260, DK-4000 Roskilde (Denmark); Christensen, Knud V.; Norddahl, Birgir [Institute of Chemical Engineering, Biotechnology and Environmental Technology, University of Southern Denmark, Campusvej 55, DK-5230 Odense M (Denmark)

    2010-03-30

    Isothermal calorimetry (ITC) was used to investigate solvent-free enzymatic biodiesel production. The transesterification of rapeseed oil with methanol and ethanol was catalyzed by immobilized lipase Novozym 435 at 40 {sup o}C. The aim of the study was to determine reaction enthalpy for the enzymatic transesterification and to elucidate the mass transfer and energetic processes taking place. Based on the measured enthalpy and composition change in the system, the heat of reaction at 40 {sup o}C for the two systems was determined as -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 was used. Simple Michaelis-Menten kinetics was not an appropriate choice for describing the kinetics of this heterogeneous system. The experiments demonstrated the possibility of investigating complex reaction mixtures using ITC. Although it is possible to determine thermodynamic properties such as reaction enthalpy and reaction rate, the difficulty in actually measuring the true non-mass-transfer-limited reaction kinetics is exposed by the high time resolution of ITC.

  19. Estudo da preparação do catalisador Cp2ZrCl2 suportado em sílica utilizando um planejamento de experimentos Preparation conditions of Cp2ZrCl2 supported on silica using an experimental planning

    Directory of Open Access Journals (Sweden)

    Anunciata Conte

    2001-03-01

    Full Text Available O monômero eteno foi polimerizado através dos sistemas catalíticos Cp2ZrCl2/SiO2 e Cp2ZrCl2/MAO/SiO2. Foi elaborado um planejamento estatístico de experimentos a fim de se identificar as melhores condições de preparo dos catalisadores heterogêneos. As variáveis utilizadas foram a concentração de metilaluminoxano (MAO no pré-tratamento do suporte, a concentração e a temperatura de imobilização do metaloceno. Os catalisadores suportados foram analisados por espectrometria de emissão com plasma acoplado indutivamente e as resinas produzidas foram caracterizadas por cromatografia de permeação em gel (GPC e calorimetria de varredura diferencial (DSC. Foi observado que quanto maior a concentração de zircônio fixada na superfície do suporte, menor foi a atividade catalítica, na faixa de variáveis estudadas.Ethylene was polymerized with the catalytic systems Cp2ZrCl2/SiO2 and Cp2ZrCl2/MAO/SiO2. A experimental planning model was developed in order to identify the best conditions for the preparation of metallocene heterogeneous catalysts. The variables used were methylaluminoxane (MAO concentration of the support treatment, concentration and temperature of metallocene immobilization. The supported catalysts were analyzed by inductively coupled plasma emission spectometry and the polyethylene (PE produced was characterized by gel permeation calorimetry (GPC and differential scanning calorimetry (DSC. It was observed that the higher the zirconium concentration fixed on the support surface, the lower the catalyst activity, in the studied variables range.

  20. DSC investigation of the effect of the new sigma ligand PPCC on DMPC lipid membrane.

    Science.gov (United States)

    Sarpietro, Maria Grazia; Accolla, Maria Lorena; Cova, Annamaria; Prezzavento, Orazio; Castelli, Francesco; Ronsisvalle, Simone

    2014-07-20

    The new sigma ligand cis-(±)-methyl (1R,2S/1S,2R)-2-[(4-hydroxy-4-phenylpiperidin-1-yl) methyl]-1-(4-methylphenyl) cyclopropanecarboxylate [(±)-PPCC] is a promising tool for the treatment of various diseases. With the aim to investigate the absorption of (±)-PPCC by the cell membranes, in this study we evaluated the influence on thermotropic behavior of membrane model exerted by PPCC both as free base or as oxalic salt. To fulfill this purpose differential scanning calorimetry was used. The findings highlight that PPCC affects the thermodynamic parameters of phospholipids in different manner depending on whether it is in the salt or base form as well as function of the amount of drugs dispersed in the lipid matrix. The salt form of PPCC was uptaken by the membrane model faster than the free base. In addition, preliminary information on the use of a lipophilic carrier for PPCC was obtained.

  1. Comparison study of trapped water in human erythrocytes by EPC and DSC method and its application

    Institute of Scientific and Technical Information of China (English)

    ZHAO; Gang; HE; Liqun; GUO; Xiaojie; LIU; Zhong; LUO; Dawei

    2004-01-01

    The novel differential scanning calorimetry method for determining trapped water volume of human red blood cell during freezing process has been reexamined. Results show that the final erythrocyte volume is 53% of its isotonic volume after freezing to -40℃. An electronic particle counter (MultisizerTM III, Beckman Coulter Inc., USA) was used to measure cell volume changes in response to hypertonic solution. Using this approach, when extracellular solution was 3186 mOsm, the equilibrium cell volume was found to be 57% of its isotonic value. Both results indicate that 34%-40% of intracellular water is trapped and cannot respond to osmotic difference between intra- and extracellular solution. These findings are consistent with the published data: at least 20%-32% of the isotonic cell water volume is retained within RBCs during freezing. Some applications of the values of trapped water are addressed.

  2. DSC study of phase transitions of cephalin pseudo-binary systems in excess water

    Institute of Scientific and Technical Information of China (English)

    王邦宁; 谈夫

    1999-01-01

    The gel-liquid crystal phase transitions of the pseudo-binary systems of cephalins DMPE and DHPE in excess water were studied by differential scanning calorimetry. The phase diagram of the pseudo-binary systems has been given. The experiments showed that the partial phase separation in gel phase might occur at least at the mole fractions of DHPE below 0.1. The analysis by the model of ideal solution showed that both the cephalins were non-ideally miscible both in the gel phases and in the liquid crystal phases. The analysis by the model of regular solution showed that all the non-ideality parameters in the gel phases were larger than those in the liquid crystal phases at the same temperature. All the non-ideality parameters were not constant, but rather dependent on temperature.

  3. Mechanisms of fibrinogen-acebutolol interactions: Insights from DSC, CD and LS.

    Science.gov (United States)

    Hassan, Natalia; Ruso, Juan M; Somasundaran, P

    2011-02-01

    The complex formed due to the interaction of the amphiphilic betablocker acebutolol with fibrinogen in a buffer solution (50mN glycine, pH of 8.5) has been investigated using a multipronged physicochemical approach. Differential scanning calorimetry measurements of the complexes have shown no reversibility of thermal denaturation as indicated by the three observed peaks and the opposite role that acebutolol plays in the folding different domains of the fibrinogen molecule and the stability of such domains. While circular dichroism measurements have revealed that interaction of acebutolol with fibrinogen affects the protein secondary structure to a different extent depending on the temperature and drug concentration, dynamic light scattering analysis showed evidence for protein aggregation mainly to tetramers and dimers.

  4. Localization and interaction of hydroxyflavones with lipid bilayer model membranes: a study using DSC and multinuclear NMR.

    Science.gov (United States)

    Sinha, Ragini; Joshi, Akshada; Joshi, Urmila J; Srivastava, Sudha; Govil, Girjesh

    2014-06-10

    The localization and interaction of six naturally occurring flavones (FLV, 5HF, 6HF, 7HF, CHY and BLN) in DPPC bilayers were studied using DSC and multi-nuclear NMR. DSC results indicate that FLV and 6HF interact with alkyl chains. The (1)H NMR shows interaction of flavones with the sn-glycero region. Ring current induced chemical shifts indicate that 6HF and BLN acquire parallel orientation in bilayers. 2D NOESY spectra indicate partitioning of the B-ring into the alkyl chain region. The DSC, NMR and binding studies indicate that 5HF and 7HF are located near head group region, while 6HF, CHY and BLN are located in the vicinity of sn-glycero region, and FLV is inserted deepest in the membrane.

  5. PREFACE: XIV International Conference on Calorimetry in High Energy Physics

    Science.gov (United States)

    Wang, Yifang

    2011-03-01

    The International Conferences on Calorimetry in High Energy Physics (also known as the Calor Conference series, started in October 1990 at Fermilab) address all aspects of calorimetric particle detection and measurement, with an emphasis on high energy physics experiments. The XIV International Conference on Calorimetry in High Energy Physics (Calor 2010) was held at the campus of the Institute of High Energy Physics, Beijing, China, from May 10-14, 2010. This conference brought together more than 110 participants from 20 countries, including senior scientists and young physicists. During the five days of the conference, 98 presentations were given in seven plenary sessions. The attendees had in-depth discussions on the latest developments and innovations in calorimetry, including the exciting new LHC results. From the presentations, 83 papers were published in this proceedings. The success of the conference was due to the participants' enthusiasm and the excellent talks given by the speakers, and to the conveners for organizing the individual sessions. We would like to thank the International Advisory Committee for giving us the opportunity to host this Conference in Beijing. Finally we would like to thank all the people involved in the organization of the Conference, who have provided valuable local support. Yifang WangChair of Local Organizing Committee International Advisory Committee M DanilovITEP Moscow M DiemozINFN Roma I A EreditatoBern F L FabbriINFN Frascati T KobayashiICEPP Tokyo M LivanPavia University & INFN P LubranoINFN Perugia S MagillANL Argonne A MaioLIPP Lisbon H OberlackMPI Munich A ParaFermilab R WigmansTTU Lubbock R YoshidaANL Argonne R ZhuCaltech Local Organizing Committee Y WangIHEP (Chair) Y GaoTshinghua University T HuIHEP (Scientific secretary) C LiUSTC W LiIHEP J LuIHEP P WangIHEP T XuIHEP L ZhouIHEP Session Conveners 1) Materials and detectors - Junguang Lu (IHEP), Francesca Nessi (CERN) 2) Algorithm and simulation - Nural Akchurin

  6. 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.

  7. Experimental investigation of phase equilibria in the Cu–Ni–Si ternary system

    International Nuclear Information System (INIS)

    Highlights: •Three isothermal sections of the Cu–Ni–Si system have been investigated. •The ternary compound τ1 and the liquid phase are confirmed at 1073 K. •The γ (Cu5Si) and θ (Ni2Si) phases can be stabilized at higher or lower temperatures. -- Abstract: The phase equilibria in the Cu–Ni–Si ternary system have been investigated experimentally by means of electron probe microanalysis (EPMA), X-ray diffraction (XRD) and differential scanning calorimetry (DSC) analysis on equilibrated ternary alloys. Three isothermal sections at 1073, 1173 and 1273 K are determined in the whole composition range. The existence of liquid phase and the ternary compound τ1 is confirmed at 1073 K. The binary γ (Cu5Si), γ (Ni31Si12), δ (Ni2Si) and θ (Ni2Si) phases exhibit a considerable solubility of a third element. In addition, the γ (Cu5Si) and θ (Ni2Si) phases can be stabilized by the addition of Ni and Cu, respectively

  8. Calorimetry at the international linear collider. From simulation to reality

    Energy Technology Data Exchange (ETDEWEB)

    Wattimena, Nanda

    2010-02-15

    Calorimetry plays a crucial role in ongoing and upcoming high-energy physics experiments. To build a powerful calorimetric system with a performance tailored to the expected physics signatures, demands dedicated research and development of new readout technologies as well as dedicated reconstruction algorithms. The presented design of a calorimetric system which meets the high demands of precision physics at the future linear collider ILC, follows the paradigm of particle ow. Particle ow is a reconstruction principle that relies on a calorimetric system with high spatial granularity. In the detector optimisation process, the development of hardware and software are interlinked and cannot be judged independently. This thesis addresses two different aspects of detector optimisation, a test of the detector design against one example physics scenario and the development of a stable calibration procedure. In the rst part, a gauge-mediated Supersymmetry breaking scenario is used to test the design of the electromagnetic calorimeter in a full detector simulation study. The reconstruction of the neutralino properties, each decaying into a photon and a gravitino, requires a good energy resolution, as well as excellent position and angular resolution. The error bounds on the neutralino mass is strongly linked to the energy resolution, while the position and angular reconstruction of neutral particles is essential for the determination of the neutralino lifetime. The second part of this thesis focuses on the calibration procedure for a prototype of the hadron calorimeter. 7608 novel photodetectors are operated and tested in this prototype. They are exposed to beams of well de ned particle type and energy. The calibration is tested with a detailed study of electromagnetic showers inside the cubic-metre-sized prototype, with special attention paid towards the non-linearity correction. (orig.)

  9. Calorimetry at the international linear collider. From simulation to reality

    International Nuclear Information System (INIS)

    Calorimetry plays a crucial role in ongoing and upcoming high-energy physics experiments. To build a powerful calorimetric system with a performance tailored to the expected physics signatures, demands dedicated research and development of new readout technologies as well as dedicated reconstruction algorithms. The presented design of a calorimetric system which meets the high demands of precision physics at the future linear collider ILC, follows the paradigm of particle ow. Particle ow is a reconstruction principle that relies on a calorimetric system with high spatial granularity. In the detector optimisation process, the development of hardware and software are interlinked and cannot be judged independently. This thesis addresses two different aspects of detector optimisation, a test of the detector design against one example physics scenario and the development of a stable calibration procedure. In the rst part, a gauge-mediated Supersymmetry breaking scenario is used to test the design of the electromagnetic calorimeter in a full detector simulation study. The reconstruction of the neutralino properties, each decaying into a photon and a gravitino, requires a good energy resolution, as well as excellent position and angular resolution. The error bounds on the neutralino mass is strongly linked to the energy resolution, while the position and angular reconstruction of neutral particles is essential for the determination of the neutralino lifetime. The second part of this thesis focuses on the calibration procedure for a prototype of the hadron calorimeter. 7608 novel photodetectors are operated and tested in this prototype. They are exposed to beams of well de ned particle type and energy. The calibration is tested with a detailed study of electromagnetic showers inside the cubic-metre-sized prototype, with special attention paid towards the non-linearity correction. (orig.)

  10. Assessing Coupled Protein Folding and Binding Through Temperature-Dependent Isothermal Titration Calorimetry.

    Science.gov (United States)

    Sahu, Debashish; Bastidas, Monique; Lawrence, Chad W; Noid, William G; Showalter, Scott A

    2016-01-01

    Broad interest in the thermodynamic driving forces of coupled macromolecular folding and binding is motivated by the prevalence of disorder-to-order transitions observed when intrinsically disordered proteins (IDPs) bind to their partners. Isothermal titration calorimetry (ITC) is one of the few methods available for completely evaluating the thermodynamic parameters describing a protein-ligand binding event. Significantly, when the effective ΔH° for the coupled folding and binding process is determined by ITC in a temperature series, the constant-pressure heat capacity change (ΔCp) associated with these coupled equilibria is experimentally accessible, offering a unique opportunity to investigate the driving forces behind them. Notably, each of these molecular-scale events is often accompanied by strongly temperature-dependent enthalpy changes, even over the narrow temperature range experimentally accessible for biomolecules, making single temperature determinations of ΔH° less informative than typically assumed. Here, we will document the procedures we have adopted in our laboratory for designing, executing, and globally analyzing temperature-dependent ITC studies of coupled folding and binding in IDP interactions. As a biologically significant example, our recent evaluation of temperature-dependent interactions between the disordered tail of FCP1 and the winged-helix domain from Rap74 will be presented. Emphasis will be placed on the use of publically available analysis programs written in MATLAB that facilitate quantification of the thermodynamic forces governing IDP interactions. Although motivated from the perspective of IDPs, the experimental design principles and data fitting procedures presented here are general to the study of most noncooperative ligand binding equilibria.

  11. ESTIMATION OF THE CRITICAL RATE OF TEMPERATURE INCREASE OF THERMAL EXPLOSION OF NITROCELLULOSE USING NON-ISOTHERMAL DSC

    Institute of Scientific and Technical Information of China (English)

    Rorng-zu Hu; Peng-jiang Guo; Sheng-li Gao; Hai Zhang; Zhi-ming Xia; Bin-ke Ning; Yan Fang; Qi-zhen Shi; Rong Liu

    2003-01-01

    A method of estimating the critical rate of temperature increase of thermal explosion for the first order autocatalytic decomposition reaction system using non-isothermal DSC is presented. Information is obtained on the increasing rate of temperature in nitrocellulose containing 13.54% of nitrogen when the first order autocatalytic decomposition converts into thermal explosion.

  12. SIMULTANEOUS SAXS/WAXS/DSC STUDIES ON MICROSTRUCTURE OF CONVENTIONAL AND METALLOCENE-BASED ETHYLENE-BUTENE COPOLYMERS

    Institute of Scientific and Technical Information of China (English)

    Jun-ting Xu; Bo-tao Li; Zhi-qiang Fan; Anthony J. Ryan

    2004-01-01

    The fractions of one metallocene-based (mPE) and one conventional (znPE) ethylene-butene copolymer eluted at 80-82℃ from temperature rising elution fractionation were selected for DSC and time-resolved small angle X-ray scattering (SAXS) and wide angle X-ray scattering (WAXS) characterization. The DSC and WAXS results show that two crystal structures exist in both mPE and znPE: structure A with higher melting temperature and structure B with lower melting temperature. It was found that original znPE (s-znPE) contains more highly ordered structure A than original mPE (s-mPE)in spite of the higher comonomer content of znPE. Another structure C is also identified because of higher crystallinity measured by WAXS than by DSC and is attributed to the interfacial region. The SAXS data were analyzed with correlation function and two maxima were observed in s-mPE and s-znPE, in agreement with the conclusion of two crystal populations drawn from DSC and WAXS results. These two crystal populations have close long periods in s-mPE, but very different long periods in s-znPE. In contrast, freshly crystallized mPE and znPE (f-mPE and f-znPE) contain only a single crystal population with a broader distribution of long period.

  13. A Shortened Norwegian Adaptation of the Lie Scale for Children (LSC) and the Defensiveness Scale for Children (DSC)

    Science.gov (United States)

    Haugen, Richard

    1978-01-01

    Ten items consisting of five DSC items and five LSC items were translated into Norwegian in order (a) to control the verbal anxiety responses from defensive tendencies, (b) to handle the problem of response set (the tendency to answer a questionnaire in a stereotyped way), and (c) to permit research concerning the nature of defensiveness itself.…

  14. Study on the non-isothermal curing kinetics of a polyfurfuryl alcohol bioresin by DSC using different amounts of catalyst

    DEFF Research Database (Denmark)

    Dominguez Toribio, Juan Carlos; Grivel, Jean-Claude; Madsen, Bo

    2012-01-01

    The curing kinetics of a biomass-based polyfurfuryl alcohol resin with three different amounts of catalyst was studied by DSC non-isothermal measurements using seven heating rates. The change of the activation energy of the curing process was obtained by the isoconversional methods of Kissinger...

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

    Science.gov (United States)

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

    2013-07-01

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

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

    Science.gov (United States)

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

    2013-07-01

    Non-invasive pulsed arterial spin labeling (PASL) MRI is a method to study brain perfusion that does not require the administration of a contrast agent, which makes it a valuable diagnostic tool as it reduces cost and side effects. The purpose of the present study was to establish the viability of PASL as an alternative to dynamic susceptibility contrast (DSC-MRI) and other perfusion imaging methods in characterizing changes in perfusion patterns caused by seizures in epileptic patients. We evaluated 19 patients with PASL. Of these, the 9 affected by high-frequency seizures were observed during the peri-ictal period (within 5hours since the last seizure), while the 10 patients affected by low-frequency seizures were observed in the post-ictal period. For comparison, 17/19 patients were also evaluated with DSC-MRI and CBF/CBV. PASL imaging showed focal vascular changes, which allowed the classification of patients in three categories: 8 patients characterized by increased perfusion, 4 patients with normal perfusion and 7 patients with decreased perfusion. PASL perfusion imaging findings were comparable to those obtained by DSC-MRI. Since PASL is a) sensitive to vascular alterations induced by epileptic seizures, b) comparable to DSC-MRI for detecting perfusion asymmetries, c) potentially capable of detecting time-related perfusion changes, it can be recommended for repeated evaluations, to identify the epileptic focus, and in follow-up and/or therapy-response assessment. PMID:23623332

  17. A DSC study of deterioration caused by environmental chemical pollutants to parchment, a collagen-based material

    Energy Technology Data Exchange (ETDEWEB)

    Budrugeac, Petru [National R and D Institute for Electrical Engineering, INCDIE-ICPE-CA, Splaiul Unirii 313, 030138 Bucharest (Romania); Badea, Elena, E-mail: elena.badea@unito.it [Department of Chemistry IFM, University of Turin, via Pietro Giuria 9, 10125 Torino (Italy); Gatta, Giuseppe Della [Department of Chemistry IFM, University of Turin, via Pietro Giuria 9, 10125 Torino (Italy); Miu, Lucretia [National R and D Institute for Textile and Leather-Div. Leather and Footwear, INCDTP-ICPI, str Ion Minulescu 93, 031215 Bucharest (Romania); Comanescu, Alina [National R and D Institute for Electrical Engineering, INCDIE-ICPE-CA, Splaiul Unirii 313, 030138 Bucharest (Romania)

    2010-03-10

    A DSC study of new parchments exposed at 25 {sup o}C for 1-16 weeks to controlled atmospheres containing 50 ppm of gaseous chemical pollutants (NO{sub 2}, SO{sub 2}, NO{sub 2} + SO{sub 2}) and 50% relative humidity (RH) was performed. Samples were exposed to chemical pollutants alone, as well as after previous heating at 100 {sup o}C for 2-16 days and/or irradiating with visible light (1.7 x 10{sup 5} lx) for 4-16 h. DSC measurements were performed in both sealed crucibles in static air atmosphere at 25-200 {sup o}C and open crucibles under gas flow (nitrogen, oxygen, synthetic air) at 25-280 {sup o}C. Analysis of DSC curves provided the variation induced by ageing on the thermodynamic parameters associated with both parchment denaturation and softening of collagen crystalline fraction. All the ageing procedures decreased both temperature and enthalpy of denaturation and increased broadness of DSC peak in function of ageing time. The occurrence of thermal oxidation peaks and/or lower temperature endothermic peaks was observed. The temperature of the first softening peak always indicated a general tendency to decrease as a function of ageing time. Shrinkage temperature of collagen fibres measured by thermomicroscopy also decreased as a result of accelerated ageing treatments.

  18. A DSC study of deterioration caused by environmental chemical pollutants to parchment, a collagen-based material

    International Nuclear Information System (INIS)

    A DSC study of new parchments exposed at 25 oC for 1-16 weeks to controlled atmospheres containing 50 ppm of gaseous chemical pollutants (NO2, SO2, NO2 + SO2) and 50% relative humidity (RH) was performed. Samples were exposed to chemical pollutants alone, as well as after previous heating at 100 oC for 2-16 days and/or irradiating with visible light (1.7 x 105 lx) for 4-16 h. DSC measurements were performed in both sealed crucibles in static air atmosphere at 25-200 oC and open crucibles under gas flow (nitrogen, oxygen, synthetic air) at 25-280 oC. Analysis of DSC curves provided the variation induced by ageing on the thermodynamic parameters associated with both parchment denaturation and softening of collagen crystalline fraction. All the ageing procedures decreased both temperature and enthalpy of denaturation and increased broadness of DSC peak in function of ageing time. The occurrence of thermal oxidation peaks and/or lower temperature endothermic peaks was observed. The temperature of the first softening peak always indicated a general tendency to decrease as a function of ageing time. Shrinkage temperature of collagen fibres measured by thermomicroscopy also decreased as a result of accelerated ageing treatments.

  19. Thermodynamic Study on the Protonation Reactions of Glyphosate in Aqueous Solution: Potentiometry, Calorimetry and NMR spectroscopy.

    Science.gov (United States)

    Liu, Bijun; Dong, Lan; Yu, Qianhong; Li, Xingliang; Wu, Fengchang; Tan, Zhaoyi; Luo, Shunzhong

    2016-03-10

    Glyphosate [N-(phosphonomethyl)glycine] has been described as the ideal herbicide because of its unique properties. There is some conflicting information concerning the structures and conformations involved in the protonation process of glyphosate. Protonation may influence the chemical and physical properties of glyphosate, modifying its structure and the chemical processes in which it is involved. To better understand the species in solution associated with changes in pH, thermodynamic study (potentiometry, calorimetry and NMR spectroscopy) about the protonation pathway of glyphosate is performed. Experimental results confirmed that the order of successive protonation sites of totally deprotonated glyphosate is phosphonate oxygen, amino nitrogen, and finally carboxylate oxygen. This trend is in agreement with the most recent theoretical work in the literature on the subject ( J. Phys. Chem. A 2015, , 119 , 5241 - 5249 ). The result is important because it confirms that the protonated site of glyphosate in pH range 7-8, is not on the amino but on the phosphonate group instead. This corrected information can improve the understanding of the glyphosate chemical and biochemical action. PMID:26862689

  20. Study on the Interaction of Zinc Ion Binding with Human Serum Albumin using Isothermal Titration Calorimetry

    International Nuclear Information System (INIS)

    The interaction between zinc ion and human serum albumin (HSA) was investigated by nano-Watt- scale isothermal titration calorimetry (ITC). From the analysis of the ITC data, the binding characteristics and thermodynamic properties of the system were obtained and the binding mechanism was discussed. It was found that the experimental data fit well with the Langmuir's binding theory and the system behaved as a system with two classes of binding sites (high-affinity and low-affinity binding site). The binding number of high-affinity binding site (N1) is 1.40 and the binding constant (K1) is 2.72*105 L/mol. For the low-affinity binding site, the binding number (N2) is 1.55 and the binding constant (K2) is 3.78*103 L/mol. Moreover, it was indicated by the thermodynamic analysis that the binding processes of both types of binding sites were exothermic and spontaneous. The high-affinity binding was an enthalpy-entropy synergically driven process and the electrostatic interaction was the main force, while the low-affinity binding was an enthalpy driven process and this process was mainly driven by the van der Waals forces. (author)

  1. Application of Differential Scanning Calorimetry to Evaluate Thermal Properties and Study of Microstructure of Biodegradable Films

    Science.gov (United States)

    Aguilar-Méndez, M. A.; Martin-Martínez, E. San; Ortega-Arroyo, L.; Cruz-Orea, A.

    2010-03-01

    The glass transition temperature ( T g) and melting temperature ( T m) of gelatin-starch films were determined using differential scanning calorimetry. Also, the microstructure was observed using scanning electron microscopy (SEM) and the crystalline structure by means of X-ray diffraction (XRD). The effect of starch and glycerol concentrations in films on the thermal properties was evaluated through response surface methodology (RSM). The highest values of T m were obtained at starch concentration intervals of (0.26 to 0.54) %w/w and glycerol concentrations lower than 0.5 (%w/w). On the other hand, the T g values diminished as the glycerol concentration increased. Mathematical models for both transitions were fitted to the experimental data. The micrographs obtained by SEM show the influence of glycerol in the microstructure of the films, being more “gummy” as the content of the plasticizer increased. The XRD patterns of the films demonstrate the existence of some pseudo-crystalline regions in the biodegradable materials.

  2. Ring-shaped Calorimetry Information for a Neural eGamma Identification with ATLAS Detector

    CERN Document Server

    Da Fonseca Pinto, Joao Victor; The ATLAS collaboration; Oliveira Damazio, Denis; Seixas, Jose

    2016-01-01

    \\title{Ring-shaped Calorimetry Information for a Neural e/$\\gamma$ Identification with ATLAS Detector} After the successful operation of the Large Hadron Collider resulting with the discovery of the Higgs boson, a new data-taking period (Run 2) has started. For the first time, collisions are produced with energies of 13 TeV in the centre of mass. It is foreseen the luminosity increase, reaching values as high as $10^{34}cm^{-2}s^{-1}$ yet in 2015. These changes in experimental conditions bring a proper environment for possible new physics key-findings. ATLAS is the largest LHC detector and was designed for general-purpose physics studies. Many potential physics channels have electrons or photons in their final states. For efficient studies on these channels precise measurement and identification of such particles is necessary. The identification task consists of disentangling those particles (signal) from collimated hadronic jets (background). Reported work concerns the identification process based on the cal...

  3. Thermodynamic Study on the Protonation Reactions of Glyphosate in Aqueous Solution: Potentiometry, Calorimetry and NMR spectroscopy.

    Science.gov (United States)

    Liu, Bijun; Dong, Lan; Yu, Qianhong; Li, Xingliang; Wu, Fengchang; Tan, Zhaoyi; Luo, Shunzhong

    2016-03-10

    Glyphosate [N-(phosphonomethyl)glycine] has been described as the ideal herbicide because of its unique properties. There is some conflicting information concerning the structures and conformations involved in the protonation process of glyphosate. Protonation may influence the chemical and physical properties of glyphosate, modifying its structure and the chemical processes in which it is involved. To better understand the species in solution associated with changes in pH, thermodynamic study (potentiometry, calorimetry and NMR spectroscopy) about the protonation pathway of glyphosate is performed. Experimental results confirmed that the order of successive protonation sites of totally deprotonated glyphosate is phosphonate oxygen, amino nitrogen, and finally carboxylate oxygen. This trend is in agreement with the most recent theoretical work in the literature on the subject (J. Phys. Chem. A 2015, 119, 5241-5249). The result is important because it confirms that the protonated site of glyphosate in pH range 7-8, is not on the amino but on the phosphonate group instead. This corrected information can improve the understanding of the glyphosate chemical and biochemical action.

  4. High Temperature Heat Capacity of Alloy D9 Using Drop Calorimetry Based Enthalpy Increment Measurements

    Science.gov (United States)

    Banerjee, Aritra; Raju, S.; Divakar, R.; Mohandas, E.

    2007-02-01

    Alloy D9 is a void-swelling resistant nuclear grade austenitic stainless steel (SS) based on AISI type 316-SS in which titanium constitutes an added predetermined alloying composition. In the present study, the high-temperature enthalpy values of alloy D9 with three different titanium-to-carbon mass percent ratios, namely Ti/C = 4, 6, and 8, have been measured using inverse drop calorimetry in the temperature range from 295 to 1323 K. It is found that within the level of experimental uncertainty, the enthalpy values are independent of the Ti-C mass ratio. The temperature dependence of the isobaric specific heat C P is obtained by a linear regression of the measured enthalpy data. The measured C P data for alloy D9 may be represented by the following best-fit expression: C_P(J \\cdot kg^{-1}\\cdot K^{-1})= 431 + 17.7 × 10^{-2}T + 8.72 × 10^{-5}/T^2. It is found that the measured enthalpy and specific heat values exhibit good agreement with reported data on 316 and other related austenitic stainless steels.

  5. Changes in polymer foils used in food packaging tested by using differential scanning calorimetry

    Indian Academy of Sciences (India)

    J Gajdoš Kljusurić

    2003-12-01

    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), poly(D-(-)--hydroxybutyrate) (powder), two-layered polypropylene (0.064 mm), and two-layered polypropylene with poly-vinylidene-chloride (0.012/0.021). The polymer stability was checked by simulation of conditions during food preparation in microwave ovens, sterilisation or rapid freezing. The materials were tested in the temperature range from 40 to 200°C at different scan rates from 2 to 30° C min-1 during heating or cooling. The enthalpies show a high correlation coefficient (0.964) with scan rate. All samples undergo phase change in the temperature range from 107 to 173°C during heating and enthalpies are in the range from 31.8 to 71.1 J g−1 Upon subsequent cooling from 200°C, the temperature range of phase changes is shifted to lower temperatures from 86 to 102°C with enthalpies ranging from 30.4 to 57.8 J g−1. Experiments with exposure of polymers to microwave radiation and freezing prove that the phase change considering the temperature range is very similar in all experiments.

  6. Single-crystal adsorption calorimetry and density functional theory of CO chemisorption on fcc Co{110}.

    Science.gov (United States)

    Liao, Kristine; Fiorin, Vittorio; Gunn, David S D; Jenkins, Stephen J; King, David A

    2013-03-21

    Using single-crystal adsorption calorimetry (SCAC) and density functional theory (DFT), the interaction of carbon monoxide on fcc Co{110} is reported for the first time. The results indicate that adsorption is consistent with molecular chemisorption at all coverages. The initial heat of adsorption of 140 kJ mol(-1) is found in the range of heat values calorimetrically measured on other ferromagnetic metal surfaces, such as nickel and iron. DFT adsorption energies are in good agreement with the experimental results, and comparison between SCAC and DFT for CO on other ferromagnetic surfaces is made. The calculated dissociation barrier of 2.03 eV implies that dissociation at 300 K is unlikely even at the lowest coverage. At high coverages during the adsorption-desorption steady state regime, a pre-exponential factor for CO desorption of 1.2 × 10(17) s(-1) is found, implying a localised molecular adsorbed state prior to desorption in contrast to what we found with Ni surfaces. This result highlights the importance of the choice of the pre-exponential factor in evaluating the activation energy for desorption.

  7. TG/DSC-FTIR and Py-GC investigation on pyrolysis characteristics of petrochemical wastewater sludge.

    Science.gov (United States)

    Chen, Jianbiao; Mu, Lin; Jiang, Bo; Yin, Hongchao; Song, Xigeng; Li, Aimin

    2015-09-01

    The pyrolysis characteristics of petrochemical wastewater sludge (PS) were evaluated using TG/DSC-FTIR and fixed-bed reactor with GC. TGA experiments indicated that the pyrolysis of PS proceeded in three phases, and the thermographs shifted to higher temperatures with increasing heating rate. Chars FTIR showed that the absorption of O-H, C-H, C=O and C-C decreased with pyrolysis temperatures increasing. Gases FTIR correspondingly showed that H2O, CO, and CH4 generated at higher temperatures. For the fixed-bed reactor tests, H2 and CO were relatively higher in the pyrolysis gases, and CH4 was negligible at 436K. The kinetic triplets of PS pyrolysis were estimated by Flynn-Wall-Ozawa, Kissinger-Akahira-Sunose, and integral master-plots method. The results suggested that the most potential kinetic models for the first and second phase were the order reaction model, while the random nucleation and nuclei growth model for the third phase.

  8. 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

  9. Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime Using Controlled Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Don W. Miller; Andrew Kauffmann; Eric Kreidler; Dongxu Li; Hanying Liu; Daniel Mills; Thomas D. Radcliff; Joseph Talnagi

    2001-12-31

    A comprehensive description of the accomplishments of the DOE grant titled, ''Local Measurement of Fuel Energy Deposition and Heat Transfer Environment During Fuel Lifetime using Controlled Calorimetry''.

  10. Uranium-liquid argon calorimetry: preliminary results from the DO tests

    International Nuclear Information System (INIS)

    The motivations for using uranium and liquid argon in sampling calorimetry are reviewed and the pros and cons of the technique are discussed. Preliminary results of the DO uranium-liquid argon test program are presented. 9 refs., 7 figs

  11. Determination of Heats of Fusion: Using Differential Scanning Calorimetry for the AP Chemistry Courses.

    Science.gov (United States)

    Temme, Susan M.

    1995-01-01

    Describes an exercise designed to be used in an Advanced Placement (AP) chemistry course to accompany the study of thermodynamics. Uses Differential Scanning Calorimetry in teaching the concepts of thermochemistry and thermodynamics. (JRH)

  12. An Integrated-Circuit Temperature Sensor for Calorimetry and Differential Temperature Measurement.

    Science.gov (United States)

    Muyskens, Mark A.

    1997-01-01

    Describes the application of an integrated-circuit (IC) chip which provides an easy-to-use, inexpensive, rugged, computer-interfaceable temperature sensor for calorimetry and differential temperature measurement. Discusses its design and advantages. (JRH)

  13. DSC study of phase transition of anhydrous phospholipid DHPC and influence of water content

    Institute of Scientific and Technical Information of China (English)

    王邦宁; 谈夫

    1997-01-01

    The phase transition behavior of 1,2-di-n-heptadecanoyl phosphatidylcholme (DHPC)with and without water has been studied by use of differential scanning calorimetry It was found by experiment that the glass transition occurred at first during the first heating of a sample of DHPC without water and then the sample underwent melting as an ordinary crystal.Therefore the sample of DHPC without water was a glassy crystal However,the DHPC sample crystallizing from melt was an ordinary crystal From the relationship between the total melting enthalpy Qf of freezable water and the water content h,it was concluded that the water contained in the DHPC samples might exist in three states recognizable thermodynamically.The water in the first state was an unfreezable water It was the water bound directly with the head groups of the phospholipid,i.e.the primary hydration water Every head group might bind seven such molecules of water.The water in the second state was the secondary hydration water,us melt ing point was

  14. DSC and TG Analysis of a Blended Binder Based on Waste Ceramic Powder and Portland Cement

    Science.gov (United States)

    Pavlík, Zbyšek; Trník, Anton; Kulovaná, Tereza; Scheinherrová, Lenka; Rahhal, Viviana; Irassar, Edgardo; Černý, Robert

    2016-03-01

    Cement industry belongs to the business sectors characteristic by high energy consumption and high {CO}2 generation. Therefore, any replacement of cement in concrete by waste materials can lead to immediate environmental benefits. In this paper, a possible use of waste ceramic powder in blended binders is studied. At first, the chemical composition of Portland cement and ceramic powder is analyzed using the X-ray fluorescence method. Then, thermal and mechanical characterization of hydrated blended binders containing up to 24 % ceramic is carried out within the time period of 2 days to 28 days. The differential scanning calorimetry and thermogravimetry measurements are performed in the temperature range of 25°C to 1000°C in an argon atmosphere. The measurement of compressive strength is done according to the European standards for cement mortars. The thermal analysis results in the identification of temperature and quantification of enthalpy and mass changes related to the liberation of physically bound water, calcium-silicate-hydrates dehydration and portlandite, vaterite and calcite decomposition. The portlandite content is found to decrease with time for all blends which provides the evidence of the pozzolanic activity of ceramic powder even within the limited monitoring time of 28 days. Taking into account the favorable results obtained in the measurement of compressive strength, it can be concluded that the applied waste ceramic powder can be successfully used as a supplementary cementing material to Portland cement in an amount of up to 24 mass%.

  15. Transfer kinetics from colloidal drug carriers and liposomes to biomembrane models: DSC studies

    Directory of Open Access Journals (Sweden)

    Maria Grazia Sarpietro

    2011-01-01

    Full Text Available The release of bioactive molecules by different delivery systems has been studied. We have proposed a protocol that takes into account a system that is able to carry out the uptake of a bioactive molecule released during the time, resembling an in vivo-like system, and for this reason we have used biomembrane models represented by multi-lamellar and unilamellar vesicles. The bioactive molecule loaded delivery system has been put in contact with the biomembrane model and the release has been evaluated, to consider the effect of the bioactive molecule on the biomembrane model thermotropic behavior, and to compare the results with those obtained when a pure drug interacts with the biomembrane model. The differential scanning calorimetry technique has been employed. Depending on the delivery system used, our research permits to evaluate the effect of different parameters on the bioactive molecule release, such as pH, drug loading degree, delivery system swelling, crosslinking agent, degree of cross-linking, and delivery system side chains.

  16. Effect of a bioactive curcumin derivative on DPPC membrane: A DSC and Raman spectroscopy study

    Energy Technology Data Exchange (ETDEWEB)

    Gardikis, Kostantinos [Department of Pharm. Technology, School of Pharmacy, University of Athens, Athens (Greece); Hatziantoniou, Sophia [Department of Pharm. Technology, School of Pharmacy, University of Athens, Athens (Greece); Viras, Kyriakos [Laboratory of Physical Chemistry, Department of Chemistry, University of Athens, Athens (Greece); Demetzos, Costas [Department of Pharm. Technology, School of Pharmacy, University of Athens, Athens (Greece)]. E-mail: demetzos@pharm.uoa.gr

    2006-08-01

    Interactions of dimethoxycurcumin (1) a lipophilic bioactive curcumin derivative with dipalmitoyl phosphatidylcholine (DPPC) were investigated. The thermodynamic changes caused by (1) and its location into DPPC lipid bilayers were monitored by differential scanning calorimetry and Raman spectroscopy. The results reveal that (1) influences the thermotropic properties of DPPC lipid membrane causing abolition of the pretransition and broadening of the phase-transition profile and slightly decreases the T {sub m} at increasing concentrations. The Raman height intensity ratios of the peaks I {sub 2935/2880}, I {sub 2844/2880} and I {sub 1090/1130} are representative of the interaction of (1) with the alkyl chains and furnish information about the ratio between disorder and order that exists in the conformation of the alkyl chain. The intensity changes of the peak at 715 cm{sup -1} indicates interaction between the choline head group and (1). The Raman spectroscopy results are in agreement with the thermal analysis results. Biologically active lipophilic molecules such as (1) should be studied in terms of their interaction with lipid bilayers prior to the development of advanced lipid carrier systems such as liposomes. The results of these studies provide information on the membrane integrity and physicochemical properties that are essential for the rational design lipidic drug delivery systems.

  17. Factors influencing the crystallisation of highly concentrated water-in-oil emulsions: A DSC study

    Directory of Open Access Journals (Sweden)

    Irina Masalova

    2012-03-01

    Full Text Available Highly concentrated emulsions are used in a variety of applications, including the cosmetics, food and liquid explosives industries. The stability of these highly concentrated water-in-oil emulsions was studied by differential scanning calorimetry. Crystallisation of the emulsions was initiated by exposing the emulsions to a low temperature. The effects of surfactant type, electrolyte concentration and electrolyte composition in the aqueous phase on emulsion crystallisation temperature were studied. Surfactant type affected the emulsion crystallisation temperature in the following order: PIBSA-MEA=PIBSA-UREA < PIBSA-MEA/SMO < PIBSA-IMIDE < SMO. These results are in the same sequence as results obtained for the stability of these emulsions in aging studies, that is, PIBSA-MEA was the most stable with age and SMO was the least. The effect of the surfactant type on emulsion crystallisation can probably be attributed to the differing strengths of the surfactant–electrolyte interactions, which result in different molecular packing geometry and differing mobility of the surfactant lipophilic portion at the interface. These results enhance our understanding of the factors that affect the stability of explosive emulsions.

  18. Relaxation process of Fe(CuNb)SiB amorphous alloys investigated by dynamical calorimetry

    OpenAIRE

    Zhu, J.; Clavaguera-Mora, M. T.; Clavaguera, N.

    1997-01-01

    Differential scanning calorimetry and dynamic differential scanning calorimetry were used to analyze the relaxation process of Fe(CuNb)SiB amorphous alloys. The Curie temperature(TC) evolution of the amorphous phase during relaxation as a function of heating rate, time and pre-annealing temperature were measured. Two distinct relaxation processes are observed, consequent with topological and chemical short range order changes.

  19. INDIRECT CALORIMETRY IN THE ASSESSMENT OF THE ENERGY REQUIREMENT IN OVERWEIGHT AND OBESE WOMEN

    OpenAIRE

    Ewa Lange; Dominika Głąbska; Dariusz Włodarek

    2013-01-01

    Individual total energy expenditure may be calculated as a sum of basal energy requirement and energy expenditure associated with physical activity. Measurement of basal energy requirement is not often conducted in dietetic practice, but may be applied using indirect calorimetry. The aim of the analysis was to present the possibilities of using the Fitmate PRO monitor in the assessment of resting metabolic rate and basal energy expenditure with a method of indirect calorimetry in a group of 9...

  20. Relaxation process of Fe(CuNb)SiB amorphous alloys investigated by dynamical calorimetry

    International Nuclear Information System (INIS)

    Differential scanning calorimetry and dynamic differential scanning calorimetry were used to analyze the relaxation process of Fe(CuNb)SiB amorphous alloys. The Curie temperature (TC) evolution of the amorphous phase during relaxation as a function of heating rate, time and pre-annealing temperature were measured. Two distinct relaxation processes are observed, consequent with topological and chemical short range order changes. copyright 1997 American Institute of Physics

  1. 差示扫描量热分析测定外掺氧化镁水泥浆体中的氢氧化镁%Determination of Magnesium Hydroxide in Cement Paste Added with Magnesia by Differential Scanning Calorimetry

    Institute of Scientific and Technical Information of China (English)

    陈福松; 徐玲玲

    2011-01-01

    This paper introduces the differential scanning calorimetry(DSC) incremental method which is used to determine magnesium hydroxide in cement paste added with magnesia and on this basis, proposes the once-incement method used to determine magnesium hydroxide also. Besides the paper evaluates the accuracy of these two methods by recovery rate. The result shows that the recovery rate of magnesium hydroxide in cement paste added with magnesia is more than 98.5% by DSC incremental method and more than 97.5% by once-incement method. Though the DSC incremental method has high accuracy in determination of magnesium hydroxide in cement paste added with magnesia and the once-incement method is slightly lower in accuracy, the once-incement method is superior to the DSC incremental method in simplified operation and can be used to determine magnesium hydroxide also.%本文介绍了一种利用差示扫描量热分析(DSC)测定外掺氧化镁水泥浆体中氢氧化镁(Mg(OH))的方法-DSC增量法,在DSC增量法基础上提出采用一次增量测定水泥浆体中Mg(OH),并用回收率评价了这两种方法的准确性.结果表明:DSC增量法测定水泥浆体中Mg(OH)的回收率大于98.5%,此法准确度较高,测定外掺氧化镁水泥浆体中Mg(OH)是可行的;一次增量法测定Mg(OH)的回收率为97.5%以上,准确度较DSC增量法略低,但此法操作简单,也可对水泥浆体中Mg(OH)进行定量测定.

  2. Isobaric specific heat capacity of typical lithium chloride liquid desiccants using scanning calorimetry

    International Nuclear Information System (INIS)

    Highlights: • Typical lithium chloride liquid desiccants were concerned. • Up to date heat capacity data of high quality were measured. • Scanning calorimetry technology was applied. • A universal empirical formula was correlated for the heat capacity of solutions. -- Abstract: Three kinds of lithium chloride desiccants were selected, which are considered to be potential and interesting working fluids for a desiccant/dehumidification or absorption refrigeration system, and their isobaric specific heat capacities were determined in this context. Experiments were conducted at a high accuracy twin-cell scanning calorimeter. The temperature accuracy and heat flux resolution of the calorimeter are ±0.05 K and 0.1 μW respectively. The data of lithium chloride + water and lithium chloride + triethylene glycol (TEG)/propylene glycol (PG) + water systems were achieved at temperatures from 308.15 K to 343.15 K and atmospheric pressure. The mass fraction of LiCl ranged from 15% to 45% in the LiCl + H2O system, and the mass fraction of LiCl and glycol ranged from 10% to 23.3% and 20% to 46.7% in the ternary systems respectively. Based on the experimental heat capacity data, a universal empirical formula was correlated as a function of temperature and solute mass fraction. In the experimental mass fractions and temperatures range, the average absolute deviation (AAD) between experiment results and calculated values is no more than 0.15%, and maximum absolute deviation (MAD) is within 0.38%. These thermodynamic data of lithium chloride solutions can be effectively used for analysis and design of desiccant/dehumidification systems and absorption refrigeration systems in both refrigeration and chemical industry

  3. Two decoupling methods for non-isothermal DSC results of AIBN decomposition

    International Nuclear Information System (INIS)

    Highlights: • DSC curves of liquid-state AIBN were obtained by a solvent decoupling method. • A mathematical method was introduced to solve the coupling phenomenon by MATLAB. • The overlapping area of heat absorption and generation was determined. • True characteristic parameters of AIBN’s melting and decomposition were obtained. - Abstract: During thermal decomposition of azobisisobutyronitrile (AIBN), the endothermic process of phase transition disturbed exothermic decomposition, which brought deformation in its thermal graphs. Therefore, exact kinetic parameters of the decomposition could not be obtained by the existing kinetics analytic models, and the accurate enthalpy data of the decomposition and phase transition were not available. Two methods, i.e., a solvent method and a mathematical method, were introduced in this paper to resolve the coupling phenomenon. In the former method, AIBN was dissolved into aniline to eliminate the endothermic process and obtain curves of the liquid-state decomposition. In the latter method, MATLAB software was employed to get the “pure” exothermic decomposition curve without the influence of phase transition by fitting coupling curves within the section after the transition point and extrapolating to the initial stage of decomposition. Moreover, the kinetic parameters of the “pure” exothermic decomposition of AIBN obtained by the mathematical fitting agreed with the results from the solvent method, verifying the accuracy of the decoupling. The research is of great significance for comprehending the exact characteristics of thermal behaviors and safety parameters of AIBN. It also provides a great help to determine the safe operating temperature and alarm temperature for processes in industry

  4. Establishment of Heat Treatment Process for Modified 440A Martensitic Stainless Steel Using Differential Scanning Calorimetry and Thermo-Calc Calculation

    Directory of Open Access Journals (Sweden)

    Huei-Sen Wang

    2015-12-01

    Full Text Available To provide a suitable microstructure and mechanical properties for modified Grade 440A martensitic stainless steel (MSS, which could facilitate the further cold deformation process (e.g., cold rolling, this work used differential scanning calorimetry (DSC and Thermo-Calc software to determine three soaking temperatures for annealing heat treatment processes (HT1, HT2 and HT3. To verify the feasibility of the proposed annealing heat treatment processes, the as-received samples were initially heated to 1050 °C (similar to the on-line working temperature for 30 min and air quenched to form a martensitic structure. The air-quenched samples were then subjected to three developed annealing heat treatment conditions. The microstructure and mechanical properties of the heat-treated samples were then investigated. Test results showed that considering the effects of the microstructure and the hardness, the HT1, the HT2 or the soaking temperatures between the HT1 and HT2 were the most recommended processes to modified Grade 440A MSS. When using the recommended processes, their carbides were fine and more evenly distributed, and the microhardness was as low as 210 Hv, which can be applied to the actual production process.

  5. Low temperature (down to 450 C) annealed TiAl contacts on N-type gallium nitride characterized by differential scanning calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Thierry-Jebali, Nicolas [Laboratoire des Multimateriaux et Interfaces, UMR-CNRS 5615, Universite Claude Bernard Lyon 1, 43 Boulevard du 11 Novembre 1918, 69622 Villeurbanne Cedex (France); STMicroelectronics, R and D department, 11 rue Pierre et Marie Curie, 37100 Tours (France); Menard, Olivier [STMicroelectronics, R and D department, 11 rue Pierre et Marie Curie, 37100 Tours (France); Laboratoire de Microelectronique de Puissance, Universite Francois Rabelais de Tours, 1 rue Pierre et Marie Curie, 37100 Tours (France); Chiriac, Rodica; Brylinski, Christian [Laboratoire des Multimateriaux et Interfaces, UMR-CNRS 5615, Universite Claude Bernard Lyon 1, 43 Boulevard du 11 Novembre 1918, 69622 Villeurbanne Cedex (France); Collard, Emmanuel [STMicroelectronics, R and D department, 11 rue Pierre et Marie Curie, 37100 Tours (France); Cayrel, Frederic; Alquier, Daniel [Laboratoire de Microelectronique de Puissance, Universite Francois Rabelais de Tours, 1 rue Pierre et Marie Curie, 37100 Tours (France)

    2011-02-15

    This work reports on Differential Scanning Calorimetry (DSC) measurements performed on Ti-Al metallic layers stacks deposited on n{sup +}-GaN. The aim is to get better understanding of the mechanisms leading to ohmic contact formation during the annealing stage. Two exothermic peaks were found, one below 500 C and the other one around 660 C. They can be respectively attributed to Al{sub 3}Ti and Al{sub 2}Ti compounds formation. The locations of these peaks provide clear evidence of solid-solid reactions. Lowest contact resistance is well correlated with the presence of Al{sub 3}Ti compound, corresponding to Al(200nm)/Ti(50nm) stoichiometric ratio. Subsequently, Al(200 nm)Ti(50 nm) stacks on n{sup +}-GaN were annealed from 400 C to 650 C. Specific Contact Resistivity (SCR) values stay in the mid 10{sup -5} {omega}.cm{sup 2} range for annealing temperatures between 450 C and 650 C. Such low-temperature annealed contacts on n+-GaN may open new device processing routes, simpler and cheaper, in which Ohmic and Schottky contacts are annealed together. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  6. Entalpia reticular, entalpia de fusão e temperatura de fusão de adutos: algumas correlações empíricas utilizando DSC

    Directory of Open Access Journals (Sweden)

    Farias Robson Fernandes de

    1999-01-01

    Full Text Available By using DSC data is shown that there are empirical correlations between lattice enthalpy, melting enthalpy and the temperature of melting for adducts, and that is possible, using only a single DSC curve, estimate the value of DM Hmq.

  7. Experimental study of partially-cured Z-pins reinforced foam core composites:K-Cor sandwich structures

    Institute of Scientific and Technical Information of China (English)

    Zheng Yingying; Xiao Jun; Duan Mufeng; Li Yong

    2014-01-01

    This paper presents an experimental study of a novel K-Cor sandwich structure rein-forced with partially-cured Z-pins. The influence of pultrusion processing parameters on Z-pins characteristics was studied and the effect of Z-pins on mechanical properties was disclosed. Differential scanning calorimetry (DSC) and optical microscopy (OM) methods were employed to determine the curing degree of as-prepared Z-pins and observe the implanted Z-pins in the K-Cor structure. These partially-cured Z-pins were treated with a stronger bonding link between face sheets and the foam core by means of a hot-press process, thereby decreasing burrs and cracking defects when the Z-pins were implanted into the Rohacell foam core. The results of the out-of-plane tensile tests and the climbing drum peel (CDP) tests showed that K-Cor structures exhibited superior mechanical performance as compared to X-Cor and blank foam core. The observed results of failure modes revealed that an effective bonding link between the foam core and face sheets that was provided from partially-cured Z-pins contributed to the enhanced mechan-ical performances of K-Cor sandwich structures.

  8. Thermophysical properties of solid phase ruthenium measured by the pulse calorimetry technique over a wide temperature range

    Energy Technology Data Exchange (ETDEWEB)

    Milosevic, Nenad; Nikolic, Ivana [Belgrade Univ. (Serbia). Vinca Institute of Nuclear Sciences

    2015-04-15

    This paper presents experimental results on four thermophysical properties of pure polycrystalline ruthenium samples over a wide temperature range. Specific heat capacity and specific electrical resistivity were measured from 250 to 2 500 K, while hemispherical total emissivity and normal spectral emissivity at 900 nm were measured from 1 300 to 2 500 K. All the properties were obtained by using the pulse calorimetry technique. The 200 mm long specimens were in the form of a thin rod, of about 3 mm in diameter. For necessary corrections, literature data on thermal linear expansion were applied. The results are compared with available literature data and discussed. The specific heat capacity and specific electrical resistivity measurements did not indicate any allotropic transformation of the samples over the entire temperature range.

  9. The use of DSC curves to determine the acetylation deg.ree of chitin/chitosan samples

    International Nuclear Information System (INIS)

    The use of DSC curves is proposed as an alternative method to determine the deg.ree of N-acetylation (DA) in chitin/chitosan samples, based in both peak area and height of the decomposition signal. Samples with DA from 74 to 16% were prepared from a chitin commercial sample and the DA was determined by 1H NMR, 13C CP/MAS NMR and IR spectra. The effect of water content, heating rate, sample mass and gas flow on the DSC peaks were evaluated and optimized. Using optimized conditions a linear relationship between peak area and height with the DA could be achieved with linear correlation coefficients of -0.998 and -0.999 (n = 7), respectively. The calibration graphs were used to determine the DA of a commercial chitosan sample with relative errors ranging from 2 to 3% for both peak area and peak height, when compared with the DA determined by 1H NMR method

  10. Formation of Cholesterol Bilayer Domains Precedes Formation of Cholesterol Crystals in Cholesterol/Dimyristoylphosphatidylcholine Membranes: EPR and DSC Studies

    OpenAIRE

    Mainali, Laxman; Raguz, Marija; Subczynski, Witold K.

    2013-01-01

    Saturation-recovery EPR along with DSC were used to determine the cholesterol content at which pure cholesterol bilayer domains (CBDs) and cholesterol crystals begin to form in dimyristoylphosphatidylcholine (DMPC) membranes. To preserve compositional homogeneity throughout the membrane suspension, lipid multilamellar dispersions were prepared using a rapid solvent exchange method. The cholesterol content increased from 0 to 75 mol%. With spin-labeled cholesterol analogs it was shown that the...

  11. Tg-Confinement Effects in Polymer Thin Films, Nanotubes, and Nanospheres as Measured by DSC, Ellipsometry and Fluorescence

    Science.gov (United States)

    Torkelson, John; Tan, Anthony; Chen, Lawrence

    The effect of nanoscale confinement on the glass transition temperature (Tg) of supported and free-standing polymer films has been studied for two decades by various techniques. However, conventional DSC, which is the most common method for measuring Tg of bulk polymers, is not well suited for such measurements. Here, we demonstrate that Tg-confinement effects measured by conventional DSC in nanotubes of polymer supported in anodic aluminum oxide (AAO) templates compare well with with Tg-confinement effects measured in supported polymer films by ellipsometry and fluorescence. We further show that Tg-confinement effect data for nanotubes obtained by fluorescence agree well with data obtained by DSC. Finally, we draw comparisons between the Tg-confinement behavior of nanoprecipitated polymer nanospheres as measured by fluorescence to Tg-confinement effects for both supported and free-standing polymer films. The roles, if any, of confinement dimensionality (1-D vs 2-D vs 3-D) and measurement technique on the observed Tg-confinement effect will be discussed.

  12. Engineering design of dosimeter prototype based on graphite calorimetry for electron radiation dose measurement

    International Nuclear Information System (INIS)

    he engineering design of a dosimeter prototype based on graphite calorimetry for electron radiation dose measurement at electron energy of at most 300 keV and maximum dose of 60 kGy have been carried out. The graphite core is a cylinder shape with diameter and thickness of 30 mm and 2 mm respectively, surrounded by a guard ring made of the same graphite material. Dosimeter based on graphite calorimetry is equipped with a styrofoam for thermal insulation, temperature sensors and instrumentation based on micro controller. The characteristics of dosimeter based on graphite calorimetry are obtained by means of calculation and computer simulations using Penelope 2003 software and ANSYS computer program. The dosimeter based on graphite calorimetry has been designed to perform real time measurement of the average of absorbed and surface dose, it was expected that dosimeter based on graphite calorimetry can operate well. Compared with the cellulose tri acetate (CTA) dose measurement it gives relative differences of 18.9% and 9.1% at the experiments of energy variation and electron beam current alteration of the electron beam machine (EBM) respectively. (author

  13. 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. PMID:18970276

  14. Enzyme kinetics determined by single-injection isothermal titration calorimetry.

    Science.gov (United States)

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

    2015-04-01

    The purposes of this paper are (a) to examine the effect of calorimeter time constant (τ) on heat rate data from a single enzyme injection into substrate in an isothermal titration calorimeter (ITC), (b) to provide information that can be used to predict the optimum experimental conditions for determining the rate constant (k2), Michaelis constant (KM), and enthalpy change of the reaction (ΔRH), and (c) to describe methods for evaluating these parameters. We find that KM, k2 and ΔRH can be accurately estimated without correcting for the calorimeter time constant, τ, if (k2E/KM), where E is the total active enzyme concentration, is between 0.1/τ and 1/τ and the reaction goes to at least 99% completion. If experimental conditions are outside this domain and no correction is made for τ, errors in the inferred parameters quickly become unreasonable. A method for fitting single-injection data to the Michaelis-Menten or Briggs-Haldane model to simultaneously evaluate KM, k2, ΔRH, and τ is described and validated with experimental data. All four of these parameters can be accurately inferred provided the reaction time constant (k2E/KM) is larger than 1/τ and the data include enzyme saturated conditions.

  15. A novel compound DSC suppresses lipopolysaccharide-induced inflammatory responses by inhibition of Akt/NF-κB signalling in macrophages.

    Science.gov (United States)

    Liu, Xin-Hua; Pan, Li-Long; Jia, Yao-Ling; Wu, Dan; Xiong, Qing-Hui; Wang, Yang; Zhu, Yi-Zhun

    2013-05-15

    A novel compound [4-(2-acetoxy-3-((R)-3-(benzylthio)-1-methoxy-1-oxopropan-2-ylamino)-3-oxopropyl)-1,2-phenylene diacetate (DSC)], derived from Danshensu, exerted cytoprotective effects by anti-oxidative and anti-apoptotic activities in vitro. Herein, we reported the protective effects of DSC on lipopolysaccharide (LPS)-induced inflammatory responses in murine RAW264.7 macrophages and the underlying mechanisms. We showed that DSC concentration-dependently attenuated nitric oxide (NO) production and inducible nitric oxide synthase (iNOS) expression with less cytotoxicity. Signal transduction studies indicated that DSC significantly inhibited LPS-induced phosphorylation of Akt, but not c-Jun N-terminal kinase 1/2, p38, or extracellular signal-regulated kinase 1/2. Meanwhile, LPS-induced nuclear translocation of nuclear factor-κB (NF-κB) p65 was decreased by DSC. Furthermore, a phosphatidylinositol 3-kinase (PI3K) inhibitor LY294002 significantly suppressed LPS-induced NF-κB p65 nuclear translocation, iNOS expression, and NO production, which was also mimicked by pretreatment with DSC. These results suggested that DSC attenuated LPS-induced inflammatory response in macrophages, at least in part, through suppression of PI3K/Akt signaling and NF-κB activation.

  16. 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

  17. Use of calorimetry for routine dose measurement in E-beam sterilization

    Energy Technology Data Exchange (ETDEWEB)

    Coomber, Allen; Lambert, Byron J.; Riggs, Brian; Tang, Fuh-Wei; Volpone, Michael [Guidant Coporation, Ynez Rd, Temecula, CA (United States); Allen, Tom; Shaffer, Harry; Williams, C.Brian [Titan Scan Systems (United States); Miller, Arne [Riso National Laboratory, Roskilde (Denmark)

    2000-07-01

    Calorimetry is an inherently simple, accurate and precise dosimeter. Calorimetry possesses the capability to be used in e-beam sterilization facilities for both reference and routine dosimetry dose measurement. Its use for routine dosimetry has been made simple and practical at Guidant VI's small, self-shielded 10 MeV, 4 kW e-beam sterilization system due to the combination of 4 factors: Simple and convenient calorimeters. A well understood dose calibration process. A small oval conveyor design. A powerful and convenient control system for the e-beam sterilizer. Benefits of using calorimeter instead of spectrophotometric methods for routine dosimetry include increased consistency and quality of dosimetry results and reduced labor requirements (both for processing dosimeters and investigating dosimetry issues). A downside of using calorimetry is lowered efficiency of the sterilization system by about 1%, since the calorimeters take up some beam time to process. (author)

  18. Incorporación de materiales de cambio de fase en placas de yeso para almacenamiento de energía térmica mediante calor latente: caracterización térmica del material mediante la técnica DSC

    Directory of Open Access Journals (Sweden)

    Oliver, A.

    2011-06-01

    Full Text Available Differential Scanning Calorimetry (DSC is a thermal analysis technique which has been used for more than three decades to measure the temperatures and heat flows associated with transitions in materials as a function of time. Other techniques, are Differential Thermal Analysis DTA and Conventional Calorimetry. There is great uncertainty in the values supplied by the manufacturers (because they are referred to pure substances and the DSC should be used to get more accurate values. It will be analyzed the thermal storage capacity depending on temperature for several compound materials formed by some aggregates, mainly gypsum and phase change materials, in various proportions. The results have been compared with other building materials such as gypsum boards and brick layer. The suitability of the new construction material for thermal energy storage will be assessed in comparison with other materials traditionally used for this purpose.

    La Calorimetría Diferencial de Barrido es una técnica de análisis térmico, usada desde hace décadas, para medir la entalpía asociada al cambio de fase de un material como función del tiempo y de la temperatura. Otras técnicas menos utilizadas son la Calorimetría Convencional el Análisis Térmico Diferencial. Existe una gran incertidumbre en los valores de propiedades suministrados por los fabricantes (puesto que éstos se refieren a las sustancias puras y es conveniente utilizar DSC para tener valores más exactos. Se va a analizar la capacidad de almacenamiento térmico en función de la temperatura de varios materiales compuestos formados por los mismos agregados -principalmente yeso y material de cambio de fase- en distintas proporciones. Los valores obtenidos se comparan con otros materiales constructivos, yeso laminado y ladrillo. También se verifica la idoneidad del nuevo material constructivo para el almacenamiento de energía térmica frente a otros materiales utilizados

  19. Kinetics of Enzymatic High-Solid Hydrolysis of Lignocellulosic Biomass Studied by Calorimetry

    DEFF Research Database (Denmark)

    Olsen, Søren Nymand; Rasmussen, Erik Lumby; McFarland, K.C.;

    2011-01-01

    . In the current work, we have investigated the application of isothermal calorimetry to study the kinetics of enzymatic hydrolysis of two substrates (pretreated corn stover and Avicel) at high-solid contents (up to 29% w/w). It was found that the calorimetric heat flow provided a true measure of the hydrolysis...... rate with a detection limit of about 500 pmol glucose s−1. Hence, calorimetry is shown to be a highly sensitive real-time method, applicable for high solids, and independent on the complexity of the substrate. Dose–response experiments with a typical cellulase cocktail enabled a multidimensional...

  20. Conductivity, calorimetry and phase diagram of the NaHSO4–KHSO4 system

    DEFF Research Database (Denmark)

    Hind, Hamma-Cugny; Rasmussen, Søren Birk; Rogez, J.;

    2006-01-01

    Physico-chemical properties of the binary system NaHSO4-KHSO4 were studied by calorimetry and conductivity, The enthalpy of mixing has been measured at 505 K in the full composition range and the phase diagram calculated. The phase diagram has also been constructed from phase transition temperatu......Physico-chemical properties of the binary system NaHSO4-KHSO4 were studied by calorimetry and conductivity, The enthalpy of mixing has been measured at 505 K in the full composition range and the phase diagram calculated. The phase diagram has also been constructed from phase transition...

  1. Analysis of calorimetry in ultra relativistic heavy ion collisions at 200 GeV per nucleon

    International Nuclear Information System (INIS)

    We draw up in this thesis the statement of the calorimetry analysis in ultra relativistic heavy ion collisions at 200 GeV/A. NA38 experiment studies the production of dimuons correlated with neutral transverse energy flow detected by an electromagnetic calorimeter. J/Ψ suppression in central collisions could be a signature of the quark-gluon plasma (Q.G.P.). Characteristics and limits of the apparatus are briefly described. On the other hand, calorimetry measurements and analysis methods are studied in details and future developments are proposed

  2. Estimation of activity related energy expenditure and resting metabolic rate in freely moving mice from indirect calorimetry data.

    Directory of Open Access Journals (Sweden)

    Jan Bert Van Klinken

    Full Text Available Physical activity (PA is a main determinant of total energy expenditure (TEE and has been suggested to play a key role in body weight regulation. However, thus far it has been challenging to determine what part of the expended energy is due to activity in freely moving subjects. We developed a computational method to estimate activity related energy expenditure (AEE and resting metabolic rate (RMR in mice from activity and indirect calorimetry data. The method is based on penalised spline regression and takes the time dependency of the RMR into account. In addition, estimates of AEE and RMR are corrected for the regression dilution bias that results from inaccurate PA measurements. We evaluated the performance of our method based on 500 simulated metabolic chamber datasets and compared it to that of conventional methods. It was found that for a sample time of 10 minutes the penalised spline model estimated the time-dependent RMR with 1.7 times higher accuracy than the Kalman filter and with 2.7 times higher accuracy than linear regression. We assessed the applicability of our method on experimental data in a case study involving high fat diet fed male and female C57Bl/6J mice. We found that TEE in male mice was higher due to a difference in RMR while AEE levels were similar in both groups, even though female mice were more active. Interestingly, the higher activity did not result in a difference in AEE because female mice had a lower caloric cost of activity, which was likely due to their lower body weight. In conclusion, TEE decomposition by means of penalised spline regression provides robust estimates of the time-dependent AEE and RMR and can be applied to data generated with generic metabolic chamber and indirect calorimetry set-ups.

  3. 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)

  4. Isothermal Titration Calorimetry Measurements of Metal Ions Binding to Proteins.

    Science.gov (United States)

    Quinn, Colette F; Carpenter, Margaret C; Croteau, Molly L; Wilcox, Dean E

    2016-01-01

    ITC measurements involving metal ions are susceptible to a number of competing reactions (oxidation, precipitation, and hydrolysis) and coupled reactions involving the buffer and protons. Stabilization and delivery of the metal ion as a well-defined and well-characterized complex with the buffer, or a specific ligand, can suppress undesired solution chemistry and, depending on the stability of the metal complex, allow accurate measurements of higher affinity protein-binding sites. This requires, however, knowledge of the thermodynamics of formation of the metal complex and accounting for its contribution to the experimentally measured values (KITC and ΔHITC) through a post hoc analysis that provides the condition-independent binding thermodynamics (K, ΔG(o), ΔH, ΔS, and ΔCP). This analysis also quantifies the number of protons that are displaced when the metal ion binds to the protein.

  5. Experimental determination of the temperature dependence of water activities for a selection of aqueous organic solutions

    Directory of Open Access Journals (Sweden)

    G. Ganbavale

    2014-05-01

    Full Text Available This work presents experimental data of the temperature dependence of water activity in aqueous organic solutions relevant for tropospheric conditions (200–273 K. Water activity (aw at low temperatures (T is a crucial parameter for predicting homogeneous ice nucleation. We investigated temperature dependent water activities, ice freezing and melting temperatures of solutions, and vapour pressures of a selection of atmospherically relevant aqueous organic systems. To measure aw over a wide composition range and with a focus on low temperatures, we use various aw measurement techniques and instruments: a dew point water activity meter, an electrodynamic balance (EDB, differential scanning calorimetry (DSC, and a setup to measure the total gas phase pressure at equilibrium over aqueous solutions. Water activity measurements were performed for aqueous multicomponent and multifunctional organic mixtures containing the functional groups typically found in atmospheric organic aerosols, such as hydroxyl, carboxyl, ketone, ether, ester, and aromatic groups. The aqueous organic systems studied at several fixed compositions over a considerable temperature range differ significantly in their temperature dependence. Aqueous organic systems of 1,4-butanediol and methoxyacetic acid show a moderate decrease in aw with decreasing temperature. The aqueous M5 system (a multicomponent system containing five different dicarboxylic acids and aqueous 2-(2-ethoxyethoxyethanol solutions both show a strong increase of water activity with decreasing temperature at high solute concentrations for TTaw can be reversed at low temperatures and that linear extrapolations of high temperature data may lead to erroneous predictions. To avoid this, experimentally determined aw at low temperature are needed to improve thermodynamic models towards lower temperatures and for improved predictions of the ice nucleation ability of organic–water systems.

  6. NorLeu3-Angiotensin (1-7) [DSC127] as a Therapy for the Healing of Diabetic Foot Ulcers

    Science.gov (United States)

    Rodgers, Kathleen E.; Bolton, Laura L.; Verco, Shelagh; diZerega, Gere S.

    2015-01-01

    Significance: Diabetes is a disorder that is well known to delay wound repair resulting in the formation of colonized chronic wounds. Over their lifetime, diabetic patients have a 25% incidence of foot ulcers (DFUs), which contribute to increased risk of morbidity, including osteomyelitis and amputations, and increased burden to the healthcare system. Recent Advances: The only active product approved for the treatment of diabetic ulcers, Regranex®, is not widely used due to minimal proven efficacy and recent warnings added to the Instructions for Use. A novel topical agent that accelerates healing and increases the proportion of fully healed DFUs, DSC127 [aclerastide; active ingredient, NorLeu3-angiotensin (1-7) (NorLeu3-A(1-7))], is recruiting patients in Phase III clinical trials (NCT01830348 and NCT01849965). NorLeu3-A(1-7) is an analog of the naturally occurring peptide, angiotensin 1-7. The mechanisms of action include induction of progenitor proliferation, accelerated vascularization, collagen deposition, and re-epithelialization. Critical Issues: Current modalities for the treatment of DFUs include strict offloading, bandaging, debridement and, on a limited basis, application of Regranex. Novel potent therapies are needed to combat this significant burden to the diabetic patient and the healthcare system. Future Direction: Preclinical and clinical research shows that DSC127 is highly effective in the closure of diabetic wounds and is superior to Regranex in animal studies. Clinical development of DSC127 as a topical agent for the healing of DFU is underway. Further investigation into the mechanisms by which this product accelerates healing is warranted. PMID:26029484

  7. Dysspondyloenchondromatosis (DSC) associated with COL2A1 mutation: Clinical and radiological overlap with spondyloepimetaphyseal dysplasia-Strudwick type (SEMD-S).

    Science.gov (United States)

    Merrick, Blair; Calder, Alistair; Wakeling, Emma

    2015-12-01

    Dysspondyloenchondromatosis (DSC) is a rare skeletal dysplasia characterized by enchondroma-like lesions and anisospondyly. The former leads to discrepancies in limb length, and the latter, to progressive kyphoscoliosis. Two recent cases have highlighted the genetic heterogeneity of DSC, one demonstrating the presence and, the other, the absence of a COL2A1 mutation. This may have important clinical implications, for example, screening for complications including atlanto-axial instability associated with type II collagenopathies, as well as long-term patient management. We report on a case with radiographic features of DSC with overlap into the type II collagenopathy spondyloepimetaphyseal dysplasia, Strudwick type, who was found to carry a novel heterozygous mutation in the COL2A1 gene. Testing for COL2A1 mutations should be performed in all patients with radiological features of DSC. Further research is needed to identify the underlying molecular cause in cases where no COL2A1 mutation is identified.

  8. DSC及IR联合测定环氧树脂-双氰胺体系固化工艺参数%Determination of Curing Parameter for Epoxy Resin-Dicyandiamide System by DSC and IR

    Institute of Scientific and Technical Information of China (English)

    蔡晋; 董如林; 陈智栋; 金长春; 方敏

    2011-01-01

    The effect of the amount of dicyandiamide on the curing reaction of epoxy resin has been investigated , using non-isothermal DSC method and the reaction kinetics of the epoxy resin -dicyandiamide system has been studied, using DSC curves measured at different heating rates. Simultaneously, the optimum curing condition has been established , using DSC and IR analytical technique. The experimental results indicate that the optimum amount of dicyandiamide is 5. 6%, curing temperature 403K and curing time 70 min. The activation energy and reaction rate for the curing reaction of the epoxy resin-dicyandiamide system were calculated to be 96. 82 Kj/mol and 0. 93, respectively.%采用非等温DSC法研究了固化剂用量对环氧树脂固化反应的影响,同时利用不同升温速率下测得的DSC曲线研究了环氧树脂-双氰胺体系的固化反应动力学,并由DSC及IR分析技术确定了该体系的最佳反应条件.实验结果表明:固化剂双氰胺最佳用量为5.6%,最佳固化温度为403 K,固化时间为70 min,该体系的反应活化能为96.82 kJ/mol,反应级数为0.93.

  9. 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

  10. Thermoreversible gelation of cellulose acetate solutions studied by differential scanning calorimetry

    NARCIS (Netherlands)

    Altena, F.W.; Schroder, J.S.; Huls, van de R.; Smolders, C.A.

    1986-01-01

    Thermoreversible gels of cellulose acetate can be obtained by cooling concentrated cellulose acetate solutions in solvent-nonsolvent mixtures of dioxane and water. Upon heating the gels, endothermic effects were observed with differential scanning calorimetry. The heat effects are ascribed to the me

  11. Thermodynamic profiling of Peptide membrane interactions by isothermal titration calorimetry: a search for pores and micelles

    DEFF Research Database (Denmark)

    Henriksen, Jonas Rosager; Andresen, Thomas Lars

    2011-01-01

    in mixed peptide-lipid micelles. We have investigated the mode of action of the antimicrobial peptide mastoparan-X using isothermal titration calorimetry (ITC) and cryo-transmission electron microscopy (cryo-TEM). The results show that mastoparan-X induces a range of structural transitions of POPC/POPG (3...

  12. Simulating SiD Calorimetry: Software Calibration Procedures and Jet Energy Resolution

    OpenAIRE

    Cassell, Ron

    2009-01-01

    Simulated calorimeter performance in the SiD detector is examined. The software calibration procedures are described, as well as the perfect pattern recognition PFA reconstruction. Performance of the SiD calorimeters is summarized with jet energy resolutions from calorimetry only, perfect pattern recognition and the SiD PFA algorithm. Presented at LCWS08[1].

  13. Monolithic junction field-effect transistor charge preamplifier for calorimetry at high luminosity hadron colliders

    International Nuclear Information System (INIS)

    The outstanding noise and radiation hardness characteristics of epitaxial-channel junction field-effect transistors (JFET) suggest that a monolithic preamplifier based upon them may be able to meet the strict specifications for calorimetry at high luminosity colliders. Results obtained so far with a buried layer planar technology, among them an entire monolithic charge-sensitive preamplifier, are described

  14. 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...

  15. Levitation calorimetry. IV - The thermodynamic properties of liquid cobalt and palladium.

    Science.gov (United States)

    Treverton, J. A.; Margrave, J. L.

    1971-01-01

    Some of the thermodynamic properties of liquid cobalt and palladium investigated by means of levitation calorimetry are reported and discussed. The presented data include the specific heats and heats of fusion of the liquid metals, and the emissivities of the liquid metal surfaces.

  16. Determination of ice content in hardened concrete by low-temperature calorimetry

    DEFF Research Database (Denmark)

    Wu, Min; Johannesson, Björn; Geiker, Mette Rica

    2014-01-01

    Low-temperature calorimetry has been used to determine the ice content in concrete at different temperatures when exposed to low-temperature environments. However, the analysis of the ice content from the measured data of heat flow is not straightforward. In this study, two important factors...

  17. Impact of sample saturation on the detected porosity of hardened concrete using low temperature calorimetry

    DEFF Research Database (Denmark)

    Wu, Min; Johannesson, Björn

    2014-01-01

    The present work studied the impact of sample saturation on the analysis of pore volume and pore size distribution by low temperature (micro-)calorimetry. The theoretical background was examined, which emphasizes that the freezing/melting temperature of water/ice confined in non-fully saturated...

  18. Partitioning of late gestation energy expenditure in ewes using indirect calorimetry and a linear regression approach

    DEFF Research Database (Denmark)

    Kiani, Alishir; Chwalibog, André; Nielsen, Mette O;

    2007-01-01

    study metabolizable energy (ME) intake ranges for twin-bearing ewes were 220-440, 350- 700, 350-900 kJ per metabolic body weight (W0.75) at week seven, five, two pre-partum respectively. Indirect calorimetry and a linear regression approach were used to quantify EE(gest) and then partition to EE...

  19. Student Learning of Thermochemical Concepts in the Context of Solution Calorimetry.

    Science.gov (United States)

    Greenbowe, Thomas J.; Meltzer, David E.

    2003-01-01

    Analyzes student performance on solution calorimetry problems in an introductory university chemistry class. Includes data from written classroom exams for 207 students and an extensive longitudinal interview with a student. Indicates learning difficulties, most of which appear to originate from failure to understand, that net increases and…

  20. Gamma Polari-Calorimetry with SOI pixels for proposals at Extreme Light Infrastructure (ELI-NP)

    CERN Document Server

    Homma, Kensuke

    2015-01-01

    We introduce the concept of Gamma Polari-Calorimetry (GPC) dedicated for proposals at Extreme Light Infrastructure in the Romanian site (ELI-NP). A simulation study shows that an assembly of thin SOI pixel sensors can satisfy our requirements to GPC.