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Sample records for scanning calorimetry dsc

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

    Science.gov (United States)

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

    2007-12-01

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

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

    DEFF Research Database (Denmark)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-05-25

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

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

    Science.gov (United States)

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

    2018-06-01

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

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

    International Nuclear Information System (INIS)

    Marinescu, R.; Mincu, M.

    2015-01-01

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

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

    Directory of Open Access Journals (Sweden)

    R. Przeliorz

    2010-04-01

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

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

    OpenAIRE

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

    2002-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Nassu, Renata Tieko

    1999-02-01

    Full Text Available Melting point of fats is used to characterize oils and fats and is related to their physical properties, such as hardness and thermal behaviour. The present work shows the utilization of DSC technique on the determination of melting point of fats. In a comparison with softening point (AOCS method Cc 3-25, DSC values were higher than those obtained by AOCS method. It has occurred due to the fact that values obtained by DSC technique were taken when the fat had melted completely. DSC was also useful for determining melting point of liquid oils, such as soybean and cottonseed ones.

    El punto de fusión de grasas es usado para caracterizar aceites y grasas, y está relacionado con sus propiedades físicas, tales como dureza y comportamiento térmico. El presente trabajo muestra la utilización de la técnica de Calorimetría Diferencial de Barrido (DSC en la determinación del punto de fusión de grasas. En comparación con el punto de ablandamiento (AOCS método Cc 3-25, los valores de DSC fueron más altos que los obtenidos por los métodos de AOCS. Esto ha ocurrido debido al hecho que los valores obtenidos por la técnica de DSC fueron tomados cuando la grasa había fundido completamente. DSC fue también útil para determinar puntos de fusión de aceites líquidos, tales como los de soya y algodón.

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

    International Nuclear Information System (INIS)

    Dantas, J.M.; Abrao, A.

    1981-04-01

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

  11. Differential scanning calorimetry techniques: applications in biology and nanoscience.

    Science.gov (United States)

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

    2010-12-01

    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.

  12. 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.

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

    International Nuclear Information System (INIS)

    Arii, T.; Kishi, A.

    1999-01-01

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

  14. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-01

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

  16. 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.

  17. 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

  18. Analyzing Protein Denaturation using Fast Differential Scanning Calorimetry

    NARCIS (Netherlands)

    Splinter, R.; Van Herwaarden, A.W.; Iervolino, E.; Vanden Poel, G.; Istrate, D.; Sarro, P.M.

    2012-01-01

    This paper investigates the possibility to measure protein denaturation with Fast Differential Scanning Calorimetry (FDSC). Cancer can be diagnosed by measuring protein denaturation in blood plasma using Differential Scanning Calorimetry (DSC). FDSC can reduce diagnosis time from hours to minutes,

  19. 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....... The bovine serum measurements show two main peaks, in good agreement with standard DSC measurements. Olive oil has been measured, with good agreement for the cooling curve and qualitative agreement for the heater curve, compared to DSC measurements....

  20. Physicochemical characterization of pitches by differential scanning calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Lahaye, J.; Ehrburger, P.; Saint-Romain, J.L.; Couderc, P.

    1987-11-01

    The glass transition characterization of pitches has been studied by differential scanning calorimetry (d.s.c.). Experimental results and theoretical considerations indicate that: (1) the average molecular mass of pitches can be characterized by the apparent activation energy of the relaxation phenomenon of pitch molecules; (2) the molecular polydispersity is correlated with the width of the glass transition. Characterization of pitch by d.s.c. is well adapted to follow pitch transformation during heat treatment. 6 refs., 6 figs., 4 tabs.

  1. Characterization of pitches by differential scanning calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Ehrburger, P.; Martin, C.; Lahaye, J.; Saint-Romain, J.L.; Couderc, P.

    1988-12-01

    Pitch materials have generally a very complex composition with molecular mass ranging from a few hundred to several thousands units. In order to characterize these materials their properties related to the glassy transformation, in particular to enthalpy relaxation, have been investigated. Solvent soluble fractions have been characterized by differential scanning calorimetry (DSC). As with polymeric materials, enthalpy relaxation can provide information about pitches and the interactions occurring between the different types of molecules present in the pitch: mean molecular size, structural factor, molecular-size distribution. The determination of glass transition properties provides a useful means for the characterization of pitch and of their solvent extracts. It also permits insight into the complex reactions which occur when pitch materials are heat-treated. 7 refs., 2 figs., 3 tabs.

  2. Differential scanning calorimetry of bacteria.

    Science.gov (United States)

    Miles, C A; Mackey, B M; Parsons, S E

    1986-04-01

    Thermograms obtained by differential scanning calorimetry of a range of bacteria of different heat resistances were compared. Equations were derived to calculate the rate at which the numbers of viable organisms in a calorimeter decline as the temperature is raised at a constant rate. Vegetative bacteria scanned at 10 degrees C min-1 showed multi-peaked thermograms with four major peaks (denoted m, n, p and q) occurring in the regions 68-73, 77-84, 89-99 and 105-110 degrees C respectively. Exceptions were that peak m (the largest peak) occurred at 79-82 degrees C in Bacillus stearothermophilus and an additional peak, r, was detected in Escherichia coli at 119 degrees C. At temperatures below the main peak m there were major differences in thermograms between species. There was a direct relationship between the onset of thermal denaturation and the thermoresistance of different organisms. Heat-sensitive organisms displayed thermogram features which were absent in the more heat-resistant types. When samples were cooled to 5 degrees C and re-heated, a small endothermic peak, pr, was observed at the same temperature as p. Peaks p and pr were identified as the melting endotherms of DNA. In all vegetative organisms examined, maximum death rates, computed from published D and z values, occurred at temperatures above the onset of thermal denaturation, i.e. cell death and irreversible denaturation of cell components occurred within the same temperature range.

  3. Parallelism between gradient temperature raman spectroscopy and differential scanning calorimetry results

    Science.gov (United States)

    Temperature dependent Raman spectroscopy (TDR) applies the temperature gradients utilized in differential scanning calorimetry (DSC) to Raman spectroscopy, providing a straightforward technique to identify molecular rearrangements that occur just prior to phase transitions. Herein we apply TDR and D...

  4. Probing Free-Energy Surfaces with Differential Scanning Calorimetry

    Science.gov (United States)

    Sanchez-Ruiz, Jose M.

    2011-05-01

    Many aspects of protein folding can be understood in terms of projections of the highly dimensional energy landscape onto a few (or even only one) particularly relevant coordinates. These free-energy surfaces can be probed conveniently from experimental differential scanning calorimetry (DSC) thermograms, as DSC provides a direct relation with the protein partition function. Free-energy surfaces thus obtained are consistent with two fundamental scenarios predicted by the energy-landscape perspective: (a) well-defined macrostates separated by significant free-energy barriers, in some cases, and, in many other cases, (b) marginal or even vanishingly small barriers, which furthermore show a good correlation with kinetics for fast- and ultrafast-folding proteins. Overall, the potential of DSC to assess free-energy surfaces for a wide variety of proteins makes it possible to address fundamental issues, such as the molecular basis of the barrier modulations produced by natural selection in response to functional requirements or to ensure kinetic stability.

  5. Review of MEMS differential scanning calorimetry for biomolecular study

    Science.gov (United States)

    Yu, Shifeng; Wang, Shuyu; Lu, Ming; Zuo, Lei

    2017-12-01

    Differential scanning calorimetry (DSC) is one of the few techniques that allow direct determination of enthalpy values for binding reactions and conformational transitions in biomolecules. It provides the thermodynamics information of the biomolecules which consists of Gibbs free energy, enthalpy and entropy in a straightforward manner that enables deep understanding of the structure function relationship in biomolecules such as the folding/unfolding of protein and DNA, and ligand bindings. This review provides an up to date overview of the applications of DSC in biomolecular study such as the bovine serum albumin denaturation study, the relationship between the melting point of lysozyme and the scanning rate. We also introduce the recent advances of the development of micro-electro-mechanic-system (MEMS) based DSCs.

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

    Science.gov (United States)

    Ford, James L; Mann, Timothy E

    2012-04-01

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

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

    DEFF Research Database (Denmark)

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

    1997-01-01

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

  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

  9. 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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  11. Enzymatic hydrolysis of Amaranth flour - differential scanning calorimetry and scanning electron microscopy studies

    Energy Technology Data Exchange (ETDEWEB)

    Barba de la Rosa, A.P.; Paredes-Lopez, O.; Carabez-Trejo, A.; Ordorica-Falomir, C. (Instituto Politecnico Nacional, Irapuato (Mexico). Centro de Investigacion y de Estudios Avanzados)

    1989-11-01

    High-protein amaranth flour (HPAF) and carbohydrate rich fraction (CRF) were produced from raw flour in a single-step process using a heat-stable alpha-amylase preparation. Protein content of flour increased from 15 to about 30 or 39% at liquefaction temperatures of 70 or 90{sup 0}C, respectively and 30 min hydrolysis time. CRF exhibited 14-22 DE. Enzymatic action at 70{sup 0}C increased endotherm temperature and gelatinization enthalpy of HPAF, in relation to gelatinized flour, as assessed by differential scanning calorimetry (DSC). Hydrolysis at 90{sup 0}C did not affect significantly (P > 0.05) DSC peak temperature. It is suggested that these changes in DSC performance might result from differences in amount and type of low-molecular weight carbohydrates and residual starch. Scanning electron microscopy (SEM) demonstrated that hydrolysis temperature changed substantially the structural appearance of flour particles. HPAF and CRF might find applications as dry milk extender and sweetener, respectively. (orig.).

  12. Novel Technique for Quantitative Fast Scanning Calorimetry on Electrospun Fibers

    Science.gov (United States)

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

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

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

    Science.gov (United States)

    Gan, Lei; Zhang, Chunxia; Shangguan, Fangqin; Li, Xiuping

    2012-06-01

    The continuous cooling crystallization of a blast furnace slag was studied by the application of the differential scanning calorimetry (DSC) method. A kinetic model describing the correlation between the evolution of the degree of crystallization with time was obtained. Bulk cooling experiments of the molten slag coupled with numerical simulation of heat transfer were conducted to validate the results of the DSC methods. The degrees of crystallization of the samples from the bulk cooling experiments were estimated by means of the X-ray diffraction (XRD) and the DSC method. It was found that the results from the DSC cooling and bulk cooling experiments are in good agreement. The continuous cooling transformation (CCT) diagram of the blast furnace slag was constructed according to crystallization kinetic model and experimental data. The obtained CCT diagram characterizes with two crystallization noses at different temperature ranges.

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

    International Nuclear Information System (INIS)

    Rady, Mohamed

    2009-01-01

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

  15. Characterization of the phase transformations in shape-memory alloys by modulated differential scanning calorimetry

    International Nuclear Information System (INIS)

    Wei, Z.G.; Sandstroem, R.

    1999-01-01

    Modulated differential scanning calorimetry (MDSC) is a recently developed calorimetric technique, which has demonstrated some significant advantages over the conventional differential scanning calorimetry (DSC). By separating the reversing quantity from the non-reversing component in the total thermal events, it provides some new information that can not be obtained from the conventional DSC. The technique has been applied to various polycrystalline and single crystalline shape-memory alloys, including Cu-Zn-Al, Cu-Al-Ni, Ti-Ni(Cu), Ni-Mn-Ga and Fe-Mn-Si, to characterize the martensitic transformations, bainitic transformation, chemical and magnetic ordering transitions, atomic reordering and other kinetic relaxation processes in the alloys. The preliminary results of the MDSC measurements are summarized and the interpretation of the MDSC results and some factors affecting the results are discussed. (orig.)

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

  17. 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 ...

  18. Thermal behavior and phase identification of Valsartan by standard and temperature-modulated differential scanning calorimetry.

    Science.gov (United States)

    Skotnicki, Marcin; Gaweł, Agnieszka; Cebe, Peggy; Pyda, Marek

    2013-10-01

    Thermal behavior of angiotensin II type 1 (AT1) receptor antagonist, Valsartan (VAL), was examined employing thermogravimetric analysis (TGA), standard differential scanning calorimetry (DSC) and temperature-modulated differential scanning calorimetry (TMDSC). The stability of VAL was measured by TGA from 25 to 600°C. Decomposition of Valsartan starts around 160°C. The DSC curve shows two endotherms, occurring around 80°C and 100°C, related to evaporation of water and enthalpy relaxation, respectively. Valsartan was identified by DSC as an amorphous material and it was confirmed by X-ray powder diffraction. The glass transition of fresh Valsartan appears around 76°C (fictive temperature). TMDSC allows separation of the total heat flow rate into reversing and nonreversing parts. The nonreversing curve corresponds to the enthalpy relaxation and the reversing curve shows changes of heat capacity around 94°C. In the second run, TMDSC curve shows the glass transition process occurring at around 74°C. Results from standard DSC and TMDSC of Valsartan were compared over the whole range of temperature.

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

    International Nuclear Information System (INIS)

    Dantas, J.M.

    1983-01-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  2. Silk I and Silk II studied by fast scanning calorimetry

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-06-01

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

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

    OpenAIRE

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

    1998-01-01

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

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

    DEFF Research Database (Denmark)

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

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

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

    DEFF Research Database (Denmark)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  7. 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.

  8. Glass transition of anhydrous starch by fast scanning calorimetry.

    Science.gov (United States)

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

    2017-10-01

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

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

    Science.gov (United States)

    Verevkin, Sergey P; Emel'yanenko, Vladimir N; Zaitsau, Dzmitry H; Ralys, Ricardas V; Schick, Christoph

    2012-04-12

    Differential scanning calorimetry (DSC) has been used to measure enthalpies of synthesis reactions of the 1-alkyl-3-methylimidazolium bromide [C(n)mim][Br] ionic liquids from 1-methylimidazole and n-alkyl bromides (with n = 4, 5, 6, 7, and 8). The optimal experimental conditions have been elaborated. Enthalpies of formation of these ionic liquids in the liquid state have been determined using the DSC results according to the Hess Law. The ideal-gas enthalpies of formation of [C(n)mim][Br] were calculated using the methods of quantum chemistry. They were used together with the DSC results to derive indirectly the enthalpies of vaporization of the ionic liquids under study. In order to validate the indirect determination, the experimental vaporization enthalpy of [C(4)mim][Br] was measured by using a quartz crystal microbalance (QCM). The combination of reaction enthalpy measurements by DSC with modern high-level first-principles calculations opens valuable indirect thermochemical options to obtain values of vaporization enthalpies of ionic liquids.

  10. Study of gamma irradiated polyethylenes by temperature modulated differential scanning calorimetry

    International Nuclear Information System (INIS)

    Secerov, B.; Galovic, S.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

    2011-01-01

    Complete text of publication follows. The various polyethylenes (PEs) and effects of high energy radiation on theirs structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we applied the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and nonreversing part enabled to observed the low temperature enthalpy relaxation (related to the existence of the 'rigid amorphous phase') and recrystallization processes as well as to follow their and/or radiation-induced evolution of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

  11. A study of gamma-irradiated polyethylenes by temperature modulated differential scanning calorimetry

    Science.gov (United States)

    Galovic, S.; Secerov, B.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

    2012-09-01

    Various polyethylenes (PEs) and the effects of high-energy radiation on their structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we used the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of the initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and non-reversing part enabled us to observe the low-temperature enthalpy relaxation (related to the existence of the "rigid amorphous phase") and recrystallisation processes, as well as to follow their radiation-induced evolution and/or that of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

  12. Silk I and Silk II studied by fast scanning calorimetry.

    Science.gov (United States)

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

    2017-06-01

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

  13. Evaluation of aluminosilicate glass sintering during differential scanning calorimetry

    International Nuclear Information System (INIS)

    Souza, Juliana Pereira de

    2015-01-01

    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 SiO 2 .10,5 Al 2 O 3 . 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)

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

    Directory of Open Access Journals (Sweden)

    Ion Dranca

    2011-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Stéphane Gibout

    2018-01-01

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

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

    OpenAIRE

    Ion Dranca; Tudor Lupascu

    2009-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Ion Dranca

    2009-12-01

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

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

    Directory of Open Access Journals (Sweden)

    Harry O'Hanley

    2012-01-01

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

  19. Calorimetry

    International Nuclear Information System (INIS)

    Pope, B.

    1983-01-01

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

  20. Calorimetry

    International Nuclear Information System (INIS)

    McDonald, J.C.

    1978-01-01

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

  1. 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.

  2. 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.

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

    Science.gov (United States)

    Schubnell, M; Schawe, J E

    2001-04-17

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

  4. Calorimetry

    International Nuclear Information System (INIS)

    Anon.

    1982-01-01

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

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

    Science.gov (United States)

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

    2010-05-19

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Directory of Open Access Journals (Sweden)

    ATUS BUKU

    2017-02-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  9. 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

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

    Science.gov (United States)

    Boehm, K; Rösgen, J; Hinz, H-J

    2006-02-15

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

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

    Science.gov (United States)

    Toyran, Neslihan; Severcan, Feride

    2007-08-01

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

  12. 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

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

    International Nuclear Information System (INIS)

    Przeliorz, R; Piatkowski, J

    2011-01-01

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

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

    Science.gov (United States)

    Badkar, Aniket; Yohannes, Paulos; Banga, Ajay

    2006-02-17

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

  15. 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.

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

    International Nuclear Information System (INIS)

    Morris, A.; Lipe, T.

    1996-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Alexander M. Brannan

    2015-12-01

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

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

    Science.gov (United States)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2005-02-07

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    DEFF Research Database (Denmark)

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

    2000-01-01

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

  2. Temperature modulated differential scanning calorimetry. Modelling and applications

    International Nuclear Information System (INIS)

    Jiang, Z.

    2000-01-01

    DSC. Some shortcomings of TMDSC have been noticed in both modelling and application work. Firstly, any experiments for purpose of either understanding or the quantitative measurements of TMDSC output quantities should be performed under carefully selected conditions which can satisfy the linear response assumption. Secondly, some signals in particular those associated with kinetic processes may not be fully sampled by TMDSC due to the limit of the observing window of a modulation. Thirdly, the TMDSC evaluation procedure introduces mathematical artefacts into the output signals. As a consequence, it is preferable to include as many temperature modulations as possible within any transition being studied in order obtain good quality experimental signals by eliminating or minimising these artefacts. (author)

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

    Directory of Open Access Journals (Sweden)

    Gernot K.-H. Kolb

    2016-08-01

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

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2015-06-01

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

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

    International Nuclear Information System (INIS)

    Fernandez, A.M.

    2012-01-01

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

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

    Science.gov (United States)

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

    2011-01-12

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

  8. Study of phase transition in hard microcrystalline waxes and wax blends by differential scanning calorimetry

    Czech Academy of Sciences Publication Activity Database

    Kumar, S.; Agrawal, K. M.; Khan, H. U.; Sikora, Antonín

    2004-01-01

    Roč. 22, 3 & 4 (2004), s. 337-345 ISSN 1091-6466 R&D Projects: GA AV ČR KSK4050111 Institutional research plan: CEZ:AV0Z4050913 Keywords : phase transition * hard microscrystalline waxes * differential scanning calorimetry Subject RIV: CD - Macromolecular Chemistry Impact factor: 0.312, year: 2004

  9. Examination of water phase transitions in Loblolly pine and cell wall components by differential scanning calorimetry

    Science.gov (United States)

    Samuel L. Zelinka; Michael J. Lambrecht; Samuel V. Glass; Alex C. Wiedenhoeft; Daniel J. Yelle

    2012-01-01

    This paper examines phase transformations of water in wood and isolated wood cell wall components using differential scanning calorimetry with the purpose of better understanding "Type II water" or "freezable bound water" that has been reported for cellulose and other hydrophilic polymers. Solid loblolly pine (Pinus taeda...

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

    Directory of Open Access Journals (Sweden)

    Eva García-Millán

    2017-12-01

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

  11. 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.

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

    Science.gov (United States)

    Gouni, Sreeja Reddy

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

  13. Pengaruh pengawetan kulit ikan buntal (Arothon reticularis terhadap suhu kerut ditinjau melalui analisis differential scanning calorimeter (DSC

    Directory of Open Access Journals (Sweden)

    RLM. Satrio Ari Wibowo

    2015-12-01

    Full Text Available The aim of this study was to determine the effect of the skin preservation type against shrinkage temperature of leather. The material used in this study was the skin of pufferfish (Arothon reticularis that have been preserved by salting, formaldehyde and pickling and also raw skin as a reference. The method used to measure the shrinkage temperature was thermal analysis using Differential Scanning Calorimeter (DSC that operated from 4°C up to 440°C with nitrogen stream. DSC measurement results showed that shrinkage temperature of puffer fish preserved with formaldehyde was higher than salting and pickling, which is 63.64°C; 47.95°C; 57.37oC respectively. The advantage of using formaldehyde compared to others preservation technique was not only can protect the skin from damage by microorganisms, but also can create a bond with the collagen .

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Science.gov (United States)

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

    2008-07-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  17. 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.

  18. Influência de alguns parâmetros experimentais nos resultados de análises calorimétricas diferenciais - DSC

    OpenAIRE

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

    2002-01-01

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

  19. Influência de alguns parâmetros experimentais nos resultados de análises calorimétricas diferenciais - DSC

    Directory of Open Access Journals (Sweden)

    Bernal Cláudia

    2002-01-01

    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.

  20. 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

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

    International Nuclear Information System (INIS)

    Rojas, Aaron; Orozco, Eulogio

    2003-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Luis Octavio Martínez Álvarez

    2013-03-01

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

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

    Science.gov (United States)

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

    2018-04-01

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

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

    Science.gov (United States)

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

    2002-01-01

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

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

    International Nuclear Information System (INIS)

    Van Humbeeck, J.; Planes, A.

    1996-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

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

    DEFF Research Database (Denmark)

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

    2003-01-01

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

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

    Science.gov (United States)

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

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

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

    Science.gov (United States)

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

    2017-10-01

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

  14. Differential scanning microcalorimetry of intrinsically disordered proteins.

    Science.gov (United States)

    Permyakov, Sergei E

    2012-01-01

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

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

    Science.gov (United States)

    Fix, I; Steffens, K J

    2004-05-01

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

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-06-01

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

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

    Science.gov (United States)

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

    2016-04-01

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

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

    International Nuclear Information System (INIS)

    Almagor, M.; Cole, R.D.

    1989-01-01

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

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

    Science.gov (United States)

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

    1989-04-18

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

  1. Measurement for commercial exposives with SC-DSC test. Sangyoyo bakuhayaku no SC-DSC sokutei

    Energy Technology Data Exchange (ETDEWEB)

    Yabashi, H.; Wada, Y.; Hwang, D.; Akutsu, Y.; Tamura, M.; Yoshida, T. (The University of Tokyo, Tokyo (Japan). Faculty of Engineering); Matsuzawa, T. (Nippon Kayaku Co. Ltd., Tokyo (Japan))

    1991-08-30

    The sealed cell differential scanning calorimetry (SC-DSC) was sintroduced of commercial blasting explosives. As a series of testing the commercial blasting explosives in performance, an SC-DSC test was made to compare the critical detonability line with that resulting therefrom. From the result of SC-DSC measurement, the critical dilution rate was estimated of commercial blasting explosives to become without detonating propagation. As a result, all the explosives with exception of ANFO one were assumed to have a possibility of detonating propagation so that the ANFO explosive was known to be material, unable to exactly evaluate the detonability by the SC-DSC test. The explosion heat, then calculated by the REITP2 in order to assume how the reaction proceeded in the DSC cell, was compared with the reaction heat measured by the SC-DSC test. As a result, the calculated value was known to be almost equal to or slightly larger than the measured one. 15 refs., 4 figs., 2 tabs.

  2. Forensic characterization of HDPE pipes by DSC.

    Science.gov (United States)

    Sajwan, Madhuri; Aggarwal, Saroj; Singh, R B

    2008-03-05

    The melting behavior of 28 high density polyethylene (HDPE) pipe samples manufactured and supplied by 13 different manufacturers in India was examined by 'differential scanning calorimetry (DSC)' to find out if this parameter could be used in differentiating between these HDPE pipe samples which are chemically the same and being manufactured by different manufacturer. The results indicate that the melting temperature may serve as the useful criteria for differentiating HDPE (i) pipe samples from different sources and (ii) samples of different diameter from the same source.

  3. Non-isothermal dehydration kinetic study of aspartame hemihydrate using DSC, TGA and DSC-FTIR microspectroscopy

    Directory of Open Access Journals (Sweden)

    Wei-hsien Hsieh

    2018-05-01

    Full Text Available Three thermal analytical techniques such as differential scanning calorimetry (DSC, thermal gravimetric analysis (TGA using five heating rates, and DSC-Fourier Transform Infrared (DSC-FTIR microspectroscopy using one heating rate, were used to determine the thermal characteristics and the dehydration process of aspartame (APM hemihydrate in the solid state. The intramolecular cyclization process of APM anhydrate was also examined. One exothermic and four endothermic peaks were observed in the DSC thermogram of APM hemihydrate, in which the exothermic peak was due to the crystallization of some amorphous APM caused by dehydration process from hemihydrate to anhydride. While four endothermic peaks were corresponded to the evaporation of absorbed water, the dehydration of hemihydrate, the diketopiperazines (DKP formation via intramolecular cyclization, and the melting of DKP, respectively. The weight loss measured in TGA curve of APM hemihydrate was associated with these endothermic peaks in the DSC thermogram. According to the Flynn–Wall–Ozawa (FWO model, the activation energy of dehydration process within 100–150 °C was about 218 ± 11 kJ/mol determined by TGA technique. Both the dehydration and DKP formation processes for solid-state APM hemihydrate were markedly evidenced from the thermal-responsive changes in several specific FTIR bands by a single-step DSC-FTIR microspectroscopy. Keywords: Aspartame (APM hemihydrate, DSC/TGA, DSC-FTIR, Dehydration, Activation energy, DKP formation

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  5. 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.

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

    Science.gov (United States)

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

    2017-04-01

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

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

    Science.gov (United States)

    Kõiv, A; Mustonen, P; Kinnunen, P K

    1994-03-31

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

  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. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    NARCIS (Netherlands)

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

    2000-01-01

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

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

    DEFF Research Database (Denmark)

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

    2006-01-01

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

  12. 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...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

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

    International Nuclear Information System (INIS)

    Hirakawa, Satoru; Morimoto, Yoshiaki; Honda, Hisashi

    2015-01-01

    Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C x H (2x+1) OSO 3 Li (x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C x H (2x+1) OSO 3 Na and n-C x H (2x+1) OSO 3 K (x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (ΔS). For n-C 18 H 37 OSO 3 Li and n-C 20 H 41 OSO 3 Li salts, each melting point produced a small ΔS mp value compared with the total entropy change in the solid phases (ΔS tr1 +ΔS tr2 ). Additionally, Li + ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. 7 Li NMR spectra of n-C 18 H 37 OSO 3 Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals

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

    Science.gov (United States)

    Hirakawa, Satoru; Morimoto, Yoshiaki; Honda, Hisashi

    2015-04-01

    Electrical conductivity ( σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C x H (2 x+1) OSO 3Li ( x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C x H (2 x+1) OSO 3Na and n-C x H (2 x+1) OSO 3K ( x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (Δ S). For n-C 18 H 37 OSO 3Li and n-C 20 H 41 OSO 3Li salts, each melting point produced a small Δ S mp value compared with the total entropy change in the solid phases (Δ S tr1+Δ S tr2). Additionally, Li + ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. 7Li NMR spectra of n-C 18 H 37 OSO 3Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals.

  17. Determination of the oxidizing property: proposal of an alternative method based on differential scanning calorimetry

    International Nuclear Information System (INIS)

    Gigante, L.; Dellavedova, M.; Pasturenzi, C.; Lunghi, A.; Mattarella, M.; Cardillo, P.

    2008-01-01

    Determination of chemical-physical and hazardous properties of substances is a very important matter in the chemical industry, considering the growing attention of public opinion regarding safety and eco-compatibility aspects of products. In the present work, attention was focused on characterization of oxidizing properties. In case of solid compounds, the current method (Dir 84/449/CEE 6) compares the maximum combustion rate of the examined substance to the maximum combustion rate of a reference mixture. This method shows a lot of disvantages and does not provide a quantitative result. In the following work an alternative method, based on DSC measurements, is proposed for the determination of oxidizing properties. [it

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    Science.gov (United States)

    Hourston, Douglas J.; Song, Mo

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

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

    Science.gov (United States)

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

    2017-09-01

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

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

    International Nuclear Information System (INIS)

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

    1982-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    1994-01-01

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

  4. 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.

  5. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  7. Investigation on caloric requirement of biomass pyrolysis using TG-DSC analyzer

    Energy Technology Data Exchange (ETDEWEB)

    He Fang [Institute of Utilization of Biomass, Shandong University of Technology, No. 12, Zhangzhou Road, Zibo, Shandong 255049 (China)]. E-mail: hf@sdut.edu.cn; Yi Weiming [Institute of Utilization of Biomass, Shandong University of Technology, No. 12, Zhangzhou Road, Zibo, Shandong 255049 (China); Bai Xueyuan [Institute of Utilization of Biomass, Shandong University of Technology, No. 12, Zhangzhou Road, Zibo, Shandong 255049 (China)

    2006-09-15

    The caloric requirement of biomass pyrolysis has an important influence on the course of the thermal conversion. However, precise data are difficult to achieve by the current calculation method because of the complexity of the process. A new method for achieving the caloric requirement of the process by integrating the differential scanning calorimetry (DSC) curves was proposed after the simultaneous thermal analyzer (TG-DSC) and DSC curves were investigated. Experiments were conducted for wheat straw, cotton stalk, pine and peanut shell on a Netsch STA 449C analyzer. Powder samples were put into a platinum crucible with a lid on a high accuracy DSC-cp sample holder in the furnace and then heated from ambient temperature up to the maximum temperature of 973 K at the heating rate of 10 K/min in the analyzer. The product gases were swept away by 25 ml/min nitrogen. Mass changes (TG) and calorimetric effects (DSC) were recorded and analyzed. The process was investigated in detail through comparison of the DTG (differential thermogravimetric) and DSC curves of wheat straw. After the water influence in the DSC was eliminated, the relationship of the caloric requirement with the temperature of the aforementioned dry biomass was obtained by integrating the DSC curve. The results showed that 523 kJ, 459 kJ, 646 kJ and 385 kJ were required, respectively, to increase the temperature of 1 kg of dried wheat straw, cotton stalk, pine and peanut from 303 K to 673 K.

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

    NARCIS (Netherlands)

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

    1977-01-01

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

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

    NARCIS (Netherlands)

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

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

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

    NARCIS (Netherlands)

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

    2006-01-01

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

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

    Science.gov (United States)

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

    2015-06-01

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

  12. A discussion of the principles and applications of Modulated Temperature DSC (MTDSC).

    Science.gov (United States)

    Verdonck, E; Schaap, K; Thomas, L C

    1999-12-01

    The benefits of Modulated Temperature DSC (MTDSC) over conventional differential scanning calorimetry (DSC) for studying thermal transitions in materials are reviewed by means of examples. These include the separation of overlapping phenomena such as melting/recrystallization in semi-crystalline materials, the heat capacity variation and enthalpic relaxation at the glass transition, and transitions from the different components of a blend. In addition, examples are presented demonstrating the ability of MTDSC to detect subtle transitions more readily and without loss of resolution. The possibility of measuring heat capacity in quasi-isothermal conditions and the evaluation of the thermal conductivity of a material are explained.

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

    Science.gov (United States)

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

    2013-12-01

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

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

    NARCIS (Netherlands)

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

    2014-01-01

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

  15. 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

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

    Science.gov (United States)

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

    2011-05-01

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

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

    International Nuclear Information System (INIS)

    Xiao, Kechao; Vlassak, Joost J.

    2015-01-01

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

  18. Nano-DTA and nano-DSC with cantilever-type calorimeter

    International Nuclear Information System (INIS)

    Nakabeppu, Osamu; Deno, Kohei

    2016-01-01

    Highlights: • Nanocalorimetry with original cantilever type calorimeters. • The calorimeters showed the enthalpy resolution of 200 nJ level. • Nano-DTA of a binary alloy captured a probabilistic peak after solidification. • Power compensation DSC of a microgram level sample was demonstrated. • The DSC and DTA behavior were explained with a lumped model. - Abstract: Differential thermal analysis (DTA) and differential scanning calorimetry (DSC) of the minute samples in the range of microgram to nanogram were studied using original cantilever-type calorimeters. The micro-fabricated calorimeter with a heater and thermal sensors was able to perform a fast temperature scan at above 1000 K/s and a high-resolution heat measurement. The DTA of minuscule metal samples demonstrated some advances such as the thermal analysis of a 20 ng level indium and observation of a strange phase transition of a binary alloy. The power compensation type DSC using a thermal feedback system was also performed. Thermal information of a microgram level sample was observed as splitting into the DSC and DTA signals because of a mismatch between the sample and the calorimeter. Although there remains some room for improvement in terms of the heat flow detection, the behavior of the compensation system in the DSC was theoretically understood through a lumped model. Those experiments also produced some findings, such as a fin effect with sample loading, a measurable weight range, a calibration of the calorimeter and a product design concept. The development of the nano-DTA and nano-DSC will enable breakthroughs for the fast calorimetry of the microscopic size samples.

  19. A study of phase separation in peptide-loaded HPMC films using T(zero)-modulated temperature DSC, atomic force microscopy, and scanning electron microscopy.

    Science.gov (United States)

    Hussain, Samana; Grandy, David B; Reading, Mike; Craig, Duncan Q M

    2004-07-01

    Despite the widespread use of drug-loaded polymeric systems, there is still considerable uncertainty with regard to the nature of the distribution of the drug within the polymer matrix. The aim of this investigation was to develop thermal and microscopic techniques whereby the miscibility and spatial distribution of a model peptide, cyclosporin A (CyA), in hydroxypropyl methylcellulose (HPMC) films may be studied. The new technique of T(zero)-modulated temperature differential scanning calorimetry (T(zero) MTDSC), scanning electron microscopy (SEM), and pulse force mode atomic force microscopy (PFM-AFM) were used in conjunction to study films prepared using a solvent evaporation process, with a solvent extraction study performed to elucidate the nature of the observed phases. T(zero) MTDSC studies showed glass transitions for both the HPMC and CycA, with the T(g) for the HPMC and CycA seen for the mixed systems. SEM showed two spherical phases of differing electron density. PFM-AFM also showed spheres of differing adhesion that increased in size on addition of drug. Pixel intensity analysis indicated that the smaller spheres corresponded to CycA. Exposure of the films to dichloromethane, in which CycA is soluble but HPMC is not, resulted in the presence of voids that corresponded well to the spheres suggested to correspond to the drug. It was concluded that the system had undergone extensive or complete phase separation, and that the thermal and microscopic techniques outlined above are an effective means by which this issue may be studied. Copyright 2004 Wiley-Liss, Inc. and the American Pharmacists Association J Pharm Sci 93:1672-1681, 2004

  20. Determining the thermodynamic melting parameters of sulfamethoxazole, trimethoprim, urea, nicodin, and their double eutectics by differential scanning calorimetry

    Science.gov (United States)

    Agafonova, E. V.; Moshchenskii, Yu. V.; Tkachenko, M. L.

    2013-08-01

    The literature data on the thermodynamic melting characteristics of sulfamethoxazole, urea, trimethoprim, and nicodin are analyzed for individual compounds. Their enthalpies and melting points, either individually or in the composition of eutectics, are found by means of DSC. The entropies of fusion and the cryoscopic constants of individual compounds are calculated.

  1. Identification of nanostructural development in epoxy polymer layered silicate nanocomposites from the interpretation of differential scanning calorimetry and dielectric spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Roman, Frida, E-mail: roman@mmt.upc.edu [Laboratori de Termodinamica, Departament de Maquines i Motors Termics, ETSEIAT, Universitat Politecnica de Catalunya, Carrer Colom 11, 08222 Terrassa (Spain); Calventus, Yolanda, E-mail: calventus@mmt.upc.edu [Laboratori de Termodinamica, Departament de Maquines i Motors Termics, ETSEIAT, Universitat Politecnica de Catalunya, Carrer Colom 11, 08222 Terrassa (Spain); Colomer, Pere, E-mail: colomer@mmt.upc.edu [Laboratori de Termodinamica, Departament de Maquines i Motors Termics, ETSEIAT, Universitat Politecnica de Catalunya, Carrer Colom 11, 08222 Terrassa (Spain); Hutchinson, John M., E-mail: hutchinson@mmt.upc.edu [Laboratori de Termodinamica, Departament de Maquines i Motors Termics, ETSEIAT, Universitat Politecnica de Catalunya, Carrer Colom 11, 08222 Terrassa (Spain)

    2012-08-10

    Highlights: Black-Right-Pointing-Pointer Comparison of DSC and DRS in the cure of epoxy nanocomposites. Black-Right-Pointing-Pointer Dependence of exfoliation of nanocomposite on clay content. Black-Right-Pointing-Pointer Anionically initiated homopolymerisation in PLS nanocomposites. - Abstract: The effect of nanoclay on the non-isothermal cure kinetics of polymer layered silicate nanocomposites based upon epoxy resin is studied by calorimetric techniques (DSC and TGA) and by dielectric relaxation spectroscopy (DRS) in non-isothermal cure at constant heating rate. The cure process takes place by homopolymerisation, initiated anionically using 3 wt% dimethylaminopyridine (DMAP), and the influence of the nanoclay content has been analysed. Interesting differences are observed between the nanocomposites with 2 wt% and 5 wt% clay content. At low heating rates, these samples vitrify and then devitrify during the cure. For the sample with 2 wt% clay, the devitrification is accompanied by a thermally initiated homopolymerisation, which can be identified by DRS but not by DSC. The effect of this is to improve the exfoliation of the nanocomposite with 2 wt% clay, as verified by transmission electron microscopy, with a corresponding increase in the glass transition temperature. These observations are interpreted in respect of the nanocomposite preparation method and the cure kinetics.

  2. Identification of nanostructural development in epoxy polymer layered silicate nanocomposites from the interpretation of differential scanning calorimetry and dielectric spectroscopy

    International Nuclear Information System (INIS)

    Román, Frida; Calventus, Yolanda; Colomer, Pere; Hutchinson, John M.

    2012-01-01

    Highlights: ► Comparison of DSC and DRS in the cure of epoxy nanocomposites. ► Dependence of exfoliation of nanocomposite on clay content. ► Anionically initiated homopolymerisation in PLS nanocomposites. - Abstract: The effect of nanoclay on the non-isothermal cure kinetics of polymer layered silicate nanocomposites based upon epoxy resin is studied by calorimetric techniques (DSC and TGA) and by dielectric relaxation spectroscopy (DRS) in non-isothermal cure at constant heating rate. The cure process takes place by homopolymerisation, initiated anionically using 3 wt% dimethylaminopyridine (DMAP), and the influence of the nanoclay content has been analysed. Interesting differences are observed between the nanocomposites with 2 wt% and 5 wt% clay content. At low heating rates, these samples vitrify and then devitrify during the cure. For the sample with 2 wt% clay, the devitrification is accompanied by a thermally initiated homopolymerisation, which can be identified by DRS but not by DSC. The effect of this is to improve the exfoliation of the nanocomposite with 2 wt% clay, as verified by transmission electron microscopy, with a corresponding increase in the glass transition temperature. These observations are interpreted in respect of the nanocomposite preparation method and the cure kinetics.

  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. 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)

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

    Science.gov (United States)

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

    2017-01-01

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

  6. A DSC analysis of inverse salt-pair explosive composition

    Energy Technology Data Exchange (ETDEWEB)

    Babu, E. Suresh; Kaur, Sukhminder [Central Forensic Science Laboratory, Explosives Division, Ramanthapur, Hyderabad 500013 (India)

    2004-02-01

    Alkali nitrates are used as an ingredient in low explosive compositions and pyrotechnics. It has been suggested that alkali nitrates can form inverse salt-pair explosives with the addition of ammonium chloride. Therefore, the thermal behavior of low explosive compositions containing potassium nitrate mixed with ammonium chloride has been studied using Differential Scanning Calorimetry (DSC). Results provide information about the ion exchange reaction between these two chemical substances and the temperature region at which the formation of a cloud of salt particles of potassium chloride takes place. Furthermore, the addition of ammonium chloride quenches the flame of deflagrating compositions and causes the mixture to undergo explosive decomposition at relatively low temperatures. (Abstract Copyright [2004], Wiley Periodicals, Inc.)

  7. The influence of glass fibers on the morphology of β-nucleated isotactic polypropylene evaluated by differential scanning calorimetry

    Directory of Open Access Journals (Sweden)

    Janevski Aco

    2015-01-01

    Full Text Available The presence of fillers/fibers can significantly affect the polymorphic behavior of semi-crystalline polymers. The influence of glass fibers on morphology of β-nucleated iPP during isothermal and nonisothermal crystallization was analyzed in detail by DSC, and the kinetics and thermodynamic parameters were determined for the systems containing 10-60 % glass fibers. The presence of glass fibers in model composites with β-iPP has insignificant effect on the morphology of the polymer. Thermodynamic and kinetics parameters of crystallization of iPP in model composites are close to those obtained for the nucleated polymer. The relative content of β-crystalline phase is slightly affected by increasing glass fiber’s content from 10 % mas to 60 % mas, due to appearance of α-crystallites. However, the stability of β-crystalline phase is decreased by the increasing glass fibers content and there appeared certain amount of β1 and β2 phases which are known as disposed to recrystallization.

  8. Stochastic temperature modulation: A new technique in temperature-modulated DSC

    International Nuclear Information System (INIS)

    Schawe, J.E.K.; Huetter, T.; Heitz, C.; Alig, I.; Lellinger, D.

    2006-01-01

    A new temperature-modulated differential scanning calorimetry (TMDSC) technique is introduced. The technique is based on stochastic temperature modulation and has been developed as a consequence of a generalized theory of a temperature-modulated DSC. The quasi-static heat capacity and the frequency-dependent complex heat capacity can be determined over a wide frequency range in one single measurement without further calibration. Furthermore, the reversing and non-reversing heat flows are determined directly from the measured data. Examples show the frequency dependence of the glass transition, the isothermal curing of thermosets and a solid-solid transition

  9. STRUCTURAL AND MECHANICAL CHARACTERIZATION OF DEFORMED POLYMER USING CONFOCAL RAMAN MICROSCOPY AND DSC

    Directory of Open Access Journals (Sweden)

    Birgit Neitzel

    2016-02-01

    Full Text Available Polymers have various interesting properties, which depend largely on their inner structure. One way to influence the macroscopic behaviour is the deformation of the polymer chains, which effects the change in microstructure. For analyzing the microstructure of non-deformed and deformed polymer materials, Raman spectroscopy as well as differential scanning calorimetry (DSC were used. In the present study we compare the results for crystallinity measurements of deformed polymers using both methods in order to characterize the differences in micro-structure due to deformation. The study is ongoing, and we present the results of the first tests.

  10. Study of thermal transitions in polymers by a multifrequency modulated DSC technique

    OpenAIRE

    Fraga Rivas, Iria

    2010-01-01

    Premi extraordinari doctorat curs 2009-2010, àmbit de Ciències Differential Scanning Calorimetry (DSC) is one of the most widely used thermal analysis techniques for the study of transitions and relaxation processes in polymers and also in other materials. It measures the heat flow as a function of time and/or temperature, and determines the energy released or absorbed by a sample when it is heated (cooled) or maintained at a constant temperature. Its advantages are that it is fast a...

  11. X-ray and DSC studies on the melt-recrystallization process of poly(butylene naphthalate)

    International Nuclear Information System (INIS)

    Yasuniwa, Munehisa; Tsubakihara, Shinsuke; Fujioka, Takashi

    2003-01-01

    Melt-recrystallization in the heating process of poly(butylene naphthalate) (PBN) was studied with X-ray analysis and differential scanning calorimetry (DSC). DSC melting curve of an isothermally crystallized sample showed double endothermic peaks. With increasing the temperature, wide-angle X-ray diffraction (WAXD) patterns of the sample were obtained successively. Crystal structure did not change during the double melting process. The X-ray diffraction intensity decreased gradually in the temperature region up to about 200 deg. C, and then increased distinctly before steep decrease due to the final melting. This increase is interpreted as a proof of recrystallization. The temperature derivative curve of the diffraction intensity was similar to the DSC melting curve

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Woolley, E.M.

    2007-01-01

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

  16. DSC and HRTEM investigation of the precipitates in Al-1.0%Mg{sub 2} Si-0.5%Ag alloy

    Energy Technology Data Exchange (ETDEWEB)

    Gaber, A.; Ali, A.M.; Zou, Y. [Toyama University (Japan). Venture Business Laboratory; Matsuda, K.; Ikeno, S. [Toyama University (Japan). Faculty of Engineering

    2004-12-15

    The understanding and control of nanoscale precipitation in an Al-1.0 wt-%Mg{sub 2} Si-0.5 wt-% Ag alloy during artificial aging is critical for achieving optimum mechanical properties. To achieve this objective, both differential scanning calorimetry (DSC) and high resolution transmission electron microscopy (HRTEM) have been utilised. The non-isothermal DSC thermograms exhibited eight reaction peaks; six are exothermic (precipitation) and two are endothermic (dissolution) reactions. The activation energies associated with the individual precipitates are determined. With the aid of HRTEM, the evolved precipitates have been characterised. (author)

  17. A DSC study of zinc binding to bovine serum albumin (BSA

    Directory of Open Access Journals (Sweden)

    SANJA OSTOJIC

    2007-04-01

    Full Text Available The thermal denaturation of bovine serum albumin (BSA is a kinetically and thermodynamically controlled process. The effects of zinc binding to bovine serum albumin (BSA, followed by differential scanning calorimetry (DSC, were investigated in this work, with the purpose of obtaining a better understanding of the albumin/zinc interaction. From the DSC curves, the thermodynamic parameters of protein denaturation were obtained, i.e., the temperature of thermal transition maximum (Tm, calorimetric enthalpy (DHcal, van't Hoff enthalpy (DHvH, the number of binding sites (I, II, the binding constants for each binding site (KbI, KbII and the average number of ligands bound per mole of native protein XN. The thermodynamic data of protein unfolding showed that zinc binding to bovine serum albumin increases the stability of the protein (higher values of DHcal and the different ratio DHcal/DHvH indicates the perturbation of the protein during thermal denaturation.

  18. In-situ study of the thermal properties of hydrate slurry by high pressure DSC

    Energy Technology Data Exchange (ETDEWEB)

    Sari, O.; Hu, J.; Brun, F.; Erbeau, N. [Institute of Thermal Engineering, University of Applied Sciences of Western Switzerland, Yverdon-les-Bains (Switzerland); Homsy, P. [Nestec, Vevey (Switzerland); Logel, J.-C. [Axima Refrigeration, Bischheim (France)

    2008-07-01

    Knowing the enthalpy of hydrate slurry is very essential for energy balance and industrial applications. No direct measurement processes had been developed in this field in the past time. A new experimental method with special device has been developed to carry out on-line measurement of the thermal properties for hydrate slurry under dynamic conditions. With this special device, it is possible to deliver the hydrate slurry to the high pressure DSC (Differential Scanning Calorimetry) directly from the production tank or pipes. Thermal data acquisition will be performed afterwards by DSC. The investigated conditions were at pressure of 30 bar and temperature of {approx}+7 {sup o}C. The dissociation enthalpy of CO{sub 2} hydrate slurry was about 54 kJ/kg, corresponding 10.8% of solid fraction. The on-line measurement results for CO{sub 2} hydrate slurry give a good tendency to apply this phase change slurry to the industrial refrigeration process. (author)

  19. Comparing Single-Point and Multi-point Calibration Methods in Modulated DSC

    Energy Technology Data Exchange (ETDEWEB)

    Van Buskirk, Caleb Griffith [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-06-14

    Heat capacity measurements for High Density Polyethylene (HDPE) and Ultra-high Molecular Weight Polyethylene (UHMWPE) were performed using Modulated Differential Scanning Calorimetry (mDSC) over a wide temperature range, -70 to 115 °C, with a TA Instruments Q2000 mDSC. The default calibration method for this instrument involves measuring the heat capacity of a sapphire standard at a single temperature near the middle of the temperature range of interest. However, this method often fails for temperature ranges that exceed a 50 °C interval, likely because of drift or non-linearity in the instrument's heat capacity readings over time or over the temperature range. Therefore, in this study a method was developed to calibrate the instrument using multiple temperatures and the same sapphire standard.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-04-15

    Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C {sub x}H{sub (2x+1)}OSO{sub 3}Li (x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C {sub x}H{sub (2x+1)}OSO{sub 3}Na and n-C {sub x}H{sub (2x+1)}OSO{sub 3}K (x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (ΔS). For n-C {sub 18}H{sub 37}OSO{sub 3}Li and n-C {sub 20}H{sub 41}OSO{sub 3}Li salts, each melting point produced a small ΔS{sub mp} value compared with the total entropy change in the solid phases (ΔS{sub tr1}+ΔS{sub tr2}). Additionally, Li {sup +} ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. {sup 7}Li NMR spectra of n-C {sub 18}H{sub 37}OSO{sub 3}Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li {sup +} ions are localized at asymmetric sites in the crystals.

  1. 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

  2. Unique cold-crystallization behavior and kinetics of biodegradable poly[(butylene succinate)-co adipate] nanocomposites: a high speed differential scanning calorimetry study

    CSIR Research Space (South Africa)

    Bandyopadhyay, J

    2014-08-01

    Full Text Available . The effect of such structural changes on the cold-crystallization behavior and kinetics of PBSANCs were investigated using a high-speed DSC. Surprisingly, the DSC thermograms revealed that the characteristic cold-crystallization peak of neat PBSA shifts...

  3. Rheological and DSC study of sol-gel transition in aqueous dispersions of industrially important polymers and colloids

    Energy Technology Data Exchange (ETDEWEB)

    Nishinari, K. [Osaka City Univ. (Japan). Dept. of Food and Nutrition

    1997-12-01

    Gelation kinetics, mechanical spectra, thermal scanning rheology (TSR), and differential scanning calorimetry (DSC) in aqueous solutions of gelling polymers and colloids such as seaweed polysaccharides (agarose, carrageenans), microbial polysaccharides (gellan, curdlan), plant polysaccharides (methylcellulose), globular proteins (casein, glycinin, {beta}-conglycinin), fibrous proteins (gelatin, fibrin), and polyvinyl alcohol, which are related to foods, cosmetics, biomedical and pharmaceutical applications, are described. Some gelation processes at a constant temperature have been treated successfully by an equation of first order kinetics or by other modified equations, and the molecular mechanism of gel formation is discussed briefly. For water-soluble polymers, the criterion of the gel or sol based on the frequency dependence of storage and loss moduli gives valuable informations. TSR and DSC are complementary, and the combination of these methods has been proved to be useful. (orig.) 81 refs.

  4. 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.

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

    International Nuclear Information System (INIS)

    Matricarde Falleiro, Rafael M.; Akisawa Silva, Luciana Y.; Meirelles, Antonio J.A.; Krähenbühl, Maria A.

    2012-01-01

    Highlights: ► Vapor pressure data of fatty acids were measured by Differential Scanning Calorimetry. ► The DSC technique is especially advantageous for expensive chemicals. ► High heating rate was used for measuring the vapor pressure data. ► Antoine constants were obtained for the selected fatty acids. - Abstract: The vapor pressure data for lauric (C 12:0 ), myristic (C 14:0 ), palmitic (C 16:0 ), stearic (C 18:0 ) and oleic (C 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 −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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-07-14

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

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Hourston Douglas J.

    2001-01-01

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

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

    Science.gov (United States)

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

    2017-01-01

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

  10. ceramics by differential scanning calorimetry

    Indian Academy of Sciences (India)

    Administrator

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

  11. The Use of Quasi-Isothermal Modulated Temperature Differential Scanning Calorimetry for the Characterization of Slow Crystallization Processes in Lipid-Based Solid Self-Emulsifying Systems

    OpenAIRE

    Otun, Sarah O.; Meehan, Elizabeth; Qi, Sheng; Craig, Duncan Q. M.

    2014-01-01

    Purpose Slow or incomplete crystallization may be a significant manufacturing issue for solid lipid-based dosage forms, yet little information is available on this phenomenon. In this investigation we suggest a novel means by which slow solidification may be monitored in Gelucire 44/14 using quasi-isothermal modulated temperature DSC (QiMTDSC). Methods Conventional linear heating and cooling DSC methods were employed, along with hot stage microscopy (HSM), for basic thermal profiling of Geluc...

  12. 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.

  13. AC susceptibility, XRD and DSC studies of Sm1-xGdxMn2Si2 silicides

    International Nuclear Information System (INIS)

    Kervan, S.; Kilic, A.; Gencer, A.

    2004-01-01

    X-ray powder diffraction, AC susceptibility and differential scanning calorimetry (DSC) studies were performed on the polycrystalline Sm 1-x Gd x Mn 2 Si 2 (0≤x≤1) compounds. All compounds investigated crystallize in the body-centered tetragonal ThCr 2 Si 2 -type structure with the space group I4/mmm. Substitution of Gd for Sm leads to a linear decrease of the lattice constants and the unit cell volume. The lattice constants and the unit cell volume obey Vegard's law. At low temperatures, the rare earth sublattice orders and reconfigures the ordering in the Mn sublattice. The samples with x=0.6 and 0.8 exhibit spin reorientation phenomenon. The Neel temperature T N (Mn) determined by DSC technique and the Curie temperature T C (RE) increase linearly with increasing Gd content x. The results are summarized in the x-T magnetic phase diagram

  14. DSC studies of retrogradation and amylose-lipid transition taking place in gamma-irradiated wheat starch

    International Nuclear Information System (INIS)

    Ciesla, K.; Gluszewski, W.; Eliasson, A.C.

    2006-01-01

    It has been already shown that degradation resulting from gamma irradiation induces a decrease in order of starch granules and influences gelatinisation taking place during heating of starch and flour suspensions. In presented paper, DSC (differential scanning calorimetry) studies were carried out for wheat starch, non-irradiated and irradiated using doses in the range from 5 to 30 kGy. The influence of the conditions applied during DSC measurements on the possibility to observe differences between the amylose-lipid complex transition and retrogradation taking place in the non-irradiated and particularly irradiated starch samples was checked. The better differentiation between the amylose-lipid complex transition taking place in particular samples accompanied by the better reproducity were obtained in the case of dense suspensions as compared to the watery suspensions as well as during the first analysis performed for the recrystallised gels

  15. DSC analysis of irradiated proteins from Crotalus durissus terrificus

    International Nuclear Information System (INIS)

    Oliveira, Karina Corleto de; Silva, Monica Nascimento da; Goncalves, Karina de Oliveira; Spencer, Patrick Jack; Nascimento, Nanci do

    2011-01-01

    Full text: Snake bites are a serious public health problem, especially in subtropical countries. In Brazil, the serum, the only effective treatment in case of snake bites, is produced in horses which, despite the large size, have a reduced lifespan due to the high toxicity of the antigen. It is known that ionizing radiation effects - direct and indirect - can modify the molecular structure, affecting the biological properties of proteins. Ionizing radiation has been employed to attenuate the toxicity of snake venoms, aiming to generate an improved antigen with low toxicity. Two proteins, purified from Crotalus durissus terrificus (Cdt) venom were tested in this work: crotoxin and crotamine. Crotoxin, the main toxic compound of Cdt venom, is a heterodimeric protein composed of two subunits: crotapotin and phospholipase A2. Crotamine is a highly basic polypeptide (pI - 10.3), with myotoxic activity and molecular weight of 4882 Da. It is composed of 42 amino acids residues and reticulated by three disulfide bonds. This study aimed to investigate the effects of radiation on crotoxin and crotamine using Differential Scanning Calorimetry (DSC). After isolation of the toxins by chromatographic techniques, they were irradiated with 2.0 kGy from 60 Co source. The thermodynamics analysis, carried out in a METTLER TOLEDO, DSC 822e calorimeter, showed that irradiation promoted changes of the calorimetric profile. These changes suggest that, although radiation induced structural modifications of the protein, denaturation was only partial, since transition states could still be detected, suggesting that some structural elements were still present after irradiation. Taken together, our data suggest that following irradiation, the molecules underwent conformational changes, and that the remaining structural elements displayed a lower enthalpy, clearly indicating that the previously described loss of toxicity of irradiated toxins can be mostly ascribed to structural changes

  16. DSC analysis of irradiated proteins from Crotalus durissus terrificus

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina Corleto de; Silva, Monica Nascimento da; Goncalves, Karina de Oliveira; Spencer, Patrick Jack; Nascimento, Nanci do [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    Full text: Snake bites are a serious public health problem, especially in subtropical countries. In Brazil, the serum, the only effective treatment in case of snake bites, is produced in horses which, despite the large size, have a reduced lifespan due to the high toxicity of the antigen. It is known that ionizing radiation effects - direct and indirect - can modify the molecular structure, affecting the biological properties of proteins. Ionizing radiation has been employed to attenuate the toxicity of snake venoms, aiming to generate an improved antigen with low toxicity. Two proteins, purified from Crotalus durissus terrificus (Cdt) venom were tested in this work: crotoxin and crotamine. Crotoxin, the main toxic compound of Cdt venom, is a heterodimeric protein composed of two subunits: crotapotin and phospholipase A2. Crotamine is a highly basic polypeptide (pI - 10.3), with myotoxic activity and molecular weight of 4882 Da. It is composed of 42 amino acids residues and reticulated by three disulfide bonds. This study aimed to investigate the effects of radiation on crotoxin and crotamine using Differential Scanning Calorimetry (DSC). After isolation of the toxins by chromatographic techniques, they were irradiated with 2.0 kGy from {sup 60}Co source. The thermodynamics analysis, carried out in a METTLER TOLEDO, DSC 822e calorimeter, showed that irradiation promoted changes of the calorimetric profile. These changes suggest that, although radiation induced structural modifications of the protein, denaturation was only partial, since transition states could still be detected, suggesting that some structural elements were still present after irradiation. Taken together, our data suggest that following irradiation, the molecules underwent conformational changes, and that the remaining structural elements displayed a lower enthalpy, clearly indicating that the previously described loss of toxicity of irradiated toxins can be mostly ascribed to structural changes

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

    International Nuclear Information System (INIS)

    Stavrou, Elissaios; Kripotou, Sotiria; Raptis, Constantine; Turrell, Sylvia; Syassen, Karl

    2011-01-01

    Raman scattering and differential scanning calorimetry (DSC) measurements have been carried out in four mixed (TeO 2 ) 1-x (ZnO) 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 g , were Q is the heating rate) plots, and the glass transition width ΔT g . Also, from the low-frequency Raman scattering, and in particular the boson peak intensity of the glasses at T g , we have estimated the fragility ratio r R (T g ) = I min /I max whose value serves as another (empirical) fragility criterion. Finally, from high pressure Raman measurements on the glasses, we have estimated the Grueneisen parameter γ T for each glass, which constitutes the fourth fragility parameter adopted in this work. Considering the four parameters ΔT g , m, r (T g ) and γ 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.)

  18. The use of quasi-isothermal modulated temperature differential scanning calorimetry for the characterization of slow crystallization processes in lipid-based solid self-emulsifying systems.

    Science.gov (United States)

    Otun, Sarah O; Meehan, Elizabeth; Qi, Sheng; Craig, Duncan Q M

    2015-04-01

    Slow or incomplete crystallization may be a significant manufacturing issue for solid lipid-based dosage forms, yet little information is available on this phenomenon. In this investigation we suggest a novel means by which slow solidification may be monitored in Gelucire 44/14 using quasi-isothermal modulated temperature DSC (QiMTDSC). Conventional linear heating and cooling DSC methods were employed, along with hot stage microscopy (HSM), for basic thermal profiling of Gelucire 44/14. QiMTDSC experiments were performed on cooling from the melt, using a range of incremental decreases in temperature and isothermal measurement periods. DSC and HSM highlighted the main (primary) crystallization transition; solid fat content analysis and kinetic analysis were used to profile the solidification process. The heat capacity profile from QiMTDSC indicated that after an initial energetic primary crystallisation, the lipid underwent a slower period of crystallization which continued to manifest at much lower temperatures than indicated by standard DSC. We present evidence that Gelucire 44/14 undergoes an initial crystallization followed by a secondary, slower process. QIMTDSC appears to be a promising tool in the investigation of this secondary crystallization process.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-06-10

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

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

    Science.gov (United States)

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

    2006-03-09

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

  2. Development of a certified reference material for calibration of DSC and DTA below room temperature: NMIJ CRM 5401-a, Cyclohexane for Thermal Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Shimizu, Yoshitaka, E-mail: y-shimizu@aist.go.jp; Ohte, Yoko; Kato, Kenji

    2013-09-20

    Highlights: • We developed a new CRM for quality assurance of DSC and DTA below room temperature. • Certified values are temperatures and enthalpies of two phase transitions. • Certified values agree with literature values. • Certified values are determined by adiabatic calorimetry and traceable to the SI. • Purity of this CRM was confirmed more than 0.9999. - Abstract: For the quality assurance of performance of differential scanning calorimeters (DSC) and differential thermal analyzers (DTA) below room temperature, we have developed “NMIJ CRM 5401-a, Cyclohexane for Thermal Analysis” applicable to calibration of DSC and DTA in the low temperature. Adiabatic calorimetry was used to measure the temperatures and enthalpies of solid–solid phase transition and fusion as certified values, and to determine the purity in amount of substance fraction as information. The certified values are consistent with their corresponding literature values within expanded uncertainties and have traceability to the SI. Purity in amount of substance fraction was measured by fractional melting method based on freezing point depression method and was confirmed to be more than 0.9999. NMIJ CRM 5401-a was produced based on a quality system in compliance with ISO Guide 34: 2000. We demonstrate the usefulness of NMIJ CRM 5401-a in the calibration, quality control, and validation aspects of DSC and DTA.

  3. Nucleation in As2Se3 glass studied by DSC

    International Nuclear Information System (INIS)

    Svoboda, Roman; Málek, Jiří

    2014-01-01

    Highlights: • Nucleation behavior of As 2 Se 3 glass was studied by DSC in dependence on particle size. • Correlation between the enthalpies of fusion and crystallization were confirmed. • Apart from classical heterogeneous nucleation a second nucleation mechanism was found. • Rapid formation of crystallization centers from a damaged glassy structure occurs. • Mechanical defects seem to partially suppress the CNT nucleation process. - Abstract: Differential scanning calorimetry was used to study nucleation behavior in As 2 Se 3 glass, dependent on particle size. The nucleation process was examined for a series of different coarse powders; the nucleation rate was estimated from the proportion of the crystalline material fraction. The enthalpy of fusion was utilized in this respect, and a correlation between ΔH m and ΔH c was confirmed. Two mechanisms of nucleus formation were found: classical heterogeneous nucleation (following CNT) and so-called “activation” of mechanically-induced defects. The latter appears to represent rapid formation of crystallization centers from a damaged glassy structure, where complete saturation occurs for fine powders in the range of 195–235 °C. A high amount of mechanical defects, on the other hand, was found to partially suppress the CNT nucleation process

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

    Energy Technology Data Exchange (ETDEWEB)

    Tseng, J.M.; Huang, S.T. [Institute of Safety and Disaster Prevention Technology, Central Taiwan University of Science and Technology, 666, Buzih Road, Beitun District, Taichung 40601, Taiwan, ROC (China); Duh, Y.S.; Hsieh, T.Y.; Sun, Y.Y. [Department of Safety Health and Environmental Engineering, National United University, Miaoli, Taiwan, ROC (China); Lin, J.Z. [Institute of Safety and Disaster Prevention Technology, Central Taiwan University of Science and Technology, 666, Buzih Road, Beitun District, Taichung 40601, Taiwan, ROC (China); Wu, H.C. [Institute of Occupational Safety and Health, Council of Labor Affairs, Taipei, Taiwan, ROC (China); Kao, C.S., E-mail: jcsk@nuu.edu.tw [Department of Safety Health and Environmental Engineering, National United University, Miaoli, Taiwan, ROC (China)

    2013-08-20

    Highlights: • Metal nanopowders are common and frequently employed in industry. • Nano iron powder experimental results of T{sub o} 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 (T{sub o}), peak of temperature (T{sub p}), and heat of reaction (ΔH). The nano iron powder experimental results of T{sub o} 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.

  5. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-08-10

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

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

    Science.gov (United States)

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

    2003-10-01

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

  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. Evaluation of the interaction of surfactants with stratum corneum model membrane from Bothrops jararaca by DSC.

    Science.gov (United States)

    Baby, André Rolim; Lacerda, Aurea Cristina Lemos; Velasco, Maria Valéria Robles; Lopes, Patrícia Santos; Kawano, Yoshio; Kaneko, Telma Mary

    2006-07-06

    The interaction of surfactants sodium dodecyl sulfate (SDS), cetyl trimethyl ammonium chloride (CTAC) and lauryl alcohol ethoxylated (12 mol ethylene oxide) (LAE-12OE) was evaluated on the stratum corneum (SC) of shed snake skins from Bothrops jararaca, used as model membrane, and thermal characterized by differential scanning calorimetry (DSC). Surfactant solutions were employed above of the critical micellar concentration (CMC) with treatment time of 8h. The SDS interaction with the SC model membrane has increased the characteristic transition temperature of 130 degrees C in approximately 10 degrees C for the water loss and keratin denaturation, indicating an augmentation of the water content. Samples treated with CTAC have a decrease of the water loss temperature, while, for the LAE-12OE treated samples, changes on the transition temperature have not been observed.

  10. The Study of Phase Transformations of AlSi9Cu3 Alloy by DSC Method

    Directory of Open Access Journals (Sweden)

    Piątkowski J.

    2016-12-01

    Full Text Available With the use of differential scanning calorimetry (DSC, the characteristic temperatures and enthalpy of phase transformations were defined for commercial AlSi9Cu3 cast alloy (EN AC-46000 that is being used for example for pressurized castings for automotive industry. During the heating with the speed of 10°C·min−1 two endothermic effects has been observed. The first appears at the temperature between 495 °C and 534 °C, and the other between 555 °C and 631 °C. With these reactions the phase transformation enthalpy comes up as +6 J g−1 and +327 J g−1. During the cooling with the same speed, three endothermic reactions were observed at the temperatures between 584 °C and 471 °C. The total enthalpy of the transitions is – 348 J g−1.

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

    International Nuclear Information System (INIS)

    Iijima, Mika; Hatakeyama, Tatsuko; Hatakeyama, Hyoe

    2012-01-01

    Research highlights: ► Locust bean gum forms hydrogels by freezing and thawing. ► Syneresis was observed when freezing and thawing cycle (n) increased. ► Dynamic Young's modulus increased with increasing n. ► Non-freezing water content restrained by hydrogels decreased with increasing n. ► 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′) 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.

  12. Comparison between DSC and TMDSC in the investigation into frozen aqueous cryoprotectants solutions.

    Science.gov (United States)

    Santoveña, A; Piñero, M J; Llabrés, M

    2010-12-01

    The influence of thermal parameters in the observation of thermal events and in the calculation of heat transformation in aqueous cryoprotectant solutions after freezing was investigated using conventional differential scanning calorimetry (DSC) and temperature-modulated DSC (TMDSC), respectively. The systems under study were formed by pure water and diluted aqueous solutions of mannitol, trehalose, sucrose, sorbitol, and glycine. The influence of different combinations of frequency and amplitude was analyzed in heating-cooling and heating-iso TMDSC scans. Trehalose, sucrose, and sorbitol present a lesser critical temperature of primary drying than other cryoprotectants studied. The calorimetric variables selection is crucial to detect or not the thermal events, or to detect so with different numerical values. Then, the values of the calorimetric parameters determined are different if measured in a mode of heating-cooling or heating-iso. The TMDSC method-1 used in this study employs a higher number of cycles in each thermal event. The use of Lissajous figures and the study of the C(p in-phase) signal evolution will allow us to understand the complexity of the events detected. The comparative study of both techniques points to the selection of conventional or modulated technique depending on the type of system and the nature of the studied events.

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

    International Nuclear Information System (INIS)

    Zvetkov, V.L.; Djoumaliisky, S.; Simeonova-Ivanova, E.

    2013-01-01

    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. The Application of ATD and DSC Methods to Study of the EN AC-48000 Alloy Phase Transformations

    Directory of Open Access Journals (Sweden)

    Piątkowski J.

    2017-06-01

    Full Text Available Tests concerning EN AC 48000 (AlSi12CuNiMg alloy phase transition covered (ATD thermal analysis and (DSC differential scanning calorimetry specifying characteristic temperatures and enthalpy of transformations. ATD thermal analysis shows that during cooling there exist: pre-eutectic crystallization effect of Al9Fe2Si phase, double eutectic and crystallization α(Al+β(Si and multi-component eutectic crystallization. During heating, DSC curve showed endothermic effect connected with melting of the eutectic α(Al+β(Si and phases: Al2Cu, Al3Ni, Mg2Si and Al9Fe2Si being its components. The enthalpy of this transformation constitutes approx. +392 J g-1. During freezing of the alloy, DSC curve showed two exothermal reactions. One is most likely connected with crystallization of Al9Fe2Si phase and the second one comes from freezing of the eutectic α(Al+β(Si. The enthalpy of this transformation constitutes approx. -340 J g-1. Calorimetric test was accompanied by structural test (SEM conducted with the use of optical microscope Reichert and scanning microscope Hitachi S-4200. There occurred solution’s dendrites α(Al, eutectic silicon crystal (β and two types of eutectic solution: double eutectic α(Al+β(Si and multi-component eutectic α+AlSiCuNiMg+β.

  16. Crystallization of Polymers Investigated by Temperature-Modulated DSC

    OpenAIRE

    Maria Cristina Righetti

    2017-01-01

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

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

    DEFF Research Database (Denmark)

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

    1996-01-01

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

  18. 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

  19. Simultaneous formation and detection of the reaction product of solid-state aspartame sweetener by FT-IR/DSC microscopic system.

    Science.gov (United States)

    Lin, S Y; Cheng, Y D

    2000-10-01

    The solid-state stability of aspartame hemihydrate (APM) sweetener during thermal treatment is important information for the food industry. The present study uses the novel technique of Fourier transform infrared microspectroscopy equipped with differential scanning calorimetry (FT-IR/DSC microscopic system) to accelerate and determine simultaneously the thermal-dependent impurity formation of solid-state APM. The results indicate a dramatic change in IR spectra from 50, 110 or 153 degrees C, which was respectively attributed to the onset temperature of water evaporation, dehydration and cyclization processes. It is suggested that the processes of dehydration and intramolecular cyclization occurred in the solid-state APM during the heating process. As an impurity, 3-carboxymethyl-6-benzyl-2,5-diketopiperazine (DKP) degraded from solid state APM via intramolecular cyclization and liberation of methanol. This was evidenced by this novel FT-IR/DSC microscopic system in a one-step procedure.

  20. 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.

  1. Hydriding properties of amorphous Ni-B alloy studied by DSC and thermogravimetry

    International Nuclear Information System (INIS)

    Spassov, T.; Rangelova, V.

    1999-01-01

    The hydrogenation behaviour of melt-spun Ni 81.5 B 18.5 amorphous alloy was studied by means of differential scanning calorimetry (DSC) and thermogravimetry (TG) and compared with the hydriding properties of a Fe-B-Si glass. It was found that the amorphous Ni-B alloy absorbs larger amounts of hydrogen than the Fe-B-Si glass, as the initial kinetics of hydrogen absorption and desorption of both the alloys are comparable. Hydrogen absorption and desorption reactions in Ni-B were observed to proceed with similar rates at ca. 300 K. The hydrogen desorption is revealed in DSC as an endothermic peak in the 350-450 K range, preceding the crystallization peak of the amorphous alloy. The enthalpy of hydrogen desorption (ΔH des =22 kJ/mol H 2 ) for Ni-B was found to be smaller than that for the Fe-B-Si glass, which finding is in contrast to the results on hydrogen diffusion in crystalline αFe and Fe-based alloys and Ni and Ni-based alloys. The hydrogen desorption temperature and enthalpy for Ni 81.5 B 18.5 were found to be independent of the amount of hydrogen absorbed. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  2. 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. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    McCabe, J F; Wilson, H J

    1980-03-01

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

  4. Estudio cinético del efecto de polifenilsulfona sobre el curado de una resina epoxi/amina mediante calorimetría diferencial de barrido convencional y modulada con temperatura: parte II Kinetic study on the effect of curing polyphenylsulfone epoxy resin/amina by differential calorimetry scanning conventional and modulated temperature: part II

    Directory of Open Access Journals (Sweden)

    Asdrúbal J. Cedeño

    2010-01-01

    Full Text Available En este trabajo se estudió el efecto de la adición del termoplástico lineal polifenilsulfona (PPSU, sobre la cinética de reacción y las propiedades térmicas de una resina epoxídica basada en diglicidil éter de bisfenol - A (DGEBA, curada con diaminodifenilsulfona (DDS. El estudio cinético y la caracterización se realizaron mediante calorimetría diferencial de barrido, DSC estándar y modulado, bajo condiciones isotérmicas y dinámicas. La cinética del curado se discutió en el marco de tres modelos cinéticos: Kissinger, Flynn-Wall-Ozawa y el modelo cinético de orden n. Para describir la reacción de curado en su última etapa, se usó la relación semiempírica propuesta por Chern y Poehlein para considerar la influencia de la difusión sobre la rapidez de reacción. El mecanismo de curado, para todos los sistemas, se ajustó a una cinética de orden n, a pesar del contenido de PPSU, y se observó que éste se hace muy controlado por la difusión conforme aumenta el contenido de PPSU y conforme la temperatura de curado disminuye. El tiempo de vitrificación de los sistemas exhibió una fuerte dependencia con el contenido de PPSU.In this work we studied the effect of the addition of the linear thermoplastic polyphenyl sulfone (PPSU on the cure kinetics and the thermal properties of a resin based on diglycidyl ether of bisphenol-A (DGEBA, cured with 4,4´-diaminodiphenyl sulfone (DDS. The kinetic study and the characterization process have been carried out by using differential scanning calorimetry, DSC, and temperature modulated DSC (TMDSC, under isothermal and dynamic conditions. The curing kinetics was discussed in the framework of three kinetic models: Kissinger, Flynn-Wall-Ozawa, and the model of reaction of order n. To describe the cured reaction in its last stage, we have used the semiempirical relationship proposed by Chern and Poehlein to take into account the influence of diffusion on the reaction rate. The cure mechanism

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

    Directory of Open Access Journals (Sweden)

    Luis Octavio Martínez Álvarez

    2011-03-01

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

  6. 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)

  7. 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

    2014-08-08

    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. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Application of in-situ nano-scanning calorimetry and X-ray diffraction to characterize Ni–Ti–Hf high-temperature shape memory alloys

    Energy Technology Data Exchange (ETDEWEB)

    McCluskey, Patrick J., E-mail: mccluske@ge.com [GE Global Research, One Research Circle, Niskayuna, NY 12309 (United States); Xiao, Kechao [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States); Gregoire, John M. [Joint Center for Artificial Photosynthesis, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Dale, Darren [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Vlassak, Joost J. [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States)

    2015-03-10

    Combinatorial nanocalorimetry and synchrotron X-ray diffraction were combined to study the martensite–austenite (M–A) phase transformation behavior of Ni–Ti–Hf shape memory alloys. A thin-film library of Ni–Ti–Hf samples with a range of compositions was deposited on a parallel nano-scanning calorimeter device using sputter deposition. Crystallization of each amorphous as-deposited sample by local heating at approximately 10{sup 4} K/s produced a nanoscale grain structure of austenite and martensite. Individual samples were then cycled through the M–A transformation, while the transformation enthalpy was measured by nanocalorimetry and the low- and high-temperature phase compositions were determined by X-ray diffraction. The techniques enable correlation of the observed behavior during thermal cycling with the thermodynamic and structural properties of the samples.

  9. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-03-01

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

  12. Improving a variation of the DSC technique for measuring the boiling points of pure compounds at low pressures

    International Nuclear Information System (INIS)

    Troni, Kelly L.; Damaceno, Daniela S.; Ceriani, Roberta

    2016-01-01

    Highlights: • Improvement of a variation of the DSC technique for boiling points at low pressures. • Use of a ballpoint pen ball over the pinhole of the DSC crucible. • Effects of configuration variables of the DSC technique accounted by factorial design. • An optimized region was obtained and tested for selected compounds. - Abstract: This study aims to improve a variation of the differential scanning calorimetry (DSC) technique for measuring boiling points of pure compounds at low pressures. Using a well-known n-paraffin (n-hexadecane), experimental boiling points at a pressure of 3.47 kPa with u(P) = 0.07 kPa were obtained by using a variation of the DSC technique, which consists of placing samples inside hermetically sealed aluminum crucibles, with a pinhole (diameter of 0.8 mm) made on the lid and a tungsten carbide ball with a diameter of 1.0 mm over it. Experiments were configured at nine different combinations of heating rates (K·min"−"1) and sample sizes (mg) following a full factorial design (2"2 trials plus a star configuration and three central points). Individual and combined effects of these two independent variables on the difference between experimental and estimated boiling points (NIST Thermo Data Engine v. 5.0 – Aspen Plus v. 8.4) were investigated. The results obtained in this work reveal that although both factors affect individually the accuracy of this variation of the DSC technique, the effect of heating rate is the most important. An optimized region of combinations of heating rate and sample size for determining boiling points of pure compounds at low pressures was obtained using the response-surface methodology (RSM). Within this optimized region, a selected condition, combining a heating rate of 24.52 K·min"−"1 and a sample size of (4.6 ± 0.5) mg, was tested for six different compounds (92.094–302.37 g mol"−"1) comprising four fatty compounds (tributyrin, monocaprylin, octanoic acid and 1-octadecanol), glycerol and n

  13. 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.

  14. 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)

    International Nuclear Information System (INIS)

    Gonzalez, Lidia; Ramis, Xavier; Salla, Josep Maria; Mantecon, Ana; Serra, Angels

    2007-01-01

    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 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 3 .MEA and lanthanide triflates initiated curing systems follow a complete different kinetic model. Among lanthanide triflates, ytterbium is the most active initiator

  15. 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.

  16. Scintillator plate calorimetry

    International Nuclear Information System (INIS)

    Price, L.E.

    1990-01-01

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

  17. 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.

  18. Calorimetry for the SSC

    International Nuclear Information System (INIS)

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

    1984-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  20. Combination of (M)DSC and surface analysis to study the phase behaviour and drug distribution of ternary solid dispersions.

    Science.gov (United States)

    Meeus, Joke; Scurr, David J; Chen, Xinyong; Amssoms, Katie; Davies, Martyn C; Roberts, Clive J; Van den Mooter, Guy

    2015-04-01

    Miscibility of the different compounds that make up a solid dispersion based formulation play a crucial role in the drug release profile and physical stability of the solid dispersion as it defines the phase behaviour of the dispersion. The standard technique to obtain information on phase behaviour of a sample is (modulated) differential scanning calorimetry ((M)DSC). However, for ternary mixtures (M)DSC alone is not sufficient to characterize their phase behaviour and to gain insight into the distribution of the active pharmaceutical ingredient (API) in a two-phased polymeric matrix. MDSC was combined with complementary surface analysis techniques, specifically time-of-flight secondary ion mass spectrometry (ToF-SIMS) and atomic force microscopy (AFM). Three spray-dried model formulations with varying API/PLGA/PVP ratios were analyzed. MDSC, TOF-SIMS and AFM provided insights into differences in drug distribution via the observed surface coverage for 3 differently composed ternary solid dispersions. Combining MDSC and surface analysis rendered additional insights in the composition of mixed phases in complex systems, like ternary solid dispersions.

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

    Science.gov (United States)

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

    2007-06-29

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

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

    Science.gov (United States)

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

    2009-01-01

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

  3. Calorimetry at the SSC

    International Nuclear Information System (INIS)

    Wigmans, R.

    1988-01-01

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

  4. Calorimetry at the SSC

    International Nuclear Information System (INIS)

    Wigmans, R.

    1987-09-01

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

  5. 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.

  6. Two DSC Glass Transitions in Miscible Blends of Polyisoprene / Poly(4-tert-butyl styrene)

    Science.gov (United States)

    Zhao, Junshu; Sun, Ye; Yu, Lian; Ediger, Mark

    2009-03-01

    Conventional and temperature modulated differential scanning calorimetry experiments have been carried out on miscible blends of polyisoprene (PI) and poly(4-tert-butyl styrene) (P4tBS) over a broad composition range. This system is characterized by an extraordinarily large component Tg difference (˜215 K) between the two homopolymers. Two distinct calorimetric Tgs were observed in blends with an intermediate composition range (25%˜50% PI) by both conventional and temperature modulated DSC. Good agreement was found between the Tg values measured by the two methods. Fitting of the measured Tgs to the Lodge-McLeish model gives a φself of 0.62˜0.64 for PI in this blend and 0.02˜0.05 for P4tBS. The extracted φself for PIis comparable to reported values for PEO in blends with PMMA and is significantly larger than those reported for other PI blends with smaller component Tg differences. This observation suggests the presence of a confinement effect in PI/P4tBS blends, which results in enhanced fast component dynamics below the effective Tg of the slow component.

  7. TG-FTIR, DSC and quantum chemical studies of the thermal decomposition of quaternary methylammonium halides

    International Nuclear Information System (INIS)

    Sawicka, Marlena; Storoniak, Piotr; Skurski, Piotr; Blazejowski, Jerzy; Rak, Janusz

    2006-01-01

    The thermal decomposition of quaternary methylammonium halides was studied using thermogravimetry coupled to FTIR (TG-FTIR) and differential scanning calorimetry (DSC) as well as the DFT, MP2 and G2 quantum chemical methods. There is almost perfect agreement between the experimental IR spectra and those predicted at the B3LYP/6-311G(d,p) level: this has demonstrated for the first time that an equimolar mixture of trimethylamine and a methyl halide is produced as a result of decomposition. The experimental enthalpies of dissociation are 153.4, 171.2, and 186.7 kJ/mol for chloride, bromide and iodide, respectively, values that correlate well with the calculated enthalpies of dissociation based on crystal lattice energies and quantum chemical thermodynamic barriers. The experimental activation barriers estimated from the least-squares fit of the F1 kinetic model (first-order process) to thermogravimetric traces - 283, 244 and 204 kJ/mol for chloride, bromide and iodide, respectively - agree very well with theoretically calculated values. The theoretical approach assumed in this work has been shown capable of predicting the relevant characteristics of the thermal decomposition of solids with experimental accuracy

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-10-15

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  10. RheoDSC: A hyphenated technique for the simultaneous measurement of calorimetric and rheological evolutions

    OpenAIRE

    Kiewiet, S; Janssens, V; Miltner, H. E; Van Assche, Gert; Van Puyvelde, Peter; Van Mele, B

    2008-01-01

    A newly developed hyphenated technique is presented combining an existing rheometer and differential scanning calorimeter into a single experimental setup. Through the development of a fixation accessory for differential scanning calorimeter (DSC) crucibles and a novel rotor, the simultaneous measurement is performed inside the well-controlled thermal environment of a Tzero (TM) DSC cell. Hence, the evolution of thermal and flow properties of a material can be simultaneously measured using st...

  11. Recent developments in silicon calorimetry

    International Nuclear Information System (INIS)

    Brau, J.E.

    1990-11-01

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

  12. Crystallization of Polymers Investigated by Temperature-Modulated DSC

    Directory of Open Access Journals (Sweden)

    Maria Cristina Righetti

    2017-04-01

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

  13. DSC, FT-IR, NIR, NIR-PCA and NIR-ANOVA for determination of chemical stability of diuretic drugs: impact of excipients

    Directory of Open Access Journals (Sweden)

    Gumieniczek Anna

    2018-03-01

    Full Text Available It is well known that drugs can directly react with excipients. In addition, excipients can be a source of impurities that either directly react with drugs or catalyze their degradation. Thus, binary mixtures of three diuretics, torasemide, furosemide and amiloride with different excipients, i.e. citric acid anhydrous, povidone K25 (PVP, magnesium stearate (Mg stearate, lactose, D-mannitol, glycine, calcium hydrogen phosphate anhydrous (CaHPO4 and starch, were examined to detect interactions. High temperature and humidity or UV/VIS irradiation were applied as stressing conditions. Differential scanning calorimetry (DSC, FT-IR and NIR were used to adequately collect information. In addition, chemometric assessments of NIR signals with principal component analysis (PCA and ANOVA were applied.

  14. Scintillating-fibre calorimetry

    International Nuclear Information System (INIS)

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

    1995-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

    Sližová, M.; Raab, Miroslav

    2013-01-01

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

  16. DSC Studies of Retrogradation and Amylose-Lipid Complex Transition Taking Place in Gamma Irradiated Wheat Starch

    International Nuclear Information System (INIS)

    Ciesla, K.

    2006-01-01

    Degradation resulting from gamma irradiation induces decrease in order of starch granules and influences the processes occurring in starch-water system. Differential scanning calorimetry (DSC) was applied at present for studying the effect of radiation with doses of 5 - 30 kGy on amylose-lipid complex transition and retrogradation occurring in wheat starch gels. Influence of the conditions applied during DSC measurements and intermediate storage was tested on the possibility to observe radiation effect. Wheat starch was irradiated with 60 C o gamma rays in a gamma cell Issledovatiel placed in the Department of Radiation Chemistry, INCT. DSC measurements were performed for ca. 50% and ca. 20% gels during heating - cooling - heating cycles (up to 3 cycles) in the temperature range 10 - 150 degree at heating and cooling rates of 10, 5 and 2.5 degree min - 1. The Seiko DSC 6200 calorimeter was used. Decrease in amylose-lipid complex transition temperature was found already after irradiation of wheat starch with a dose of 5 kGy showing modificatin of the complex structure. The differences between the irradiated and the non-irradiated samples became the easier seen in the every foregoing heating or cooling cycle as compared to the preceeding one. It is because that thermal treatment causes decrease of transition temperature in all the irradiated samples, with no effect or increase of that temperature observed in the non-irradiated ones. Irradiation hinders retrogradation taking place in ca. 50% gels but facilitates retrogradation occurring in ca. 20 % gels. Moreover, the expanded differences between the amylose-lipid complex formed in the irradiated and non-irradiated gels result due to their recrystallisation. Storage of the gels induces decrease in the temperature of the complex transition as compared to the last cycle of the first analysis. That decrease was, however, more significant in the case of all the irradiated samples than in the case of the initial sample. In

  17. Laser-flash calorimetry

    International Nuclear Information System (INIS)

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

    1982-01-01

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

  18. 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

  19. TOPEM, a new temperature modulated DSC technique - Application to the glass transition of polymers

    OpenAIRE

    Fraga Rivas, Iria; Montserrat Ribas, Salvador; Hutchinson, John M.

    2007-01-01

    TOPEM is a new temperature modulated DSC technique, introduced by Mettler-Toledo in late 2005, in which stochastic temperature modulations are superimposed on the underlying rate of a conventional DSC scan. These modulations consist of temperature pulses, of fixed magnitude and alternating sign, with random durations within limits specified by the user. The resulting heat flow signal is analysed by a parameter estimation method which yields a so-called ‘quasi-static’ specific heat capac...

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

    International Nuclear Information System (INIS)

    Cunico, Larissa P.; Damaceno, Daniela S.; Matricarde Falleiro, Rafael M.; Sarup, Bent; Abildskov, Jens; Ceriani, Roberta; Gani, Rafiqul

    2015-01-01

    Highlights: • Novel VLE data for binary mixtures involving a partial acylglycerol (monocaprylin). • Use of a promising technique for measuring VLE/vapour pressure data (DSC technique). • The consistency of experimental data is analysed by a proposed methodology. • Regressed parameters are given for excess Gibbs thermodynamic models. • New regressed parameters are presented for UNIFAC to account for nonidealities. - Abstract: 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 Wilson, NRTL and UNIQUAC models. The original UNIFAC group contribution method is also considered and new binary interaction parameters for the main groups CH 2 , CCOO, OH and COOH are regressed, to account for the non-idealities found in these lipid systems. Established thermodynamic consistency tests are applied and attest the quality of the measured data. In terms of relevance of the selected components, system 1 can be found in the purification and deodorization steps during the production of edible oils, while, system 2 can be found in the purification steps of biodiesel. It should be noted that no such data could be found in the open literature, not only for the specific components selected but also for the combination of the classes of components considered; that is, acylglycerol plus fatty acid or fatty ester.

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

    International Nuclear Information System (INIS)

    Lang, Peter; Wojcik, Tomasz; Povoden-Karadeniz, Erwin; Falahati, Ahmad; Kozeschnik, Ernst

    2014-01-01

    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

  2. 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.

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

    Science.gov (United States)

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

    2012-01-05

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

  4. The effects of urea and n-propanol on collagen denaturation: using DSC, circular dicroism and viscosity

    International Nuclear Information System (INIS)

    Usha, R.; Ramasami, T.

    2004-01-01

    The effect of urea and n-propanol on circular dichroism (CD) and viscosity of purified type1 collagen solution at various temperatures and differential scanning calorimetry (DSC) of rat-tail tendon (RTT) collagen fibre have been studied. CD reveals a spectrum with a positive peak at around 220 nm and a negative peak at 200 nm characteristics of collagen triple helix. The molar ellipticity decreases as the concentration of urea increases up to particular concentration (collagen solution treated with 265 μM of urea) and after that it increases (collagen solution treated with 500 μM of urea). There is a linear decrease in molar ellipticity as the concentration of n-propanol increases. Denaturation temperature of urea and n-propanol treated with purified collagen solution has been studied using viscosity method. Additives such as urea and n-propanol decrease the thermal stability of collagen triple helix in solution and in RTT collagen fibre. Thermal helix to coil transition of urea and n-propanol treated collagen depends on the degree of hydration and the concentration of these additives. Thermodynamic parameters such as the peak temperature, enthalpy of activation, and energy of activation for collagen-gelatin transition for native, urea and n-propanol treated RTT collagen fibre has been calculated using DSC. The change in the thermodynamic parameters has been observed for native, urea and n-propanol treated RTT collagen fibres. The experimental results show that the change in the water structure, dehydration and desolvation induced by different additives such as urea and n-propanol on RTT may vary with the type of denaturation

  5. 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. Copyright © 2013 Wiley Periodicals, Inc.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-12-01

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

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  8. 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. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Magoń, A.; Pyda, M.

    2013-01-01

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

  10. Dynamics of Polymorphic Transformations in Palm Oil, Palm Stearin and Palm Kernel Oil Characterized by Coupled Powder XRD-DSC.

    Science.gov (United States)

    Zaliha, Omar; Elina, Hishamuddin; Sivaruby, Kanagaratnam; Norizzah, Abd Rashid; Marangoni, Alejandro G

    2018-06-01

    The in situ polymorphic forms and thermal transitions of refined, bleached and deodorized palm oil (RBDPO), palm stearin (RBDPS) and palm kernel oil (RBDPKO) were investigated using coupled X-ray diffraction (XRD) and differential scanning calorimetry (DSC). Results indicated that the DSC onset crystallisation temperature of RBDPO was at 22.6°C, with a single reflection at 4.2Å started to appear from 23.4 to 17.1°C, and were followed by two prominent exothermic peaks at 20.1°C and 8.5°C respectively. Further cooling to -40°C leads to the further formation of a β'polymorph. Upon heating, a of β'→βtransformation was observed between 32.1 to 40.8°C, before the sample was completely melted at 43.0°C. The crystallization onset temperature of RBDPS was 44.1°C, with the appearance of the α polymorph at the same temperature as the appearance of the first sharp DSC exothermic peak. This quickly changed from α→β´ in the range 25 to 21.7°C, along with the formation of a small β peak at -40°C. Upon heating, a small XRD peak for the β polymorph was observed between 32.2 to 36.0°C, becoming a mixture of (β´+ β) between 44.0 to 52.5°C. Only the β polymorph survived further heating to 59.8°C. For RBDPKO, the crystallization onset temperature was 11.6°C, with the formation of a single sharp exothermic peak at 6.5°C corresponding to the β' polymorphic form until the temperature reached -40°C. No transformation of the polymorphic form was observed during the melting process of RBDPKO, before being completely melted at 33.2°C. This work has demonstrated the detailed dynamics of polymorphic transformations of PKO and PS, two commercially important hardstocks used widely by industry and will contribute to a greater understanding of their crystallization and melting dynamics.

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Science.gov (United States)

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

    2009-01-01

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

  13. 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...

  14. Calorimetry end-point predictions

    International Nuclear Information System (INIS)

    Fox, M.A.

    1981-01-01

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

  15. Development of Resistive Micromegas for Sampling Calorimetry

    Science.gov (United States)

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

    2018-02-01

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

  16. DSC and Raman studies of silver borotellurite glasses

    Science.gov (United States)

    Kaur, Amandeep; Khanna, Atul; Gonzàlez, Fernando

    2016-05-01

    Silver borotellurite glasses of composition: xAg2O-yB2O3-(100-x-y)TeO2 (x=20-mol%, y = 0, 10, 20 and 30-mol%) were prepared and characterized by density, X-ray diffraction (XRD), differential scanning calorimetry, and Raman spectroscopy. XRD confirmed the amorphous structure of all samples. Density of glasses decreases while the glass transition temperature increases with increase in B2O3 content from 10 to 30-mol%. Raman study shows that coordination number of Te with oxygen decreases steadily from 3.42 to 3.18 on adding B2O3 due to the transformation of TeO4 into TeO3 units.

  17. Evaluation of the quasi-isothermal method of modulated DSC for heat capacity measurement

    International Nuclear Information System (INIS)

    Venkata Krishnan, R.; Nagarajan, K.

    2004-01-01

    Heat capacity measurements were carried out on ThO 2 by Modulated Differential Scanning Calorimetry (MDSC) using quasi-isothermal method in the temperature range 323-723 K. The highest accuracy of the heat capacity data obtained by this method was ± 2-3% which is much lower than that reported in the literature. (author)

  18. 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

  19. Competitive crystallization of a propylene/ethylene random copolymer filled with a β-nucleating agent and multi-walled carbon nanotubes. Conventional and ultrafast DSC study.

    Science.gov (United States)

    Papageorgiou, Dimitrios G; Papageorgiou, George Z; Zhuravlev, Evgeny; Bikiaris, Dimitrios; Schick, Christoph; Chrissafis, Konstantinos

    2013-11-27

    A propylene/ethylene polymeric matrix was reinforced by the simultaneous addition of a β-nucleating agent (calcium pimelate) and multi-walled carbon nanotubes (MWCNTs) in various concentrations. The present manuscript explores the competitive crystallization tendency that is caused by the presence of the two fillers. On the one hand, calcium pimelate forces the material to crystallize predominantly in the β-crystalline form, while, on the other, the strong α-nucleating ability of MWCNTs compels the material to develop higher α-crystalline content. An in-depth study has been performed on the nanocomposite samples by means of conventional, temperature-modulated, and differential fast scanning calorimetry (DFSC) under various dynamic and isothermal conditions. The results showed that β-crystals are predominant at low MWCNT content (DSC, and the use of very high cooling rates by UFDSC made it possible to achieve and study the nucleation of the samples. The presence of MWCNTs enabled the nanocomposites to crystallize faster under both isothermal and dynamic conditions. The activation energy of the samples was also calculated according to Friedman's theory.

  20. Water calorimetry: The heat defect

    International Nuclear Information System (INIS)

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

    1997-01-01

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

  1. Calorimetric sensitivity and thermal resolution of a novel miniaturized ceramic DSC chip in LTCC technology

    Energy Technology Data Exchange (ETDEWEB)

    Missal, Wjatscheslaw, E-mail: wmissal@gmx.net [Department of Functional Materials, University of Bayreuth, 95440 Bayreuth (Germany); Kita, Jaroslaw [Department of Functional Materials, University of Bayreuth, 95440 Bayreuth (Germany); Wappler, Eberhard [wsk Mess- und Datentechnik GmbH, Gueterbahnhofstr. 1, 63450 Hanau (Germany); Bechtold, Franz [VIA electronic GmbH, Robert-Friese-Str. 3, 07629 Hermsdorf (Germany); Moos, Ralf [Department of Functional Materials, University of Bayreuth, 95440 Bayreuth (Germany)

    2012-09-10

    Highlights: Black-Right-Pointing-Pointer Unique vertical design of a DSC device manufactured in the low-cost LTCC technology and therefore capable of one-way use. Black-Right-Pointing-Pointer Fully functional DSC device with a size of only 1.5 mm Multiplication-Sign 11 mm Multiplication-Sign 39 mm enabling very low power consumption. Black-Right-Pointing-Pointer Comparable measurement performance as conventional DSC whilst also suitable for mobile thermal analysis. Black-Right-Pointing-Pointer Thermal resolution is 0.12 (TAWN test). Repeatability of the peak area is within 0.3% for indium samples. Black-Right-Pointing-Pointer Calorimetric sensitivity: linear with regard to temperature and independent from sample mass and heating rate in wide ranges. - Abstract: The calorimetric properties of a novel miniaturized ceramic differential scanning calorimeter device (MC-DSC) with integrated heater and crucible are presented. All features of a conventional DSC apparatus (including oven) are integrated into this DSC device of the size 11 mm Multiplication-Sign 39 mm Multiplication-Sign 1.5 mm. The MC-DSC device is suitable for one-way use, since it is fully manufactured in the low-cost planar low temperature co-fired ceramics technology. First characterization of this device is performed using indium, tin and zinc samples. The calorimetric sensitivity at 156.6 Degree-Sign C is 0.24 J/ Degree-Sign C s. It depends linearly on temperature in the range of at least 150 Degree-Sign C and 420 Degree-Sign C. The calorimetric sensitivity is constant up to an enthalpy of fusion of at least {Delta}H = 750 mJ (at 156.6 Degree-Sign C). The thermal analysis of indium in direct contact to the crucible of the chip even reveals a constant calorimetric sensitivity up to an enthalpy of fusion of at least {Delta}H = 1000 mJ. The repeatability of the peak area is within {+-}0.3% (11 mg indium, 10 measurements). The thermal resolution determined using 4,4 Prime -azoxyanisole under TAWN test

  2. 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 ...

  3. Tritium inventory measurements using calorimetry

    International Nuclear Information System (INIS)

    Kapulla, H.; Kraemer, R.; Heine, R.

    1992-01-01

    In the past calorimetry has been developed as a powerful tool in radiometrology. Calorimetric methods have been applied for the determination of activities, half lives and mean energies released during the disintegration of radioactive isotopes. The fundamental factors and relations which determine the power output of radioactive samples are presented and some basic calorimeter principles are discussed in this paper. At the Kernforschungszentrum Karlsruhe (KfK) a family of 3 calorimeters has been developed to measure the energy release from radiative waste products arising from reprocessing operations. With these calorimeters, radiative samples with sizes from a few cm 3 to 2 ·10 5 cm 3 and heat ratings ranging from a few nW to kW can be measured. After modifications of tits inner part the most sensitive calorimeter among the three calorimeters mentioned above would be best suited for measuring the tritium inventory in T-getters of the Amersham-type

  4. Detection of irradiated food by differential scanning calorimetry

    International Nuclear Information System (INIS)

    Nesvadba, P.; Kent, M.

    1991-01-01

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

  5. Analytical methods for lignin characterization - Differential scanning calorimetry

    NARCIS (Netherlands)

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

    2006-01-01

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

  6. Analysis of Siderite Thermal Decomposition by Differential Scanning Calorimetry

    Science.gov (United States)

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

    2000-01-01

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

  7. Ultra-Fast Hadronic Calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Denisov, Dmitri [Fermilab; Lukić, Strahinja [VINCA Inst. Nucl. Sci., Belgrade; Mokhov, Nikolai [Fermilab; Striganov, Sergei [Fermilab; Ujić, Predrag [VINCA Inst. Nucl. Sci., Belgrade

    2017-12-18

    Calorimeters for particle physics experiments with integration time of a few ns will substantially improve the capability of the experiment to resolve event pileup and to reject backgrounds. In this paper time development of hadronic showers induced by 30 and 60 GeV positive pions and 120 GeV protons is studied using Monte Carlo simulation and beam tests with a prototype of a sampling steel-scintillator hadronic calorimeter. In the beam tests, scintillator signals induced by hadronic showers in steel are sampled with a period of 0.2 ns and precisely time-aligned in order to study the average signal waveform at various locations w.r.t. the beam particle impact. Simulations of the same setup are performed using the MARS15 code. Both simulation and test beam results suggest that energy deposition in steel calorimeters develop over a time shorter than 3 ns providing opportunity for ultra-fast calorimetry. Simulation results for an "ideal" calorimeter consisting exclusively of bulk tungsten or copper are presented to establish the lower limit of the signal integration window.

  8. WA80 BGO calorimetry electronics

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  9. A Research Agenda on Data Supply Chains (DSC)

    OpenAIRE

    Spanaki, K; Adams, R; Mulligan, C; Lupu, E

    2016-01-01

    Competition among organizations supports initiatives and collaborative use of data while creating value based on the strategy and best performance of each data supply chain. Supporting this direction, and building on the theoretical background of the supply chain, we propose the Data Supply Chain (DSC) as a novel concept to aid investigations for data-driven collaboration impacting organizational performance. In this study we initially propose a definition for the DSC paying particular attent...

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

    Science.gov (United States)

    Roy, Debmalya; Shastri, Babita; Mukhopadhyay, K

    2012-07-12

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

  11. Liquid ionization calorimetry: review and preview

    International Nuclear Information System (INIS)

    Fabjan, C.W.

    1995-01-01

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

  12. XRD and DSC study of the formation and the melting of a new zeolite like borosilicate CsBSi5O12 and (Cs,Rb)BSi5O12 solid solutions

    International Nuclear Information System (INIS)

    Bubnova, R.S.; Ugolkov, V.L.; Krzhizhanovskaya, M.G.; Filatov, S.K.; Paufler, P.

    2007-01-01

    Polycrystalline CsBSi 5 O 12 was prepared from a stoichiometric mixture by solid-state reaction above 1000 C. The solid solutions Cs 1-x Rb x BSi 5 O 12 were obtained at 1000 C during a long heat treatment of polycrystalline Cs 1-x Rb x BSi 2 O 6 boropollucites (x Rb = 0, 0.05, 0.2, 0.4). A new borosilicate compound and its solid solutions were studied using X-ray powder diffraction (XRD), annealing, differential scanning calorimetry (DSC), and thermogravimetry (TG). For Cs,Rb-boropollucites the new phase formation is accompanied by significant mass losses detected by DSC and TG. The following mechanism of phase transformations is assumed: (Cs,Rb)BSi 2 O 6 → (Cs,Rb)BSi 5 O 12 + (Cs,Rb)BO 2 ↑. The zeolite phase forms as a result of the boropollucite decomposition over 1000 C. Zeolite decomposes also on further heating and the SiO 2 reflections are observed in the XRD pattern only. Thus above 1000 C both boropollucite and zeolite phases are unstable presumably due to the ability of the alkali cations to leave the structure. Using XRD the unit cell parameters of CsBSi 5 O 12 have been determined in the orthorhombic crystal system: a = 16.242(4) A, b = 13.360(4) A, c = 4.874(1) A. The compound is isostructural with the zeolite compound CsAlSi 5 O 12 . In the crystal structure of Cs 1-x Rb x BSi 5 O 12 solid solutions the changes of cell parameters are insignificant under the substitution of Cs by Rb atoms that indicates a very limited substitution range. (orig.)

  13. Morphology of blends of linear and long-chain-branched polyethylenes in the solid state: A study by SANS, SAXS, and DSC

    International Nuclear Information System (INIS)

    Wignall, G.D.; Londono, J.D.; Lin, J.S.; Alamo, R.G.; Galante, M.J.; Mandelkern, L.

    1995-01-01

    Differential scanning calorimetry (DSC), small-angle neutron scattering (SANS), and X-ray scattering (SAXS) have been used to investigate the solid-state morphology of blends of linear (high density) and long-chain-branched (low-density) polyethylenes (HDPE/LDPE). The blends are homogeneous in the melt, as previously demonstrated by SANS using the contrast obtained by deuterating the linear polymer. However, due to the structural and melting point differences (∼ 20 C) between HDPE and LDPE, the components may phase segregate on slow cooling (0.75 C/min). For high concentrations (φ ≥ 0.5) of HDPE, relatively high rates of crystallization of the linear component lead to the formation of separate stacks of HDPE and LDPE lamellae, as indicated by two-peak SAXS curves. For predominantly branched blends, the difference in crystallization rate of the components becomes smaller and only one SAXS peak is observed, indicating that the two species are in the same lamellar stack. Moreover, the phases no longer consist of the pure component and the HDPE lamellae contain up to 15--20% LDPE (and vice versa). Rapid quenching into dry ice/2-propanol (-78 C) produces only one SAXS peak (and hence one lamellar stack) over the whole concentration range. The blends show extensive cocrystallization, along with a tendency for the branched material to be preferentially located in the amorphous interlamellar regions. For high concentrations (φ > 0.5) of HDPE-D, the overall scattering length density (SLD) is high and the excess concentration of LDPE between the lamellae enhances the SLD contrast between the crystalline and amorphous phases. Thus, the interlamellar spacing (long period) is clearly visible in the SANS pattern. The blend morphology is a strong function of the quenching rate, and samples quenched less rapidly (e.g., into water at 23 C) are similar to slowly cooled blends

  14. Fragility Variation of Lithium Borate Glasses Studied by Temperature-Modulated DSC

    Science.gov (United States)

    Matsuda, Yu; Fukawa, Yasuteru; Kawashima, Mitsuru; Kojima, Seiji

    2008-02-01

    The fragility of lithium borate glass system has been investigated by Temperature-Modulated Differential Scanning Calorimetry (TMDSC). The frequency and temperature dependences of dynamic specific heat have been observed in the vicinity of a glass transition temperature Tg. It is shown that the value of the fragility index m can be determined from the temperature dependence of the α-relaxation times observed by TMDSC, when the raw phase angle is properly corrected. The composition dependence of the fragility has been also discussed.

  15. Correlation of the penetration enhancement with the influence of an alcohol/tocopheryl polyethylene glycol succinate (TPGS) cosolvent system on the molecular structure of the stratum corneum of nude mouse skin as examined by microscopic FTIR/DSC

    Science.gov (United States)

    Liou, Yi-Bo; Ho, Hsiu-O.; Chen, Shin-Yi; Sheu, Ming-Thau

    2009-10-01

    Tocopheryl polyethylene glycol succinate (TPGS) is a water-soluble derivative of natural source of vitamin E, which possesses a dual nature of lipophilicity and hydrophilicity, similar to a surface-active agent. The penetration enhancement of estradiol by an ethanol and TPGS cosolvent system (EtOH/TPGS) has been confirmed. In this study, the correlation of the penetration enhancement with the influence of the EtOH/TPGS cosolvent system on biophysical changes of the stratum corneum (SC) as examined by Fourier transformation infrared spectrometry differential scanning calorimetry (FTIR/DSC) was investigated. Thermotropic changes in the asymmetrical and symmetrical C-H stretching of hydrocarbon chains of lipids, and amide I and II bands that characterize the protein structure of the SC treated with different concentrations of the EtOH/TPGS cosolvent were examined in this investigation. Results demonstrated that a strong correlation of the influence on biophysical changes of the SC treated with the EtOH/TPGS cosolvent system with the penetration enhancement of estradiol by the corresponding cosolvent system was not evident. It was concluded that the incorporation of TPGS in the cosolvent system seemed only to have insignificantly modified the structural features of the SC. It was not obvious that the penetrant had encountered these modifications resulting in an improvement in the penetration of estradiol by TPGS.

  16. DSC, Raman and impedance spectroscopy studies on the xB2O3 - (90 - x)TeO2 - 10TiO2 (where x = 0 to 50 mol%) glass system

    Science.gov (United States)

    Sripada, Suresh; Rani, D. Esther Kalpana; Upender, G.; Pavani, P. Gayathri

    2013-03-01

    Titanium boro tellurite glasses in the xB2O3 -(90- x) TeO2 - 10TiO2 (where x = 0 to 50 mol%) system were prepared by using the conventional melt-quenching technique. Glass transition temperatures were measured with differential scanning calorimetry (DSC) and found to be in the range of 300-370 °C. The Raman spectra showed a cleavage of the continuous TeO4 (tbp) network by breaking of the Te-O-Te linkages. The relative transition of TeO4 - groups to TeO3 - groups is accompanied by a change in the oxygen coordination of the boron from 3 to 4 (BO3 - to BO4 -). The impedance plots Z″( ω) versus Z'( ω) for all the glass samples were recorded and found to exhibit a single circle. The AC conductivity of all glass samples was studied in the frequency range from 100 Hz to 1 MHz and in the temperature range from room temperature (RT) to 375 °C. The AC conductivity decreased by about one order in magnitude with increasing B2O3 content. The conductivity was found to be on the order of 10-4.5 to 10-6 (Ωcm)-1 at 375 °C and 1 MHz for 10 mol% and 50 mol% B2O3 contents, respectively. The relaxation behavior in these glass samples is discussed based on the complex modulus and impedance data.

  17. Calorimetry energy measurement in particle physics

    CERN Document Server

    Wigmans, Richard

    2017-01-01

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

  18. Study of asphaltene precipitation by Calorimetry

    DEFF Research Database (Denmark)

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

    2007-01-01

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

  19. 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

  20. Evaluation of the physical stability and local crystallization of amorphous terfenadine using XRD-DSC and micro-TA

    International Nuclear Information System (INIS)

    Yonemochi, Etsuo; Hoshino, Takafumi; Yoshihashi, Yasuo; Terada, Katsuhide

    2005-01-01

    It is very difficult to follow rapid changes in polymorphic transformation and crystallization and to estimate the species recrystallized from the amorphous form. The aim of this study was to clarify the structural changes of amorphous terfenadine and to evaluate the polymorphs crystallized from amorphous samples using XRD-DSC and an atomic force microscope with a thermal probe (micro-TA). Amorphous samples were prepared by grinding or rapid cooling of the melt. The rapid structural transitions of samples were followed by the XRD-DSC system. On the DSC trace of the quenched terfenadine, two exotherms were observed, while only one exothermic peak was observed in the DSC scan of a ground sample. From the in situ data obtained by the XRD-DSC system, the stable form of terfenadine was recrystallized during heating of the ground amorphous sample, whereas the metastable form was recrystallized from the quenched amorphous sample and the crystallized polymorph changed to the stable form. Obtained data suggested that recrystallized species could be related to the homogeneity of samples. When the stored sample surface was scanned by atomic force microscopy (AFM), heterogeneous crystallization was observed. By using micro-TA, melting temperatures at various points were measured, and polymorph forms I and II were crystallized in each region. The percentages of the crystallized form I stored at 120 and 135 deg C were 47 and 79%, respectively. This result suggested that increasing the storage temperature increased the crystallization of form I, the stable form, confirming the temperature dependency of the crystallized form. The crystallization behavior of amorphous drug was affected by the annealing temperature. Micro-TA would be useful for detecting the inhomogeneities in polymorphs crystallized from amorphous drug

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

    Science.gov (United States)

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

    2008-07-10

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

  2. New crystals for dual-readout calorimetry

    Czech Academy of Sciences Publication Activity Database

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

    2009-01-01

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

  3. 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…

  4. Liquid argon calorimetry for the SSC

    International Nuclear Information System (INIS)

    Gordon, H.A.

    1990-01-01

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

  5. Monte Carlo studies of uranium calorimetry

    International Nuclear Information System (INIS)

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

    1985-01-01

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

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

    International Nuclear Information System (INIS)

    Pielichowska, Kinga; Król, Piotr; Król, Bożena; Pagacz, Joanna

    2012-01-01

    Highlights: ► TOPEM DSC method was employed to investigate the glass transition (T g ) region of fluorinated polyurethane cationomers. ► Introduction of fluorine compounds significantly changes thermal behaviour of cationomers in the T g 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.

  7. 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

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

    Science.gov (United States)

    Lee, Ae-Ri Cho; Moon, Hee Kyung

    2007-11-01

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

  9. Calorimetry and thermodynamics of living systems

    International Nuclear Information System (INIS)

    Lamprecht, Ingolf

    2003-01-01

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

  10. The use of calorimetry for plutonium assay

    International Nuclear Information System (INIS)

    Mason, J.A.

    1982-12-01

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

  11. Use of DSC and DMA Techniques to Help Investigate a Material Anomaly for PTFE Used in Processing a Piston Cup for the Urine Processor Assembly (UPA) on International Space Station (ISS)

    Science.gov (United States)

    Wingard, Doug

    2010-01-01

    Human urine and flush water are eventually converted into drinking water with the Urine Processor Assembly (UPA) aboard the International Space Station (ISS). This conversion is made possible through the Distillation Assembly (DA) of the UPA. One component of the DA is a molded circular piston cup made of virgin polytetrafluoroethylene (PTFE). The piston cup is assembled to a titanium component using eight fasteners and washers. Molded PTFE produced for spare piston cups in the first quarter of 2010 was different in appearance and texture, and softer than material molded for previous cups. For the suspect newer PTFE material, cup fasteners were tightened to only one-half the required torque value, yet the washers embedded almost halfway into the material. The molded PTFE used in the DA piston cup should be Type II, based on AMS 3667D and ASTM D4894 specifications. The properties of molded PTFE are considerably different between Type I and II materials. Engineers working with the DA thought that if Type I PTFE was molded by mistake instead of Type II material, that could have resulted in the anomalous material properties. Typically, the vendor molds flat sheet PTFE from the same material lot used to mold the piston cups, and tensile testing as part of quality control should verify that the PTFE is Type II material. However, for this discrepant lot of material, such tensile data was not available. Differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) were two of the testing techniques used at the NASA/Marshall Space Flight Center (MSFC) to investigate the anomaly for the PTFE material. Other techniques used on PTFE specimens were: Shore D hardness testing, tensile testing on dog bone specimens and a qualitative estimation of porosity by optical and scanning electron microscopy.

  12. Thermal behavior of biflorin by beans TG and a DSC photovisual system

    Directory of Open Access Journals (Sweden)

    C. F. S. Aragão

    Full Text Available This work proposes thermal characterization, of the biflorine, orto-quinon of Capraria biflora L., through the TG and DSC photovisual data. The thermogravimetric results showed that the decomposition reaction biflorine occurs three steps under air atmosphere, The DSC of biflorin presented five peaks relating to phase transitions. The DSC photovisual system demonstrated changes in biflorin.

  13. Intercomparative tests on phase change materials characterisation with differential scanning calorimeter

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  14. 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.

  15. Thermodynamic study of ibuprofen by adiabatic calorimetry and thermal analysis

    International Nuclear Information System (INIS)

    Xu Fen; Sun Lixian; Tan Zhicheng; Liang Jianguo; Li Ruilian

    2004-01-01

    Molar heat capacities of ibuprofen were precisely measured with a small sample precision automated adiabatic calorimeter over the temperature range from 80 to 400 K. The polynomial functions of C p,m (J K -1 mol -1 ) versus T were established on the heat capacity measurements by means of the least fitting square method. The functions are as follows: for solid ibuprofen, at the temperature range of 79.105 K≤T≤333.297 K, C p,m =144.27+77.046X+3.5171X 2 +10.925X 3 +11.224X 4 , where X=(T-206.201)/127.096; for liquid ibuprofen, at the temperature range of 353.406 K≤T≤378.785 K, C p,m =325.79+8.9696X-1.6073X 2 -1.5145X 3 , where X=(T-366.095)/12.690. A fusion transition at T=348.02 K was found from the C p -T curve. The molar enthalpy and entropy of the fusion transition were determined to be 26.65 kJ mol -1 and 76.58 J mol -1 K -1 , respectively. The thermodynamic functions on the base of the reference temperature of 298.15 K, (H T -H 298.15 ) and (S T -S 298.15 ), were derived. Thermal characteristic of ibuprofen was studied by thermo-gravimetric analysis (TG-DTG) and differential scanning calorimeter (DSC). The temperature of fusion, the molar enthalpy and entropy of fusion obtained by DSC were well consistent with those obtained by adiabatic calorimeter. The evaporation process of ibuprofen was investigated further by TG and DTG, and the activation energy of the evaporation process was determined to be 80.3±1.4 kJ mol -1

  16. 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.

  17. 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.....

  18. Fabrication of 12% 240Pu calorimetry standards

    International Nuclear Information System (INIS)

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

    1995-01-01

    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% 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% 240 Pu oxide with a wattage of about 6 to 8 watts

  19. A guide to automation techniques in calorimetry

    International Nuclear Information System (INIS)

    Renz, D.P.; Wetzel, J.R.; Breakall, K.L.; James, S.J.; Kasperski, P.W.

    1992-01-01

    Many improvements occurring in calorimetry measurement technology in the past few years will help current users of calorimeters to achieve better use of their existing systems. These include a more user friendly operator computer interface, a more detailed printout at the end of each run, improved data processing to eliminate operator error, and improved system monitoring to detect system or environmental problems. In addition, an electrical calibration heater has been developed to replace plutonium-238 heat standards for calibrating calorimeters, and several automation systems allow for easier and safer system operation

  20. 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....

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

    Science.gov (United States)

    Brewer, J M; Wampler, J E

    2001-03-14

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

  2. Synergies between electromagnetic calorimetry and PET

    International Nuclear Information System (INIS)

    Moses, William W.

    2002-01-01

    The instrumentation used for the nuclear medical imaging technique of Positron Emission Tomography (PET) shares many features with the instrumentation used for electromagnetic calorimetry. Both fields can certainly benefit from technical advances in many common areas, and this paper discusses both the commonalties and the differences between the instrumentation needs for the two fields. The overall aim is to identify where synergistic development opportunities exist. While such opportunities exist in inorganic scintillators, photodetectors, amplification and readout electronics, and high-speed computing, it is important to recognize that while the requirements of the two fields are similar, they are not identical, and so it is unlikely that advances specific to one field can be transferred without modification to the other

  3. Silicon calorimetry for the SSC[ Superconducting Supercollider

    International Nuclear Information System (INIS)

    Bertrand, C.; Borchi, E.; Brau, J.E.

    1989-01-01

    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

  4. 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...

  5. CMS Forward Calorimetry R&D

    Energy Technology Data Exchange (ETDEWEB)

    Bilki, Burak [Univ. of Iowa, Iowa City, IA (United States); Argonne National Lab. (ANL), Argonne, IL (United States)

    2013-11-11

    This is a technical scope of work (TSW) between the Fermi National Accelerator Laboratory (Fermilab) and the experimenters of the CMS Forward Calorimetry Taskforce (FCAL group) who have committed to participate in beam tests to be carried out during the 2013-2016 Fermilab Test Beam Facility program. The TSW is intended primarily for the purpose of recording expectations for budget estimates and work allocations for Fermilab, the funding agencies and the participating institutions. It reflects an arrangement that currently is satisfactory to the parties; however, it is recognized and anticipated that changing circumstances of the evolving research program will necessitate revisions. The parties agree to modify this scope of work to reflect such required adjustments. Actual contractual obligations will be set forth in separate documents.

  6. Study of lamellar structure and crystallization behavior of poly(butylene terephthalate (PBT) in PBT/ABS and PBT/ABS/MMA-GMA blends using DSC, SAXS and DMTA

    International Nuclear Information System (INIS)

    Mantovani, Gerson L.; Pessan, Luiz A.; Hage, Elias; Torriani, Iris L.

    2001-01-01

    The effects of processing conditions and blend composition in the crystallization behaviour and lamellar structure of poly(butylene terephthalate) (PBT) in blends with acrylonitrile-butadiene-styrene copolymer (ABS) were studied. Differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS) and dynamic mechanical thermal analysis (DMTA) were used to observe those effects. Addition of reactive acrylic compatibilizer to the PBT/ABS blends has promoted an increase in the heat of crystallization of the related blends. The Long Period (L), obtained from the peak in the Lorentz-corrected SAXS pattern, was used to observe the effect in the lamellar structure of PBT phase in the blends. The results were in good agreement with the calculated values from de correlation function and the values of L do not show a significant dependence with the PBT mass fraction, either in the binary blends (PBT/ABS) or in the compatibilized blends. A slight but clear increase of the long period (from 3 to 5 angstrom) is noted for the systems injection molded at 240 deg C when compared to the ones molded at 260 deg C, although PBT crystallinity in the blends does not change significantly with blend composition or processing conditions. DMTA curves show a slight shift in the temperature of the tan δ main peaks for both PBT and ABS phases in the compatibilized blends, thereby indicating changes in the degree of miscibility or interaction between phases of those blends. Changes in the compatibilized blends miscibility may be responsible by the effects in the crystallization behaviour and lamellar structure of the PBT/ABS blends. (author)

  7. Study of lamellar structure and crystallization behavior of poly(butylene terephthalate (PBT) in PBT/ABS and PBT/ABS/MMA-GMA blends using DSC, SAXS and DMTA

    Energy Technology Data Exchange (ETDEWEB)

    Mantovani, Gerson L.; Pessan, Luiz A.; Hage, Elias [Sao Carlos Univ., SP (Brazil). Dept. de Engenharia de Materiais]. E-mail: elias@power.ufscar.br; Plivelic, Tomas S. [Laboratorio Nacional de Luz Sincrotron (LNLS), Campinas, SP (Brazil); Torriani, Iris L. [Universidade Estadual de Campinas, SP (Brazil). Inst. de Fisica Gleb Wataghin

    2001-07-01

    The effects of processing conditions and blend composition in the crystallization behaviour and lamellar structure of poly(butylene terephthalate) (PBT) in blends with acrylonitrile-butadiene-styrene copolymer (ABS) were studied. Differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS) and dynamic mechanical thermal analysis (DMTA) were used to observe those effects. Addition of reactive acrylic compatibilizer to the PBT/ABS blends has promoted an increase in the heat of crystallization of the related blends. The Long Period (L), obtained from the peak in the Lorentz-corrected SAXS pattern, was used to observe the effect in the lamellar structure of PBT phase in the blends. The results were in good agreement with the calculated values from de correlation function and the values of L do not show a significant dependence with the PBT mass fraction, either in the binary blends (PBT/ABS) or in the compatibilized blends. A slight but clear increase of the long period (from 3 to 5 angstrom) is noted for the systems injection molded at 240 deg C when compared to the ones molded at 260 deg C, although PBT crystallinity in the blends does not change significantly with blend composition or processing conditions. DMTA curves show a slight shift in the temperature of the tan {delta} main peaks for both PBT and ABS phases in the compatibilized blends, thereby indicating changes in the degree of miscibility or interaction between phases of those blends. Changes in the compatibilized blends miscibility may be responsible by the effects in the crystallization behaviour and lamellar structure of the PBT/ABS blends. (author)

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    This paper describes the design and development of tandem dye-sensitized/Cu(In, Ga)Se (DSC/CIGS) PV modules. The tandem PV module comprised of the top DSC module and a bottom commercial 0,8 m 2 CIGS module. The top DSC module was made of 10 DSC mini-modules with the field size of 20 × 20 cm 2 each. Tandem DSC/CIGS PV modules were used for providing the long-term monitoring of energy yield and electrical parameters in comparison with standalone CIGS modules under outdoor conditions. The outdoor test facility, containing solar modules of both types and a measurement unit, was located on the roof of the Institute of Biochemical Physics in Moscow. The data obtained during monitoring within the 2014 year period has shown the advantages of the designed tandem DSC/CIGS PV-modules over the conventional CIGS modules, especially for cloudy weather and low-intensity irradiation conditions. (paper)

  9. Characterization of the evolution of the volume fraction of precipitates in aged AlMgSiCu alloys using DSC technique

    International Nuclear Information System (INIS)

    Esmaeili, Shahrzad; Lloyd, David J.

    2005-01-01

    Differential scanning calorimetry is used to quantify the evolution of the volume fraction of precipitates during age hardening in AlMgSiCu alloys. The calorimetry tests are run on alloy samples after aging for various times at 180 deg. C and the change in the collective heat effects from the major precipitation and dissolution processes in each run are used to determine the precipitation state of the samples. The method is implemented on alloys with various thermal histories prior to artificial aging, including commercial pre-aging histories. The estimated values for the relative volume fraction of precipitates are compared with the results from a newly developed analytical method using isothermal calorimetry and a related quantitative transmission electron microscopy work. Excellent agreement is obtained between the results from various methods

  10. Infrared spectra, Raman laser, XRD, DSC/TGA and SEM ...

    Indian Academy of Sciences (India)

    Administrator

    cussed and the X-ray diffraction, scanning electron microscopy (SEM) and atomic force microscope (AFM) ... acetamide as a simple organic compound at high tempera- ture has less ..... properties of selenium surface, AFM-microscopy tapping.

  11. Loading of praziquantel in the crystal lattice of solid lipid nanoparticles - studies by DSC and SAXS

    Energy Technology Data Exchange (ETDEWEB)

    Souza, A.L.R.; Cassimiro, D.L.; Almeida, A.E.; Ribeiro, C.A.; Gremiao, M.P.D. [UNESP, Araraquara, SP (Brazil); Sarmento, V.H.V. [Universidade Federal de Sergipe (UFS), Itabaiana, SE (Brazil); Andreani, T.; Silva, A.M.; Souto, E.B. [Universidade de Tras-os-Montes e Alto Douro, Vila Real (Portugal)

    2012-07-01

    Full text: Praziquantel (PZQ) is the drug of choice for oral treatment of schistosomiasis and other fluke infections that affect humans. Its low oral bioavailability demands the development of innovative strategies to overcome the first pass metabolism. In this work, solid lipid nanoparticles loaded with PZQ (PZQ-SLN) were prepared by a modified oil-in-water microemulsion method selecting stearic acid as lipid phase after solubility screening studies. The mean particle size (Z-Ave) and zeta potential (ZP) were 500 nm and -34.0 mV, respectively. Morphology and shape of PZQ-SLN were analysed by scanning electron microscopy revealing the presence of spherical particles with smooth surface. Differential scanning calorimetry suggested that SLN comprised a less ordered arrangement of crystals and the drug was molecularly dispersed in the lipid matrix. No supercooled melts were detected. The entrapment efficiency (EE) and loading capacity of PZQ, determined by high performance liquid chromatography, were 99.0 and 17.5, respectively. Effective incorporation of PZQ into the particles was confirmed by small angle X-ray scattering revealing the presence of a lipid lamellar structure. Stability parameters of PZQ-SLN stored at room temperature (25 deg C) and at 4 deg C were checked by analysing Z-Ave, ZP and the EE for a period of 60 days Results showed a relatively long-term physical stability after storage at 4 deg C, without drug expulsion. (author)

  12. Loading of praziquantel in the crystal lattice of solid lipid nanoparticles - studies by DSC and SAXS

    International Nuclear Information System (INIS)

    Souza, A.L.R.; Cassimiro, D.L.; Almeida, A.E.; Ribeiro, C.A.; Gremiao, M.P.D.; Sarmento, V.H.V.; Andreani, T.; Silva, A.M.; Souto, E.B.

    2012-01-01

    Full text: Praziquantel (PZQ) is the drug of choice for oral treatment of schistosomiasis and other fluke infections that affect humans. Its low oral bioavailability demands the development of innovative strategies to overcome the first pass metabolism. In this work, solid lipid nanoparticles loaded with PZQ (PZQ-SLN) were prepared by a modified oil-in-water microemulsion method selecting stearic acid as lipid phase after solubility screening studies. The mean particle size (Z-Ave) and zeta potential (ZP) were 500 nm and -34.0 mV, respectively. Morphology and shape of PZQ-SLN were analysed by scanning electron microscopy revealing the presence of spherical particles with smooth surface. Differential scanning calorimetry suggested that SLN comprised a less ordered arrangement of crystals and the drug was molecularly dispersed in the lipid matrix. No supercooled melts were detected. The entrapment efficiency (EE) and loading capacity of PZQ, determined by high performance liquid chromatography, were 99.0 and 17.5, respectively. Effective incorporation of PZQ into the particles was confirmed by small angle X-ray scattering revealing the presence of a lipid lamellar structure. Stability parameters of PZQ-SLN stored at room temperature (25 deg C) and at 4 deg C were checked by analysing Z-Ave, ZP and the EE for a period of 60 days Results showed a relatively long-term physical stability after storage at 4 deg C, without drug expulsion. (author)

  13. Thermodynamic study of ibuprofen by adiabatic calorimetry and thermal analysis

    Energy Technology Data Exchange (ETDEWEB)

    Xu Fen; Sun Lixian; Tan Zhicheng; Liang Jianguo; Li Ruilian

    2004-03-23

    Molar heat capacities of ibuprofen were precisely measured with a small sample precision automated adiabatic calorimeter over the temperature range from 80 to 400 K. The polynomial functions of C{sub p,m} (J K{sup -1} mol{sup -1}) versus T were established on the heat capacity measurements by means of the least fitting square method. The functions are as follows: for solid ibuprofen, at the temperature range of 79.105 K{<=}T{<=}333.297 K, C{sub p,m}=144.27+77.046X+3.5171X{sup 2}+10.925X{sup 3}+11.224X{sup 4}, where X=(T-206.201)/127.096; for liquid ibuprofen, at the temperature range of 353.406 K{<=}T{<=}378.785 K, C{sub p,m}=325.79+8.9696X-1.6073X{sup 2}-1.5145X{sup 3}, where X=(T-366.095)/12.690. A fusion transition at T=348.02 K was found from the C{sub p}-T curve. The molar enthalpy and entropy of the fusion transition were determined to be 26.65 kJ mol{sup -1} and 76.58 J mol{sup -1} K{sup -1}, respectively. The thermodynamic functions on the base of the reference temperature of 298.15 K, (H{sub T}-H{sub 298.15}) and (S{sub T}-S{sub 298.15}), were derived. Thermal characteristic of ibuprofen was studied by thermo-gravimetric analysis (TG-DTG) and differential scanning calorimeter (DSC). The temperature of fusion, the molar enthalpy and entropy of fusion obtained by DSC were well consistent with those obtained by adiabatic calorimeter. The evaporation process of ibuprofen was investigated further by TG and DTG, and the activation energy of the evaporation process was determined to be 80.3{+-}1.4 kJ mol{sup -1}.

  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. Current status of tritium calorimetry at TLK

    International Nuclear Information System (INIS)

    Buekki-Deme, A.; Alecu, C.G.; Kloppe, B.; Bornschein, B.

    2015-01-01

    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)

  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. The CLEO-III Trigger: Calorimetry and tracking

    International Nuclear Information System (INIS)

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

    1996-01-01

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

  18. Forward calorimetry in the upgraded UA1 experiment

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  19. 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.

  20. 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.

  1. 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.

  2. Nuclear Scans

    Science.gov (United States)

    Nuclear scans use radioactive substances to see structures and functions inside your body. They use a special ... images. Most scans take 20 to 45 minutes. Nuclear scans can help doctors diagnose many conditions, including ...

  3. Micro-XRD and temperature-modulated DSC investigation of nickel-titanium rotary endodontic instruments.

    Science.gov (United States)

    Alapati, Satish B; Brantley, William A; Iijima, Masahiro; Schricker, Scott R; Nusstein, John M; Li, Uei-Ming; Svec, Timothy A

    2009-10-01

    Employ Micro-X-ray diffraction and temperature-modulated differential scanning calorimetry to investigate microstructural phases, phase transformations, and effects of heat treatment for rotary nickel-titanium instruments. Representative as-received and clinically used ProFile GT and ProTaper instruments were principally studied. Micro-XRD analyses (Cu Kalpha X-rays) were performed at 25 degrees C on areas of approximately 50 microm diameter near the tip and up to 9 mm from the tip. TMDSC analyses were performed from -80 to 100 degrees C and back to -80 degrees C on segments cut from instruments, using a linear heating and cooling rate of 2 degrees C/min, sinusoidal oscillation of 0.318 degrees C, and period of 60s. Instruments were also heat treated 15 min in a nitrogen atmosphere at 400, 500, 600 and 850 degrees C, and analyzed. At all Micro-XRD analysis regions the strongest peak occurred near 42 degrees , indicating that instruments were mostly austenite, with perhaps some R-phase and martensite. Tip and adjacent regions had smallest peak intensities, indicative of greater work hardening, and the intensity at other sites depended on the instrument. TMDSC heating and cooling curves had single peaks for transformations between martensite and austenite. Austenite-finish (A(f)) temperatures and enthalpy changes were similar for as-received and used instruments. Heat treatments at 400, 500 and 600 degrees C raised the A(f) temperature to 45-50 degrees C, and heat treatment at 850 degrees C caused drastic changes in transformation behavior. Micro-XRD provides novel information about NiTi phases at different positions on instruments. TMDSC indicates that heat treatment might yield instruments with substantial martensite and improved clinical performance.

  4. 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. ...

  5. Characterisation of the glass transition of an amorphous drug using modulated DSC.

    Science.gov (United States)

    Royall, P G; Craig, D Q; Doherty, C

    1998-07-01

    The use of modulated differential scanning calorimetry (MDSC) as a novel means of characterising the glass transition of amorphous drugs has been investigated, using the protease inhibitor saquinavir as a model compound. In particular, the effects of measuring variables (temperature cycling, scanning period, heating mode) have been examined. Saquinavir samples of known moisture content were examined using a TA Instruments 2920 MDSC at a heating rate of 2 degrees C/min and an amplitude of +/-0.159 degrees C with a period of 30 seconds. These conditions were used to examine the effects of cycling between - 50 degrees C and 150 degrees C. A range of periods between 20 and 50 seconds were then studied. Isothermal measurements were carried out between 85 degrees C and 120 degrees C using an amplitude of +/-0.159 degrees C with a period of 30 seconds. MDSC showed the glass transition of saquinavir (0.98 +/- 0.05%w/w moisture content) in isolation from the relaxation endotherm to give an apparent glass transition temperature of 107.0 degrees C +/- 0.4 degrees C. Subsequent temperature cycling gave reproducible glass transition temperatures of approximately 105 degrees C for both cooling and heating cycles. The enthalpic relaxation peak observed in the initial heating cycle had an additional contribution from a Tg "shift" effect brought about by the difference in response to the glass transition of the total and reversing heat flow signals. Isothermal studies yield a glass transition at 105.9 degrees C +/- 0.1 degrees C. MDSC has been shown to be capable of separating the glass transition of saquinavir from the relaxation endotherm, thereby facilitating measurement of this parameter without the need for temperature cycling. However, the Tg "shift" effect and the number of modulations through the transition should be taken into account to avoid drawing erroneous conclusions from the experimental data. MDSC has been shown to be an effective method of characterising the glass

  6. 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.

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

    Science.gov (United States)

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

    2018-01-01

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

  8. Characterisation of moisture uptake effects on the glass transitional behaviour of an amorphous drug using modulated temperature DSC.

    Science.gov (United States)

    Royall, P G; Craig, D Q; Doherty, C

    1999-12-01

    The purpose of this study was to investigate the depression of the glass transition temperature, T(g), of the protease inhibitor saquinavir in the first heating scan as a function of the quantity of sorbed water by the application of modulated temperature differential scanning calorimetry (MTDSC). Samples of amorphous saquinavir were pretreated under various humidity conditions and the quantity of sorbed water measured by thermogravimetric analysis. MTDSC runs were performed using hermetically and non-hermetically sealed pans in order to determine the glass transition temperature. MTDSC allowed the separation of the glass transition from the enthalpic relaxation, thereby allowing clear visualisation of T(g) for amorphous saquinavir in the first heating scan. The plasticizing effects of water were assessed, with the depression in T(g) related to the mole fraction of water sorbed via the Gordon-Taylor relationship. An expression has been derived which allows estimation of the water content which lowers the T(g) to the storage temperature, thereby considerably increasing the risk of recrystallisation. It is argued that this model may aid prediction of the optimal storage conditions for amorphous drugs.

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

    Science.gov (United States)

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

    2017-09-01

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

  10. Fast sampling calorimetry with solid argon ionization chambers

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  11. Optimization of crystals for applications in dual-readout calorimetry

    Czech Academy of Sciences Publication Activity Database

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

    2010-01-01

    Roč. 621, 1-3 (2010), 212-221 ISSN 0168-9002 Institutional research plan: CEZ:AV0Z10100521 Keywords : calorimetry * Cherenkov light * High-Z scintillating crystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.142, year: 2010

  12. 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…

  13. Hadronic shower development in iron-scintillator tile calorimetry

    Czech Academy of Sciences Publication Activity Database

    Amaral, P.; Amorim, A.; Anderson, K.; Lokajíček, Miloš; Němeček, Stanislav

    2000-01-01

    Roč. 443, - (2000), s. 51-70 ISSN 0168-9002 R&D Projects: GA MPO RP-4210/69 Institutional research plan: CEZ:AV0Z1010920 Keywords : ATLAS Iron-Scintillator * hadron calorimeter * shower parametrisation * calorimetry * computer data analysis Subject RIV: BL - Plasma and Gas Discharge Physics Impact factor: 0.964, year: 2000

  14. Particle flow calorimetry at the international linear collider

    Indian Academy of Sciences (India)

    Particle flow calorimetry at the international linear ... It is widely believed that the most promising strategy for achieving a jet ... this level of performance for two main reasons. Firstly ... (i) Tracking: For the studies presented in this paper, the track pattern ... that particles propagating outward from the interaction region will cross ...

  15. Differential Binding Models for Direct and Reverse Isothermal Titration Calorimetry.

    Science.gov (United States)

    Herrera, Isaac; Winnik, Mitchell A

    2016-03-10

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

  16. Indirect calorimetry: assessing animal response to heat and cold stress

    NARCIS (Netherlands)

    Gaughan, J.B.; Heetkamp, M.J.W.; Hendriks, P.

    2015-01-01

    Calorimetric thermal stress studies where indirect calorimetry is used as a tool to estimate energy expenditure have been undertaken since this technique was developed. Some examples of these studies are presented in this chapter. The measurement of gas exchange by means of an open-circuit

  17. The development of the code package PERMAK--3D//SC--1

    International Nuclear Information System (INIS)

    Bolobov, P. A.; Oleksuk, D. A.

    2011-01-01

    Code package PERMAK-3D//SC-1 was developed for performing pin-by-pin coupled neutronic and thermal hydraulic calculation of the core fragment of seven fuel assemblies and was designed on the basis of 3D multigroup pin-by-pin code PERMAK-3D and 3D (subchannel) thermal hydraulic code SC-1 The code package predicts axial and radial pin-by-pin power distribution and coolant parameters in stimulated region (enthalpies,, velocities,, void fractions,, boiling and DNBR margins).. The report describes some new steps in code package development. Some PERMAK-3D//SC-1 outcomes of WWER calculations are presented in the report. (Authors)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-03-10

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

  19. What does calorimetry and thermodynamics of living cells tell us?

    Science.gov (United States)

    Maskow, Thomas; Paufler, Sven

    2015-04-01

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

  20. The application of differential scanning calorimetry and ice nucleation spectrometry to ecophysiological studies of algae

    Czech Academy of Sciences Publication Activity Database

    Worland, M. R.; Lukešová, Alena

    2001-01-01

    Roč. 123, - (2001), s. 571-583 ISSN 1438-9134 Institutional research plan: CEZ:AV0Z6066911 Keywords : Antarctic * cold tolerance * terrestrial algae Subject RIV: EH - Ecology, Behaviour Impact factor: 0.488, year: 2000

  1. Differential scanning calorimetry as a screening technique in compatibility studies of acyclovir extended release formulations

    International Nuclear Information System (INIS)

    Barboza, Fernanda M.; Vecchia, Debora D.; Tagliari, Monika P.; Ferreira, Andrea Granada; Silva, Marcos A.S.; Stulzer, Hellen K.

    2009-01-01

    Acyclovir (ACV) has been investigated during the past years, mainly due to its antiviral activity. Assessment of possible incompatibility between an active component and different excipients along with the evaluation of thermal stability are crucial parts of a normal study prior to the final formulation setting of a medicine. Thermal analysis studies were used as important and complementary tools during pre-formulation to determine the compatibility of drug excipients with the purpose of developing an acyclovir extended release formulation. Fourier transform infrared spectroscopy and X-ray powder diffraction analyses were also realized. The results showed that ACV only exhibited interaction which could influence the stability of the product in the binary mixtures of ACV/magnesium stearate. (author)

  2. Crystallization Kinetics of Nanocrystalline Materials by Combined X-ray Diffraction and Differential Scanning Calorimetry Experiments

    Czech Academy of Sciences Publication Activity Database

    Gil-González, E.; Perejón, A.; Sánchez-Jiménez, P. E.; Medina-Carrasco, S.; Kupčík, Jaroslav; Šubrt, Jan; Criado, J. M.; Pérez-Maqueda, L. A.

    2018-01-01

    Roč. 18, č. 5 (2018), s. 3107-3116 ISSN 1528-7483 Institutional support: RVO:61388980 Keywords : nanocrysalline alloys * combined X ray diffraction * crystallization kinetics Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 4.055, year: 2016

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

    NARCIS (Netherlands)

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

    2009-01-01

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

  4. Differential scanning calorimetry studies of Se85Te15–xPbx (x = 4, 6 ...

    Indian Academy of Sciences (India)

    Unknown

    2000-06-14

    Jun 14, 2000 ... Matusita's equation while 102–139 kJ/mol by modified Kissinger's equation. The Hruby number ... to n-type in Ge–Se–Pb system (Toghe et al 1987) is observed in spite ... determine the activation energy of structural relaxation.

  5. A New Energy-Efficient Data Transmission Scheme Based on DSC and Virtual MIMO for Wireless Sensor Network

    OpenAIRE

    Li, Na; Zhang, Liwen; Li, Bing

    2015-01-01

    Energy efficiency in wireless sensor network (WSN) is one of the primary performance parameters. For improving the energy efficiency of WSN, we introduce distributed source coding (DSC) and virtual multiple-input multiple-output (MIMO) into wireless sensor network and then propose a new data transmission scheme called DSC-MIMO. DSC-MIMO compresses the source data using distributed source coding before transmitting, which is different from the existing communication schemes. Data compression c...

  6. Renal scan

    Science.gov (United States)

    ... this page: //medlineplus.gov/ency/article/003790.htm Renal scan To use the sharing features on this ... anaphylaxis . Alternative Names Renogram; Kidney scan Images Kidney anatomy Kidney - blood and urine flow References Chernecky CC, ...

  7. CT Scan

    Science.gov (United States)

    ... disease, lung nodules and liver masses Monitor the effectiveness of certain treatments, such as cancer treatment Detect ... scan done in a hospital or an outpatient facility. CT scans are painless and, with newer machines, ...

  8. Morphology evaluation of biodegradable copolyesters based on dimerized fatty acid studied by DSC, SAXS and WAXS

    Czech Academy of Sciences Publication Activity Database

    Kozlowska, A.; Gromadzki, Daniel; El Fray, M.; Štěpánek, Petr

    2008-01-01

    Roč. 16, č. 6 (2008), s. 85-88 ISSN 1230-3666 Institutional research plan: CEZ:AV0Z40500505 Keywords : multiblock copolymers * DSC * WAXS Subject RIV: CD - Macromolecular Chemistry Impact factor: 0.439, year: 2008

  9. Multispectral Image Compression Based on DSC Combined with CCSDS-IDC

    Directory of Open Access Journals (Sweden)

    Jin Li

    2014-01-01

    Full Text Available 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.

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

    International Nuclear Information System (INIS)

    Hsu, C.-H.; Lin, S.-Y.

    2009-01-01

    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 -1 for water liberated and at 1701 cm -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

  12. Scintillating glasses for total absorption dual readout calorimetry

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-01-01

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

  13. Inherent limitations of fixed time servo-controlled radiometric calorimetry

    International Nuclear Information System (INIS)

    Wetzel, J.R.; Duff, M.F.; Lemming, J.F.

    1987-01-01

    There has been some interest in low precision, short run time calorimetry measurements. This type of calorimetry measurement has been proposed for use when high precision measurements are not required, for example, to screen scrap containers to determine if there is enough material to be measured more accurately of for confirmatory measurements that only require low precision results. The equipment needed to make these measurements is a servo-controlled calorimeter with a sample preequilibration bath. The preequilibration bath temperature is set to the internal temperature of the calorimeter running at a fixed servo-controlled wattage level. The sample power value is determined at a fixed time form the sample loading into the calorimeter. There are some limitations and areas of uncertainties in the use of data obtained by this method. Data collected under controlled conditions demonstrate the limitations. Sample packaging, preequilibration time, and item wattage were chosen as the variables most likely to be encountered in a plant environment

  14. The upgraded CDF front end electronics for calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Drake, G.; Frei, D.; Hahn, S.R.; Nelson, C.A.; Segler, S.L.; Stuermer, W.

    1991-11-01

    The front end electronics used in the calorimetry of the CDF detector has been upgraded to meet system requirements for higher expected luminosity. A fast digitizer utilizing a 2 {mu}Sec, 16 bit ADC has been designed and built. Improvements to the front end trigger circuitry have been implemented, including the production of 900 new front end modules. Operational experience with the previous system is presented, with discussion of the problems and performance goals.

  15. The upgraded CDF front end electronics for calorimetry

    International Nuclear Information System (INIS)

    Drake, G.; Frei, D.; Hahn, S.R.; Nelson, C.A.; Segler, S.L.; Stuermer, W.

    1991-11-01

    The front end electronics used in the calorimetry of the CDF detector has been upgraded to meet system requirements for higher expected luminosity. A fast digitizer utilizing a 2 μSec, 16 bit ADC has been designed and built. Improvements to the front end trigger circuitry have been implemented, including the production of 900 new front end modules. Operational experience with the previous system is presented, with discussion of the problems and performance goals

  16. The Philosophy and Feasibility of Dual Readout Calorimetry

    International Nuclear Information System (INIS)

    Hauptman, John

    2006-01-01

    I will discuss the general physical ideas behind dual-readout calorimetry, their implementation in DREAM (Dual REAdout Module) with exact separation of scintillation and Cerenkov light, implementation with mixed light in DREAM fibers, anticipated implementation in PbWO4 crystals with applications to the 4th Concept detector and to CMS, use in high energy gamma-ray and cosmic ray astrophysics with Cerenkov and N2 fluorescent light, and implementation in the 4th Concept detector for muon identification

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

    International Nuclear Information System (INIS)

    Wai, Y.C.; Labov, S.E.; Silver, E.H.

    1990-01-01

    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

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

    Science.gov (United States)

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

    2015-03-01

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

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

    Science.gov (United States)

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

    2012-07-14

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

  20. Experimental and theoretical evidence of a supercritical-like transition in an organic semiconductor presenting colossal uniaxial negative thermal expansion† †Electronic supplementary information (ESI) available: Diffraction and crystallography, Cambridge Structural Database survey, DFT computational details, UV spectroscopy, differential scanning calorimetry, and optical microscopy. CCDC 1810678–1810688. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c8sc00159f

    Science.gov (United States)

    Roche, Gilles H.; Wantz, Guillaume; Moreau, Joël J. E.; Dautel, Olivier J.; Filhol, Jean-Sébastien

    2018-01-01

    Thermal expansion coefficients of most materials are usually small, typically up to 50 parts per million per kelvin, and positive, i.e. materials expand when heated. Some materials show an atypical shrinking behavior in one or more crystallographic directions when heated. Here we show that a high mobility thiophene-based organic semiconductor, BHH-BTBT, has an exceptionally large negative expansion between 95 and 295 K (–216 BTBT, a much studied organic semiconductor with a closely related molecular formula and 3D crystallographic structure. Complete theoretical characterization of BHH-BTBT using ab initio molecular dynamics shows that below ∼200 K two different α and β domains exist of which one is dominant but which dynamically exchange around and above 210 K. A supercritical-like transition from an α dominated phase to a β dominated phase is observed using DSC measurements, UV-VIS spectroscopy, and X-ray diffraction. The origin of the extreme negative and positive thermal expansion is related to steric hindrance between adjacent tilted thiophene units and strongly enhanced by attractive S···S and S···C interactions within the highly anharmonic mixed-domain phase. This material could trigger the tailoring of optoelectronic devices highly sensitive to strain and temperature. PMID:29780527

  1. An evaluation of the use of modulated temperature DSC as a means of assessing the relaxation behaviour of amorphous lactose.

    Science.gov (United States)

    Craig, D Q; Barsnes, M; Royall, P G; Kett, V L

    2000-06-01

    To evaluate the use of Modulated Temperature DSC (MTDSC) as a means of assessing the relaxation behaviour of amorphous lactose via measurement of the heat capacity, glass transition (Tg) and relaxation endotherm. Samples of amorphous lactose were prepared by freeze drying. MTDSC was conducted using a TA Instruments 2920 MDSC using a heating rate of 2 degrees C/minute, a modulation amplitude of +/-0.3 degrees C and a period of 60 seconds. Samples were cycled by heating to 140 degrees C and cooling to a range of annealing temperatures between 80 degrees C and 100 degrees C, followed by reheating through the Tg region. Systems were then recooled to allow for correction of the Tg shift effect. MTDSC enabled separation of the glass transition from the relaxation endotherm, thereby facilitating calculation of the relaxation time as a function of temperature. The relative merits of using MTDSC for the assessment of relaxation processes are discussed. In addition, the use of the fictive temperature rather than the experimentally derived Tg is outlined. MTDSC allows assessment of the glass transition temperature, the magnitude of the relaxation endotherm and the value of the heat capacity, thus facilitating calculation of relaxation times. Limitations identified with the approach include the slow scanning speed, the need for careful choice of experimental parameters and the Tg shift effect.

  2. Melting and crystallization of in-situ polymerized cyclic butylene terephthalates with and without organoclay: a modulated DSC study

    Directory of Open Access Journals (Sweden)

    2007-02-01

    Full Text Available The polymerization of cyclic butylene terephthalate oligomers (CBT were studied in presence (in 5 wt.% and absence of an organoclay (Cloisite® 30B by modulated DSC (MDSC. The organoclay containing samples were produced by dry and melt blending, respectively. The first heating, causing the polymerization of the CBT catalyzed by an organotin compound, was followed by cooling prior to the second heating. The MDSC scans covered the temperature interval between 0 and 260°C. The aim of this protocol was to study the crystallization and melting behavior of the resulting polybutylene terephthalate (pCBT and its organoclay modified nanocomposites. It was found that the thermal behaviors of the polymerizing and polymerized CBT (pCBT were strongly affected by the sample preparation. The organoclay suppressed the crystallization of the pCBT produced during the first heating. However, results from the second heating suggest that more perfect crystallites were formed in the organoclay modified pCBT variants. The organoclay also affected the conversion and mean molecular mass of the resulting pCBT which were slightly lower than those of the plain pCBT polymerized under identical conditions.

  3. 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)

  4. Cooperative scans

    NARCIS (Netherlands)

    M. Zukowski (Marcin); P.A. Boncz (Peter); M.L. Kersten (Martin)

    2004-01-01

    textabstractData mining, information retrieval and other application areas exhibit a query load with multiple concurrent queries touching a large fraction of a relation. This leads to individual query plans based on a table scan or large index scan. The implementation of this access path in most

  5. Contribution of modulated DSc to study the thermal behaviour of PET films drawn in hot water

    International Nuclear Information System (INIS)

    Zumalian, Abubaker

    2003-01-01

    PET films uni-axially drawn in hot water are studied by means of conventional DSc and modulated DSc. The glass transition is studied by modulated DSc which allows access to the values of the glass transition temperature T g and the variations of δ C p = C p 1-C p g (difference between thermal capacity in the liquid-like and glassy states at T = T g ). Variations of T g with the water content (which act as plasticizer) and with the drawing (which rigidifies the amorphous phase) are discussed in regard to the structure engaged in these materials. The variations of δ C p are also interpreted with the help of a three phase model and a strong-fragile glass former liquid concept. We show that the fragility of the medium increases by the conjugated effects of deformation and water as soon as a strain induced crystalline phase is obtained, and it decreases drastically when the rigid amorphous phase occurs. (author)

  6. Calorimetry exchange program annual data report for 1992

    International Nuclear Information System (INIS)

    Barnett, T.M.

    1992-01-01

    The goals of the Calorimetry Sample Exchange Program are: discuss measurement differences; review and improve analytical measurements and methods; discuss new measurement capabilities; provide data to DOE on measurement capabilities to evaluate shipper-receiver differences; provide characterized or standard materials as necessary for exchange participants; and provide a measurement control program for plutonium analysis. A sample of PuO 2 powder is available at each participating site for NDA measurement, including either or both calorimetry and high-resolution gamma-ray spectroscopy, the elements which are typically combined to provide a calorimetric assay of plutonium. The facilities measure the sample as frequently and to the level of precision which they desire, and then submit the data to the Exchange for analysis. The data report includes summary tables for each measurement and charts showing the performance of each laboratory. Comparisons are made to the accepted values for the exchange sample and to data previously reported by that laboratory. This information is presented, in the form of quarterly and annual reports, intended for use by Exchange participants in measurement control programs, or to indicate when bias corrections may be appropriate. No attempt, however, has been made to standardize methods or frequency of data collection, calibration, or operating procedures. Direct comparisons between laboratories may, therefore, be misleading since data have not been collected to the same precision or for the same time periods. A meeting of the participants of the Calorimetry Exchange is held annually at EG ampersand G Mound Applied Technologies. The purposes of this meeting are to discuss measurement differences, problems, and new measurement capabilities, and to determine the additional activities needed to fulfill the goals of the Exchange. This document provides data for 1992

  7. Radionuclide scanning

    International Nuclear Information System (INIS)

    Shapiro, B.

    1986-01-01

    Radionuclide scanning is the production of images of normal and diseased tissues and organs by means of the gamma-ray emissions from radiopharmaceutical agents having specific distributions in the body. The gamma rays are detected at the body surface by a variety of instruments that convert the invisible rays into visible patterns representing the distribution of the radionuclide in the body. The patterns, or images, obtained can be interpreted to provide or to aid diagnoses, to follow the course of disease, and to monitor the management of various illnesses. Scanning is a sensitive technique, but its specificity may be low when interpreted alone. To be used most successfully, radionuclide scanning must be interpreted in conjunction with other techniques, such as bone radiographs with bone scans, chest radiographs with lung scans, and ultrasonic studies with thyroid scans. Interpretation is also enhanced by providing pertinent clinical information because the distribution of radiopharmaceutical agents can be altered by drugs and by various procedures besides physiologic and pathologic conditions. Discussion of the patient with the radionuclide scanning specialist prior to the study and review of the results with that specialist after the study are beneficial

  8. Neutral-beam aiming and calorimetry for MFTF-B

    International Nuclear Information System (INIS)

    Goldner, A.I.; Margolies, D.

    1981-01-01

    The vessel for the Tandem Mirror Fusion Test Facility (MFTF-B) will have up to eleven 0.5-s-duration neutral-beam injectors for the initial heating of the MFTF-B plasma. Knowing the exact alignment of the beams and their total power is critical to the performance of the experiment. Using prototype aiming and calorimetry systems on the High Voltage Test Stand (HVTS) at Lawrence Livermore National Laboratory (LLNL), we hope to prove our ability to obtain an aiming accuracy of +-1 cm at the plasma and a calorimetric accuracy of +-5% of the actual total beam energy

  9. A custom floating point format ADC for LHC calorimetry

    International Nuclear Information System (INIS)

    Hermel, V.; Lecoq, J.; Bohner, G.

    1996-01-01

    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)

  10. Thermal behavior of native and hydrophobized wheat gluten, gliadin and glutenin-rich fractions by modulated DSC.

    Science.gov (United States)

    Micard, V; Guilbert, S

    2000-06-13

    The glass transition temperature (T(g)) of hydrophobized and native wheat gluten and its protein fractions, with water mass fraction from 0 to 0.2, was studied using modulated differential scanning calorimetry. The T(g) values of unplasticized products were approximately 175 degrees C whatever the treatment (hydrophobization) or the fraction tested, except for the gliadin-rich fraction (162 degrees C). Experimental change in heat capacity at the glass transition (DeltaC(p)) ranged from 0.32 to 0. 50 J/g/ degrees C depending on the gluten fractions. The Gordon-Taylor fit of T(g) evolution as a function of water content showed that glutenin-rich fractions were more sensitive to water plasticization than the gliadin-rich fraction. The Kwei equation gave better fit to experimental data and demonstrated that the water plasticization of gluten and its fractions is influenced by secondary interactions. However, the application of the Couchman-Karasz equation without fitting predicts satisfactorily the plasticization of gluten proteins by water.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  12. Distributing functionality in the Drift Scan Camera System

    International Nuclear Information System (INIS)

    Nicinski, T.; Constanta-Fanourakis, P.; MacKinnon, B.; Petravick, D.; Pluquet, C.; Rechenmacher, R.; Sergey, G.

    1993-11-01

    The Drift Scan Camera (DSC) System acquires image data from a CCD camera. The DSC is divided physically into two subsystems which are tightly coupled to each other. Functionality is split between these two subsystems: the front-end performs data acquisition while the host subsystem performs near real-time data analysis and control. Yet, through the use of backplane-based Remote Procedure Calls, the feel of one coherent system is preserved. Observers can control data acquisition, archiving to tape, and other functions from the host, but, the front-end can accept these same commands and operate independently. The DSC meets the needs for such robustness and cost-effective computing

  13. The Pandora Software Development Kit for Particle Flow Calorimetry

    International Nuclear Information System (INIS)

    Marshall, J S; Thomson, M A

    2012-01-01

    Pandora is a robust and efficient framework for developing and running pattern-recognition algorithms. It was designed to perform particle flow calorimetry, which requires many complex pattern-recognition techniques to reconstruct the paths of individual particles through fine granularity detectors. The Pandora C++ software development kit (SDK) consists of a single library and a number of carefully designed application programming interfaces (APIs). A client application can use the Pandora APIs to pass details of tracks and hits/cells to the Pandora framework, which then creates and manages named lists of self-describing objects. These objects can be accessed by Pandora algorithms, which perform the pattern-recognition reconstruction. Development with the Pandora SDK promotes the creation of small, re-usable algorithms containing just the kernel of a specific operation. The algorithms are configured via XML and can be nested to perform complex reconstruction tasks. As the algorithms only access the Pandora objects in a controlled manner, via the APIs, the framework can perform most book-keeping and memory-management operations. The Pandora SDK has been fully exploited in the implementation of PandoraPFA, which uses over 60 algorithms to provide the state of the art in particle flow calorimetry for ILC and CLIC.

  14. Tritium inventory measurements by 'in-bed' gas flowing calorimetry

    International Nuclear Information System (INIS)

    Hayashi, T.; Suzuki, T.; Yamada, M.; Okuno, K.

    1996-01-01

    In order to establish the 'in-bed' tritium accounting technology for the ITER scale tritium storage system, a gas flowing calorimetry has been studied using a scaled ZrCo bed (25 g tritium capacity). The basic calorimetric characteristics, steady state temperature raise of He gas stream flowing through a secondary coil line fixed in the ZrCo tritide, was measured and correlated with the stored tritium inventory. The results shows that about 4 degrees raise of He stream temperature can be detected for each gram of tritium storage. The sensitivity of this calorimetry is about 0.05 g of tritium, calculated by 0.2 degrees of temperature sensor error. The accuracy is better than 0.25 g of tritium on 25 g storage, evaluated by 2 times of standard deviation from the repeat measurements. This accuracy of < 1% on full storage capacity is satisfied the target accountability to measure ± 1 gram of tritium on 100 g storage for ITER. 13 refs., 7 figs

  15. 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

  16. Advanced ion beam calorimetry for the test facility ELISE

    International Nuclear Information System (INIS)

    Nocentini, R.; Fantz, U.; Franzen, P.; Fröschle, M.; Heinemann, B.; Riedl, R.; Ruf, B.; Wünderlich, D.; Bonomo, F.; Pimazzoni, A.; Pasqualotto, R.

    2015-01-01

    The negative ion source test facility ELISE (Extraction from a Large Ion Source Experiment) is in operation since beginning of 2013 at the Max-Planck-Institut für Plasmaphysik (IPP) in Garching bei München. The large radio frequency driven ion source of ELISE is about 1×1 m 2 in size (1/2 the ITER source) and can produce a plasma for up to 1 h. Negative ions can be extracted and accelerated by an ITER-like extraction system made of 3 grids with an area of 0.1 m 2 , for 10 s every 3 minutes. A total accelerating voltage of up to 60 kV is available, i.e. a maximum ion beam power of about 1.2 MW can be produced. ELISE is equipped with several beam diagnostic tools for the evaluation of the beam characteristics. In order to evaluate the beam properties with a high level of detail, a sophisticated diagnostic calorimeter has been installed in the test facility at the end of 2013, starting operation in January 2014. The diagnostic calorimeter is split into 4 copper plates with separate water calorimetry for each of the plates. Each calorimeter plate is made of 15×15 copper blocks, which act as many separate inertial calorimeters and are attached to a copper plate with an embedded cooling circuit. The block geometry and the connection with the cooling plate are optimized to accurately measure the time-averaged power of the 10 s ion beam. The surface of the blocks is covered with a black coating that allows infrared (IR) thermography which provides a 2D profile of the beam power density. In order to calibrate the IR thermography, 48 thermocouples are installed in as many blocks, arranged in two vertical and two horizontal rows. The paper describes the beam calorimetry in ELISE, including the methods used for the IR thermography, the water calorimetry and the analytical methods for beam profile evaluation. It is shown how the maximum beam inhomogeneity amounts to 13% in average. The beam divergence derived by IR thermography ranges between 1° and 4° and

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

    CERN Multimedia

    CERN. Geneva

    2010-01-01

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

  18. Characterisation of 1,3-diammonium propylselenate monohydrate by XRD, FT-IR, FT-Raman, DSC and DFT studies

    Science.gov (United States)

    Thirunarayanan, S.; Arjunan, V.; Marchewka, M. K.; Mohan, S.; Atalay, Yusuf

    2016-03-01

    The crystals of 1,3-diammonium propylselenate monohydrate (DAPS) were prepared and characterised X-ray diffraction (XRD), FT-IR, FT-Raman spectroscopy, and DFT/B3LYP methods. It comprises protonated propyl ammonium moieties (diammonium propyl cations), selenate anions and water molecule which are held together by a number of hydrogen bonds and form infinite chains. The XRD data confirm the transfer of two protons from selenic acid to 1,3-diaminopropane molecule. The DAPS complex is stabilised by the presence of O-H···O and N-H···O hydrogen bonds and the electrostatic interactions as well. The N···O and O···O bond distances are 2.82-2.91 and 2.77 Å, respectively. The FT-IR and FT-Raman spectra of 1,3-diammonium propyl selenate monohydrate are recorded and the complete vibrational assignments have been discussed. The geometry is optimised by B3LYP method using 6-311G, 6-311+G and 6-311+G* basis sets and the energy, structural parameters, vibrational frequencies, IR and Raman intensities are determined. Differential scanning colorimetry (DSC) data were also presented to analyse the possibility of the phase transition. Complete natural bonding orbital (NBO) analysis is carried out to analyse the intramolecular electronic interactions and their stabilisation energies. The electrostatic potential of the complex lies in the range +1.902e × 10-2 to -1.902e × 10-2. The limits of total electron density of the complex is +8.43e × 10-2 to -8.43e × 10-2.

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

    Energy Technology Data Exchange (ETDEWEB)

    Liu Lijun [Mary Kay O' Connor Process Safety Center, Artie McFerrin Department of Chemical Engineering, Texas A and M University System, College Station, TX 77843-3122 (United States); Wei Chunyang [BASF Corporation, Wyandotte, MI 48192 (United States); Guo Yuyan; Rogers, William J. [Mary Kay O' Connor Process Safety Center, Artie McFerrin Department of Chemical Engineering, Texas A and M University System, College Station, TX 77843-3122 (United States); Sam Mannan, M. [Mary Kay O' Connor Process Safety Center, Artie McFerrin Department of Chemical Engineering, Texas A and M University System, College Station, TX 77843-3122 (United States)], E-mail: mannan@tamu.edu

    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.

  20. 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......-sized pores of approximately 14 nm saturated with either distilled water or a sodium chloride solution, as well as on water, the salt solution, and an artificial pore solution, alone. It was found that supercooling is unavoidable during the liquid-solid phase transition, and that even at low temperature...... to limit transport of liquid, whereas heating should be undertaken at a low rate to limit the effect of non-equilibrium....

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

    International Nuclear Information System (INIS)

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

    2009-01-01

    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

  2. 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...

  3. Prospects for and tests of hadron calorimetry with silicon

    International Nuclear Information System (INIS)

    Brau, J.E.; Gabriel, T.A.; Rancoita, P.G.

    1989-03-01

    Hadron calorimetry with silicon may provide crucial capabilities in experiments at the high luminosity, high energy colliders of the future, particularly due to silicon's fast intrinsic speed and absolute calibration. The important underlying processes of our understanding of hadron calorimeters are reviewed to set the framework for the presentation of recent calculations of the expected performance of silicon detector based hadron calorimeters. Such devices employing uranium are expected to achieve the compensation condition (that is, the ratio of the most probable electron signal to hadron signal (e/h) is ∼1.0) based on the understanding that has been derived from the uranium-liquid argon and uranium-plastic scintillator systems. In fact, even lead-silicon calorimeters are found to achieve the attractive value for the e/h ratio of 1.16 at 10 GeV. An experimental test of these predictions is underway at CERN by the SICAPO Collaboration. 64 refs., 19 figs

  4. The importance of calorimetry for highly-boosted jet substructure

    Energy Technology Data Exchange (ETDEWEB)

    Coleman, Evan [Brown U.; Freytsis, Marat [Oregon U.; Hinzmann, Andreas [Hamburg U.; Narain, Meenakshi [Brown U.; Thaler, Jesse [MIT, Cambridge, CTP; Tran, Nhan [Fermilab; Vernieri, Caterina [Fermilab

    2017-09-25

    Jet substructure techniques are playing an essential role in exploring the TeV scale at the Large Hadron Collider (LHC), since they facilitate the efficient reconstruction and identification of highly-boosted objects. Both for the LHC and for future colliders, there is a growing interest in using jet substructure methods based only on charged-particle information. The reason is that silicon-based tracking detectors offer excellent granularity and precise vertexing, which can improve the angular resolution on highly-collimated jets and mitigate the impact of pileup. In this paper, we assess how much jet substructure performance degrades by using track-only information, and we demonstrate physics contexts in which calorimetry is most beneficial. Specifically, we consider five different hadronic final states - W bosons, Z bosons, top quarks, light quarks, gluons - and test the pairwise discrimination power with a multi-variate combination of substructure observables. In the idealized case of perfect reconstruction, we quantify the loss in discrimination performance when using just charged particles compared to using all detected particles. We also consider the intermediate case of using charged particles plus photons, which provides valuable information about neutral pions. In the more realistic case of a segmented calorimeter, we assess the potential performance gains from improving calorimeter granularity and resolution, comparing a CMS-like detector to more ambitious future detector concepts. Broadly speaking, we find large performance gains from neutral-particle information and from improved calorimetry in cases where jet mass resolution drives the discrimination power, whereas the gains are more modest if an absolute mass scale calibration is not required.

  5. 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

    We have investigated the thermal stability of the heteroleptic ruthenium complex C106 employed as a sensitizer in dye-sensitized solar cells. The C106 was adsorbed on TiO2 particles and exposed to 2 different iodide/triidode based redox electrolytes A and B at 80 °C for up to 1500 h in sealed glass......) 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...

  6. Scanning table

    CERN Multimedia

    1960-01-01

    Before the invention of wire chambers, particles tracks were analysed on scanning tables like this one. Today, the process is electronic and much faster. Bubble chamber film - currently available - (links can be found below) was used for this analysis of the particle tracks.

  7. Scan Statistics

    CERN Document Server

    Glaz, Joseph

    2009-01-01

    Suitable for graduate students and researchers in applied probability and statistics, as well as for scientists in biology, computer science, pharmaceutical science and medicine, this title brings together a collection of chapters illustrating the depth and diversity of theory, methods and applications in the area of scan statistics.

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

    International Nuclear Information System (INIS)

    Don W. Miller; Andrew Kauffmann; Eric Kreidler; Dongxu Li; Hanying Liu; Daniel Mills; Thomas D. Radcliff; Joseph Talnagi

    2001-01-01

    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''

  9. Base adsorption calorimetry for characterising surface acidity: a comparison between pulse flow and conventional ''static'' techniques

    International Nuclear Information System (INIS)

    Felix, S.P.; Savill-Jowitt, C.; Brown, D.R.

    2005-01-01

    A pulsed flow adsorption microcalorimeter (pulse-FMC) has been developed by modifying a Setaram 111. It is tested in comparison with a conventional pulsed static adsorption microcalorimeter (pulse-SMC) for characterising surface acidity of solid acid catalysts. Small pulses of 1% ammonia in helium are delivered to an activated catalyst sample and its surface acidity is differentially profiled in terms of the molar enthalpy of ammonia adsorption (ΔH ads o ) using a combination of differential scanning calorimeter (DSC) and a downstream thermal conductivity detector (TCD). The pulsing action and its sequences are controlled by in-house developed software and the TCD output also is logged into a PC. Thus, the pulse-FMC is fully automated. Two sulfonated polystyrene resin-type catalysts, Amberlyst 15 and Amberlyst 35, a zeolite of the type H + -ZSM-5 (CT 410) and an acid activated clay (Fulcat 220) are characterised at appropriate temperatures using both the new technique and the conventional static base adsorption method. ΔH ads o versus surface coverage profiles of all the four catalysts obtained from both pulse-FMC and the conventional method are found to be comparable. Results are interpreted in terms of the extent to which NH 3 adsorption on the catalysts surface is under thermodynamic control in the two methods

  10. Quantum-chemical insight into structure-reactivity relationship in 4,5,6,7-tetrahalogeno-1H-benzimidazoles: a combined X-ray, DSC, DFT/QTAIM, Hirshfeld surface-based, and molecular docking approach.

    Science.gov (United States)

    Latosińska, Jolanta Natalia; Latosińska, Magdalena; Maurin, Jan Krzysztof; Orzeszko, Andrzej; Kazimierczuk, Zygmunt

    2014-03-20

    The weak interaction patterns in 4,5,6,7-tetrahalogeno-1H-benzimidazoles, protein kinase CK2 inhibitors, in solid state are studied by the X-ray method and quantum chemistry calculations. The crystal structures of 4,5,6,7-tetrachloro- and 4,5,6,7-tetrabromo-1H-benzimidazole are determined by X-ray diffraction and refined to a final R-factor of 3.07 and 3.03%, respectively, at room temperature. The compound 4,5,6,7-tetrabromo-1H-benzimidazole, which crystallizes in the I41/a space group, is found to be isostructural with previously studied 4,5,6,7-tetraiodo-1H-benzimidazole in contrast to 4,5,6,7-tetrachloro-1H-benzimidazole, which crystallizes as triclinic P1̅ with 4 molecules in elementary unit. For 4,5,6,7-tetrachloro-1H-benzimidazole, differential scanning calorimetry (DSC) revealed a second order glassy phase transition at Tg = 95°/106° (heating/cooling), an indication of frozen disorder. The lack of 3D isostructurality found in all 4,5,6,7-tetrahalogeno-1H-benzimidazoles is elucidated on the basis of the intra- and intermolecular interactions (hydrogen bonding, van der Waals contacts, and C-H···π interactions). The topological Bader's Quantum Theory of Atoms in Molecules (QTAIM) and Spackman's Hirshfeld surface-based approaches reveal equilibration of electrostatic matching and dispersion van der Waals interactions between molecules consistent with the crystal site-symmetry. The weakening of van der Waals forces accompanied by increasing strength of the hydrogen bond (N-H···N) result in a decrease in the crystal site-symmetry and a change in molecular packing in the crystalline state. Crystal packing motifs were investigated with the aid of Hirshfeld surface fingerprint plots. The ordering 4,5,6,7-tetraiodo > 4,5,6,7-tetrabromo > 4,5,6,7-tetrachloro > 4,5,6,7-tetrafluoro reflects not only a decrease in crystal symmetry but also increase in chemical reactivity (electronic activation), which could explain some changes in biological activity of

  11. Solvent deuteration enhancement of hydrophobicity: DSC study of the inverse temperature transition of elastin-based polypeptides

    International Nuclear Information System (INIS)

    Chihao Luan; Urry, D.W.

    1991-01-01

    As previously shown, the polypentapeptide of elastin, (Val 1 -Pro 2 -Gly 3 -Val 4 -Gly 5 ) n or simply poly(VPGVG), undergoes an inverse temperature transition which is seen macroscopically as a phase separation with a dense viscoelastic phase of about 60% water, 40% peptide by weight and which is characterized molecularly by increase in intra- and intermolecular order as evidenced by formation of specific hydrophobic contacts. Furthermore, from an extensive study of polypentapeptides of the composition poly[f x (VPGXG), f v (VPGVG)], where f x + f v = 1 and X is any of the amino acid residues with apolar (hydrophobic) side chains, it has been shown that the temperature of the transition decreases and the heat of the transition increases with increased hydrophobicity. In the present paper differential scanning calorimetry has been utilized to determine the effect of D 2 O on the temperature and heats of the inverse temperature transitions for poly(VPGVG), poly(IPGVG), poly(LPGVG), and poly(VPAVG) and in the latter case in the presence of 0.5 and 1.0 N NaCl and of 1,2, and 3 M urea. In all cases, the effect of D 2 O as compared to H 2 O is to lower the transition temperature about 2 C and to increase the heat of the transition about 10%, and this occurs also in the presence of NaCl, which itself lowers the temperature and increases the heat, and in the presence of urea, which itself raises the temperature and decreases the heat of the transition. It is concluded that the effect of replacement of H 2 O by D 2 O by D 2 O in these polypeptides is to effect a small but consistent increase in the expression of hydrophobicity

  12. Scanning holograms

    International Nuclear Information System (INIS)

    Natali, S.

    1984-01-01

    This chapter reports on the scanning of 1000 holograms taken in HOBC at CERN. Each hologram is triggered by an interaction in the chamber, the primary particles being pions at 340 GeV/c. The aim of the experiment is the study of charm production. The holograms, recorded on 50 mm film with the ''in line'' technique, can be analyzed by shining a parallel expanded laser beam through the film, obtaining immediately above it the real image of the chamber which can then be scanned and measured with a technique half way between emulsions and bubble chambers. The results indicate that holograms can be analyzed as quickly and reliably as in other visual techniques and that to them is open the same order of magnitude of large scale experiments

  13. Bone scans

    International Nuclear Information System (INIS)

    Hetherington, V.J.

    1989-01-01

    Oftentimes, in managing podiatric complaints, clinical and conventional radiographic techniques are insufficient in determining a patient's problem. This is especially true in the early stages of bone infection. Bone scanning or imaging can provide additional information in the diagnosis of the disorder. However, bone scans are not specific and must be correlated with clinical, radiographic, and laboratory evaluation. In other words, bone scanning does not provide the diagnosis but is an important bit of information aiding in the process of diagnosis. The more useful radionuclides in skeletal imaging are technetium phosphate complexes and gallium citrate. These compounds are administered intravenously and are detected at specific time intervals postinjection by a rectilinear scanner with minification is used and the entire skeleton can be imaged from head to toe. Minification allows visualization of the entire skeleton in a single image. A gamma camera can concentrate on an isolated area. However, it requires multiple views to complete the whole skeletal image. Recent advances have allowed computer augmentation of the data received from radionucleotide imaging. The purpose of this chapter is to present the current radionuclides clinically useful in podiatric patients

  14. Multiple-specimen absolute paleointensity determination with the MSP-DSC protocol: Advantages and drawbacks.

    Science.gov (United States)

    Camps, P.; Fanjat, G.; Poidras, T.; Carvallo, C.; Nicol, P.

    2012-04-01

    The MSP-DSC protocol (Dekkers & Bohnel, 2006, EPSL; Fabian & Leonhardt, 2010, EPSL) is a recent development in the methodology for documenting the intensity of the ancient Earth magnetic field. Applicable both on rocks or archaeological artifacts it allows us to use samples that until now were not measured because their magnetic properties do not meet selection criteria required by conventional methods. However, this new experimental protocol requires that samples be heated and cooled under a field parallel to its natural remanent magnetization (NRM). Currently, standard paleointensity furnaces do not match precisely this constraint. Yet, such new measurement protocol seems very promising since it would possibly double the number of available data. We are developing in Montpellier (France), a very fast-heating oven with infrared dedicated to this protocol. Two key points determine its characteristics. The first is to heat uniformly a rock sample of a 10-cc-standard volume as fast as possible. The second is to apply to the sample during the heating (and the cooling) a precise magnetic induction field, perfectly controlled in 3D. We tested and calibrated a preliminary version of this oven along with the MSP-DSC protocol with 3 historical lava flows, 2 from Reunion Island (erupted in 2002 and 2007) and one from Etna (erupted in 1983). These lava flows were selected because they have different magnetic behaviors. Reunion 2002 is rather SD-PSD-like, while Reunion 2007 is PSD-MD-like, and Etna 1983 is MD-like. The paleointensity determinations obtained with the original protocol of Dekkers and Bohnel (2006, EPSL) are within +- 1 μT of the known field for the three lava flows. The same precision is obtained when we applied the fraction correction (MSP-FC protocol). However, we systematically observed a loss in the linearity of the MSP-FC plots. In addition, like Muxworthy and Taylor (2011, GJI), we found that the Domain State Correction is difficult to apply since alpha

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

    Science.gov (United States)

    Blume, A; Tuchtenhagen, J

    1992-05-19

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

  16. Physiochemical properties of the complex of myricetin and ...

    African Journals Online (AJOL)

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

  17. Kenaf fiber-reinforced copolyester biocomposites

    CSIR Research Space (South Africa)

    Mokhothu, Thabang H

    2011-12-01

    Full Text Available scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), tensile properties, environmental scanning electron microscopy (ESEM), and biodegradability. The extent of silane initiated grafting was followed by gel content...

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

    CERN Document Server

    Mavromanolakis, G; Lecoq, P

    2011-01-01

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

  19. Improvement in Performance of ZnO based DSC Prepared by Spraying Method

    Directory of Open Access Journals (Sweden)

    Rangga Winantyo

    2013-09-01

    Full Text Available This paper reports the effect of TiCl4 on the performance of ZnO based DSC. ZnO was used due to its stability against photo-corrosion  and  photochemical  properties  similar  to  TiO2.  Thin  films  of  nanocrystalline  ZnO  were  deposited  on transparent conducting oxide glass using spray  method. The ZnO  films  were treated using TiCl4. The cell’s efficiency was found to be 2.5% with TiCl4 post-treatment and 1.9% without TiCl4 post-treatment.

  20. Synthesis, characterization and TG-DSC study of cadmium halides adducts with caffeine

    Energy Technology Data Exchange (ETDEWEB)

    Farias, Robson F. de; Silva, Ademir O. da; Silva, Umberto G. da

    2003-11-28

    The synthesis, characterization and TG-DSC study of the compounds CdX{sub 2}{center_dot}ncaff, for which X: Cl, Br and I; n=1 and 2 and caff: caffeine is reported. It is verified that caffeine is coordinated through more than one coordination site, despite the fact that the nitrogen of the imidazole ring is the main coordination site. The following thermal stability trend is observed: Cl>Br>I and monoadducts are more stable than bisadducts. The thermal degradation (td) enthalpies have the values (kJ mol{sup -1}): 58.2 and 71.5; 74.9 and 91.4; 31.1 and 47.5 for Cl, Br and I mono and bisadducts, respectively.

  1. Complex Heat Capacity of Lithium Borate Glasses Studied by Modulated DSC

    Science.gov (United States)

    Matsuda, Yu; Matsui, Chihiro; Ike, Yuji; Kodama, Masao; Kojima, Seiji

    2006-05-01

    Complex heat capacity, Cp* = Cp' - iCp″, of lithium borate glasses Li2Oṡ(1-x)B2O3 (x = 0.00 - 0.33) has been investigated by Modulated DSC (MDSC). We have successfully observed the frequency dependent Cp* by MDSC in the frequency range 0.01 to 0.1 Hz, and the average relaxation time of glass transition has been determined as a function of temperature. Moreover, the composition dependence of the thermal properties has been investigated. The calorimetric glass transition temperatures become higher with the increase of concentration of Li2O and show the board maximum around x = 0.26-0.28. The width of glass transition region becomes narrower as Li2O increases. These results relate to the change of the fragility of the system. It has been proven that the complex heat capacity spectroscopy by MDSC is a powerful tool to investigate the glass transition phenomena.

  2. Front-End Electronics in calorimetry: from LHC to ILC

    International Nuclear Information System (INIS)

    De La Taille, Ch.

    2009-09-01

    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 Si-W electromagnetic

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  4. An investigation of calibration methods for solution calorimetry.

    Science.gov (United States)

    Yff, Barbara T S; Royall, Paul G; Brown, Marc B; Martin, Gary P

    2004-01-28

    Solution calorimetry has been used in a number of varying applications within pharmaceutical research as a technique for the physical characterisation of pharmaceutical materials, such as quantifying small degrees of amorphous content, identifying polymorphs and investigating interactions between drugs and carbohydrates or proteins and carbohydrates. A calibration test procedure is necessary to validate the instrumentation; a few of the suggested calibration reactions are the enthalpies of solution associated with dissolving Tris in 0.1 M HCl or NaCl, KCl or propan-1-ol in water. In addition, there are a number of different methods available to determine enthalpies of solution from the experimental data provided by the calorimeter, for example, the Regnault-Pfaundler's method, a graphical extrapolation based on the Dickinson method, or a manual integration-based method. Thus, the aim of the study was to investigate how each of these methods influences the values for the enthalpy of solution. Experiments were performed according to the method outlined by Hogan and Buckton [Int. J. Pharm. 207 (2000) 57] using KCl (samples of 50, 100 and 200 mg), Tris and sucrose as calibrants. For all three materials the manual integration method was found to be the most consistent with the KCl in water (sample mass of 200 mg) being the most precise. Thus, this method is recommended for the validation of solution calorimeters.

  5. 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.

  6. Isothermal reaction calorimetry as a tool for kinetic analysis

    International Nuclear Information System (INIS)

    Zogg, Andreas; Stoessel, Francis; Fischer, Ulrich; Hungerbuehler, Konrad

    2004-01-01

    Reaction calorimetry has found widespread application for thermal and kinetic analysis of chemical reactions in the context of thermal process safety as well as process development. This paper reviews the most important reaction calorimetric principles (heat-flow, heat-balance, power-compensation, and Peltier principle) and their applications in commercial or scientific devices. The discussion focuses on the different dynamic behavior of the main calorimetric principles during an isothermal reaction measurement. Examples of available reaction calorimeters are further compared considering their detection limit, time constant as well as temperature range. In a second part, different evaluation methods for the isothermally measured calorimetric data are reviewed and discussed. The methods will be compared, focusing especially on the fact that reaction calorimetric data always contains additional informations not directly related to the actual chemical reaction such as heat of mixing, heat of phase-transfer/change processes or simple measurement errors. Depending on the evaluation method applied such disturbances have a significant influence on the calculated reaction enthalpies or rate constants

  7. Thermodynamic properties of soddyite from solubility and calorimetry measurements

    International Nuclear Information System (INIS)

    Gorman-Lewis, Drew; Mazeina, Lena; Fein, Jeremy B.; Szymanowski, Jennifer E.S.; Burns, Peter C.; Navrotsky, Alexandra

    2007-01-01

    The release of uranium from geologic nuclear waste repositories under oxidizing conditions can only be modeled if the thermodynamic properties of the secondary uranyl minerals that form in the repository setting are known. Toward this end, we synthesized soddyite ((UO 2 ) 2 (SiO 4 )(H 2 O) 2 ), and performed solubility measurements from both undersaturation and supersaturation. The solubility measurements rigorously constrain the value of the solubility product of synthetic soddyite, and consequently its standard-state Gibbs free energy of formation. The log solubility product (lg K sp ) with its error (1σ) is (6.43 + 0.20/-0.37), and the standard-state Gibbs free energy of formation is (-3652.2 ± 4.2 (2σ)) kJ mol -1 . High-temperature drop solution calorimetry was conducted, yielding a calculated standard-state enthalpy of formation of soddyite of (-4045.4 ± 4.9 (2σ)) kJ . mol -1 . The standard-state Gibbs free energy and enthalpy of formation yield a calculated standard-state entropy of formation of soddyite of (-1318.7 ± 21.7 (2σ)) J . mol -1 . K -1 . The measurements and associated thermodynamic calculations not only describe the T = 298 K stability and solubility of soddyite, but they also can be used in predictions of repository performance through extrapolation of these properties to repository temperatures

  8. Test of calorimetry for high burn-up plutonium

    International Nuclear Information System (INIS)

    Beets, C.; Carchon, R.; Fettweis, P.

    1984-01-01

    In recent times, the interest of applying calorimetry for safeguards purpose is steadily increasing. Calorimetric measurements have been performed on a set of high burn-up (25000 MWd/t) Pu samples, ranging in mass between 60 g and 2.5 kg Pu, distributed as PuO 2 powder embedded in stainless steel containers. The powers produced by these containers ranged between 0.8 W and 36 W. The calorimeter used was the Mound 150 type, and the isotopics and the Am content have been determined earlier by mass spectroscopy, completed with α and γ counting, and were later verified by the same methods. Watts/gram measurements were made on twelve 60 g samples of the same plutonium lot to demonstrate the Pu elemental and isotopic homogeneity, and hence, its suitability for subsequent NDA experiments. These samples were also measured in a stacked way to fill up the mass and wattage gaps between 60 g (0.8W) and 1 kg (14W). Calorimetric assay values, obtained with both isotopic measurements are discussed

  9. Prospects for and tests of hadron calorimetry with silicon

    Energy Technology Data Exchange (ETDEWEB)

    Brau, James E. [Univ. of Oregon, OR (United States). Dept. of Physics; Gabriel, Tony A. [Oak Ridge National Lab., TN (United States); Rancoita, P. G. [INFN, Milan (Italy)

    1989-03-01

    Hadron calorimetry with silicon may provide crucial capabilities in experiments at the high luminosity, high energy colliders of the future, particularly due to silicon's fast intrinsic speed and absolute calibration. The important underlying processes of our understanding of hadron calorimeters are reviewed to set the framework for the presentation of recent calculations of the expected performance of silicon detector based hadron calorimeters. Such devices employing uranium are expected to achieve the compensation condition (that is, the ratio of the most probable electron signal to hadron signal (e/h) is approx.1.0) based on the understanding that has been derived from the uranium-liquid argon and uranium-plastic scintillator systems. In fact, even lead-silicon calorimeters are found to achieve the attractive value for the e/h ratio of 1.16 at 10 GeV. An experimental test of these predictions is underway at CERN by the SICAPO Collaboration. 64 refs., 19 figs.

  10. 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...

  11. Estimation of water-coal surface interaction during heat treatment of coal by use of FTir and DSC; FTir to DSC wo mochiita sekitan-mizu kan sogo sayo no teiryoteki hyoka

    Energy Technology Data Exchange (ETDEWEB)

    Miura, K.; Mae, K.; Morozumi, F.; Kusakawa, T. [Kyoto University, Kyoto (Japan)

    1997-10-30

    The authors have recently presented a method to estimate the strength distribution of hydrogen bondings in coal using FTir and DSC. The method was applied to estimate the strength of coal-water interaction in two different coals and to estimate the enthalpy change deriving from the change in hydrogen bondings during the desorption of water. The estimated enthalpy change was compared with the total enthalpy change estimated by DSC measurement to examine the importance of hydrogen bondings during the desertion of water. 1 ref., 6 figs.

  12. 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.)

  13. Calorimetry at the international linear collider. From simulation to reality

    International Nuclear Information System (INIS)

    Wattimena, Nanda

    2010-02-01

    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.)

  14. Laser-Driven Calorimetry Measurements of Petroleum and Biodiesel Fuels.

    Science.gov (United States)

    Presser, Cary; Nazarian, Ashot; Millo, Amit

    2018-02-01

    Thermochemical characteristics were determined for several National Institute of Standards and Technology standard-reference-material petroleum and biodiesel fuels, using a novel laser-heating calorimetry technique. Measurements focused on the sample thermal behavior, specific heat release rate, and total specific heat release. The experimental apparatus consists of a copper sphere-shaped reactor mounted within a chamber, along with laser-beam-steering optical components, gas-supply manifold, and a computer-controlled data-acquisition system. At the center of the reactor, liquid sample is injected onto a copper pan substrate that rests and is in contact with a fine-wire thermocouple. A second thermocouple is in contact with the inner reactor sphere surface. The reactor is heated from opposing sides by a continuous-wave, near-infrared laser to achieve nearly uniform sample temperature. The change in temperature with time (thermogram) is recorded for both thermocouples, and compared to a baseline thermogram (without liquid in the pan). The thermograms are then processed (using an equation for thermal energy conservation) for the thermochemical information of interest. The results indicated that the energy reaching the pan is dominated by radiative heat transfer processes, while the dominant thermal process for the reactor sphere is the stored (internal) thermal energy within the sphere material. Sufficient laser power is necessary to detect the fuel thermal-related characteristics, and the required power can differ from one fuel to another. With sufficient laser power, one can detect the preferential vaporization of the lighter and heavier fuel fractions. The total specific heat release obtained for the different conventional and biodiesel fuels used in this investigation were similar to the expected values available in the literature.

  15. Application of calorimetry and thermodynamics to critical problems in materials science

    International Nuclear Information System (INIS)

    Atake, Tooru

    2009-01-01

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

  16. Application of prediction of equilibrium to servo-controlled calorimetry measurements

    International Nuclear Information System (INIS)

    Mayer, R.L. II

    1987-01-01

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

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

    International Nuclear Information System (INIS)

    Presoly, P; Bernhard, C; Six, J

    2016-01-01

    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 (T Liquid , T Solid , T Perit , T γ→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. (paper)

  18. 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.

  19. FTIR, XRD and DSC studies of nanochitosan, cellulose acetate and polyethylene glycol blend ultrafiltration membranes.

    Science.gov (United States)

    Vinodhini, P Angelin; K, Sangeetha; Thandapani, Gomathi; P N, Sudha; Jayachandran, Venkatesan; Sukumaran, Anil

    2017-11-01

    In the present work, a series of novel nanochitosan/cellulose acetate/polyethylene glycol (NCS/CA/PEG) blend flat sheet membranes were fabricated in different ratios (1:1:1, 1:1:2, 2:1:1, 2:1:2, 1:2:1, 2:2:1) in a polar solvent of N,N'-dimethylformamide (DMF) using the most popular phase inversion method. Nanochitosan was prepared by the ionotropic gelation method and its average particle size has been analyzed using Dynamic Light Scattering (DLS) method. The effect of blending of the three polymers was investigated using FTIR and XRD studies. FTIR results confirmed the formation of well-blended membranes and the XRD analysis revealed enhanced amorphous nature of the membrane ratio 2:1:2. DSC study was conducted to find out the thermal behavior of the blend membranes and the results clearly indicated good thermal stability and single glass transition temperature (T g ) of all the prepared membranes. Asymmetric nature and rough surface morphology was confirmed using SEM analysis. From the results it was evident that the blending of the polymers with higher concentration of nanochitosan can alter the nature of the resulting membranes to a greater extent and thus amorphous membranes were obtained with good miscibility and compatibility. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. DSC and X-ray diffraction investigations of phase transitions in HxBABA and NBABA

    International Nuclear Information System (INIS)

    Usha Deniz, K.; Paranjpe, A.S.; Mirza, E.B.; Parvathanathan, P.S.; Patel, K.S.

    1979-01-01

    The phase transitions and the heats of transformation, of the hexyl (HxBABA) and nonyl (NBABA) members of the series of compounds, p-n-Alkoxybenzylidene-p-Aminobenzoic Acids, have been studied by DSC in the temperature range, - 100 0 C to 300 0 C. A scheme of transitions has been proposed for each of the compounds. X-ray diffraction measurements have been done in the smectic C(Ssub(c)) and nematic (N) phases of these materials. The results reveal that (1) the Ssub(c) phase in both compounds is of the C 1 -type, (2) Ssub(c)-type order is seen throughout the nematic phase in HxBABA, whereas in NBABA, it is seen only in the neighbourhood of the Ssub(c)-N transition, (3) the temperature dependence of the smectic layer thickness, d, and of the directly measured tilt angle, theta sub(t,d), reflect faithfully the strength of the first order transition, Ssub(c)-N, and (4) there is a marked difference between the values and the temperature variations of theta sub(t,d) and theta sub(t,c) (tilt angle calculated from d) which is not completely understood, at present

  1. Development and validation of an open source quantification tool for DSC-MRI studies.

    Science.gov (United States)

    Gordaliza, P M; Mateos-Pérez, J M; Montesinos, P; Guzmán-de-Villoria, J A; Desco, M; Vaquero, J J

    2015-03-01

    This work presents the development of an open source tool for the quantification of dynamic susceptibility-weighted contrast-enhanced (DSC) perfusion studies. The development of this tool is motivated by the lack of open source tools implemented on open platforms to allow external developers to implement their own quantification methods easily and without the need of paying for a development license. This quantification tool was developed as a plugin for the ImageJ image analysis platform using the Java programming language. A modular approach was used in the implementation of the components, in such a way that the addition of new methods can be done without breaking any of the existing functionalities. For the validation process, images from seven patients with brain tumors were acquired and quantified with the presented tool and with a widely used clinical software package. The resulting perfusion parameters were then compared. Perfusion parameters and the corresponding parametric images were obtained. When no gamma-fitting is used, an excellent agreement with the tool used as a gold-standard was obtained (R(2)>0.8 and values are within 95% CI limits in Bland-Altman plots). An open source tool that performs quantification of perfusion studies using magnetic resonance imaging has been developed and validated using a clinical software package. It works as an ImageJ plugin and the source code has been published with an open source license. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Complex Heat Capacity of Lithium Borate Glasses Studied by Modulated DSC

    International Nuclear Information System (INIS)

    Matsuda, Yu; Ike, Yuji; Matsui, Chihiro; Kodama, Masao; Kojima, Seiji

    2006-01-01

    Complex heat capacity, C p * = C p ' - iC p '', of lithium borate glasses Li2O·(1-x)B2O3 (x = 0.00 - 0.33) has been investigated by Modulated DSC (MDSC). We have successfully observed the frequency dependent C p * by MDSC in the frequency range 0.01 to 0.1 Hz, and the average relaxation time of glass transition has been determined as a function of temperature. Moreover, the composition dependence of the thermal properties has been investigated. The calorimetric glass transition temperatures become higher with the increase of concentration of Li2O and show the board maximum around x = 0.26-0.28. The width of glass transition region becomes narrower as Li2O increases. These results relate to the change of the fragility of the system. It has been proven that the complex heat capacity spectroscopy by MDSC is a powerful tool to investigate the glass transition phenomena

  3. Raman scattering and modulated-DSC experiments on Potassium Germanate glasses*

    Science.gov (United States)

    Wang, N.; Novita, D.; Boolchand, P.

    2006-03-01

    We have synthesized titled glasses in the 0 modulated-DSC (MDSC) experiments. Raman lineshapes observed in the present work are quite similar to those reported by Henderson and Wang ^1. Preliminary MDSC experiments reveal glass transition temperatures, Tg(x), starting from a value of 570 C at x = 0, to decrease to 508 C near x = 0.06, and to increase thereafter almost linearly to 552 C as x increases to 0.15. On the other hand, the non-reversing enthalpy associated with Tg provides evidence of a global minimum in the 0.08 0.10 as Floppy, while those in the reversibility window as representing the Intermediate Phase^2. The space filling nature of the Intermediate Phase is, independently, corroborated by trends in molar volumes which show a broad global minimum in the 9-11% range. Identification of the three elastic phases provides a physical basis to understand the origin of the Germanate anomaly, and the electrical conductivity threshold when glasses become mechanically floppy. *Supported by NSF grant DMR 04-56472. ^1 G.S.Henderson and H.M.Wang, Eur. J. Mineral. 14, 733 (2002). ^2 P.Boolchand, G.Lucovsky, J.C. Phillips and M.F.Thorpe, Phil. Mag 85,3823 (2005).

  4. A DSC study of deterioration caused by environmental chemical pollutants to parchment, a collagen-based material

    International Nuclear Information System (INIS)

    Budrugeac, Petru; Badea, Elena; Gatta, Giuseppe Della; Miu, Lucretia; Comanescu, Alina

    2010-01-01

    A DSC study of new parchments exposed at 25 o C for 1-16 weeks to controlled atmospheres containing 50 ppm of gaseous chemical pollutants (NO 2 , SO 2 , NO 2 + SO 2 ) and 50% relative humidity (RH) was performed. Samples were exposed to chemical pollutants alone, as well as after previous heating at 100 o C for 2-16 days and/or irradiating with visible light (1.7 x 10 5 lx) for 4-16 h. DSC measurements were performed in both sealed crucibles in static air atmosphere at 25-200 o C and open crucibles under gas flow (nitrogen, oxygen, synthetic air) at 25-280 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.

  5. 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. Copyright © 2013 Elsevier Inc. All rights reserved.

  6. 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.

  7. Psychometric Evaluation of the Diabetes Symptom Checklist-Revised (DSC-R)-A Measure of Symptom Distress

    NARCIS (Netherlands)

    Arbuckle, R.A.; Humphrey, L.; Vardeva, K.; Arondekar, B.; Scott, J.A.; Snoek, F.J.

    2009-01-01

    Objective: To assess the psychometric validity, reliability, responsiveness, and minimal important differences of the Diabetes Symptoms Checklist-Revised (DSC-R), a widely used patient-reported outcome measure of diabetes symptom distress. Research Design and Methods: Psychometric validity of the

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

    DEFF Research Database (Denmark)

    Jeppesen, Stinus; Linderoth, Søren; Pryds, Nini

    2008-01-01

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

  9. Head CT scan

    Science.gov (United States)

    ... scan - orbits; CT scan - sinuses; Computed tomography - cranial; CAT scan - brain ... head size in children Changes in thinking or behavior Fainting Headache, when you have certain other signs ...

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

    Science.gov (United States)

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

    2016-05-01

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

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

    Science.gov (United States)

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

    2017-04-01

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

  12. Relaxation dynamics of glass transition in PMMA + SWCNT composites by temperature-modulated DSC

    Science.gov (United States)

    Pradhan, N. R.; Iannacchione, G. S.

    2010-03-01

    The experimental technique offered by temperature-modulated differential scanning calorimeter (TMDSC) used to investigate the thermal relaxation dynamics through the glass transition as a function of frequency was studied for pure PMMA and PMMA-single wall carbon nanotubes (SWCNTs) composites. A strong dependence of the temperature dependence peak in the imaginary part of complex heat capacity (Tmax) is found during the transition from the glass-like to the liquid-like region. The frequency dependence of Tmax of the imaginary part of heat capacity (Cp) is described by Arrhenius law. The activation energy obtained from the fitting shows increases while the characteristic relaxation time decreases with increasing mass fraction (phim) of SWCNTs. The dynamics of the composites during glass transition, at slow and high scan rates, are also the main focus of this experimental study. The change in enthalpy during heating and cooling is also reported as a function of scan rate and frequency of temperature modulation. The glass transition temperature (Tg) shows increases with increasing frequency of temperature modulation and phim of SWCNTs inside the polymer host. Experimental results show that Tg is higher at higher scan rates but as the frequency of temperature modulation increases, the Tg values of different scan rates coincide with each other and alter the scan rate dependence. From the imaginary part of heat capacity, it is obvious that Tmax is not the actual glass transition temperature of pure polymer but Tmax and Tg values can be superimposed when phim increases in the polymer host or when the sample undergoes a transition with a certain frequency of temperature modulation.

  13. Picowatt Resolution Calorimetry for Micro and Nanoscale Energy Transport Studies

    Science.gov (United States)

    Sadat, Seid H.

    Precise quantification of energy transport is key to obtaining insights into a wide range of phenomena across various disciplines including physics, chemistry, biology and engineering. This thesis describes technical advancements into heat-flow calorimetry which enable measurement of energy transport at micro and nanoscales with picowatt resolution. I have developed two types of microfabricated calorimeter devices and demonstrated single digit picowatt resolution at room temperature. Both devices incorporate two distinct features; an active area isolated by a thermal conductance (GTh) of less than 1 microW/K and a high resolution thermometer with temperature resolution (DeltaTres) in the micro kelvin regime. These features enable measurements of heat currents (q) with picowatt resolution (q= Th xDeltaTres). In the first device the active area is suspended via silicon nitride beams with excellent thermal isolation (~600 nW/K) and a bimaterial cantilever (BMC) thermometer with temperature resolution of ~6 microK. Taken together this design enabled calorimetric measurements with 4 pW resolution. In the second device, the BMC thermometry technique is replaced by a high-resolution resistance thermometry scheme. A detailed noise analysis of resistance thermometers, confirmed by experimental data, enabled me to correctly predict the resolution of different measurement schemes and propose techniques to achieve an order of magnitude improvement in the resolution of resistive thermometers. By incorporating resistance thermometers with temperature resolution of ~30 microK, combined with a thermal isolation of ~150 nW/K, I demonstrated an all-electrical calorimeter device with a resolution of ~ 5 pW. Finally, I used these calorimeters to study Near-Field Radiative Heat Transfer (NF-RHT). Using these devices, we studied--for the first time--the effect of film thickness on the NF-RHT between two dielectric surfaces. We showed that even a very thin film (~50 nm) of silicon

  14. Determination of the enthalpy of formation of Ni-Al intermetallic compounds using differential scanning calorimetry technique

    International Nuclear Information System (INIS)

    Kubaski, Evaldo Toniolo; Capocchi, Jose Deodoro Trani; Cintho, Osvaldo Mitsuyuki

    2010-01-01

    The compositions Ni20Al80, Ni25Al75, Ni40Al60, Ni50Al50, Ni60Al40 and Ni75Al25 (at. %) were heated in a calibrated thermal analysis equipment. All runs were conducted at a heating rate of 10 deg C/min under a dynamic argon atmosphere. Each composition was heated until the completion of the corresponding exothermic reaction responsible for intermetallic compound formation, and, also heated to 1480 deg C. The products obtained were characterized using X ray diffraction in order to identify the intermetallic compounds that were synthesized. Moreover, the results were evaluated using variance analysis. As a result, enthalpies of formation of Ni 2 Al 3 and Ni 3 Al compounds were determined by means of this methodology. Experimental values were 167 kJ/mol and 93 kJ/mol for Ni 2 Al 3 and Ni 3 Al, respectively. The former is 18% lower than the value found on literature, while the latter is 6% greater. (author)

  15. Relaxation Dynamics of the Glass Transition in PMMA+SWCNT Composites by Temperature-Modulated DSC

    Science.gov (United States)

    Pradhan, Nihar; Iannacchione, Germano

    2010-03-01

    Temperature Modulated Differential Scanning Calorimeter (TMDSC) used to investigate the thermal relaxation dynamics of PMMA-Single wall carbon nanotubes (SWCNTs) through the glass transition as a function of frequency. A strong dependence of the temperature dependence peak in imaginary part of complex heat capacity (Tmax) was found during the transition from glass like to liquid like region and can be described by Arhenius law. The activation energy shows increases while the charactersistic time decreases with increasing mass fraction (φm) of SWCNTs. Decreasing of enthalpy, while heating and slowly increasing while cooling at 2.0 K/min scan rate was observed and as frequency of temperature modulation increases. There is no relative change of enthalpy in heating and cooling observed at sufficiently slow scan rate. The glass transition temperature (Tg) shows increases as a function of frequency of temperature modulation, φm of SWCNTs and with increasing scan rate. From imaginary part of heat capacity, it obvious that Tmax is not the actual glass transition temperature of pure polymer but Tmax and Tg values can be superimpose when φm of SWCNT increases in polymer.

  16. Longitudinal DSC-MRI for Distinguishing Tumor Recurrence From Pseudoprogression in Patients With a High-grade Glioma.

    Science.gov (United States)

    Boxerman, Jerrold L; Ellingson, Benjamin M; Jeyapalan, Suriya; Elinzano, Heinrich; Harris, Robert J; Rogg, Jeffrey M; Pope, Whitney B; Safran, Howard

    2017-06-01

    For patients with high-grade glioma on clinical trials it is important to accurately assess time of disease progression. However, differentiation between pseudoprogression (PsP) and progressive disease (PD) is unreliable with standard magnetic resonance imaging (MRI) techniques. Dynamic susceptibility contrast perfusion MRI (DSC-MRI) can measure relative cerebral blood volume (rCBV) and may help distinguish PsP from PD. A subset of patients with high-grade glioma on a phase II clinical trial with temozolomide, paclitaxel poliglumex, and concurrent radiation were assessed. Nine patients (3 grade III, 6 grade IV), with a total of 19 enhancing lesions demonstrating progressive enhancement (≥25% increase from nadir) on postchemoradiation conventional contrast-enhanced MRI, had serial DSC-MRI. Mean leakage-corrected rCBV within enhancing lesions was computed for all postchemoradiation time points. Of the 19 progressively enhancing lesions, 10 were classified as PsP and 9 as PD by biopsy/surgery or serial enhancement patterns during interval follow-up MRI. Mean rCBV at initial progressive enhancement did not differ significantly between PsP and PD (2.35 vs. 2.17; P=0.67). However, change in rCBV at first subsequent follow-up (-0.84 vs. 0.84; P=0.001) and the overall linear trend in rCBV after initial progressive enhancement (negative vs. positive slope; P=0.04) differed significantly between PsP and PD. Longitudinal trends in rCBV may be more useful than absolute rCBV in distinguishing PsP from PD in chemoradiation-treated high-grade gliomas with DSC-MRI. Further studies of DSC-MRI in high-grade glioma as a potential technique for distinguishing PsP from PD are indicated.

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

    OpenAIRE

    Fini, Adamo; Cavallari, Cristina; Ospitali, Francesca

    2010-01-01

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

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

    Science.gov (United States)

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

    2011-01-01

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

  19. 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.

  20. Characterization of Microemulsions Prepared using Isopropyl ...

    African Journals Online (AJOL)

    HP

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

  1. Physicochemical Characterization of Inclusion Complex of Catechin ...

    African Journals Online (AJOL)

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

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

    Science.gov (United States)

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

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

    NARCIS (Netherlands)

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

    2018-01-01

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

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

    African Journals Online (AJOL)

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

  5. Hydroxychalcone and Hydroxypropyl-β-Cyclodextrin

    African Journals Online (AJOL)

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

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

    Science.gov (United States)

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

  7. Triacylglycerol and melting profiles of milk fat from several species

    NARCIS (Netherlands)

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

    2012-01-01

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

  8. Brain PET scan

    Science.gov (United States)

    ... results on a PET scan. Blood sugar or insulin levels may affect the test results in people with diabetes . PET scans may be done along with a CT scan. This combination scan is called a PET/CT. Alternative Names Brain positron emission tomography; PET scan - brain References Chernecky ...

  9. Formulation and Evaluation of Spray-Dried Esomeprazole ...

    African Journals Online (AJOL)

    HP

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

  10. Infrared spectroscopy as a tool to characterise starch ordered structure--a joint FTIR-ATR, NMR, XRD and DSC study.

    Science.gov (United States)

    Warren, Frederick J; Gidley, Michael J; Flanagan, Bernadine M

    2016-03-30

    Starch has a heterogeneous, semi-crystalline granular structure and the degree of ordered structure can affect its behaviour in foods and bioplastics. A range of methodologies are employed to study starch structure; differential scanning calorimetry, (13)C nuclear magnetic resonance, X-ray diffraction and Fourier transform infrared spectroscopy (FTIR). Despite the appeal of FTIR as a rapid, non-destructive methodology, there is currently no systematically defined quantitative relationship between FTIR spectral features and other starch structural measures. Here, we subject 61 starch samples to structural analysis, and systematically correlate FTIR spectra with other measures of starch structure. A hydration dependent peak position shift in the FTIR spectra of starch is observed, resulting from increased molecular order, but with complex, non-linear behaviour. We demonstrate that FTIR is a tool that can quantitatively probe short range interactions in starch structure. However, the assumptions of linear relationships between starch ordered structure and peak ratios are overly simplistic. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Phase behavior in blends of ethylene oxide-propylene oxide copolymer and poly(ether sulfone) studied by modulated-temperature DSC and NMR relaxometry.

    Science.gov (United States)

    Van Lokeren, Luk; Gotzen, Nicolaas-Alexander; Pieters, Ronny; Van Assche, Guy; Biesemans, Monique; Willem, Rudolph; Van Mele, Bruno

    2009-01-01

    The state diagram of a blend consisting of a copolymer containing ethylene oxide and propylene oxide, P(EO-ran-PO), and poly(ether sulfone), PES, is constructed by using modulated-temperature differential scanning calorimetry (MTDSC), T(2) NMR relaxometry, and light scattering. The apparent heat capacity signal in MTDSC is used for the characterization of polymer miscibility and morphology development. T(2) NMR relaxometry is used to detect the onset of phase separation, which is in good agreement with the onset of phase separation in the apparent heat capacity from MTDSC and the cloud-point temperature as determined from light scattering. The coexistence curve can be constructed from T(2) values at various temperatures by using a few blends with well-chosen compositions. These T(2) values also allow the detection of the boundary between the demixing zones with and without interference of partial vitrification and are in good agreement with stepwise quasi-isothermal MTDSC heat capacity measurements. Important interphases are detected in the heterogeneous P(EO-ran-PO)/PES blends.

  12. The physics of compensating calorimetry and the new CALOR89 code system

    International Nuclear Information System (INIS)

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

    1989-03-01

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

  13. Application of prediction of equilibrium to servo-controlled calorimetry measurements

    International Nuclear Information System (INIS)

    Mayer, R.L. II.

    1987-01-01

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

  14. Heart PET scan

    Science.gov (United States)

    ... nuclear medicine scan; Heart positron emission tomography; Myocardial PET scan ... A PET scan requires a small amount of radioactive material (tracer). This tracer is given through a vein (IV), ...

  15. DSC (Differential Scanning Calorimerty used to follow the evolution of W/O emulsions versus time on ground and in space in the ISS

    Directory of Open Access Journals (Sweden)

    Drelich Audrey

    2018-01-01

    Full Text Available The evolution of W/O emulsion versus time in microgravity conditions has been studied in the framework of the FASES (Fundamental and Applied Studies on Emulsion Stability project sponsored by the European Space Agency (ESA. The objective of this study was to investigate the evolution of W/O emulsions made of water + paraffin oil + SPAN 80® under purely diffusive conditions (no gravity driven effects and to compare with evolution of similar emulsions observed on ground. A correlation between the state of dispersion of water and either the freezing temperature during cooling, or the freezing time at a fixed temperature was used to follow the emulsion evolution versus time. For that purpose, two identical calorimeters were built by Airbus (formerly EADS with the support of the French company SETARAM: The Flight Model (FM located onboard the International Space Station (ISS and the Engineering Model (EM located at the TELESPAZIO Centre in Naples. Dedicated cells were filled on ground with different formulations of W/O emulsions and identical experiments were performed with the FM and the EM models in order to highlight the differences in emulsion evolution. On ground, the experiments were performed by cooling and heating the calorimeter between 40 °C and −60 °C but due to technical constraints in the FM, the experiments performed in the FSL (Fluid Science Laboratory of the ISS were limited to a lowest temperature of −22 °C. The results obtained with the FM confirmed the formation of emulsions in the dedicated cell with the selected stirring system in space. These results also demonstrated that it is possible to detect the freezing and the melting of the water droplets with the designed calorimeter either during cooling and heating phases or versus time during a temperature holding period at −22 °C. Furthermore, the comparison between both results obtained with the EM on ground and with the FM in space revealed distinct behaviours. This study drove us to focus on other mechanisms than sedimentation and convection to account for the destabilization of these kinds of emulsions.

  16. Study of interactions between hyaluronan and cationic surfactants by means of calorimetry, turbidimetry, potentiometry and conductometry.

    Science.gov (United States)

    Krouská, J; Pekař, M; Klučáková, M; Šarac, B; Bešter-Rogač, M

    2017-02-10

    The thermodynamics of the micelle formation of the cationic surfactants tetradecyltrimethylammonium bromide (TTAB) and cetyltrimethylammonium bromide (CTAB) with and without the addition of hyaluronan of two molecular weights was studied in aqueous solution by titration calorimetry. Macroscopic phase separation, which was detected by calorimetry and also by conductometry, occurs when charges on the surfactant and hyaluronan are balanced. In contrast, turbidimetry and potentiometry showed hyaluronan-surfactant interactions at very low surfactant concentrations. The observed differences between systems prepared with CTAB and TTAB indicate that besides the electrostatic interactions, which probably predominate, hydrophobic effects also play a significant role in hyaluronan interactions with cationic surfactants. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Optical fibre temperature sensor technology and potential application in absorbed dose calorimetry

    International Nuclear Information System (INIS)

    Allen, P.D.; Hargrave, N.J.

    1992-09-01

    Optical fibre based sensors are proposed as a potential alternative to the thermistors traditionally used as temperature sensors in absorbed dose calorimetry. The development of optical fibre temperature sensor technology over the last ten years is reviewed. The potential resolution of various optical techniques is assessed with particular reference to the requirements of absorbed dose calorimetry. Attention is drawn to other issues which would require investigation before the development of practical optical fibre sensors for this purpose could occur. 192 refs., 5 tabs., 4 figs

  18. Thermodynamics of Surfactants, Block Copolymers and Their Mixtures in Water: The Role of the Isothermal Calorimetry

    Science.gov (United States)

    De Lisi, Rosario; Milioto, Stefania; Muratore, Nicola

    2009-01-01

    The thermodynamics of conventional surfactants, block copolymers and their mixtures in water was described to the light of the enthalpy function. The two methodologies, i.e. the van’t Hoff approach and the isothermal calorimetry, used to determine the enthalpy of micellization of pure surfactants and block copolymers were described. The van’t Hoff method was critically discussed. The aqueous copolymer+surfactant mixtures were analyzed by means of the isothermal titration calorimetry and the enthalpy of transfer of the copolymer from the water to the aqueous surfactant solutions. Thermodynamic models were presented to show the procedure to extract straightforward molecular insights from the bulk properties. PMID:19742173

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

    NARCIS (Netherlands)

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

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

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

    Directory of Open Access Journals (Sweden)

    Adamo Fini

    2010-04-01

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

  1. An autosampling differential scanning calorimeter instrument for studying molecular interactions.

    Science.gov (United States)

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

    2002-11-01

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

  2. Isothermal Titration Calorimetry and Macromolecular Visualization for the Interaction of Lysozyme and Its Inhibitors

    Science.gov (United States)

    Wei, Chin-Chuan; Jensen, Drake; Boyle, Tiffany; O'Brien, Leah C.; De Meo, Cristina; Shabestary, Nahid; Eder, Douglas J.

    2015-01-01

    To provide a research-like experience to upper-division undergraduate students in a biochemistry teaching laboratory, isothermal titration calorimetry (ITC) is employed to determine the binding constants of lysozyme and its inhibitors, N-acetyl glucosamine trimer (NAG[subscript 3]) and monomer (NAG). The extremely weak binding of lysozyme/NAG is…

  3. Subsite binding energies of an exo-polygalacturonase using isothermal titration calorimetry

    Science.gov (United States)

    Thermodynamic parameters for binding of a series of galacturonic acid oligomers to an exo-polygalacturonase, RPG16 from Rhizopus oryzae, were determined by isothermal titration calorimetry. Binding of oligomers varying in chain length from two to five galacturonic acid residues is an exothermic proc...

  4. Thermodynamic investigations of protein's behaviour with ionic liquids in aqueous medium studied by isothermal titration calorimetry.

    Science.gov (United States)

    Bharmoria, Pankaj; Kumar, Arvind

    2016-05-01

    While a number of reports appear on ionic liquids-proteins interactions, their thermodynamic behaviour using suitable technique like isothermal titration calorimetry is not systematically presented. Isothermal titration calorimetry (ITC) is a key technique which can directly measure the thermodynamic contribution of IL binding to protein, particularly the enthalpy, heat capacities and binding stoichiometry. Ionic liquids (ILs), owing to their unique and tunable physicochemical properties have been the central area of scientific research besides graphene in the last decade, and growing unabated. Their encounter with proteins in the biological system is inevitable considering their environmental discharge though most of them are recyclable for a number of cycles. In this article we will cover the thermodynamics of proteins upon interaction with ILs as osmolyte and surfactant. The up to date literature survey of IL-protein interactions using isothermal titration calorimetry will be discussed and parallel comparison with the results obtained for such studies with other techniques will be highlighted to demonstrate the accuracy of ITC technique. Net stability of proteins can be obtained from the difference in the free energy (ΔG) of the native (folded) and denatured (unfolded) state using the Gibbs-Helmholtz equation (ΔG=ΔH-TΔS). Isothermal titration calorimetry can directly measure the heat changes upon IL-protein interactions. Calculation of other thermodynamic parameters such as entropy, binding constant and free energy depends upon the proper fitting of the binding isotherms using various fitting models. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Monolithic front-end preamplifiers for a broad range of calorimetry applications

    Energy Technology Data Exchange (ETDEWEB)

    Radeka, V.; Rescia, S. [Brookhaven National Lab., Upton, NY (United States); Manfredi, P.F.; Speziali, V. [Pavia Univ. (Italy). Dipt. di Elettronica]|[INFN--Sezzione di Milano, Milano (Italy)

    1993-12-31

    The present paper summarizes the salient results of a research and development activity in the area of low noise preamplifiers for different applications in calorimetry. Design target for all circuits considered here are low noise, ability to cope with broad energy ranges and radiation hardness.

  6. Proton and Copper Binding to Humic Acids Analyzed by XAFS Spectroscopy and Isothermal Titration Calorimetry

    NARCIS (Netherlands)

    Xu, Jinling; Koopal, Luuk K.; Fang, Linchuan; Xiong, Juan; Tan, Wenfeng

    2018-01-01

    Proton and copper (Cu) binding to soil and lignite-based humic acid (HA) was investigated by combining X-ray absorption fine structure (XAFS) spectroscopy, isothermal titration calorimetry (ITC), and nonideal-competitive-adsorption (NICA) modeling. NICA model calculations and XAFS results showed

  7. Monolithic junction field-effect transistor charge preamplifier for calorimetry at high luminosity hadron colliders

    International Nuclear Information System (INIS)

    Radeka, V.; Rescia, S.; Rehn, L.A.; Manfredi, P.F.; Speziali, V.

    1991-11-01

    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

  8. 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 p...

  9. Designing a compensating quartz fiber calorimeter for low angle calorimetry at LHC

    International Nuclear Information System (INIS)

    Ferrando, A.; Fouz, M.C.; Josa, M.I.; Khan, A.; Rosowsky, A.; Salicio, J.M.

    1996-01-01

    We present a design of a compensating quartz fiber calorimeter, made of a unique active section, and ment for the specific physics requirements of the low angle calorimetry in LHC experiments. The purposed calorimeter is exemplified for the case of the CMS experiment

  10. Coulometry and Calorimetry of Electric Double Layer Formation in Porous Electrodes

    NARCIS (Netherlands)

    Janssen, Mathijs; Griffioen, Elian; Biesheuvel, P. M.; Van Roij, René; Erné, Ben

    2017-01-01

    Coulometric measurements on salt-water-immersed nanoporous carbon electrodes reveal, at a fixed voltage, a charge decrease with increasing temperature. During far-out-of-equilibrium charging of these electrodes, calorimetry indicates the production of both irreversible Joule heat and reversible

  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. Combining Diffusion Tensor Metrics and DSC Perfusion Imaging: Can It Improve the Diagnostic Accuracy in Differentiating Tumefactive Demyelination from High-Grade Glioma?

    Science.gov (United States)

    Hiremath, S B; Muraleedharan, A; Kumar, S; Nagesh, C; Kesavadas, C; Abraham, M; Kapilamoorthy, T R; Thomas, B

    2017-04-01

    Tumefactive demyelinating lesions with atypical features can mimic high-grade gliomas on conventional imaging sequences. The aim of this study was to assess the role of conventional imaging, DTI metrics ( p:q tensor decomposition), and DSC perfusion in differentiating tumefactive demyelinating lesions and high-grade gliomas. Fourteen patients with tumefactive demyelinating lesions and 21 patients with high-grade gliomas underwent brain MR imaging with conventional, DTI, and DSC perfusion imaging. Imaging sequences were assessed for differentiation of the lesions. DTI metrics in the enhancing areas and perilesional hyperintensity were obtained by ROI analysis, and the relative CBV values in enhancing areas were calculated on DSC perfusion imaging. Conventional imaging sequences had a sensitivity of 80.9% and specificity of 57.1% in differentiating high-grade gliomas ( P = .049) from tumefactive demyelinating lesions. DTI metrics ( p : q tensor decomposition) and DSC perfusion demonstrated a statistically significant difference in the mean values of ADC, the isotropic component of the diffusion tensor, the anisotropic component of the diffusion tensor, the total magnitude of the diffusion tensor, and rCBV among enhancing portions in tumefactive demyelinating lesions and high-grade gliomas ( P ≤ .02), with the highest specificity for ADC, the anisotropic component of the diffusion tensor, and relative CBV (92.9%). Mean fractional anisotropy values showed no significant statistical difference between tumefactive demyelinating lesions and high-grade gliomas. The combination of DTI and DSC parameters improved the diagnostic accuracy (area under the curve = 0.901). Addition of a heterogeneous enhancement pattern to DTI and DSC parameters improved it further (area under the curve = 0.966). The sensitivity increased from 71.4% to 85.7% after the addition of the enhancement pattern. DTI and DSC perfusion add profoundly to conventional imaging in differentiating tumefactive

  13. ATD and DSC Analysis of IN-713C and ZhS6U-VI Superalloys

    Directory of Open Access Journals (Sweden)

    Binczyk F.

    2017-03-01

    Full Text Available Paper presents the results of ATD and DSC analysis of two superalloys used in casting of aircraft engine parts. The main aim of the research was to obtain the solidification parameters, especially Tsol and Tliq, knowledge of which is important for proper selection of casting and heat treatment parameters. Assessment of the metallurgical quality (presence of impurities of the feed ingots is also a very important step in production of castings. It was found that some of the feed ingots delivered by the superalloy producers are contaminated by oxides located in shrinkage defects. The ATD analysis allows for quite precise interpretation of first stages of solidification at which solid phases with low values of latent heat of solidification are formed from the liquid. Using DSC analysis it is possible to measure precisely the heat values accompanying the phase changes during cooling and heating which, with knowledge of phase composition, permits to calculate the enthalpy of formation of specific phases like γ or γ′.

  14. Determination of the activation energy in a cast aluminium alloy by TEM and DSC

    International Nuclear Information System (INIS)

    Ovono Ovono, D.; Guillot, I.; Massinon, D.

    2007-01-01

    The precipitation behaviour and microstructure development of the A319 alloy during ageing were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM and STEM). During T5 treatment, θ' precipitates with an average size of about 18 nm were observed by TEM. The precipitate sizes increased with ageing temperature and attained an average size of 107 nm. In addition, there was a linear relationship between precipitate growth temperature and the cube of the precipitate size. This indicates that precipitate growth of the A319 alloy belongs to a thermal activated process of the Arrhenius type. The activation energy for the precipitate growth was calculated to be 140.4 ± 13.3 kJ/mol. However, under continuous heating conditions, the activation energy for the precipitate growth obtained by Kissinger plot was determined to be 119.5 ± 8.3 kJ/mol. Allowing for experimental error, both values are comparable and are related to the diffusion of Cu and/or Si in Al

  15. A DSC investigation on the changes in pore structure of skin during leather processing

    International Nuclear Information System (INIS)

    Fathima, N. Nishad; Kumar, M. Pradeep; Rao, J. Raghava; Nair, B.U.

    2010-01-01

    Leather processing involves many unit operations that modify the physical, chemical and biological properties of the raw skin/hide of an animal. One such major variation is brought to pore structure and size, which determines the breathing property of skin. Understanding this property is essential to improve the end use of the leather matrix. Thermoporometric technique has been used in this study to bring out the influence of various process steps on the pore size distribution of skin. Marked changes in the depression of freezing point are observed for each process. Scanning electron microscopy study reveals the morphological changes in the grain and cross-section of the skin during leather processing. Understanding and predictions of pore structure changes at various stages of leather processing would benefit: (a) in process control, (b) analysis of cost benefit ratio and (c) strategic planning and transport. Thus, this study aids in better understanding of the pore structure of skin to improve the functional properties of the leather.

  16. Absorbed dose to water determination with ionization chamber dosimetry and calorimetry in restricted neutron, photon, proton and heavy-ion radiation fields.

    Science.gov (United States)

    Brede, H J; Greif, K-D; Hecker, O; Heeg, P; Heese, J; Jones, D T L; Kluge, H; Schardt, D

    2006-08-07

    Absolute dose measurements with a transportable water calorimeter and ionization chambers were performed at a water depth of 20 mm in four different types of radiation fields, for a collimated (60)Co photon beam, for a collimated neutron beam with a fluence-averaged mean energy of 5.25 MeV, for collimated proton beams with mean energies of 36 MeV and 182 MeV at the measuring position, and for a (12)C ion beam in a scanned mode with an energy per atomic mass of 430 MeV u(-1). The ionization chambers actually used were calibrated in units of air kerma in the photon reference field of the PTB and in units of absorbed dose to water for a Farmer-type chamber at GSI. The absorbed dose to water inferred from calorimetry was compared with the dose derived from ionometry by applying the radiation-field-dependent parameters. For neutrons, the quantities of the ICRU Report 45, for protons the quantities of the ICRU Report 59 and for the (12)C ion beam, the recommended values of the International Atomic Energy Agency (IAEA) protocol (TRS 398) were applied. The mean values of the absolute absorbed dose to water obtained with these two independent methods agreed within the standard uncertainty (k = 1) of 1.8% for calorimetry and of 3.0% for ionometry for all types and energies of the radiation beams used in this comparison.

  17. Radiopharmaceutical scanning agents

    International Nuclear Information System (INIS)

    1976-01-01

    This invention is directed to dispersions useful in preparing radiopharmaceutical scanning agents, to technetium labelled dispersions, to methods for preparing such dispersions and to their use as scanning agents

  18. Thyroid Scan and Uptake

    Medline Plus

    Full Text Available ... Scan and Uptake Thyroid scan and uptake uses small amounts of radioactive materials called radiotracers, a special ... is a branch of medical imaging that uses small amounts of radioactive material to diagnose and determine ...

  19. Nuclear Heart Scan

    Science.gov (United States)

    ... Home / Nuclear Heart Scan Nuclear Heart Scan Also known as Nuclear Stress Test , ... Learn More Connect With Us Contact Us Directly Policies Privacy Policy Freedom of Information Act (FOIA) Accessibility ...

  20. Thyroid Scan and Uptake

    Medline Plus

    Full Text Available ... of page What will I experience during and after the procedure? Most thyroid scan and thyroid uptake ... you otherwise, you may resume your normal activities after your nuclear medicine scan. If any special instructions ...