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.

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.

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.

Nicotinamides: Evaluation of thermochemical experimental properties

International Nuclear Information System (INIS)

Zhabina, Aleksandra A.; Nagrimanov, Ruslan N.; Emel’yanenko, Vladimir N.; Solomonov, Boris N.; Verevkin, Sergey P.

2016-01-01

Highlights: • Vapor pressures measured by transpiration method. • Enthalpies of solution measured using high-precision solution calorimetry. • Enthalpies of fusion measured by DSC. • Sublimation enthalpies derived from transpiration and solution calorimetry in agreement. • Experimental results evaluated and compared with G4 calculations. - Abstract: Vapor pressures of the isomeric 2-, 3-, and 4-pyridinecarboxamides were measured by using the transpiration method. The enthalpies of sublimation/vaporization of these compounds at 298.15 K were derived from vapor pressure temperature dependences. The enthalpies of solution of the isomeric pyridinecarboxamides were measured with the high-precision solution calorimetry. The enthalpies of sublimation of 3- and 4-pyridinecarboxamides were independently derived with help of the solution calorimetry based procedure. The enthalpies of fusion of the pyridinecarboxamides were measured by the DSC. Thermochemical data isomeric pyridinecarboxamides were collected, evaluated, and tested for internal consistency. The high-level G4 quantum-chemical method was used for mutual validation of the experimental and theoretical gas phase enthalpies of formation successfully.

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.

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.

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.

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...

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.

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

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.

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

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)

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.

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...

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.

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.

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...

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.

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

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.

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

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.

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.

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.

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.)

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 ...

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)

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.

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

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.

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

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.

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.

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.

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.

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

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.

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

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.

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

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.

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)

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.

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)

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...

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

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

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.

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.

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.

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.

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.)

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

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

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.)

Numerical calibration and experimental validation of a PCM-Air heat exchanger model

International Nuclear Information System (INIS)

Stathopoulos, N.; El Mankibi, M.; Santamouris, Mattheos

2017-01-01

Highlights: • Development of a PCM-Air heat exchanger experimental unit and its numerical model. • Differential Scanning Calorimetry for PCM properties. • Ineptitude of DSC obtained heat capacity curves. • Creation of adequate heat capacity curves depending on heat transfer rates. • Confrontation of numerical and experimental results and validation of the model. - Abstract: Ambitious goals have been set at international, European and French level for energy consumption and greenhouse gas emissions decrease of the building sector. Achieving them requires renewable energy integration, a technology that presents however an important drawback: intermittent energy production. In response, thermal energy storage (TES) technology applications have been developed in order to correlate energy production and consumption of the building. Phase Change Materials (PCMs) have been widely used in TES applications as they offer a high storage density and adequate phase change temperature range. It is important to accurately know the thermophysical properties of the PCM, both for experimental (system design) and numerical (correct prediction) purposes. In this paper, the fabrication of a PCM – Air experimental prototype is presented at first, along with the development of a numerical model simulating the downstream temperature evolution of the heat exchanger. Particular focus is given to the calibration method and the validation of the model using experimental characterization results. Differential scanning calorimetry (DSC) is used to define the thermal properties of the PCM. Initial numerical results are underestimated compared to experimental ones. Various factors were investigated, pointing to the ineptitude of the heat capacity parameter, as DSC results depend on heating/cooling rates. Adequate heat capacity curves were empirically determined, depending on heat transfer rates and based on DSC results and experimental observations. The results of the proposed model

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.).

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

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.

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...

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....

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

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

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.

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)

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.

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

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.

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.

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.

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.)

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.

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

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.

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...

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.

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.

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...

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

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

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.

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

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

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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.

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

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...

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.)

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.

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.

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.

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.

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.

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.

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

Science.gov (United States)

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

2010-05-19

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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.

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.

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

International Nuclear Information System (INIS)

Jakubczyk, Michał; Sporzyński, Andrzej; Emel’yanenko, Vladimir N.; Varfolomeev, Mikhail A.; Verevkin, Sergey P.

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-09-10

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

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

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

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

International Nuclear Information System (INIS)

Bahari, Zahra; Elgadi, Mohamed; Rivet, Jacques; Dugue, Jerome

2009-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-05-27

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

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...

2D Numerical Modelling of the Resin Injection Pultrusion Process Including Experimental Resin Kinetics and Temperature Validation

DEFF Research Database (Denmark)

Rasmussen, Filip Salling; Sonne, Mads Rostgaard; Larsen, Martin

In the present study, a two-dimensional (2D) transient Eulerian thermo-chemical analysis of a carbon fibre epoxy thermosetting Resin Injection Pultrusion (RIP) process is carried out. The numerical model is implemented using the well known unconditionally stable Alternating Direction Implicit (ADI......) scheme. The total heat of reaction and the cure kinetics of the epoxy thermosetting are determined using Differential Scanning Calorimetry (DSC). A very good agreement is observed between the fitted cure kinetic model and the experimental measurements. The numerical steady state temperature predictions...

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)

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.

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

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

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

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.

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

Directory of Open Access Journals (Sweden)

Nichola C Garbett

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

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

Science.gov (United States)

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

2014-01-01

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

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.

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.

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.

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.

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

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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.

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.

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…

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...

Determination of calorific values of some renewable biofuels

Energy Technology Data Exchange (ETDEWEB)

Kumar, Jothi V.; Pratt, Benjamin C. [Department of Chemistry, North Carolina A and T State University, Greensboro, North Carolina (United States)

1996-06-01

Thermal methods such as differential scanning calorimetry (DSC), and elemental analysis (EA) were employed to determine the calorific values of some renewable biofuels either directly or indirectly. The biofuels tested were the common milkweed, dogbane, kudzu, and eucalyptus tree. The purpose of this work was to optimize the experimental conditions for DSC analysis of biofuels, improve the calorific values by adding metal oxides as catalysts, and compare the heat values between DSC and EA analyses

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.

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.

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.

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…

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.

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

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.

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.

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.

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

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

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)

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.

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.

High-energy components of 'designer gasoline and designer diesel fuel' I. Heat capacities, enthalpy increments, vapor pressures, critical properties, and derived thermodynamic functions for bicyclopentyl between the T=(10 and 600) K

International Nuclear Information System (INIS)

Chirico, R.D.; Steele, W.V.

2004-01-01

Measurements leading to the calculation of the standard thermodynamic properties for gaseous bicyclopentyl (Chemicals Abstracts registry number [1636-39-1]) are reported. Experimental methods include adiabatic heat-capacity calorimetry, comparative ebulliometry, and differential-scanning calorimetry (d.s.c.). The critical temperature was determined by d.s.c. and the critical pressure and critical density were estimated. Standard molar entropies, standard molar enthalpies, and standard molar Gibbs free energies of formation are reported at selected temperatures between T=(298.15 and 600) K. Formation properties were calculated with a literature value for the enthalpy of combustion in the liquid phase. All results are compared with available literature values

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

Fluorene: An extended experimental thermodynamic study

International Nuclear Information System (INIS)

Monte, Manuel J.S.; Pinto, Sónia P.; Lobo Ferreira, Ana I.M.C.; Amaral, Luísa M.P.F.; Freitas, Vera L.S.; Ribeiro da Silva, Maria D.M.C.

2012-01-01

Highlights: ► Experimental results of an extended thermodynamic study on fluorene are presented. ► Enthalpy of combustion and vapor pressures of liquid and crystalline phase were measured. ► Enthalpy of sublimation was derived from three different experimental methods. ► New values of enthalpies of sublimation and of formation of fluorene are recommended. - Abstract: This work reports new experimental thermodynamic results on fluorene. Vapor pressures of both crystalline and liquid phases were measured using a pressure gauge (capacitance diaphragm manometer) and Knudsen effusion methods over a wide temperature range (292.20 to 412.16) K yielding accurate determination of enthalpy and entropy of sublimation and of vaporization. The enthalpy of sublimation was also determined using Calvet microcalorimetry. The enthalpy of fusion was derived from vapor pressure results and from d.s.c. experiments. Static bomb calorimetry was used to determine the enthalpy of combustion of fluorene from which the standard enthalpy of formation in the crystalline phase was calculated. The enthalpy of formation in the gaseous phase was calculated combining the result derived for the crystalline phase with the enthalpy of sublimation.

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

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

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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.

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.

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

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

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

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.

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

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.

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

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)

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

Determination of the glass transition temperature: methods correlation and structural heterogeneity

OpenAIRE

Hutchinson, John M.

2009-01-01

The definition of the glass transition temperature, Tg, is recalled and its experimental determination by various techniques is reviewed. The diversity of values of Tg obtained by the different methods is discussed, with particular attention being paid to Differential Scanning Calorimetry (DSC) and to dynamic techniques such as Dynamic Mechanical Thermal Analysis (DMTA) and Temperature Modulated DSC (TMDSC). This last technique, TMDSC, in particular, is considered in respect of ways in which ...

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.

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...

An experimental investigation to evaluate the heating value of palm oil waste by calorimetry. Paper no. IGEC-1-040

International Nuclear Information System (INIS)

Supeni, E.E.; Megat Mohd, M.H.; Mohd Sapuan, S.; Nor Maria, A.; Ismail, M.Y.; Thoguluva, R.V.; Chuah, T.G.

2005-01-01

A palm oil mill produces palm oil and kernel palm oil as main products and biomass residue (fiber and shell). This excess biomass residue can be used as fuel in boilers to meet energy and process heat demand in the industries. Quality of the palm oil waste (POW) is characterized by low fixed carbon and relatively high moisture content which may affect the heating value (HV). By applying the principle of calorimetry, a bomb calorimeter is utilized to evaluate the heating value of POW. From the experimental results, it is found that higher heating value (HHV) varies with the moisture content (MC) and it is observed as a function of MC. (author)

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.

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

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

Energy Technology Data Exchange (ETDEWEB)

Vient, E

2006-12-15

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

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)

Calorimetry for the SSC

Energy Technology Data Exchange (ETDEWEB)

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

1984-01-01

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

Calorimetry for the SSC

International Nuclear Information System (INIS)

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

1984-01-01

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

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.

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.

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.

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

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.

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

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.

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.

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.

Theory of calorimetry

CERN Document Server

Zielenkiewicz, Wojciech

2004-01-01

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

Calorimetry end-point predictions

International Nuclear Information System (INIS)

Fox, M.A.

1981-01-01

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

Phase separation in coamorphous systems: in silico prediction and the experimental challenge of detection.

Science.gov (United States)

Pajula, Katja; Wittoek, Lieke; Lehto, Vesa-Pekka; Ketolainen, Jarkko; Korhonen, Ossi

2014-07-07

Combinatorial chemistry has enabled the production of very potent drugs that might otherwise suffer from poor solubility and low oral bioavailability. One approach to increase solubility is to make the drug amorphous, which leads to problems associated with drug stability. To improve stability, one option is to molecularly disperse the drug in a matrix. However, the primary reason for the failed stabilization with this approach is phase separation, which has been carefully studied in polymeric systems. Nevertheless, the amorphous-amorphous phase separation in coamorphous small molecule mixtures has not yet been reported. The goal of the present study was to experimentally detect the amorphous-amorphous phase separation between two small molecules. A modified in silico method for predicting miscibility by the Flory-Huggins interaction parameter is presented, where conformational variations of the studied molecules were taken into account. A series of drug-drug mixtures, with different mixture ratios, were analyzed by conventional differential scanning calorimetry (DSC(conv)) to detect possible amorphous-amorphous phase separations. The phase separation of coamorphous drug-drug mixtures was also monitored by temperature modulated DSC (MDSC) and Fourier transform infrared (FT-IR) imaging at temperatures above Tg for prolonged time periods. Amorphous-amorphous phase separation was not detected with DSC(conv), probably due to the slow kinetics of phase separation. However, the melting of the separated and subsequently crystallized phases was detected by MDSC. Furthermore, FT-IR imaging was able to detect the separation of the two amorphous phases, which demonstrates the ability of this method to detect small molecule phase separations.

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

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

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.

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...

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.

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

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...

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.

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

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...

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.

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.)

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.

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

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).

Investigation of solidification behavior of the Sn-rich ternary Sn–Bi–Zn alloys

Directory of Open Access Journals (Sweden)

S Mladenović

2017-03-01

Full Text Available Solidification properties and microstructure of six as-cast Sn–Bi–Zn alloys with 80 at.% of Sn and variable contents of Bi and Zn were experimentally investigated using the scanning electron microscopy (SEM with energy-dispersive X-ray spectroscopy (EDS and differential scanning calorimetry (DSC. The experimentally obtained results were compared with predicted phase equilibria according to the calculation of phase diagram (CALPHAD method and by the Scheil solidification simulation.

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

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.

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.

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.

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.

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

A survey of the year 2007 literature on applications of isothermal titration calorimetry

OpenAIRE

Bjelic, S; Jelesarov, I

2008-01-01

Elucidation of the energetic principles of binding affinity and specificity is a central task in many branches of current sciences: biology, medicine, pharmacology, chemistry, material sciences, etc. In biomedical research, integral approaches combining structural information with in-solution biophysical data have proved to be a powerful way toward understanding the physical basis of vital cellular phenomena. Isothermal titration calorimetry (ITC) is a valuable experimental tool facilitating ...

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.

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. ...

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.

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.

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.

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.

Experimental investigation of phase equilibria in the Cu–Ni–Si ternary system

Energy Technology Data Exchange (ETDEWEB)

Liu, Xingjun; Xiang, Shulin; Yang, Shuiyuan; Shi, Rongpei; Wang, Cuiping, E-mail: wangcp@xmu.edu.cn

2013-11-25

Highlights: •Three isothermal sections of the Cu–Ni–Si system have been investigated. •The ternary compound τ{sub 1} and the liquid phase are confirmed at 1073 K. •The γ (Cu{sub 5}Si) and θ (Ni{sub 2}Si) phases can be stabilized at higher or lower temperatures. -- Abstract: The phase equilibria in the Cu–Ni–Si ternary system have been investigated experimentally by means of electron probe microanalysis (EPMA), X-ray diffraction (XRD) and differential scanning calorimetry (DSC) analysis on equilibrated ternary alloys. Three isothermal sections at 1073, 1173 and 1273 K are determined in the whole composition range. The existence of liquid phase and the ternary compound τ{sub 1} is confirmed at 1073 K. The binary γ (Cu{sub 5}Si), γ (Ni{sub 31}Si{sub 12}), δ (Ni{sub 2}Si) and θ (Ni{sub 2}Si) phases exhibit a considerable solubility of a third element. In addition, the γ (Cu{sub 5}Si) and θ (Ni{sub 2}Si) phases can be stabilized by the addition of Ni and Cu, respectively.

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.

New experimental heat capacity and enthalpy of formation of lithium cobalt oxide

International Nuclear Information System (INIS)

Gotcu-Freis, Petronela; Cupid, Damian M.; Rohde, Magnus; Seifert, Hans J.

2015-01-01

Highlights: • LiCoO 2 heat capacity was measured in the temperature range (160 to 953) K using DSC. • Continuous/discontinuous methods were applied on different types of calorimeters. • Enthalpy increment of LiCoO 2 was determined using drop calorimetry at T = 974 K. • Enthalpies of formation were evaluated from oxide melt drop solution calorimetry. - Abstract: The heat capacity of LiCoO 2 (O3-phase), constituent material in cathodes for lithium-ion batteries, was measured using two differential scanning calorimeters over the temperature range from (160 to 953) K (continuous method). As an alternative, the discontinuous method was employed over the temperature range from (493 to 693) K using a third calorimeter. Based on the results obtained, the enthalpy increment of LiCoO 2 was derived from T = 298.15 K up to 974.15 K. Very good agreement was obtained between the derived enthalpy increment and our independent measurements of enthalpy increment using transposed temperature drop calorimetry at 974.15 K. In addition, values of the enthalpy of formation of LiCoO 2 from the constituent oxides and elements were assessed based on measurements of enthalpy of dissolution using high temperature oxide melt drop solution calorimetry. The high temperature values obtained by these measurements are key input data in safety analysis and optimisation of the battery management systems which accounts for possible thermal runaway events

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

DEFF Research Database (Denmark)

Huyghe, Raphaël; Rasmussen, Peter; Thomsen, Kaj

2004-01-01

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

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)

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.

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.

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

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.

Thermodynamics of micellization from heat-capacity measurements.

Science.gov (United States)

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

2014-06-23

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

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)

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.

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.)

Heat transfer characteristics of thermal energy storage of a composite phase change materials: Numerical and experimental investigations

International Nuclear Information System (INIS)

Aadmi, Moussa; Karkri, Mustapha; El Hammouti, Mimoun

2014-01-01

In the present study, phase change materials based on epoxy resin paraffin wax with the melting point 27 °C were used as a new energy storage system. Thermophysical properties and the process of melting of a PCM (phase change material) composite were investigated numerically and experimentally. DSC (differential scanning calorimetry) has been used for measurement of melting enthalpy and determination of PCM heat capacity. The thermophysical properties of the prepared composite have been characterized by using a new transient hot plate apparatus. The results have shown that the most important thermal properties of these composites at the solid and liquid states are like the “apparent” thermal conductivity, the heat storage capacity and the latent heat of fusion. These experimental results have been simulated by using numerical Comsol ® Multiphysiques 4.3 based models with success. The results of the experimental investigation compare favorably with the numerical results and thus serve to validate the numerical approach. - Highlights: • Phase change materials based on paraffin spheres used as new energy storage system. • Thermophysical properties and the melting process of composites were investigated. • All experimental results have been simulated using Comsol ® Multiphysiques. • The ability to store and release the thermal energy were investigated. • A very thin molten PCM (phase change material) exists which is apparently visible in the spheres

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

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

A novel calorimetry technique for monitoring electron beam curing of polymer resins

International Nuclear Information System (INIS)

Chen, J.H.; Johnston, A.; Petrescue, L.; Hojjati, M.

2006-01-01

This paper describes the development of a calorimetry-based technique for monitoring of the curing of electron beam (EB) curable resins, including design of the calorimeter hardware and the development of an analytical model for calculating resin cure rates and radiation dose. Factors affecting the performance of the calorimeter were investigated. Experimental trials monitoring the curing of epoxy resin were conducted under single pass and multiple passes of EB irradiation. Results show that the developed calorimeter is a simple, inexpensive and reasonably accurate technique for monitoring the EB curing of cationic epoxies

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

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...

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.

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.

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

Measurement of VLE data for binary lipids systems

DEFF Research Database (Denmark)

Cunico, Larissa; Ceriani, Roberta; Sarup, Bent

components and also for their mixtures. To contribute in this area, experimental data were obtained using the Differential Scanning Calorimetry (DSC) technique for isobaric vapor-liquid equilibrium (VLE) of two binary mixtures at two different pressures (1.2 and 2.5 KPa): system 1 [monoacylglycerol....... The relevance of enlarging experimental databank of lipids systems data in order to improve the performance of predictive thermodynamic models was confirmed in this work by analyzing the calculated values of original UNIFAC model. A new group for original UNIFAC model is created aiming to improve...

The use of calorimetry for plutonium assay

International Nuclear Information System (INIS)

Mason, J.A.

1982-12-01

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

New crystals for dual-readout calorimetry

Czech Academy of Sciences Publication Activity Database

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

2009-01-01

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

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

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

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.

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

Temperature-dependent structural relaxation in As{sub 40}Se{sub 60} glass

Energy Technology Data Exchange (ETDEWEB)

Golovchak, R., E-mail: roman_ya@yahoo.com [Lviv Sci. and Res. Institute of Materials of SRC ' Carat' , 202 Stryjska str., 79031 Lviv (Ukraine); Kozdras, A. [Opole University of Technology, 75, Ozimska str., Opole, PL-45370 (Poland); Academy of Management and Administration, 18 Niedzialkowski str., Opole, PL-45085 (Poland); Shpotyuk, O. [Jan Dlugosz University, 13/15, al. Armii Krajowej, 42201, Czestochowa (Poland); Gorecki, Cz. [Opole University of Technology, 75, Ozimska str., Opole, PL-45370 (Poland); Kovalskiy, A.; Jain, H. [Department of Materials Science and Engineering, Lehigh University, 5 East Packer Avenue, Bethlehem, PA 18015-3195 (United States)

2011-08-01

The origin of structural relaxation in As{sub 40}Se{sub 60} glass at different annealing temperatures is studied by differential scanning calorimetry (DSC) and in situ extended X-ray absorption fine structure (EXAFS) methods. Strong physical aging effect, expressed through the increase of endothermic peak area in the vicinity of T{sub g}, is recorded by DSC technique at the annealing temperatures T{sub a}>90{sup o}C. EXAFS data show that the observed structural relaxation is not associated with significant changes in the short-range order of this glass. An explanation is proposed for this relaxation behavior assuming temperature-dependent constraints. -- Highlights: → In this study we report experimental evidence for temperature-dependent constraints theory. → Structural relaxation of As{sub 2}Se{sub 3} glass at higher annealing temperatures is studied by DSC technique. → Accompanied changes in the structure are monitored by in situ EXAFS measurements.

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...

Experimental and Monte Carlo studies of fluence corrections for graphite calorimetry in low- and high-energy clinical proton beams

International Nuclear Information System (INIS)

Lourenço, Ana; Thomas, Russell; Bouchard, Hugo; Kacperek, Andrzej; Vondracek, Vladimir; Royle, Gary; Palmans, Hugo

2016-01-01

Purpose: The aim of this study was to determine fluence corrections necessary to convert absorbed dose to graphite, measured by graphite calorimetry, to absorbed dose to water. Fluence corrections were obtained from experiments and Monte Carlo simulations in low- and high-energy proton beams. Methods: Fluence corrections were calculated to account for the difference in fluence between water and graphite at equivalent depths. Measurements were performed with narrow proton beams. Plane-parallel-plate ionization chambers with a large collecting area compared to the beam diameter were used to intercept the whole beam. High- and low-energy proton beams were provided by a scanning and double scattering delivery system, respectively. A mathematical formalism was established to relate fluence corrections derived from Monte Carlo simulations, using the FLUKA code [A. Ferrari et al., “FLUKA: A multi-particle transport code,” in CERN 2005-10, INFN/TC 05/11, SLAC-R-773 (2005) and T. T. Böhlen et al., “The FLUKA Code: Developments and challenges for high energy and medical applications,” Nucl. Data Sheets 120, 211–214 (2014)], to partial fluence corrections measured experimentally. Results: A good agreement was found between the partial fluence corrections derived by Monte Carlo simulations and those determined experimentally. For a high-energy beam of 180 MeV, the fluence corrections from Monte Carlo simulations were found to increase from 0.99 to 1.04 with depth. In the case of a low-energy beam of 60 MeV, the magnitude of fluence corrections was approximately 0.99 at all depths when calculated in the sensitive area of the chamber used in the experiments. Fluence correction calculations were also performed for a larger area and found to increase from 0.99 at the surface to 1.01 at greater depths. Conclusions: Fluence corrections obtained experimentally are partial fluence corrections because they account for differences in the primary and part of the secondary

Experimental and Monte Carlo studies of fluence corrections for graphite calorimetry in low- and high-energy clinical proton beams

Energy Technology Data Exchange (ETDEWEB)

Lourenço, Ana, E-mail: am.lourenco@ucl.ac.uk [Department of Medical Physics and Biomedical Engineering, University College London, London WC1E 6BT, United Kingdom and Division of Acoustics and Ionising Radiation, National Physical Laboratory, Teddington TW11 0LW (United Kingdom); Thomas, Russell; Bouchard, Hugo [Division of Acoustics and Ionising Radiation, National Physical Laboratory, Teddington TW11 0LW (United Kingdom); Kacperek, Andrzej [National Eye Proton Therapy Centre, Clatterbridge Cancer Centre, Wirral CH63 4JY (United Kingdom); Vondracek, Vladimir [Proton Therapy Center, Budinova 1a, Prague 8 CZ-180 00 (Czech Republic); Royle, Gary [Department of Medical Physics and Biomedical Engineering, University College London, London WC1E 6BT (United Kingdom); Palmans, Hugo [Division of Acoustics and Ionising Radiation, National Physical Laboratory, Teddington TW11 0LW, United Kingdom and Medical Physics Group, EBG MedAustron GmbH, A-2700 Wiener Neustadt (Austria)

2016-07-15

Purpose: The aim of this study was to determine fluence corrections necessary to convert absorbed dose to graphite, measured by graphite calorimetry, to absorbed dose to water. Fluence corrections were obtained from experiments and Monte Carlo simulations in low- and high-energy proton beams. Methods: Fluence corrections were calculated to account for the difference in fluence between water and graphite at equivalent depths. Measurements were performed with narrow proton beams. Plane-parallel-plate ionization chambers with a large collecting area compared to the beam diameter were used to intercept the whole beam. High- and low-energy proton beams were provided by a scanning and double scattering delivery system, respectively. A mathematical formalism was established to relate fluence corrections derived from Monte Carlo simulations, using the FLUKA code [A. Ferrari et al., “FLUKA: A multi-particle transport code,” in CERN 2005-10, INFN/TC 05/11, SLAC-R-773 (2005) and T. T. Böhlen et al., “The FLUKA Code: Developments and challenges for high energy and medical applications,” Nucl. Data Sheets 120, 211–214 (2014)], to partial fluence corrections measured experimentally. Results: A good agreement was found between the partial fluence corrections derived by Monte Carlo simulations and those determined experimentally. For a high-energy beam of 180 MeV, the fluence corrections from Monte Carlo simulations were found to increase from 0.99 to 1.04 with depth. In the case of a low-energy beam of 60 MeV, the magnitude of fluence corrections was approximately 0.99 at all depths when calculated in the sensitive area of the chamber used in the experiments. Fluence correction calculations were also performed for a larger area and found to increase from 0.99 at the surface to 1.01 at greater depths. Conclusions: Fluence corrections obtained experimentally are partial fluence corrections because they account for differences in the primary and part of the secondary

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.

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.

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, ...

Glass transition and the rigid amorphous phase in semicrystalline blends of bacterial polyhydroxybutyrate PHB with low molecular mass atactic R,S-PHB-diol

NARCIS (Netherlands)

Hoehne, G.W.H.

2004-01-01

The glass transition and the crystallinity of blends of isotactic bacterial PHB and low molecular mass atactic R, S-PHB-diols was investigated by means of differential scanning calorimetry (DSC), temperature-modulated DSC and dielectric spectroscopy. It was found that (i) Tg of crystallized blends

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.

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

On the solid–liquid phase diagrams of binary mixtures of even saturated fatty alcohols: Systems exhibiting peritectic reaction

Energy Technology Data Exchange (ETDEWEB)

Carareto, Natália D.D. [EXTRAE, Department of Food Engineering, Food Engineering Faculty, University of Campinas, UNICAMP, CEP 13083-862 Campinas, SP (Brazil); Santos, Adenílson O. dos [Social Sciences, Health and Technology Center, University of Maranhão, UFMA, CEP 65900-410 Imperatriz, MA (Brazil); Rolemberg, Marlus P. [Institute of Science and Technology, University of Alfenas, UNIFAL, Rodovia José AurélioVilela, CEP 37715400 Poços de Caldas, MG (Brazil); Cardoso, Lisandro P. [Institute of Physics GlebWataghin, University of Campinas, UNICAMP, C.P. 6165, CEP 13083-970 Campinas, SP (Brazil); Costa, Mariana C. [School of Applied Science, University of Campinas, UNICAMP, CEP 13484-350 Limeira, SP (Brazil); Meirelles, Antonio J.A., E-mail: tomze@fea.unicamp.br [EXTRAE, Department of Food Engineering, Food Engineering Faculty, University of Campinas, UNICAMP, CEP 13083-862 Campinas, SP (Brazil)

2014-08-10

Highlights: • SLE of binary mixtures of saturated fatty alcohols was studied. • Experimental data were obtained using DSC and stepscan DSC. • Microscopy and X-ray diffraction used as complementary techniques. • Systems presented eutectic, peritectic and metatectic points. - Abstract: The solid–liquid phase diagrams of the following binary mixtures of even saturated fatty alcohols are reported in the literature for the first time: 1-octanol (C8OH) + 1-decanol (C10OH), 1-decanol + 1-dodecanol (C12OH), 1-dodecanol + 1-hexadecanol (C16OH) and 1-tetradecanol (C14OH) + 1-octadecanol (C18OH). The phase diagrams were obtained by differential scanning calorimetry (DSC) using a linear heating rate of 1 K min{sup −1} and further investigated by using a stepscan DSC method. X-ray diffraction (XRD) and polarized light microscopy were also used to complement the characterization of the phase diagrams which have shown a complex global behavior, presenting not only peritectic and eutectic reactions, but also the metatectic reaction and partial immiscibility on solid state.

On the solid–liquid phase diagrams of binary mixtures of even saturated fatty alcohols: Systems exhibiting peritectic reaction

International Nuclear Information System (INIS)

Carareto, Natália D.D.; Santos, Adenílson O. dos; Rolemberg, Marlus P.; Cardoso, Lisandro P.; Costa, Mariana C.; Meirelles, Antonio J.A.

2014-01-01

Highlights: • SLE of binary mixtures of saturated fatty alcohols was studied. • Experimental data were obtained using DSC and stepscan DSC. • Microscopy and X-ray diffraction used as complementary techniques. • Systems presented eutectic, peritectic and metatectic points. - Abstract: The solid–liquid phase diagrams of the following binary mixtures of even saturated fatty alcohols are reported in the literature for the first time: 1-octanol (C8OH) + 1-decanol (C10OH), 1-decanol + 1-dodecanol (C12OH), 1-dodecanol + 1-hexadecanol (C16OH) and 1-tetradecanol (C14OH) + 1-octadecanol (C18OH). The phase diagrams were obtained by differential scanning calorimetry (DSC) using a linear heating rate of 1 K min −1 and further investigated by using a stepscan DSC method. X-ray diffraction (XRD) and polarized light microscopy were also used to complement the characterization of the phase diagrams which have shown a complex global behavior, presenting not only peritectic and eutectic reactions, but also the metatectic reaction and partial immiscibility on solid state

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

Experimental determination of the phase equilibria in the Co-Fe-Zr ternary system

International Nuclear Information System (INIS)

Wang, C.P.; Yu, Y.; Zhang, H.H.; Hu, H.F.; Liu, X.J.

2011-01-01

Research highlights: → We determined four isothermal sections of the Co-Fe-Zr system from 1000 o C to 1300 o C. → No ternary compound was found in the Co-Fe-Zr ternary system. → The solubility of Fe in the liquid phase at 1300 o C is extremely large. → The (Co, Fe) 2 Zr phase form the continuous solution from Co-Zr side to Fe-Zr side. → The solubility of Zr in the fcc (Co, Fe) phase is extremely small. - Abstract: The phase equilibria in the Co-Fe-Zr ternary system were investigated by means of optical microscopy (OM), electron probe microanalysis (EPMA), X-ray diffraction (XRD), and differential scanning calorimetry (DSC) on equilibrated ternary alloys. Four isothermal sections of the Co-Fe-Zr ternary system at 1300 o C, 1200 o C, 1100 o C and 1000 o C were experimentally established. The experimental results indicate that (1) no ternary compound was found in this system; (2) the solubility of Fe in the liquid phase of the Co-rich corner at 1300 o C is extremely large; (3) the liquid phase in the Zr-rich corner and the (Co,Fe) 2 Zr phase form the continuous solid solutions from the Co-Zr side to the Fe-Zr side; (4) the solubility of Zr in the fcc (Co, Fe) phase is extremely small.

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.

Thermal transitions in Fe-Ti-Cr-C quaternary system used as precursor during laser in situ carbide coating

International Nuclear Information System (INIS)

Singh, Anshul; Porter, Wallace D.; Dahotre, Narendra B.

2005-01-01

The temperature range of thermal transitions within the quaternary system (Fe, Ti, Cr, and C) and the thermal stability of the evolved phases were studied with the help of differential scanning calorimetry (DSC). DSC studies indicated that the major exothermic reactions (formation of carbides) take place within 850-1150 deg. C. The evolved phases (TiC, M 7 C 3 , Fe-Cr, and Fe 3 C) were characterized using X-ray diffraction (XRD). This multicomponent powder mixture was used as a precursor for synthesizing a composite coating on the surface of steel via laser surface engineering (LSE). The intended wear applications of the coating made thermal stability investigations vital. Experimental evaluation of thermal stability of the phases formed was done

Calorimetric features of IgM gammopathies. Implication for patient’s diagnosis and monitoring

Energy Technology Data Exchange (ETDEWEB)

Krumova, Sashka; Todinova, Svetla; Danailova, Avgustina [Institute of Biophysics and Biomedical Engineering, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 21, 1113 Sofia (Bulgaria); Petkova, Violeta; Dimitrova, Keranka; Gartcheva, Lidia [National Specialized Hospital for Active Treating of Haematological Diseases, Sofia 1756 (Bulgaria); Taneva, Stefka G., E-mail: stefka.germanova@ehu.es [Institute of Biophysics and Biomedical Engineering, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., bl. 21, 1113 Sofia (Bulgaria); Unidad de Biofísica (CSIC-UPV/EHU) and Departamento de Bioquímica y Biología Molecular, Universidad del País Vasco, 48080 Bilbao (Spain)

2015-09-10

Highlights: • DSC reveals distinct calorimetric features for IgM gammopaties. • Calorimetry sets of IgM multiple myeloma and Waldenström’s macroglobulinemia patients. • DSC features correlate with the level of involved IgM heavy/light chains. • DSC and “Heavylite” are complementary methods for patients diagnostics/monitoring. - Abstract: The serum proteome of patients featuring immunoglobulin M (IgM) gammopathy and diagnosed as having IgM multiple myeloma or Waldenström’s macroglobulinemia was characterized by differential scanning calorimetry and HevyLite™ (HLC) assay. The thermodynamic properties of the thermograms and their deviation from the typical healthy thermogram were found to correlate with the monoclonal protein concentration and the level of the involved (monoclonal) IgM heavy/light chains. Patients monitoring during treatment showed that the variations in the shape of the DSC profiles corresponded to fluctuations of the IgM heavy/light chain levels verifying the two parameters as non-invasive markers for disease progression.

Thermodynamic properties of 2,7-di-tert-butylfluorene – An experimental and computational study

International Nuclear Information System (INIS)

Oliveira, Juliana A.S.A.; Freitas, Vera L.S.; Notario, Rafael; Ribeiro da Silva, Maria D.M.C.; Monte, Manuel J.S.

2016-01-01

Highlights: • Enthalpies and Gibbs energies of formation of 2,7-di-tert-butylfluorene were determined. • Vapour pressures were measured at different temperatures. • Phase transition thermodynamic properties were determined. - Abstract: This work presents a comprehensive experimental and computational study of the thermodynamic properties of 2,7-di-tert-butylfluorene. The standard (p"o = 0.1 MPa) molar enthalpy of formation in the crystalline phase was derived from the standard molar energy of combustion, measured by static bomb combustion calorimetry. The enthalpies and temperatures of transition between condensed phases were determined from DSC experiments. The vapour pressures of the crystalline and liquid phases were measured between (349.14 and 404.04) K, using two different experimental methods. From these results the standard molar enthalpies, entropies and Gibbs energies of sublimation and of vaporization were derived. The enthalpy of sublimation was also determined using Calvet microcalorimetry. The thermodynamic stability of 2,7-di-tert-butylfluorene in the crystalline and gaseous phases was evaluated by the determination of the standard Gibbs energies of formation, at the temperature 298.15 K, and compared with the ones reported in the literature for fluorene. A computational study at the G3(MP2)//B3LYP and G3 levels has been carried out. A conformational analysis has been performed and the enthalpy of formation of 2,7-di-tert-butylfluorene has been calculated, using atomization and isodesmic reactions. The calculated enthalpies of formation have been compared to the experimental values.

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.

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

The thermochemical behavior of some binary shape memory alloys by high temperature direct synthesis calorimetry

International Nuclear Information System (INIS)

Meschel, S.V.; Pavlu, J.; Nash, P.

2011-01-01

Research highlights: → We studied 14 shape memory alloys. → The enthalpies of formation and structure characteristics are summarized. → Theoretical predictions by ab initio calculations compare better with experimental measurements than Miedema's semi empirical model. - Abstract: The standard enthalpies of formation of some shape memory alloys have been measured by high temperature direct synthesis calorimetry at 1373 K. The following results (in kJ/mol of atoms) are reported: CoCr (-0.3 ± 2.9); CuMn (-3.7 ± 3.2); Cu 3 Sn (-10.4 ± 3.1); Fe 2 Tb (-5.5 ± 2.4); Fe 2 Dy (-1.6 ± 2.9); Fe 17 Tb 2 (-2.1 ± 3.1); Fe 17 Dy 2 (-5.3 ± 1.7); FePd 3 (-16.0 ± 2.7); FePt (-23.0 ± 1.9); FePt 3 (-20.7 ± 2.3); NiMn (-24.9 ± 2.6); TiNi (-32.7 ± 1.0); TiPd (-60.3 ± 2.5). The results are compared with some earlier experimental values obtained by calorimetry and by EMF technique. They are also compared with predicted values on the basis of the semi empirical model of Miedema and co-workers and with ab initio calculations when available. We will also assess the available information regarding the structures of these alloys.

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.

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)

Phase Change Humidity Control Material and its Application in Buildings

DEFF Research Database (Denmark)

Wu, Zhimin; Qin, Menghao; Chen, Zhi

2017-01-01

calorimetry (DSC). The thermal gravimetric analysis (TGA) was used to study the thermal stability. Both the moisture transfer coefficient and moisture buffer value (MBV) of the PCHCM were measured by two bottle method. The DSC results show that the super-cooling degrees of microcapsule and PCHCM are lower...

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.

Lead-free soldering: Investigation of the Cu-Sn-Sb system along the Sn:Sb = 1:1 isopleth

Energy Technology Data Exchange (ETDEWEB)

Yuan, Y. [State Key Laboratory of Powder Metallurgy, Central South University, Changsha, Hunan 410083 (China); Department of Chemistry and Industrial Chemistry, University of Genoa, INSTM UdR Genoa, Via Dodecaneso 31, I-16146 Genoa (Italy); Borzone, G., E-mail: borzone@chimica.unige.it [Department of Chemistry and Industrial Chemistry, University of Genoa, INSTM UdR Genoa, Via Dodecaneso 31, I-16146 Genoa (Italy); Zanicchi, G.; Delsante, S. [Department of Chemistry and Industrial Chemistry, University of Genoa, INSTM UdR Genoa, Via Dodecaneso 31, I-16146 Genoa (Italy)

2011-02-03

Research highlights: > In the electronics industry, the solder alloys commonly used for assembly belong to the Sn-Pb system. Fulfilment of the EU RoHS (reduction of hazardous substances) requires the development of new lead-free alloys for applications in electronics, with the same or possibly better characteristics than the traditional Sn-Pb alloys. > This research concerns the investigation of the constitutional properties of the Cu-Sn-Sb system which is considered as lead-free replacement for high-temperature applications. - Abstract: The Cu-Sn-Sb system has been experimentally investigated by a combination of optical microscopy, differential scanning calorimetry (DSC) and electron probe microanalysis (EPMA). DSC was used to identify a total number of five invariant ternary reactions and the Sn:Sb = 1:1 isopleth section up to 65 at.% Cu was constructed by combining the DSC data with the EPMA analyses of annealed alloys and literature information. The composition limits of the binary phases were detected.

Thermochemistry of organic azides revisited

International Nuclear Information System (INIS)

Emel'yanenko, Vladimir N.; Algarra, Manuel; Esteves da Silva, Joaquim C.G.; Hierrezuelo, Jesús; López-Romero, Juan M.; Verevkin, Sergey P.

2014-01-01

Highlights: • Pure samples of 4-nitro-phenyl azide, 1-octyl- and 1-decyl-azides were prepared. • Vapour pressures, sublimation and vaporization enthalpies measured by transpiration. • Enthalpy of formation of 1-alkyl azides measured by combustion calorimetry. • Enthalpy of fusion of 4-nitro-phenyl azide measured by DSC. • Experimental gas enthalpies of formation were in agreement with calculated by G4. - Abstract: Highly pure samples of 4-nitro-phenyl azide, 1-octyl azide and 1 decyl-azide were prepared for thermochemical studies. Vapour pressures over the solid and the liquid sample of 4-nitro-phenyl azide have been determined by the transpiration method. The molar enthalpies of vaporization/sublimation for this compound were derived from the temperature dependencies of vapour pressures. The molar enthalpy of fusion of 4-nitro-phenyl azide was measured by DSC. The measured data set for 4-nitro-phenyl azide was successfully checked for internal consistency. Molar enthalpies of vaporization of 1-octyl azide and 1 decyl-azide were measured by transpiration. The molar enthalpies of formation of the liquid 1-octyl azide and 1 decyl-azides were derived from the combustion calorimetry. New experimental results for these organic azides have been used to derive their molar enthalpies of formation in the gas state and for comparison with results from quantum-chemical method G4

Experimental and computational study of the thermodynamic properties of 2-nitrofluorene and 2-aminofluorene

International Nuclear Information System (INIS)

Oliveira, Juliana A.S.A.; Monte, Manuel J.S.; Notario, R.; Ribeiro da Silva, Maria D.M.C.

2014-01-01

Highlights: • A thermodynamic study of two fluorene derivatives is presented. • Vapour pressures and energies of combustion were measured. • Enthalpy, entropy and Gibbs energy of sublimation were derived. • Enthalpy and Gibbs energy of formation in crystal and gas phases were calculated. • Gas phase enthalpy of formation was also estimated by quantum chemical calculations. - Abstract: This report presents a comprehensive experimental and computational study of the thermodynamic properties of two fluorene derivatives: 2-aminofluorene and 2-nitrofluorene. The standard (p° = 0.1 MPa) molar enthalpies of formation in the crystalline phase of these compounds were derived from the standard molar energies of combustion, in oxygen, at T = 298.15 K, measured by static bomb combustion calorimetry. A Knudsen effusion method was used to perform the vapour pressure study of the referred compounds, yielding an accurate determination of the standard molar enthalpies and entropies of sublimation. The enthalpies of sublimation were also determined using Calvet microcalorimetry and the enthalpy and temperature of fusion were derived from DSC experiments. Derived results of standard enthalpy and Gibbs energy of formation in both gaseous and crystalline phases were compared with the ones reported in literature for fluorene. A theoretical study at the G3 and G4 levels has been carried out, and the calculated enthalpies of formation have been compared to the experimental values

The binary (solid + liquid) phase diagrams of (caprylic or capric acid) + (1-octanol or 1-decanol)

International Nuclear Information System (INIS)

Carareto, Natália D.D.; Castagnaro, Thamires; Costa, Mariana C.; Meirelles, Antonio J.A.

2014-01-01

Highlights: • SLE of mixtures of caprylic acid, (capric acid + 1-octanol), 1-decanol were studied. • Experimental data were obtained through DSC and Stepscan DSC. • Systems presented eutectic and peritectic points. • Liquidus line was modeled using Margules and NRTL models. • Solid phase was modeled using the Slaughter and Doherty approach. - Abstract: In the present study the phase diagrams of four (fatty acid + fatty alcohol) binary mixtures composed of caprylic (C8O2) or capric acid (C10O2) + 1-octanol (C8OH) or 1-decanol (C10OH) were obtained by differential scanning calorimetry (DSC). Eutectic and peritectic reactions occurred in the systems. In standard DSC analyses of the (C8O2 + C10OH) and (C10O2 + C8OH) systems, an exothermic transition occurs in association with the melting of a metastable phase. A Stepscan DSC method was used in order to avoid the formation of this metastable phase during the heating of the mixtures. The approach suggested by Slaughter and Doherty (1995) [24] was used for modeling the solid phase, and the Margules 2-suffix, Margules 3-suffix and NRTL models were applied for calculating the activity coefficients of the liquid phase. The best modeling results were obtained using the Margules-3-suffix with an average deviation between experimental and calculated values ranging from T = (0.3 to 0.9) K

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

NARCIS (Netherlands)

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

2016-01-01

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

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

Science.gov (United States)

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

2017-04-01

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

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.

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

Determination of Energy Characteristic and Microporous Volume by Immersion Calorimetry in Carbon Monoliths

Directory of Open Access Journals (Sweden)

Juan Carlos Moreno-Piraján

2012-01-01

Full Text Available Activated carbon monoliths disc and honeycomb type were prepared by chemical activation of coconut shell with zinc chloride at different concentrations, without using a binder. The structures were characterized by N2 adsorption at 77 K and immersion calorimetry into benzene. The experimental results showed that the activation with zinc chloride produces a wide microporous development, with micropore volume between 0,38 and 0,79 cm3g-1, apparent BET surface area between 725 and 1523 m2g-1 and immersion enthalpy between 73,5 and 164,2 Jg-1. We compared the experimental enthalpy with calculated enthalpy by equation Stoeckli-Kraehenbuehl finding a data dispersion from which can infer that the structures are not purely microporous; this fact is ratified with similar behavior that the evidence t the product EoWo.

Alternative methods of determining phase transition temperatures of phospholipids that constitute liposomes on the example of DPPC and DMPC

Energy Technology Data Exchange (ETDEWEB)

Pentak, Danuta, E-mail: danuta.pentak@us.edu.pl

2014-05-01

Highlights: • New phase transition for DMPC was found. • FT-IR method is an important addition to the DSC studies. • The proposed method for determining the T{sub C} give very consistent results. - Abstract: In this work, alternatives to differential scanning calorimetry (DSC) as a method of determining the main phospholipid phase transition temperature are presented. The bilayer phase transitions from the ripple gel phase (P{sub β{sup ′}}) to the liquid-crystal phase (L{sub α}) of 1,2-dipalmitoyl-sn-glycerol-3-phosphocholine (DPPC) and 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) were studied by differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR), nuclear magnetic resonance (NMR), and electron paramagnetic resonance (EPR) methods. In this work, two correlations between the DSC and FT-IR methods, and NMR and EPR methods are shown. The proposed methods allow for determining the T{sub C} temperature with a high degree of accuracy. Furthermore, a comparison of results obtained using the DSC and FT-IR methods allowed for an observation of a new DMPC phase transition. The liposomes analyzed in this work were obtained by the modified reverse-phase evaporation method (mREV)

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.

Thermal characterization of radiation processed contact lens material

International Nuclear Information System (INIS)

Varshney, L.; Choughule, S.V.

1998-01-01

Differential scanning calorimetry (DSC), thermomechanical analysis (TMA) and thermogravimetry analysis (TGA) were used to characterize radiation processed contact lens gel material of 2-hydroxy ethyl methacrylate(HEMA). DSC revealed two types of water in the gels. DSC and TGA in combination were used to quantitate the percentage of different types of the water in the gel material. Temperature expansion coefficients values indicate more dimensions stability in the radiation processed lenses of similar water contents. (author)

Experimental and thermodynamic study of the Mg–Sn–In–Zn quaternary system

International Nuclear Information System (INIS)

Wang, Jian; Hudon, Pierre; Kevorkov, Dmytro; Chartrand, Patrice; Jung, In-Ho; Medraj, Mamoun

2014-01-01

Highlights: • Phase equilibria in the Mg-rich region of the Mg–Sn–In are determined. • Phase equilibria in the Mg-rich region of the Mg–Sn–Zn are determined. • Evaluation and thermodynamic optimization of the Mg–Sn–In–Zn quaternary system are developed. -- Abstract: Phase equilibria in the Mg-rich region of the Mg–Sn–In (at 415 °C and 330 °C), and Mg–Sn–Zn (at 300 °C) ternary systems were determined by quenching experiments, electron probe micro-analyzer (EPMA), and X-ray diffraction (XRD) techniques. The ternary isoplethal sections with constant 5 In and 10 Sn at.% of Mg–In–Sn system, and 10 Sn at.% of Mg–In–Zn system were determined by differential scanning calorimetry (DSC). No ternary compounds were found in the Mg–Sn–Zn and Mg–Sn–In isothermal sections. Critical evaluation and thermodynamic optimization of the Mg–Sn–In–Zn quaternary system were carried out using CALPHAD (Calculation of Phase Diagrams) technique. The Modified Quasichemical Model in the Pair Approximation (MQMPA) was used for modeling the liquid solution, which exhibits a high degree of short-range ordering behavior. The solid phases were modeled with the Compound Energy Formalism (CEF). All available and reliable experimental data were reproduced within experimental error limits. A self-consistent thermodynamic database was constructed for the Mg–Sn–In–Zn quaternary system, which can be used as a guide for Mg-based alloys development

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

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.

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.

Effect of electron irradiation on poly(vinylidene fluoride-trifluoroethylene) 56/44 mol% copolymers

International Nuclear Information System (INIS)

Guo, S S; Zhao, X-Z; Lu, S G; Lau, S T; Chan, H L W

2004-01-01

High-energy electron-irradiated poly(vinylidene fluoride-trifluoroethylene) 56/44 mol% copolymers are studied in a broad dose ranging from 0 to 110 Mrad. The experimental results are obtained by differential scanning calorimetry (DSC), x-ray diffraction, dielectric constant, dc conductivity and polarization hysteresis loop based on structural changes and dielectric relaxation behaviour. All the x-ray and DSC results show that both the crystalline and polar ordering decreased after irradiation, indicating a partial recovery from trans-gauche bonds to local trans bonds (polar ordering). The dielectric relaxation peaks, obeying the Vogel-Fulcher Law, indicate that the copolymers have transformed from a normal ferroelectric to a relaxor ferroelectric. It is also found that dc conductivity can be modulated with electron irradiation, as well as the hysteresis loop characteristics

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.

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

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

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.

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.

Calorimetry using organic scintillators, 'a sideways perspective'.

Energy Technology Data Exchange (ETDEWEB)

Proudfoot, J.

1999-09-10

Over the last two decades, calorimetry baaed on organic scintillators has developed into an excellent technology for many experimental situations in high energy physics. The primary difficulty, that of extracting the light signals, has benefited from two milestone innovations. The first was the use of wavelength-shifting bars to allow light to be efficiently collected from large areas of scintillator and then readily piped to a readout device. The second of these was the extension of this approach to plastic wavelength-shifting optical fibers whose great flexibility and small diameter allowed a minimum of detector volume to be compromised by the read-out. These two innovations coupled with inventiveness have produced many varied and successful calorimeters. Equal response to both hadronic and electromagnetic showers can be realized in scintillator-based calorimeters. However, in general this is not the case and it is likely that in the search for greater performance, in the future, combined tracking and calorimeter systems will be required.

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...

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

Applying a new criterion to predict glass forming alloys in the Zr–Ni–Cu ternary system

Energy Technology Data Exchange (ETDEWEB)

Déo, L.P., E-mail: leonardopratavieira@gmail.com [Universidade de São Paulo, EESC, SMM - Av. Trabalhador São Carlense, 400 – São Carlos, SP 13566-590 (Brazil); Mendes, M.A.B., E-mail: marcio.andreato@gmail.com [Universidade Federal de São Carlos, DEMa - Rod. Washington Luiz, Km 235 – São Carlos, SP 13565-905 (Brazil); Costa, A.M.S., E-mail: alexmatos1980@gmail.com [Universidade de São Paulo, DEMAR, EEL – Polo Urbo-Industrial Gleba AI-6, s/n – Lorena, SP 12600-970 (Brazil); Campos Neto, N.D., E-mail: nelsonddcn@gmail.com [Universidade de São Paulo, EESC, SMM - Av. Trabalhador São Carlense, 400 – São Carlos, SP 13566-590 (Brazil); Oliveira, M.F. de, E-mail: falcao@sc.usp.br [Universidade de São Paulo, EESC, SMM - Av. Trabalhador São Carlense, 400 – São Carlos, SP 13566-590 (Brazil)

2013-03-15

Highlights: ► Calculation to predict and select the glass forming ability (GFA) of metallic alloys in Zr–Ni–Cu system. ► Good correlation between theoretical and experimental GFA samples. ► Combination of X-ray diffraction (XRD) and differential scanning calorimetry (DSC) techniques mainly to characterize the samples. ► Oxygen impurity dramatically reduced the GFA. ► The selection criterion used opens the possibility to obtain new amorphous alloys, reducing the experimental procedures of trial and error. -- Abstract: A new criterion has been recently proposed to predict and select the glass forming ability (GFA) of metallic alloys. It was found that the critical cooling rate for glass formation (R{sub c}) correlates well with a proper combination of two factors, the minimum topological instability (λ{sub min}) and the thermodynamic parameter (Δh). The (λ{sub min}) criterion is based on the concept of topological instability of stable crystalline structures and (Δh) depends on the average work function difference (Δϕ) and the average electron density difference Δn{sub ws}{sup 1/3} among the constituent elements of the alloy. In the present work, the selection criterion was applied in the Zr–Ni–Cu system and its predictability was analyzed experimentally. Ribbon-shaped and splat-shaped samples were produced by melt-spinning and splat-cooling techniques respectively. The crystallization content and behavior were analyzed by X-ray diffraction (XRD) and differential scanning calorimetry (DSC), respectively. The results showed a good correlation between the theoretical GFA values and the amorphous phase percentages found in different alloy compositions.

Design of Ag-Ge-Zn braze/solder alloys: Experimental thermodynamics and surface properties

Directory of Open Access Journals (Sweden)

Delsante S.

2017-01-01

Full Text Available The experimental investigation of the Ag-Ge-Zn phase diagram was performed by using combined microstructural and Differential Scanning Calorimeter (DSC analyses. The samples were subjected to thermal cycles by a heat-flux DSC apparatus with heating and cooling rate of 0.5 or 0.3°C/min. The microstructure of the samples, both after annealing and after DSC analysis, was studied by optical and scanning electron microscopy coupled with EDS (Energy Dispersive Spectroscopy analysis. Considering the slow heating and cooling rate adopted, the isothermal section at room temperature was established. No ternary compounds were observed. On the basis of the experimental investigations the invariant reactions were identified. Combining the thermodynamic data on the Ag-Ge, Ag-Zn and Ge-Zn liquid phases by means of Butler’s model the surface tension of Ag-Ge-Zn alloys was calculated.

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.

Stress corrosion crack growth rate in dissimilar metal welds; Evolucion microestructural de la ZAC en la union soldada con MIG sobre una aleacion del aluminio AA7020

Energy Technology Data Exchange (ETDEWEB)

Bloem, C. A.; Salvador, M. D.; Amigo, V.; Busquets, D.

2003-07-01

The aim of the present study is to evaluate the changes through the HAZ, analyzed under two different but complementary techniques. These are Transmission Electronic Microscopy (TEM) and Differential Scanning Calorimetry (DSC). The results shown that there are remarkable changes in size and morphology of the precipitates, being in accordance with the results obtained by DSC. (Author) 10 refs.

Stress corrosion crack growth rate in dissimilar metal welds

International Nuclear Information System (INIS)

Bloem, C. A.; Salvador, M. D.; Amigo, V.; Busquets, D.

2003-01-01

The aim of the present study is to evaluate the changes through the HAZ, analyzed under two different but complementary techniques. These are Transmission Electronic Microscopy (TEM) and Differential Scanning Calorimetry (DSC). The results shown that there are remarkable changes in size and morphology of the precipitates, being in accordance with the results obtained by DSC. (Author) 10 refs

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.

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

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.)

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)

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

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

Science.gov (United States)

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

2017-12-01

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

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

Experimental investigations on potassium permanganate doped polyvinyl alcohol - polyvinyl pyrrolidone blend

Science.gov (United States)

Veena, G.; Lobo, Blaise

2018-04-01

Potassium permanganate (KMnO4) doped polyvinyl alcohol (PVA) - polyvinyl pyrrolidone (PVP) blend films were prepared by solution casting technique, in the doping range varying from 0.01 wt % up to 4.70 wt %. The microstructural changes caused by doping, and the modified properties of these films were studied using Atomic Force Microscope (AFM) and temperature dependent direct current (DC) electrical measurements. Temperature variation of electrical resistivity was found to obey Arrhenius relation, from which activation energy was determined. The study was supported by AFM scans, which showed an increase in surface roughness and the presence of spike-like structures, due to interaction of dopant with the polymeric blend. Differential Scanning Calorimetry (DSC) scans revealed two stages of degradation in KMnO4 doped PVA - PVP blend films.

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.

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)

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.

Moisture distribution in sludges based on different testing methods

Institute of Scientific and Technical Information of China (English)

Wenyi Deng; Xiaodong Li; Jianhua Yan; Fei Wang; Yong Chi; Kefa Cen

2011-01-01

Moisture distributions in municipal sewage sludge, printing and dyeing sludge and paper mill sludge were experimentally studied based on four different methods, i.e., drying test, thermogravimetric-differential thermal analysis (TG-DTA) test, thermogravimetricdifferential scanning calorimetry (TG-DSC) test and water activity test. The results indicated that the moistures in the mechanically dewatered sludges were interstitial water, surface water and bound water. The interstitial water accounted for more than 50％ wet basis (wb) of the total moisture content. The bond strength of sludge moisture increased with decreasing moisture content, especially when the moisture content was lower than 50％ wb. Furthermore, the comparison among the four different testing methods was presented.The drying test was advantaged by its ability to quantify free water, interstitial water, surface water and bound water; while TG-DSC test, TG-DTA test and water activity test were capable of determining the bond strength of moisture in sludge. It was found that the results from TG-DSC and TG-DTA test are more persuasive than water activity test.

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

Theoretical studies of hadronic calorimetry for high luminosity, high energy colliders

Energy Technology Data Exchange (ETDEWEB)

Brau, J.E.; Gabriel, T.A.

1989-01-01

Experiments at the high luminosity, high energy colliders of the future are going to demand optimization of the state of the art of calorimetry design and construction. During the past few years, the understanding of the basic phenomenology of hadron calorimeters has advanced through paralleled theoretical and experimental investigations. The important underlying processes 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, e/h 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. 62 refs., 22 figs., 3 tabs.

Theoretical studies of hadronic calorimetry for high luminosity, high energy colliders

International Nuclear Information System (INIS)

Brau, J.E.; Gabriel, T.A.

1989-01-01

Experiments at the high luminosity, high energy colliders of the future are going to demand optimization of the state of the art of calorimetry design and construction. During the past few years, the understanding of the basic phenomenology of hadron calorimeters has advanced through paralleled theoretical and experimental investigations. The important underlying processes 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, e/h ∼ 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. 62 refs., 22 figs., 3 tabs

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.

Thermoanalytical Investigation of Terazosin Hydrochloride

Directory of Open Access Journals (Sweden)

Mona Mohamed Abdel-Moety

2013-02-01

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

CALOR2012 XVth International Conference on Calorimetry in High Energy Physics

Energy Technology Data Exchange (ETDEWEB)

Akchurin, Nural .

2015-05-04

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

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

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

Science.gov (United States)

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

2018-02-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-06-05

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

Experimentally determined standard thermodynamic properties of synthetic MgSO(4)·4H(2)O (Starkeyite) and MgSO(4)·3H(2)O: a revised internally consistent thermodynamic data set for magnesium sulfate hydrates.

Science.gov (United States)

Grevel, Klaus-Dieter; Majzlan, Juraj; Benisek, Artur; Dachs, Edgar; Steiger, Michael; Fortes, A Dominic; Marler, Bernd

2012-11-01

The enthalpies of formation of synthetic MgSO(4)·4H(2)O (starkeyite) and MgSO(4)·3H(2)O were obtained by solution calorimetry at T=298.15 K. The resulting enthalpies of formation from the elements are [Formula: see text] (starkeyite)=-2498.7±1.1 kJ·mol(-1) and [Formula: see text] (MgSO(4)·3H(2)O)=-2210.3±1.3 kJ·mol(-1). The standard entropy of starkeyite was derived from low-temperature heat capacity measurements acquired with a physical property measurement system (PPMS) in the temperature range 5 Kcalorimetry (DSC) measurements with a Perkin Elmer Diamond DSC in the temperature range 270 Klimitations of kieserite formation, metastable occurrence of starkeyite might be possible under martian conditions.

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.

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.

Thermodynamic behavior of erythritol in aqueous solutions and in gelatine gels and its quantification

International Nuclear Information System (INIS)

Tyapkova, Oxana; Bader-Mittermaier, Stephanie; Schweiggert-Weisz, Ute

2013-01-01

Highlights: • Differential scanning calorimetry as a method to determine erythritol crystallization. • Determination of crystallization using solution enthalpy. • Erythritol crystallization influenced by area of air–water-interfaces. • DSC method is applicable for both aqueous solutions and gels. • Adaption of DSC method to other, more complex food matrices is possible. - Abstract: As crystallization of erythritol can cause a sandy mouth-feel in sugar-free products, strategies to avoid crystallization or adaption of food formulation should be elucidated. However, until now erythritol crystallization was only quantified in aqueous solutions, but not in model food systems. Differential scanning calorimetry (DSC) is a simple method for the quantification of phase transition in various systems. However, no methods for the quantification of crystallization from aqueous systems based on DSC have been published until now. In the present study DSC was found to be suitable for the quantification of crystallization using supersaturated aqueous solutions of erythritol and erythritol containing gelatine gels for the first time. The developed method was validated by comparing the crystallization values determined by gravimetric measurement of erythritol crystals and the values obtained by DSC. No significant differences (p < 0.05) have been obtained between the results of the two methods if an appropriate design of measurements was applied. Additionally, the method was adapted to gelatine gels to elucidate the transferability to model food systems. Hence, the method is suitable for quantification of the amount of erythritol crystals present in aqueous solutions and gels, respectively

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.

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.

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...

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.

Energetics of metastudtite and implications for nuclear waste alteration.

Science.gov (United States)

Guo, Xiaofeng; Ushakov, Sergey V; Labs, Sabrina; Curtius, Hildegard; Bosbach, Dirk; Navrotsky, Alexandra

2014-12-16

Metastudtite, (UO2)O2(H2O)2, is one of two known natural peroxide minerals, but little is established about its thermodynamic stability. In this work, its standard enthalpy of formation, -1,779.6 ± 1.9 kJ/mol, was obtained by high temperature oxide melt drop solution calorimetry. Decomposition of synthetic metastudtite was characterized by thermogravimetry and differential scanning calorimetry (DSC) with ex situ X-ray diffraction analysis. Four decomposition steps were observed in oxygen atmosphere: water loss around 220 °C associated with an endothermic heat effect accompanied by amorphization; another water loss from 400 °C to 530 °C; oxygen loss from amorphous UO3 to crystallize orthorhombic α-UO2.9; and reduction to crystalline U3O8. This detailed characterization allowed calculation of formation enthalpy from heat effects on decomposition measured by DSC and by transposed temperature drop calorimetry, and both these values agree with that from drop solution calorimetry. The data explain the irreversible transformation from studtite to metastudtite, the conditions under which metastudtite may form, and its significant role in the oxidation, corrosion, and dissolution of nuclear fuel in contact with water.

Particle flow calorimetry at the international linear collider

Indian Academy of Sciences (India)

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

Hadronic shower development in iron-scintillator tile calorimetry

Czech Academy of Sciences Publication Activity Database

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

2000-01-01

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

Optimization of crystals for applications in dual-readout calorimetry

Czech Academy of Sciences Publication Activity Database

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

2010-01-01

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

Optical fibre temperature sensor technology and potential application in absorbed dose calorimetry

International Nuclear Information System (INIS)

Allen, P.D.; Hargrave, N.J.

1992-09-01

Optical fibre based sensors are proposed as a potential alternative to the thermistors traditionally used as temperature sensors in absorbed dose calorimetry. The development of optical fibre temperature sensor technology over the last ten years is reviewed. The potential resolution of various optical techniques is assessed with particular reference to the requirements of absorbed dose calorimetry. Attention is drawn to other issues which would require investigation before the development of practical optical fibre sensors for this purpose could occur. 192 refs., 5 tabs., 4 figs

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

Directory of Open Access Journals (Sweden)

Krstić Marko

2015-01-01

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

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.

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.

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

2017 ARL Summer Student Program Volume 2: Compendium of Abstracts

Science.gov (United States)

2017-12-01

porosimetry, bomb calorimetry, TEM, DSC, FTIR, EDS, and high- speed imaging are used to analyze the physical and energetic qualities of the...combustion reaction. Open-channel combustion experiments yield flame speed in excess of 2.5 km/s, and bomb calorimetry produces heats of combustion in the...J Matthew The properties and behaviors of energetic material ( EM ) composites are believed to be heavily influenced by their microstructure

Study of the Melting Latent Heat of Semicrystalline PVDF applied to High Gamma Dose Dosimetry

Energy Technology Data Exchange (ETDEWEB)

Batista, Adriana S.M. [Departamento de Anatomia e Imagem - IMA, Universidade Federal de Minas Gerais, Av. Prof. Alfredo Balena, 190, 30130-100, Belo Horizonte, MG (Brazil); Gual, Maritza R.; Faria, Luiz O. [Centro de Desenvolvimento da Tecnologia Nuclear - CDTN, Av. Antonio Carlos 6627, C.P. 941, 31270-901, Belo Horizonte, MG (Brazil); Lima, Claubia P.B. [Departamento de Engenharia Nuclear - DEN, Universidade Federal de Minas Gerais - UFMG, Av. Antonio Carlos 6627, 31270-970 Belo Horizonte, MG (Brazil)

2015-07-01

Poly(vinylidene fluoride) homopolymers [PVDF] homopolymers were irradiated with gamma doses ranging from 0.5 to 2.75 MGy. Differential scanning calorimetry (DSC) and FTIR spectrometry were used in order to study the effects of gamma radiation in the amorphous and crystalline polymer structures. The FTIR data revealed absorption bands at 1730 and 1853 cm{sup -1} which were attributed to the stretch of C=O bonds, at 1715 and 1754 cm{sup -1} which were attributed to the C=C stretching and at 3518, 3585 and 3673 cm{sup -1} which were associated with NH stretch of NH{sub 2} and OH. The melting latent heat (LM) measured by DSC was used to construct an unambiguous relationship with the delivered dose. Regression analyses revealed that the best mathematical function that fits the experimental calibration curve is a 4-degree polynomial function, with an adjusted Rsquare of 0.99817. (authors)

Advanced kinetics for calorimetric techniques and thermal stability screening of sulfide minerals

International Nuclear Information System (INIS)

Iliyas, Abduljelil; Hawboldt, Kelly; Khan, Faisal

2010-01-01

Thermal methods of analysis such as differential scanning calorimetry (DSC) provide a powerful methodology for the study of solid reactions. This paper proposes an improved thermal analysis methodology for thermal stability investigation of complex solid-state reactions. The proposed methodology is based on differential iso-conversional approach and involves peak separation, individual peak analysis and combination of isothermal/non-isothermal DSC measurements for kinetic analysis and prediction. The proposed thermal analysis, which coupled with Mineral Libration Analyzer (MLA) technique was employed to investigate thermal behavior of sulfide mineral oxidation. The importance of various experimental variables such as particle size, heating rate and atmosphere were investigated and discussed. The information gained from such an advanced thermal analysis method is useful for scale-up processes with potential of significant savings in plant operations, as well as in mitigating adverse environmental and safety issues arising from handling and storage of sulfide minerals.

Synthesis of Hydrophobic, Crosslinkable Resins.

Science.gov (United States)

1985-12-01

product by methanol precipitation the majority of the first oligomer was L-"- lost. 4.14 DIFFERENTIAL SCANNING CALORIMETRY. The DSC trace of a typical...polymer from the DSC traces obtained to dcte. Preliminary studies using an automated torsional pendulum indicate that the Tg of the crosslinked polymer is...enabling water to be used in the purification steps. The diethyl phosphonates are readily prepared by heating triethyl phosphite with the chloromethyl

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

International Nuclear Information System (INIS)

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

1996-01-01

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

Inherent limitations of fixed time servo-controlled radiometric calorimetry

International Nuclear Information System (INIS)

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

1987-01-01

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

Inherent limitations of fixed-time, servo-controlled radiometric calorimetry

International Nuclear Information System (INIS)

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

1987-01-01

Interest has been shown in using fixed-time, servo-controlled calorimetry to shorten the measurement times for certain samples that require low precision values (3 to 5%). This type of calorimeter measurement could be particularly useful for screening scrap samples to determine whether there is a need for a more accurate measurement or for certain confirmatory measurements for which low precision numbers are sufficient. The equipment required for this type of measurement is a servo-controlled calorimeter and a preconditioning unit. Samples to be measured are placed in the preconditioning unit, which is maintained at the internal temperature of the calorimeter. The power value for the sample is determined at a fixed time after loading into the calorimeter, for example, 30 min. When a calorimeter is operated using a fixed cutoff time, there are additional sources of uncertainty that need to be considered. The major factors affecting the uncertainty of the calorimetry power values are discussed. 2 refs., 4 figs

Thermodynamic study of selected monoterpenes III

International Nuclear Information System (INIS)

Štejfa, Vojtěch; Fulem, Michal; Růžička, Květoslav; Červinka, Ctirad

2014-01-01

Highlights: • (−)-trans-Pinane, (+)-Δ-carene, eucalyptol, and limonene were studied. • New thermodynamic data were measured and calculated. • Many of thermodynamic data are reported for the first time. - Abstract: A thermodynamic study of selected monoterpenes, (−)-trans-pinane, (+)-Δ-carene, eucalyptol, (+)-limonene, and (−)-limonene, is presented in this work. The vapor pressure measurements were performed using the static method over the environmentally important temperature range (238 to 308) K. Liquid heat capacities were measured by Tian–Calvet calorimetry in the temperature interval (258 to 355) K. The phase behavior was investigated by differential scanning calorimetry (DSC) from T = 183 K. The thermodynamic properties in the ideal-gas state were calculated by combining statistical thermodynamic and density functional theory (DFT) calculations. Calculated ideal-gas heat capacities and experimental data for vapor pressures and condensed phase heat capacities were treated simultaneously to obtain a consistent thermodynamic description

Kinetics of the lamellar gel-fluid transition in phosphatidylcholine membranes in the presence of sugars

Energy Technology Data Exchange (ETDEWEB)

Lenné, Thomas; Garvey, Christopher J.; Koster, Karen L.; Bryant, Gary [ANSTO; (USD); (RMIT)

2014-09-24

Phase diagrams are presented for dipalmitoylphosphatidylcholine (DPPC) in the presence of sugars (sucrose) over a wide range of relative humidities (RHs). The phase information presented here, determined by small angle X-ray scattering (SAXS), is shown to be consistent with previous results achieved by differential scanning calorimetry (DSC). Both techniques show a significant effect of sucrose concentration on the phase behaviour of this phospholipid bilayer. An experimental investigation into the effect of sugars on the kinetic behaviour of the gel to fluid transition is also presented showing that increasing the sugar content appears to slightly increase the rate at which the transition occurs.

Kinetics of the lamellar gel-fluid transition in phosphatidylcholine membranes in the presence of sugars

Energy Technology Data Exchange (ETDEWEB)

Lenné, Thomas; Garvey, Christopher J; Koster, Karen L; Bryant, Gary [ANSTO; (USD); (RMIT)

2010-08-04

Phase diagrams are presented for dipalmitoylphosphatidylcholine (DPPC) in the presence of sugars (sucrose) over a wide range of relative humidities (RHs). The phase information presented here, determined by small angle X-ray scattering (SAXS), is shown to be consistent with previous results achieved by differential scanning calorimetry (DSC). Both techniques show a significant effect of sucrose concentration on the phase behaviour of this phospholipid bilayer. An experimental investigation into the effect of sugars on the kinetic behaviour of the gel to fluid transition is also presented showing that increasing the sugar content appears to slightly increase the rate at which the transition occurs.

The relationship between viscosity and refinement efficiency of pure aluminum by Al-Ti-B refiner

Energy Technology Data Exchange (ETDEWEB)

Yu Lina [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, 73 Jingshi Road, Jinan 250061 (China); Liu Xiangfa [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, 73 Jingshi Road, Jinan 250061 (China)]. E-mail: xfliu@sdu.edu.cn

2006-11-30

The relationship between viscosity and refinement efficiency of pure aluminum with the addition of Al-Ti-B master alloy was studied in this paper. The experimental results show that when the grain size of solidified sample is finer the viscosity of the melt is higher after the addition of different Al-Ti-B master alloys. This indicates that viscosity can be used to approximately estimate the refinement efficiency of Al-Ti-B refiners in production to a certain extent. The main reason was also discussed in this paper by using transmission electron microscopy (TEM) analysis and differential scanning calorimetry (DSC) experiment.

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 ...

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...

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.

SU-E-T-146: Reference Dosimetry for Protons and Light-Ion Beams Based on Graphite Calorimetry.

Science.gov (United States)

Rossomme, S; Palmans, H; Thomas, R; Lee, N; Bailey, M; Shipley, D; Al-Sulaiti, L; Cirrone, P; Romano, F; Kacperek, A; Bertrand, D; Vynckier, S

2012-06-01

The IAEA TRS-398 code of practice can be applied for the measurement of absorbed dose to water under reference conditions with an ionization chamber. For protons, the combined relative standard uncertainty on those measurements is less than 2% while for light-ion beams, it is considerably larger, i.e. 3.2%, mainly due to the higher uncertainty contributions for the water to air stopping power ration and the W air-value on the beam quality correction factors kQ,Q 0 . To decrease this uncertainty, a quantification of kQ,Q 0 is proposed using a primary standard level graphite calorimeter. This work includes numerical and experimental determinations of dose conversion factors to derive dose to water from graphite calorimetry. It also reports on the first experimental data obtained with the graphite calorimeter in proton, alpha and carbon ion beams. Firstly, the dose conversion has been calculated with by Geant4 Monte-Carlo simulations through the determination of the water to graphite stopping power ratio and the fluence correction factor. The latter factor was also derived by comparison of measured ionization curves in graphite and water. Secondly, kQ,Q 0 was obtained by comparison of the dose response of ionization chambers with that of the calorimeter. Stopping power ratios are found to vary by no more than 0.35% up to the Bragg peak, while fluence correction factors are shown to increase slightly above unity close to the Bragg peak. The comparison of the calorimeter with ionization chambers is currently under analysis. For the modulated proton beam, preliminary results on W air confirm the value recommended in TRS-398. Data in both the non-modulated proton and light-ion beams indicate higher values but further investigation of heat loss corrections is needed. The application of graphite calorimetry to proton, alpha and carbon ion beams has been demonstrated successfully. Other experimental campaigns will be held in 2012. This work is supported by the BioWin program

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....

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.

Non-isothermal crystallization kinetics of As{sub 30}Te{sub 60}Ga{sub 10} glass

Energy Technology Data Exchange (ETDEWEB)

Mohamed, Mansour; Abd-Elnaiem, Alaa M.; Abdel-Rahim, M.A.; Hafiz, M.M. [Assiut University, Physics Department, Faculty of Science, Assiut (Egypt); Hassan, R.M. [Assiut University, Physics Department, Faculty of Science, Assiut (Egypt); Aden University, Physics Department, Faculty of Education-Zingiber, Aden (Yemen)

2017-08-15

The crystallization study under non-isothermal conditions of As{sub 30}Te{sub 60}Ga{sub 10} glass was investigated. The studied composition was synthesized by melt-quenching technique and characterized by different techniques such as X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and differential scanning calorimetry (DSC). The XRD analysis revealed that the as-prepared and annealed bulk glass of As{sub 30}Te{sub 60}Ga{sub 10} exhibit the amorphous, and polycrystalline nature, respectively. The DSC results showed that the heating rate affects the characteristic temperatures, for instance, the glass transition, onset, and peak crystallization temperatures. Furthermore, some thermal analysis methods such as the Kissinger and Matusita et al., approximations were employed to determine the crystallization parameters: for example Avrami exponent and the activation energies for glass transition and crystallization process. In addition, we have compared the experimental DSC data with the calculated ones based on the Johnson-Mehl-Avrami (JMA) and Sestak-Berggren SB(M,N) models. The results indicated that the SB(M,N) model is more suitable for describing the non-isothermal crystallization kinetics of the investigated composition. (orig.)

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

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.

Isothermal and non-isothermal cure of a tri-functional epoxy resin (TGAP): a stochastic TMDSC study

OpenAIRE

Hutchinson, John M.; Shiravand, Fatemeh; Calventus Solé, Yolanda; Fraga Rivas, Iria

2012-01-01

The isothermal cure of a highly reactive tri-functional epoxy resin, tri-glycidyl para-amino phenol (TGAP), with diamino diphenyl sulphone (DDS), at two different cure temperatures Tc has been studied by both conventional differential scanning calorimetry (DSC) and by a stochastic temperature modulated DSC technique, TOPEM. From a series of isothermal cure experiments for increasing cure times, the glass transition temperature Tg as a function of isothermal cure time is determined by co...

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

A combined experimental and computational thermodynamic study of fluorene-9-methanol and fluorene-9-carboxylic acid

International Nuclear Information System (INIS)

Oliveira, Juliana A.S.A.; Calvinho, Maria M.; Notario, R.; Monte, Manuel J.S.; Ribeiro da Silva, Maria D.M.C.

2013-01-01

Highlights: • A thermodynamic study of two fluorene derivatives is presented. • Vapour pressures and energies of combustion were measured. • Enthalpy, entropy and Gibbs energy of sublimation were derived. • Enthalpy and Gibbs energy of formation in crystal and gas phases were calculated. • Gas phase enthalpy of formation was also estimated by quantum chemical calculations. -- Abstract: This work reports an experimental and computational thermodynamic study performed on two 9-fluorene derivatives: fluorene-9-methanol and fluorene-9-carboxylic acid. The standard (p o = 0.1 MPa) molar enthalpies of formation in the crystalline phase of these compounds were derived from the standard molar energies of combustion, in oxygen, at T = 298.15 K, measured by static bomb combustion calorimetry. A static method, based on a capacitance diaphragm gauge, and a Knudsen effusion method were used to perform the vapour pressure study of the referred compounds, yielding accurate determination of the standard molar enthalpies and entropies of sublimation and vaporisation. For fluorene-9-carboxylic acid, the enthalpy of sublimation was also determined using Calvet microcalorimetry. The enthalpy of fusion of both compounds was derived indirectly from vapour pressure results and directly from DSC experiments. Combining the thermodynamic parameters of the compounds studied, the standard Gibbs energy of formation in crystalline and gaseous phases were derived as well as the standard molar enthalpy of formation in the gaseous phase. A theoretical study at the G3 and G4 levels has been carried out, and the calculated enthalpies of formation have been compared with the experimental values

Synthesis, thermodynamic properties and antibacterial activities of lanthanide complexes with 3,5-dimethoxybenzoic acid and 1,10-phenanthroline

Energy Technology Data Exchange (ETDEWEB)

Zheng, Jun-Ru [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Ren, Shu-Xia [Material Science and Engineering School, Shijiazhuang Tiedao University, Shijiazhaung 050043 (China); Ren, Ning [Department of Chemistry, Handan College, Handan 056005 (China); Zhang, Jian-Jun, E-mail: jjzhang6@126.com [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Zhang, Da-Hai [Department of Chemistry, Handan College, Handan 056005 (China); Wang, Shu-Ping [College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China)

2013-11-20

Graphical abstract: Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline))were synthesized and characterized by elemental analysis, IR and TG/DSC-FTIR technology. Heat capacities of the four complexes were measured by differential scanning calorimetry (DSC). The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and Candida albicans were studied by filter paper approach. - Highlights: • Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} were synthesized and characterized. • The thermal decomposition processes of the title complexes were studied using the TG/DSC–FTIR coupling techniques. • The heat capacities of the complexes were measured by (DSC). • The antibacterial action of the four complexes on Escherichia coli, Staphylococcus aureus and Candida albicans were studied. - Abstract: Four lanthanide complexes with a general formula [Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, infrared spectra (IR), and thermogravimetric, differential scanning calorimetry techniques, combined with Fourier transform infrared (TG/DSC–FTIR) technology. The thermal decomposition processes of the four complexes were investigated by TG/DSC–FTIR techniques. Heat capacities were measured by DSC. The values of the experimental heat capacities were fitted to a polynomial equation with the least-squares method. Based on the fitted polynomial, the smoothed heat capacities and thermodynamic functions (H{sub T} − H{sub 298.15} {sub K}), (S{sub T} − S{sub 298.15} {sub K}), and (G{sub T} − G{sub 298.15} {sub K}) were calculated. The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and

Curing of bisphenol A-aniline based benzoxazine using phenolic, amino and mercapto accelerators

Directory of Open Access Journals (Sweden)

A. Rucigaj

2015-07-01

Full Text Available The curing of bisphenol A-aniline based benzoxazine was studied applying different accelerators (4,4'-thiodiphenol, o-dianisidine, 2-mercaptobenzimidazole and 4-mercaptophenol to initiate the catalytic ring-opening of benzoxazine. Possible pathways of benzoxazine ring-opening, polymerization and cross-linking without and with the addition of different accelerators are presented. The curing kinetics was investigated by model-free kinetic analysis of experimental data obtained by differential scanning calorimetry (DSC. The addition of different accelerators significantly reduced the onset temperature of curing in dynamic experiments. The effects of accelerators on the results of isothermal conversion prediction were studied and discussed in detail. Among the used accelerators, thiodiphenol showed the best accelerating efficiency and was consequently used in further studies, where its amount was varied. By low heating rate DSC analysis the catalytic ring-opening, thermally accelerated ring-opening and the diffusion-controlled steps were identified. The amount of added accelerator affected particularly the ring-opening and diffusion-controlled steps.

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

Analysis of light particles correlation selected by neutron calorimetry in the reaction 208 Pb+93 Nb at 29 MeV/u

International Nuclear Information System (INIS)

Ghisalberti, C.

1994-01-01

This work deals with the analysis of light particles correlation selected by neutrons calorimetry in the reaction : 208 Pb+ 93 Nb at 29 MeV/u. In the first part are described the interest of correlation functions, the proton-proton correlation function study, the classical model developed for describing the correlations of two light particles emitted by a nucleus in thermal equilibrium, the quantum model and some notions about exclusive sources and measures. The second part is a description of the experience : 208 Pb+ 93 Nb at 29 MeV/u. The analysis of experimental data and of experimental correlation functions are given respectively in the third and the fourth parts. (O.L.). 38 refs., 82 figs., 11 tabs

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.....

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

Science.gov (United States)

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

2016-01-01

Many labs have conventional calorimeters where denaturation and binding experiments are setup and run one at a time. While these systems are highly informative to biopolymer folding and ligand interaction, they require considerable manual intervention for cleaning and setup. As such, the throughput for such setups is limited typically to a few runs a day. With a large number of experimental parameters to explore including different buffers, macromolecule concentrations, temperatures, ligands, mutants, controls, replicates, and instrument tests, the need for high-throughput automated calorimeters is on the rise. Lower sample volume requirements and reduced user intervention time compared to the manual instruments have improved turnover of calorimetry experiments in a high-throughput format where 25 or more runs can be conducted per day. The cost and efforts to maintain high-throughput equipment typically demands that these instruments be housed in a multiuser core facility. We describe here the steps taken to successfully start and run an automated biological calorimetry facility at Pennsylvania State University. Scientists from various departments at Penn State including Chemistry, Biochemistry and Molecular Biology, Bioengineering, Biology, Food Science, and Chemical Engineering are benefiting from this core facility. Samples studied include proteins, nucleic acids, sugars, lipids, synthetic polymers, small molecules, natural products, and virus capsids. This facility has led to higher throughput of data, which has been leveraged into grant support, attracting new faculty hire and has led to some exciting publications. © 2016 Elsevier Inc. All rights reserved.

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.

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

African Journals Online (AJOL)

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

Hydroxychalcone and Hydroxypropyl-β-Cyclodextrin

African Journals Online (AJOL)

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

Liquid praseodymium heat content by levitation calorimetry. [Sample size 0. 5 - 1. 5g; 1460 to 2289/sup 0/K

Energy Technology Data Exchange (ETDEWEB)

Stretz, L.A.; Bautista, R.G.

1976-01-01

The high-temperature heat content of liquid praseodymium was measured experimentally by the levitation calorimetry technique. The samples, ranging in size from 0.5 to 1.5 g, were simultaneously levitated and heated by a radiofrequency generator in an argon-helium mixture prior to being dropped into a conventional copper block drop calorimeter. Corrections were made for the convection and radiation losses during the fall of the sample from the levitation chamber into the calorimeter. The praseodymium data, from 1460 to 2289K, were fitted by the following equation where the indicated errors represent the average deviation of the experimental value from the value predicted by the equation: H/sub T/ - H/sub 298/./sub 15/ = (41.57 +- 0.29) (T - 1208) + (41733 +- 197) J/mol. (auth)

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

The upgraded CDF front end electronics for calorimetry

Energy Technology Data Exchange (ETDEWEB)

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

1991-11-01

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

The upgraded CDF front end electronics for calorimetry

International Nuclear Information System (INIS)

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

1991-11-01

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

A guide to automation techniques in calorimetry

International Nuclear Information System (INIS)

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

1992-01-01

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

Thermodynamic study of selected monoterpenes II

International Nuclear Information System (INIS)

Štejfa, Vojtěch; Fulem, Michal; Růžička, Květoslav; Červinka, Ctirad

2014-01-01

Highlights: • (−)-Borneol, (−)-camphor, (±)-camphene, and (+)-fenchone were studied. • New thermodynamic data were measured and calculated. • Most of thermodynamic data are reported for the first time. - Abstract: A thermodynamic study of selected monoterpenes, (−)-borneol, (−)-camphor, (±)-camphene, and (+)-fenchone is presented in this work. The vapor pressure measurements were performed using the static method over the environmentally important temperature range from (238 to 308) K. Heat capacities of condensed phases were measured by Tian–Calvet calorimetry in the temperature interval from (258 to 355) K. The phase behavior was investigated by differential scanning calorimetry (DSC) from subambient temperatures up to the fusion temperatures. The thermodynamic properties in the ideal-gas state were calculated by combining statistical thermodynamic and density functional theory (DFT) calculations. Calculated ideal-gas heat capacities and experimental data for vapor pressures and condensed phase heat capacities were treated simultaneously to obtain a consistent thermodynamic description

A comprehensive approach to ascertain the binding mode of curcumin with DNA

Science.gov (United States)

Haris, P.; Mary, Varughese; Aparna, P.; Dileep, K. V.; Sudarsanakumar, C.

2017-03-01

Curcumin is a natural phytochemical from the rhizoma of Curcuma longa, the popular Indian spice that exhibits a wide range of pharmacological properties like antioxidant, anticancer, anti-inflammatory, antitumor, and antiviral activities. In the published literatures we can see different studies and arguments on the interaction of curcumin with DNA. The intercalative binding, groove binding and no binding of curcumin with DNA were reported. In this context, we conducted a detailed study to understand the mechanism of recognition of dimethylsulfoxide-solubilized curcumin by DNA. The interaction of curcumin with calf thymus DNA (ctDNA) was confirmed by agarose gel electrophoresis. The nature of binding and energetics of interaction were studied by Isothermal Titration Calorimetry (ITC), Differential Scanning Calorimetry (DSC), UV-visible, fluorescence and melting temperature (Tm) analysis. The experimental data were compared with molecular modeling studies. Our investigation confirmed that dimethylsulfoxide-solubilized curcumin binds in the minor groove of the ctDNA without causing significant structural alteration to the DNA.

In Situ Techniques for the Investigation of the Kinetics of Austenitization of Supermartensitic Stainless Steel

DEFF Research Database (Denmark)

Nießen, Frank; Villa, Matteo; Apel, Daniel

2016-01-01

The austenitization and inter-critical annealing of X4CrNiMo16-5-1 (1.4418) supermartensitic stainless steel were investigated in-situ with synchrotron X-ray diffraction (XRD), dilatometry and differential scanning calorimetry (DSC) under isochronal heating conditions. Austenitization occurred...... of surface martensite formation on the XRD measurement. The applicable temperature range for DSC as well as the close proximity of the Ac1- and the Curietemperature limited the usage of the technique in the present case....

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

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...

Compositional thermodynamic modelling of crystallization in waxy crudes; Modelisation thermodynamique compositionnelle de la cristallisation des bruts paraffiniques

Energy Technology Data Exchange (ETDEWEB)

Calange, S.

1996-06-26

During waxy crudes production, the risks of solid deposits formation, mainly in wells and in transport lines, are to be considered. These risks prevention induces high exploitation costs, and sometimes production losses. A better knowledge of the phenomena involved should allow an optimization of production conditions and thus cost reduction. With such objectives, we have developed a compositional thermodynamic model which allows to compute both the Wax Appearance Temperature and the amount of precipitated solid for lower temperatures. We have also implemented an experimental procedure in order to measure the solid deposit curve for a given crude under atmospheric pressure. The model can be used by means of a computer programme called `CRYSPAR`. This model takes into account the non-ideality of the solid phase through the one-parameter Margules equation. Thus it is only necessary to fit this unique parameter on the deposit quantities measured in the laboratory. The value thus determined will further allow the prediction of the deposition curves for crudes when their composition is changed, particularly by solvent addition. The experimental technique used is Differential Scanning Calorimetry (DSC). DSC is fast, easy to use and available in the laboratories of oil companies. (author) 181 refs.

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.

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Experimental research in the phase change materials based on paraffin and expanded perlite

Science.gov (United States)

Jiesheng, Liu; Faping, Li; Xiaoqiang, Gong; Rongtang, Zhang

2018-06-01

In this study, paraffin (PA)/expanded perlite (EP) form-stable phase change material (PCM) was first fabricated using the direct impregnation method without vacuum treatment. Absorptive capacity results showed that the PA/EP composite can obtain good absorptive capacity with the temperature 80 °C and the time 2 h. Compared with the water absorption of EP, the decrease in the water absorption of PA/EP form-stable proved that the absorption of PA into porous EP has been carried out successfully. Scanning electron microscope (SEM) and Fourier transform infrared (FT-IR) results show that paraffin can be well impregnated into EP pores and has good compatibility with it. Differential scanning calorimetry (DSC) results reveal that paraffin/EP composite PCM has melting temperature and latent heat of 53.6 °C and 91.3 J/g, respectively. The durability cycles results suggest that form-stable PA/EP PCM shows good durability.

Immersion calorimetry as a tool to evaluate the catalytic performance of titanosilicate materials in the epoxidation of cyclohexene.

Science.gov (United States)

Vernimmen, Jarian; Guidotti, Matteo; Silvestre-Albero, Joaquin; Jardim, Erika O; Mertens, Myrjam; Lebedev, Oleg I; Van Tendeloo, Gustaaf; Psaro, Rinaldo; Rodríguez-Reinoso, Francisco; Meynen, Vera; Cool, Pegie

2011-04-05

Different types of titanosilicates are synthesized, structurally characterized, and subsequently catalytically tested in the liquid-phase epoxidation of cyclohexene. The performance of three types of combined zeolitic/mesoporous materials is compared with that of widely studied Ti-grafted-MCM-41 molecular sieve and the TS-1 microporous titanosilicate. The catalytic test results are correlated with the structural characteristics of the different catalysts. Moreover, for the first time, immersion calorimetry with the same substrate molecule as in the catalytic test reaction is applied as an extra means to interpret the catalytic results. A good correlation between catalytic performance and immersion calorimetry results is found. This work points out that the combination of catalytic testing and immersion calorimetry can lead to important insights into the influence of the materials structural characteristics on catalysis. Moreover, the potential of using immersion calorimetry as a screening tool for catalysts in epoxidation reactions is shown.

Laser Calorimetry Spectroscopy for ppm-level Dissolved Gas Detection and Analysis.

Science.gov (United States)

K S, Nagapriya; Sinha, Shashank; R, Prashanth; Poonacha, Samhitha; Chaudhry, Gunaranjan; Bhattacharya, Anandaroop; Choudhury, Niloy; Mahalik, Saroj; Maity, Sandip

2017-02-20

In this paper we report a newly developed technique - laser calorimetry spectroscopy (LCS), which is a combination of laser absorption spectroscopy and calorimetry - for the detection of gases dissolved in liquids. The technique involves determination of concentration of a dissolved gas by irradiating the liquid with light of a wavelength where the gas absorbs, and measuring the temperature change caused by the absorbance. Conventionally, detection of dissolved gases with sufficient sensitivity and specificity was done by first extracting the gases from the liquid and then analyzing the gases using techniques such as gas chromatography. Using LCS, we have been able to detect ppm levels of dissolved gases without extracting them from the liquid. In this paper, we show the detection of dissolved acetylene in transformer oil in the mid infrared (MIR) wavelength (3021 nm) region.

Analysis of light particles correlation selected by neutron calorimetry in the reaction {sup 208} Pb+{sup 93} Nb at 29 MeV/u; Analyse de correlation de particules legeres selectionnees par calorimetrie neutronique dans la reaction {sup 208} Pb+{sup 93} Nb a 29 MeV/u

Energy Technology Data Exchange (ETDEWEB)

Ghisalberti, C

1994-11-10

This work deals with the analysis of light particles correlation selected by neutrons calorimetry in the reaction : {sup 208} Pb+{sup 93} Nb at 29 MeV/u. In the first part are described the interest of correlation functions, the proton-proton correlation function study, the classical model developed for describing the correlations of two light particles emitted by a nucleus in thermal equilibrium, the quantum model and some notions about exclusive sources and measures. The second part is a description of the experience : {sup 208} Pb+{sup 93} Nb at 29 MeV/u. The analysis of experimental data and of experimental correlation functions are given respectively in the third and the fourth parts. (O.L.). 38 refs., 82 figs., 11 tabs.

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′.

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)

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

Science.gov (United States)

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

2018-05-01

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

Physicochemical Characterization of Inclusion Complex of Catechin ...

African Journals Online (AJOL)

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

Crystallization processes in Ge2Sb2Se4Te glass

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

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

NARCIS (Netherlands)

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

2018-01-01

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

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...

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

Comparison of calorimetry and destructive analytical measurement techniques for excess plutonium powders

International Nuclear Information System (INIS)

Welsh, T.L.

1996-01-01

In Dec. 1994, IAEA safeguards were initiated on inventory of Pu- bearing materials, originating from the US nuclear weapons complex, at vault 3 of DOE's Plutonium Finishing Plant at Hanford. Because of the diversity and heterogeneity of the Pu, plant operators have increasingly used calorimetry for accountability measurements. During the recent commencement of IAEA safeguards at vault 3, destructive (electrochemical titration) methods were used to determine Pu concentrations in subsamples of inventory items with widely ranging chemical purities. The Pu concentrations in the subsamples were determined and contribution of heterogeneity to total variability was identified. Measurement results, gathered by PFP and IAEA laboratories, showed total measurement variability for calorimetry to be comparable with or lower than those of sampling and chemical analyses

The Philosophy and Feasibility of Dual Readout Calorimetry

International Nuclear Information System (INIS)

Hauptman, John

2006-01-01

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

Synergies between electromagnetic calorimetry and PET

International Nuclear Information System (INIS)

Moses, William W.

2002-01-01

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

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

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)

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

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.

The thermodynamic properties of benzothiazole and benzoxazole

Science.gov (United States)

Steele, W. V.; Chirico, R. D.; Knipmeyer, S. E.; Nguyen, A.

1991-08-01

This research program, funded by the Department of Energy, Office of Fossil Energy, Advanced Extraction and Process Technology, provides accurate experimental thermochemical and thermophysical properties for key organic diheteroatom-containing compounds present in heavy petroleum feedstocks, and applies the experimental information to thermodynamic analyses of key hydrodesulfurization, hydrodenitrogenation, and hydrodeoxygenation reaction networks. Thermodynamic analyses, based on accurate information, provide insights for the design of cost-effective methods of heteroatom removal. The results reported here, and in a companion report to be completed, will point the way to the development of new methods of heteroatom removal from heavy petroleum. Measurements leading to the calculation of the ideal-gas thermodynamic properties are reported for benzothiazole and benzoxazole. Experimental methods included combustion calorimetry, adiabatic heat-capacity calorimetry, comparative ebulliometry, inclinded-piston gauge manometry, and differential-scanning calorimetry (d.s.c). Critical property estimates are made for both compounds. Entropies, enthalpies, and Gibbs energies of formation were derived for the ideal gas for both compounds for selected temperatures between 280 K and near 650 K. The Gibbs energies of formation will be used in a subsequent report in thermodynamic calculations to study the reaction pathways for the removal of the heteratoms by hydrogenolysis. The results obtained in this research are compared with values present in the literature. The failure of a previous adiabatic heat capacity study to see the phase transition in benzothiazole is noted. Literature vibrational frequency assignments were used to calculate ideal gas entropies in the temperature range reported here for both compounds. Resulting large deviations show the need for a revision of those assignments.

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.

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...

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

Energy Technology Data Exchange (ETDEWEB)

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

2018-01-01

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

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

Science.gov (United States)

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

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

African Journals Online (AJOL)

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

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

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

KAUST Repository

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

2016-01-01

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

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

NARCIS (Netherlands)

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

2007-01-01

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

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

NARCIS (Netherlands)

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

2007-01-01

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

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.

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)

Age hardening in mechanically alloyed Al-Mg-Li-C-O

Energy Technology Data Exchange (ETDEWEB)

Papazian, J.M. (Corporate Research Center, Grumman Corporation, Bethpage, NY (USA)); Gilman, P. (Allied-Signal Inc., Morristown, NJ (USA))

1990-05-01

The age-hardening behavior of a series of mechanically alloyed Al-Mg-Li-C-O alloys containing 3.0-4.0 wt.% Mg and 1.3-1.75 wt.% Li was studied using hardness tests, differential scanning calorimetry (DSC) and transmission electron microscopy. The hardness tests showed an increased hardness after 100degC aging in all the alloys containing at least 1.5 at.% Li. Likewise, the calorimetry results showed the presence of pronounced precipitate dissolution peaks in these same alloys after 100degC aging. The volume fraction of precipitates formed (as measured by the dissolution enthalpies of the DSC peaks) increased systematically with increasing solute content. Transmission electron microscopy after 100 and 190degC aging showed images and diffraction spots similar to those of {delta}' (Al{sub 3}Li). Comparison of the DSC results with results from binary Al-Li and Al-Mg alloys indicated that the precipitates formed in the Al-Mg-Li-C-O alloys were similar to those formed in binary Al-Li alloys, and that the primary role of the magnesium was to lower the solid solubility of lithium. (orig.).

Thermal degradation and isothermal crystalline behavior of poly(trimethylene terephthalate)

Institute of Scientific and Technical Information of China (English)

Jian Liu; Shu Guang Bian; Min Xiao; Shuan Jin Wang; Yue Zhong Meng

2009-01-01

Poly(trimethylene terephthalate)(PTT)is an excellent fiber material.Its thermal degradation and isothermal crystalline behaviors were in this study investigated using thermogravimetric analysis(TGA),thermogravimetric analysis-Fourier transform infrared spectroscopy(TGA-FTIR)analysis,differential scanning calorimetry(DSC)and X-ray diffraction(XRD).The thermal degradation mechanism of PTT follows Mclafferty rearrangement principle.The PTT with intrinsicviscosity(IV)of 0.74 dL/g has a maximum crystallinity of about 55%at 190℃,as demonstrated by DSC and XRD measurements consistently.

Synthesis and Characterization of Photo-Responsive Thermotropic Liquid Crystals Based on Azobenzene

Directory of Open Access Journals (Sweden)

Runmiao Yang

2018-03-01

Full Text Available A series of new thermotropic liquid crystals (LCs containing azobenzene units was synthesized. The structures of the compounds were characterized by means of NMR and FTIR spectroscopy. Their mesomorphic behaviors were investigated via differential scanning calorimetry (DSC and polarizing optical microscopy (POM. Based on the POM and DSC measurements, the optical properties of the Razo-ester were tested using UV-vis spectroscopy. The azobenzene side chain displayed a strong ability to influence the formation of thermotropic LCs.

Simultaneous Absorptance and Thermal-Diffusivity Determination of Optical Components with Laser Calorimetry Technique

Science.gov (United States)

Wang, Yanru; Li, Bincheng

2012-11-01

The laser calorimetry (LCA) technique is used to determine simultaneously the absorptances and thermal diffusivities of optical components. An accurate temperature model, in which both the finite thermal conductivity and the finite sample size are taken into account, is employed to fit the experimental temperature data measured with an LCA apparatus for a precise determination of the absorptance and thermal diffusivity via a multiparameter fitting procedure. The uniqueness issue of the multiparameter fitting is discussed in detail. Experimentally, highly reflective (HR) samples prepared with electron-beam evaporation on different substrates (BK7, fused silica, and Ge) are measured with LCA. For the HR-coated sample on a fused silica substrate, the absorptance is determined to be 15.4 ppm, which is close to the value of 17.6 ppm, determined with a simplified temperature model recommended in the international standard ISO11551. The thermal diffusivity is simultaneously determined via multiparameter fitting to be approximately 6.63 × 10-7 m2 · s-1 with a corresponding square variance of 4.8 × 10-4. The fitted thermal diffusivity is in reasonably good agreement with the literature value (7.5 × 10-7 m2 · s -1). Good agreement is also obtained for samples with BK7 and Ge substrates.

Subsite binding energies of an exo-polygalacturonase using isothermal titration calorimetry

Science.gov (United States)

Thermodynamic parameters for binding of a series of galacturonic acid oligomers to an exo-polygalacturonase, RPG16 from Rhizopus oryzae, were determined by isothermal titration calorimetry. Binding of oligomers varying in chain length from two to five galacturonic acid residues is an exothermic proc...

Monolithic front-end preamplifiers for a broad range of calorimetry applications

Energy Technology Data Exchange (ETDEWEB)

Radeka, V.; Rescia, S. [Brookhaven National Lab., Upton, NY (United States); Manfredi, P.F.; Speziali, V. [Pavia Univ. (Italy). Dipt. di Elettronica]|[INFN--Sezzione di Milano, Milano (Italy)

1993-12-31

The present paper summarizes the salient results of a research and development activity in the area of low noise preamplifiers for different applications in calorimetry. Design target for all circuits considered here are low noise, ability to cope with broad energy ranges and radiation hardness.

Analysis of the effects of reaction parameters upon the molecular weight of an aromatic poly(hydrazide) through experimental design

International Nuclear Information System (INIS)

Gomes, Dominique; Pinto, Jose Carlos; Borges, Cristiano P.; Nunes, Suzana P.

2001-01-01

Samples of an aromatic poly(hydrazide) were synthesized through low temperature solution polycondensation reactions. Monomers were characterized by nuclear magnetic resonance (NMR) and thermal analysis. The polymer material was characterized by intrinsic viscosity measurements and by NMR. The thermal behavior of the polymer samples was studied by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The effect of various factors that influence the course of the polymerization reaction, such as concentration of monomer and electrolyte (LiCl) in the reaction medium, purity of the monomers, reaction temperature and reaction time, were investigated. Reaction conditions were then optimized in order to allow the preparation of high molecular weight polymer resins. Values of intrinsic viscosity obtained for the poly(hydrazide) in N-methyl-2-pyrrolidone were as high as 1.51 dL/g. (author)

Ring-shaped Calorimetry Information for a Neural eGamma Identification with ATLAS Detector

CERN Document Server

Da Fonseca Pinto, Joao Victor; The ATLAS collaboration; Oliveira Damazio, Denis; Seixas, Jose

2016-01-01

\\title{Ring-shaped Calorimetry Information for a Neural e/$\\gamma$ Identification with ATLAS Detector} After the successful operation of the Large Hadron Collider resulting with the discovery of the Higgs boson, a new data-taking period (Run 2) has started. For the first time, collisions are produced with energies of 13 TeV in the centre of mass. It is foreseen the luminosity increase, reaching values as high as $10^{34}cm^{-2}s^{-1}$ yet in 2015. These changes in experimental conditions bring a proper environment for possible new physics key-findings. ATLAS is the largest LHC detector and was designed for general-purpose physics studies. Many potential physics channels have electrons or photons in their final states. For efficient studies on these channels precise measurement and identification of such particles is necessary. The identification task consists of disentangling those particles (signal) from collimated hadronic jets (background). Reported work concerns the identification process based on the cal...

Application of isothermal calorimetry and uv spectroscopy for stability monitoring of pentaerythritol tetranitrate

International Nuclear Information System (INIS)

Dosser, L.R.; Pickard, J.M.

1992-01-01

Thermal stabilities for a series of pentaerythritol-tetranitrate (PETN) samples with variable surf ace areas were monitored by isothermal calorimetry and UV spectroscopy over the temperature range of 363 to 408 K. Isothermal induction times measured with constant volume calorimetry under an air atmosphere and No evolution rates monitored by UV absorbance at 213 nm under vacuum correlated with the PETN surface area at temperatures equal to or exceeding 383 K. Rate data measured at 383 K are in accord with predictions based on detailed kinetic modeling. Below 383 K, NO evolution data suggested that additional geometric factors may be significant in controlling PETN stability. Mechanisms for influencing surface area upon the rate-determining step are addressed

Material characterization of a polyester resin system for the pultrusion process

DEFF Research Database (Denmark)

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

2014-01-01

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

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

African Journals Online (AJOL)

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

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

NARCIS (Netherlands)

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

2008-01-01

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

The Influence of Concentration and Temperature on the Formation of ¿-Oryzanol + ß-Sitosterol Tubules in Edible Oil Organogels

NARCIS (Netherlands)

Sawalha, H.I.M.; Venema, P.; Bot, A.; Flöter, E.; Linden, van der E.

2011-01-01

The gelation process of mixtures of ¿-oryzanol and sitosterol structurants in sunflower oil was studied using light scattering, rheology, and micro-scanning calorimetry (Micro-DSC). The relation between temperature and the critical aggregation concentration (CAC) of tubule formation of ¿-oryzanol

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

NARCIS (Netherlands)

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

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

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

African Journals Online (AJOL)

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

Preparation, Characterization and Antibacterial Properties of Silver ...

African Journals Online (AJOL)

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

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

NARCIS (Netherlands)

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

1997-01-01

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

Khảo sát sự tạo mixel của một số Copolyme Pluronic

DEFF Research Database (Denmark)

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

2009-01-01

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

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

Science.gov (United States)

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

Precipitate-induced R-phase in martensitic transformation of as-spun and annealed Ti51Ni49 ribbons

International Nuclear Information System (INIS)

Wu, Ling-Mei; Chang, Shih-Hang; Wu, Shyi-Kaan

2010-01-01

Differential scanning calorimetry (DSC) results indicate that a two-step B2 → R → B19' martensitic transformation and a one-step B19' → B2 transformation exhibit in as-spun and in 200-600 o C annealed Ti 51 Ni 49 ribbons. Guinier-Preston (GP) zones and Ti 2 Ni precipitates are formed in ribbons annealed at ≤300 o C and ≥400 o C, respectively, and a conspicuous increase of DSC transformation peak temperature occurs in between 300 o C and 400 o C. The sizes of GP zones and Ti 2 Ni precipitates increase with increased annealing temperature. Transmission electron microscope (TEM) observations show that GP zones can induce the R-phase and both of them are formed along B2 directions. DSC and TEM tests show that Ti 2 Ni precipitates can induce the R-phase more than GP zones and the induced R-phase plates are also found along B2 directions. Experimental results show that the growing direction of R-phase plates is strongly confined by that of GP zones and Ti 2 Ni precipitates. The length of R-phase plates can reach about 2 μm in 300 o C annealed ribbon.

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

Radiation damage study for silicon calorimetry: Summary of first year's activity

International Nuclear Information System (INIS)

Russ, J.S.

1988-01-01

In the first contract year of this activity at Carnegie-Mellon we have had two major objectives. These were to devise and test a non-intrusive means to measure the energy and spatial profiles of the neutrons generated in a hadronic cascade at high energy; and to study the calibration systematics of silicon diode detectors as a prelude to their evaluation for SSC calorimetry. These objectives have been carried out, as are described in this paper. In addition we have recoded the ORNL detector simulation program HETC to operate on a VAX and are working on the conversion of the low energy neutron transport program MORSE. These programs are used heavily at Oak Ridge (Gabriel and coworkers) for cascade studies. For silicon calorimetry one wants to have more control over the energy deposition routines, especially in MORSE. Unfortunately, MORSE is heavily-laden with machine code, and its conversion is going slowly. 11 refs., 5 figs

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.

Experimental analysis on physical and mechanical properties of thermal shock damage of granite

Directory of Open Access Journals (Sweden)

He Xiao

2017-01-01

Full Text Available The purpose of this study was to explore the changes of mechanical and physical properties of granite under different thermal loading effects. Uniaxial compression experiments studying the rules of the influence of temperature load on mechanical properties of granite were carried out. After high-temperature heating at above 600 °C, granite tended to have stronger ductility and plasticity as well as declined peak stress and compressive strength. Thermogravimetry - differential scanning calorimetry (TG-DSC analysis results showed that, thermal load at different temperatures induced reactions such as water loss, oxidation and crystallization in the microstructure of granite, which led to physical changes of granite. Hence it is concluded that, heating can significantly weaken the mechanical performance of granite, which provides an important support for the optimization of heating assisted processing of granite. It also reveals that, heating assisted cutting technique can effectively lower energy consumption and improve processing efficiency.

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

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

Kissinger method applied to the crystallization of glass-forming liquids: Regimes revealed by ultra-fast-heating calorimetry

Energy Technology Data Exchange (ETDEWEB)

Orava, J., E-mail: jo316@cam.ac.uk [Department of Materials Science & Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); WPI-Advanced Institute for Materials Research (WPI-AIMR), Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan); Greer, A.L., E-mail: alg13@cam.ac.uk [Department of Materials Science & Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom); WPI-Advanced Institute for Materials Research (WPI-AIMR), Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577 (Japan)

2015-03-10

Highlights: • Study of ultra-fast DSC applied to the crystallization of glass-forming liquids. • Numerical modeling of DSC traces at heating rates exceeding 10 orders of magnitude. • Identification of three regimes in Kissinger plots. • Elucidation of the effect of liquid fragility on the Kissinger method. • Modeling to study the regime in which crystal growth is thermodynamically limited. - Abstract: Numerical simulation of DSC traces is used to study the validity and limitations of the Kissinger method for determining the temperature dependence of the crystal-growth rate on continuous heating of glasses from the glass transition to the melting temperature. A particular interest is to use the wide range of heating rates accessible with ultra-fast DSC to study systems such as the chalcogenide Ge{sub 2}Sb{sub 2}Te{sub 5} for which fast crystallization is of practical interest in phase-change memory. Kissinger plots are found to show three regimes: (i) at low heating rates the plot is straight, (ii) at medium heating rates the plot is curved as expected from the liquid fragility, and (iii) at the highest heating rates the crystallization rate is thermodynamically limited, and the plot has curvature of the opposite sign. The relative importance of these regimes is identified for different glass-forming systems, considered in terms of the liquid fragility and the reduced glass-transition temperature. The extraction of quantitative information on fundamental crystallization kinetics from Kissinger plots is discussed.

Kissinger method applied to the crystallization of glass-forming liquids: Regimes revealed by ultra-fast-heating calorimetry

International Nuclear Information System (INIS)

Orava, J.; Greer, A.L.

2015-01-01

Highlights: • Study of ultra-fast DSC applied to the crystallization of glass-forming liquids. • Numerical modeling of DSC traces at heating rates exceeding 10 orders of magnitude. • Identification of three regimes in Kissinger plots. • Elucidation of the effect of liquid fragility on the Kissinger method. • Modeling to study the regime in which crystal growth is thermodynamically limited. - Abstract: Numerical simulation of DSC traces is used to study the validity and limitations of the Kissinger method for determining the temperature dependence of the crystal-growth rate on continuous heating of glasses from the glass transition to the melting temperature. A particular interest is to use the wide range of heating rates accessible with ultra-fast DSC to study systems such as the chalcogenide Ge 2 Sb 2 Te 5 for which fast crystallization is of practical interest in phase-change memory. Kissinger plots are found to show three regimes: (i) at low heating rates the plot is straight, (ii) at medium heating rates the plot is curved as expected from the liquid fragility, and (iii) at the highest heating rates the crystallization rate is thermodynamically limited, and the plot has curvature of the opposite sign. The relative importance of these regimes is identified for different glass-forming systems, considered in terms of the liquid fragility and the reduced glass-transition temperature. The extraction of quantitative information on fundamental crystallization kinetics from Kissinger plots is discussed

Kinetics of dihydro-dibenz[b,f]azepine derivatives sublimation

International Nuclear Information System (INIS)

Krongauz, V.V.; Ling, M.T.K.; Woo, L.; Purohit, U.

2007-01-01

Sublimation of dihydro-dibenz[b,f]azepine derivatives upon heating was studied and confirmed by thermogravimetry (TGA) and differential scanning calorimetry (DSC). DSC was used to analyze thermodynamics of melting. The kinetics of dihydro-dibenz[b,f]azepine derivatives sublimation were monitored by TGA as a function of temperature. Activation energies of sublimation were deduced and correlated with melting enthalpies and molecular structure. The results indicated that the sublimation was controlled by intermolecular forces in the crystalline lattice of dihydro-dibenz[b,f]azepine derivatives

Effect of tellurium on viscosity and liquid structure of GaSb melts

Energy Technology Data Exchange (ETDEWEB)

Ji Leilei [School of Material Science and Engineering, Jinan University, Jinan 250022 (China); Geng Haoran [School of Material Science and Engineering, Jinan University, Jinan 250022 (China)], E-mail: mse_genghr@ujn.edu.cn; Sun Chunjing [Key Laboratory of Liquid Structure and Heredity of Materials, Ministry of Education, Shandong University, Jinan 250061 (China); Teng Xinying; Liu Yamei [School of Material Science and Engineering, Jinan University, Jinan 250022 (China)

2008-04-03

The behavior of GaSb melt with tellurium addition was investigated using viscometer and differential scanning calorimetry (DSC). Normally, the viscosity of all melts measured decreased with the increasing temperature. However, anomalous transition points were observed in the temperature dependence of viscosity for Ga-Sb-Te system. Corresponded with the abnormal points on the viscosity-temperature curves, there were thermal effect peaks on the DSC curves. Furthermore, viscous activation energy and flow units of these melts and their structural features were discussed in this paper.

The archaeometry study of the chemical and mineral composition of pottery from Brazil's Northeast

International Nuclear Information System (INIS)

Santos, J.O.; Santos, J.O.; Munita, C.S.; Toyota, R.G.; Oliveira, P.M.S.; Vergne, C.; Silva, R.S.

2009-01-01

Chemical and mineralogical analysis was performed on ceramics and clay samples from Barracao archaeological site located in Baixo Sao Francisco River by means of instrumental neutron activation analysis (INAA) and by differential scanning calorimetry (DSC). The data set was studied by means of cluster analysis (CA) and discriminant analysis (DA). The results showed that the raw material used in ceramics is not local. By using DSC it was possible to discover that the principal minerals in the samples are quartz, feldspars, mica and kaolinite. (author)

Chain Extension and Thermal Behavior of Recycled Poly(Ethylene Terephthalate Modified by Reactive Extrusion with Triphenyl Phosphite

Directory of Open Access Journals (Sweden)

Qin Dan

2016-01-01

Full Text Available Reactive extrusion experiments of recycled PET fabrics (R-PET were carried out in a Haake torque rheometer with triphenyl phosphite (TPP and thermal behavior of modified R-PET was investigated by differential scanning calorimetry (DSC. The reaction mechanism which TPP acts as a cross-linker is verified by the experiment of phosphorus elemental analysis. DSC results show the presence of reaction residues may not modify melting temperature Tm and crystallization temperature Tc is controlled by the combined effect of molecular weight and reaction residues.

Thermal Analysis On The Kinetics Of Magnesium-Aluminum Layered Double Hydroxides In Different Heating Rates

Directory of Open Access Journals (Sweden)

Hongbo Y.

2015-06-01

Full Text Available The thermal decomposition of magnesium-aluminum layered double hydroxides (LDHs was investigated by thermogravimetry analysis and differential scanning calorimetry (DSC methods in argon environment. The influence of heating rates (including 2.5, 5, 10, 15 and 20K/min on the thermal behavior of LDHs was revealed. By the methods of Kissinger and Flynn-Wall-Ozawa, the thermal kinetic parameters of activation energy and pre-exponential factor for the exothermic processes under non-isothermal conditions were calculated using the analysis of corresponding DSC curves.

Influence of Si concentration on the precipitation in Al-1 at.% Mg alloy

Energy Technology Data Exchange (ETDEWEB)

Afify, N. [Physics Department, Faculty of Science, Assiut University, Assiut 71516 (Egypt)], E-mail: afify@aun.edu.eg; Gaber, A.; Mostafa, M.S.; Abbady, Gh. [Physics Department, Faculty of Science, Assiut University, Assiut 71516 (Egypt)

2008-08-25

The aging processes in Al-Mg-Si alloys have been studied by using differential scanning calorimetry (DSC), microhardness measurements (HV) and X-ray diffraction (XRD). Five processes have been detected by the DSC curves and HV behaviour. In the DSC curves, four exothermic and one endothermic reactions are developed. The sequence of processes are Guinier-Preston (G.P.) zones, dissolution of the G.P. zones, intermediate precipitation of {beta}''-phase, precipitation of {beta}'-phase and precipitation of the stable {beta}-phase + Si particles. The activation energies associated with the processes have been determined by using Kissinger method. Consequently, the nucleation mechanism of the precipitates can be explained. These phases are confirmed by XRD analysis.

Pressurization effects on the polymorphic forms of famotidine

International Nuclear Information System (INIS)

Nemet, Zoltan; Hegedues, Bela; Szantay, Csaba; Sztatisz, Janisz; Pokol, Gyoergy

2005-01-01

The effects of high static pressure on the polymorphic modifications A and B of famotidine were examined by differential scanning calorimetry, infrared and Raman spectroscopy, and X-ray powder diffractometry. The obtained effects appeared to differ significantly depending on whether they were monitored by DSC or any of the other above techniques. In particular, DSC measurements tend to deceptively amplify a tendency of the pure modification B to turn into the more stable form A under pressurization, while the spectroscopic methods and XRPD exhibit no essential change in the crystal structure of the metastable form B. The apparent morphological transformation in the pressed samples stems from the nature of the DSC method itself

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 ...

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

Revised final report for tank 241-AN-101, grab samples 1AN-95-1 through 1AN-95-7. Revision 1

International Nuclear Information System (INIS)

Esch, R.A.

1996-01-01

Six supernate grab samples and one field blank were taken from tank 241-AN-101. This report documents analyses performed in support of the Safety Screening program: differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), density by specific gravity (Sp.G.), and total alpha activity (AT)

Interactions in a blend of two polymers greatly differing in glass transition temperature

Czech Academy of Sciences Publication Activity Database

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

2011-01-01

Roč. 49, č. 14 (2011), s. 1031-1040 ISSN 0887-6266 Institutional research plan: CEZ:AV0Z40500505 Keywords : differential scanning calorimetry (DSC) * fouriertransform infrared spectroscopy (FT-IR) * glass transition temperature Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.531, year: 2011

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

African Journals Online (AJOL)

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

Development of Chitosan Acetate Films for Transdermal Delivery of ...

African Journals Online (AJOL)

Methods: Chitosan acetate was chemically modified with acetaldehyde and the solution was prepared with 1 % acetic acid, in which was dissolved propranolol hydrochloride, was cast as films in Petri dish and characterised by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC) and ...

Formulation and Evaluation of Spray-Dried Esomeprazole ...

African Journals Online (AJOL)

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

The Synthesis of Novel Enclathration Compounds : Bis(9-amino-9 ...

African Journals Online (AJOL)

The stability of the clathrate complexes has been investigated by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Competition experiments were carried out with the compounds that successfully hosted solvent molecules in order to determine their relative affinity for these solvents. One of the ...

Physicochemical properties of nanoparticles titania from alcohol ...

African Journals Online (AJOL)

The synthesized TiO2 were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal analysis (thermogravimetric analysis, TGA, and differential scanning calorimetry, DSC), and surface area Brunauer–Emmett–Teller (BET) method. The photocatalytic activity of TiO2 nanoparticles was ...

Inclusion Mechanism and Heat Stability of the Complex of 4 ...

African Journals Online (AJOL)

The physicochemical properties of the complex were evaluated by Fourier transform infrared spectroscopy (FT-IR) and x-ray diffractometry (XRD) while the heat stability of the complex was measured by thermogravimetric/differential scanning calorimetry (TG/DSC). Results: The stability constants of the complexes were ...

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

DEFF Research Database (Denmark)

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

2014-01-01

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

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...

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

Direct calorimetry of free-moving eels with manipulated thyroid status

Science.gov (United States)

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

2007-02-01

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

Indirect calorimetry in nutritional therapy. A position paper by the ICALIC study group.

Science.gov (United States)

Oshima, Taku; Berger, Mette M; De Waele, Elisabeth; Guttormsen, Anne Berit; Heidegger, Claudia-Paula; Hiesmayr, Michael; Singer, Pierre; Wernerman, Jan; Pichard, Claude

2017-06-01

This review aims to clarify the use of indirect calorimetry (IC) in nutritional therapy for critically ill and other patient populations. It features a comprehensive overview of the technical concepts, the practical application and current developments of IC. Pubmed-referenced publications were analyzed to generate an overview about the basic knowledge of IC, to describe advantages and disadvantages of the current technology, to clarify technical issues and provide pragmatic solutions for clinical practice and metabolic research. The International Multicentric Study Group for Indirect Calorimetry (ICALIC) has generated this position paper. IC can be performed in in- and out-patients, including those in the intensive care unit, to measure energy expenditure (EE). Optimal nutritional therapy, defined as energy prescription based on measured EE by IC has been associated with better clinical outcome. Equations based on simple anthropometric measurements to predict EE are inaccurate when applied to individual patients. An ongoing international academic initiative to develop a new indirect calorimeter aims at providing innovative and affordable technical solutions for many of the current limitations of IC. Indirect calorimetry is a tool of paramount importance, necessary to optimize the nutrition therapy of patients with various pathologies and conditions. Recent technical developments allow broader use of IC for in- and out-patients. Copyright © 2016 Elsevier Ltd and European Society for Clinical Nutrition and Metabolism. All rights reserved.

Bronsted acid site number evaluation using isopropylamine decomposition on Y-zeolite contaminated with vanadium in a simultaneous DSC-TGA analyzer

International Nuclear Information System (INIS)

Osorio Perez, Yonnathan; Forero, Liliam Alexandra Palomeque; Torres, Diana Vanessa Cristiano; Trujillo, Carlos Alexander

2008-01-01

Acid-site catalyzed decomposition of isopropylamine was followed in a simultaneous DSC-TGA analyzer. USY zeolite samples with and without vanadium were studied. Results show that acid sites number decreases linearly with vanadium concentration in zeolite indicating that vanadium neutralizes acid sites on catalyst and the metal is able to move on the surface of the solid. The neutralizing species probably contain only one vanadium atom. The reaction enthalpy plus desorption heat of the products show that vanadium preferentially neutralizes the strongest acid sites on the zeolite. The application of the simultaneous DSC-TGA technique to quantify Bronsted acid sites on solids by this reaction is novel

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 .

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

Use of isothermal titration calorimetry to study the interaction of short-chain alcohols with lipid membranes

DEFF Research Database (Denmark)

Trandum, Christa; Westh-Andersen, Peter; Jørgensen, Kent

1999-01-01

of short-chain alcohols on Lipid bilayers. isothermal titration calorimetry (ITC) has been used to determine the energy involved in the association of the alcohols with lipid bilayers. Pure unilamellar DMPC liposomes and DMPC liposomes incorporated with different amounts of cholesterol, sphingomyelin...... dependent on the lipid bilayer composition. In the presence of high concentrations of cholesterol, the binding enthalpy of ethanol is decreased, whereas the presence of ceramides enhances the enthalpic response of the lipid bilayer to ethanol. Isothermal titration calorimetry offers a new methodology...

Effect of the Cu and Ni content on the crystallization temperature and crystallization mechanism of La–Al–Cu(Ni metallic glasses

Directory of Open Access Journals (Sweden)

Peiyou Li

2016-02-01

Full Text Available The effect of the Cu and Ni content on the crystallization mechanism and the crystallization temperatures of La–Al–Cu(Ni metallic glasses (MGs was studied by differential scanning calorimetry (DSC. The experimental results have shown that the DSC curves obtained for the La–Al–Cu and La–Al–Ni MGs exhibit two and three crystallization temperatures, respectively. The crystallization temperatures of the La–Al–Cu and La–Al–Ni MGs result from the merging and splitting of thermal events related to the corresponding eutectic atomic pairs in the La72Cu28 and La81.6Al18.4 MGs, and La72Ni28 and La81.6Al18.4 MGs, respectively. In addition, Al- and Ni-containing clusters with weak or strong atomic interaction in the Al–Ni atomic pairs strongly affect the crystallization mechanism and thus the crystallization temperature of La–Al–Ni MGs. This study provides a novel understanding of the relation between the crystallization temperature and the underlying crystallization mechanisms in La–Al–Cu(Ni MGs.

The phase diagram of KNO3-KClO3

International Nuclear Information System (INIS)

Zhang Xuejun; Tian Jun; Xu Kangcheng; Gao Yici

2004-01-01

The binary phase diagram of KNO 3 -KClO 3 is studied by means of differential scanning calorimetry (DSC) and high-temperature X-ray diffraction. The limited solid solutions, K(NO 3 ) 1-x (ClO 3 ) x (0 3 ) 1-x (ClO 3 ) x (0.90 3 -based solid solutions and KClO 3 -based solid solutions phase, respectively. For KNO 3 -based solid solutions, KNO 3 ferroelectric phase can be stable from 423 to 223 K as a result of substituting of NO 3 by ClO 3 -radicals. The temperatures for solidus and liquidus have been determined based on limited solid solutions. Two models, Henrian solution and regular solution theory for KNO 3 -based (α) phase and KClO 3 -based (β) phase, respectively, are employed to reproduce solidus and liquidus of the phase diagram. The results are in good agreement with the DSC data. The thermodynamic properties for α and β solid solutions have been derived from an optimization procedure using the experimental data. The calculated phase diagram and optimized thermodynamic parameters are thermodynamically self-consistent

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.

Nanostructured Catalytic Hybrid Materials for Energy Conversion or Storage

Science.gov (United States)

2017-08-27

and 6) and characterized them using bomb calorimetry, DSC and XRD. - We are organizing the data to make research articles and patents . [Iron...nanofibers: Control on hydrogen generation kinetics In preparation [ Patents ] We have a plan to submit patents (regarding the second and third publications) to

New liquid crystals in the series of 1, 3, 5-triazine compounds ...

African Journals Online (AJOL)

The Series of compounds were prepared by nucleophilic addition of the primary amino nucleophile to 1,3,5-triazine electrophilic ring via alkyl spacers in presence of potassium carbonate as hydrochloride acceptor. Differencial scanning calorimetry (DSC), polarizing optical microscopy and x-ray diffraction confirmed Smectic ...

Formulation and evaluation of matrix microspheres for simultaneous ...

African Journals Online (AJOL)

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

Crystallization and melting behavior of multi-walled carbon nanotube-reinforced nylon-6 composites

NARCIS (Netherlands)

Phang, In Yee; Ma, Jianhua; Shen, Lu; Liu, Tianxi; Zhang, Wei-De

2006-01-01

The crystallization and melting behavior of neat nylon-6 (PA6) and multi-walled carbon nanotubes (MWNTs)/PA6 composites prepared by simple melt-compounding was comparatively studied. Differential scanning calorimetry (DSC) results show two crystallization exotherms (TCC, 1 and TCC, 2) for PA6/MWNTs

Structure and mechanical properties of Al-3Fe rapidly solidified alloy

International Nuclear Information System (INIS)

Karakoese, Ercan; Keskin, Mustafa

2011-01-01

The Al based Al-3 wt%Fe alloy was prepared by conventionally casting (ingot) and further processed the melt-spinning technique and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) together with energy dispersive spectroscopy (EDS), differential scanning calorimetry (DSC) and the Vickers microhardness tester. The rapidly solidified (RS) binary alloys were composed of supersaturated α-Al solid solution and finely dispersed intermetallic phases. Experimental results showed that the mechanical properties of RS alloys were enhanced, which can be attributed to significant changes in the microstructure. The dependence of microhardness H V on the solidification rate (V) was analysed. These results showed that with the increasing values of V, the values of H V increased.

Prediction of phase equilibria and thermal analysis in the Bi-Cu-Pb ternary system

Energy Technology Data Exchange (ETDEWEB)

Manasijevic, Dragan [University of Belgrade, Technical Faculty, VJ 12, 19210 Bor (Serbia); Mitovski, Aleksandra, E-mail: amitovski@tf.bor.ac.rs [University of Belgrade, Technical Faculty, VJ 12, 19210 Bor (Serbia); Minic, Dusko [University of Pristina, Faculty of Technical Sciences, 38220 Kosovska Mitrovica (Serbia); Zivkovic, Dragana; Marjanovic, Sasa [University of Belgrade, Technical Faculty, VJ 12, 19210 Bor (Serbia); Todorovic, Radisa [Institute of Mining and Metallurgy, Zeleni Bulevar 35, 19210 Bor (Serbia); Balanovic, Ljubisa [University of Belgrade, Technical Faculty, VJ 12, 19210 Bor (Serbia)

2010-05-20

The knowledge about phase diagram of the Bi-Cu-Pb ternary system is of importance in development of copper-lead based bearing materials, soldering and in refining of copper and lead. In this work, the phase diagram of the Bi-Cu-Pb ternary system was calculated by the CALPHAD method using binary thermodynamic parameters included in the COST 531 database. The results include liquidus projection, invariant equilibria and three vertical sections with molar ratio Cu:Pb = 1, Cu:Pb = 1:3 and Bi:Cu = 1. Alloys, with compositions along three predicted vertical sections, were measured using differential scanning calorimetry (DSC). The experimentally determined phase transition temperatures were compared with calculated results and good mutual agreement was noticed.

Prediction of phase equilibria and thermal analysis in the Bi-Cu-Pb ternary system

International Nuclear Information System (INIS)

Manasijevic, Dragan; Mitovski, Aleksandra; Minic, Dusko; Zivkovic, Dragana; Marjanovic, Sasa; Todorovic, Radisa; Balanovic, Ljubisa

2010-01-01

The knowledge about phase diagram of the Bi-Cu-Pb ternary system is of importance in development of copper-lead based bearing materials, soldering and in refining of copper and lead. In this work, the phase diagram of the Bi-Cu-Pb ternary system was calculated by the CALPHAD method using binary thermodynamic parameters included in the COST 531 database. The results include liquidus projection, invariant equilibria and three vertical sections with molar ratio Cu:Pb = 1, Cu:Pb = 1:3 and Bi:Cu = 1. Alloys, with compositions along three predicted vertical sections, were measured using differential scanning calorimetry (DSC). The experimentally determined phase transition temperatures were compared with calculated results and good mutual agreement was noticed.

High temperature drop calorimetric studies on La6UO12 and Nd6UO12

International Nuclear Information System (INIS)

Babu, R.; Senapati, A.; Rao, G.J.; Venkata Krishnan, R.; Ananthasivan, K.; Nagarajan, K.

2014-01-01

Rare earth elements produced in the reactor during irradiation can interact with the fuel. Under transient conditions, compounds of formula, RE 6 UO 12 with rhombohedral crystal structure are expected to be formed. Hence, thermodynamic properties of these compounds are useful in interpreting the behaviour of fuels during irradiation. Thermal expansion and heat capacities by DSC have been reported for La 6 UO 12 and Nd 6 UO 12 . There are no experimentally measured values of enthalpy. Hence, measurements on enthalpy increments of La 6 UO 12 and Nd 6 UO 12 were carried out for the first time by inverse drop calorimetry in the temperature range 534-1738 K and computed the thermodynamic functions

Síntese e caracterização de nanocompósitos de poliestireno/hidroxissal lamelar

Directory of Open Access Journals (Sweden)

Samara Boaventura de Moraes

2014-01-01

Full Text Available Polystyrene/layered hydroxide salt (LHS modified with sodium dodecyl sulfate was synthesized by in situ polymerization. The materials synthesized were characterized by gravimetry, X-ray diffraction (XRD, thermogravimetry analyses (TGA, differential scanning calorimetry (DSC and the flammability test (FT. XRD demonstrated that synthesized nanocomposites in all compositions studied showed poor global dispersion of LHS in polystyrene. TGA showed a slight decrease in thermal stability. DSC curves showed that the glass transition temperature of polystyrene and nanocomposites were similar. The FT showed that the nanocomposite with low load of LHS exhibited good results.

Synthesis and characteristics of composite phase change humidity control materials

DEFF Research Database (Denmark)

Qin, Menghao; Chen, Zhi

2017-01-01

) and the thermal gravimetric analysis (TGA) were used to determine the thermal properties and thermal stability. Both the moisture transfer coefficient and moisture buffer value (MBV) of different PCHCMs were measured by the improved cup method. The DSC results showed that the SiO2 shell can reduce the super...... synthesized with methyl triethoxysilane by the sol–gel method. The vesuvianite, sepiolite and zeolite were used as hygroscopic materials. The scanning electron microscopy (SEM) was used to measure the morphology profiles of the microcapsules and PCHCM. The differential scanning calorimetry (DSC...

Synthesis of Amorphous Powders of Ni-Si and Co-Si Alloys by Mechanical Alloying

Science.gov (United States)

Omuro, Keisuke; Miura, Harumatsu

1991-05-01

Amorphous powders of the Ni-Si and Co-Si alloys are synthesized by mechanical alloying (MA) from crystalline elemental powders using a high energy ball mill. The alloying and amorphization process is examined by X-ray diffraction, differential scanning calorimetry (DSC), and scanning electron microscopy. For the Ni-Si alloy, it is confirmed that the crystallization temperature of the MA powder, measured by DSC, is in good agreement with that of the powder sample prepared by mechanical grinding from the cast alloy ingot products of the same composition.

Radiochemical ageing of epoxy coating for nuclear plants

International Nuclear Information System (INIS)

Queiroz, D.P.R.; Fraisse, F.; Fayolle, B.; Kuntz, M.; Verdu, J.

2010-01-01

The degradation of an epoxy-amine network exposed to gamma irradiation in oxygen atmosphere has been studied by using a variety of analytical methods, including infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and sol-gel analysis. Results show that the oxidation of epoxy systems grows with the irradiation dose. Hydroperoxides, which are species resulting from oxidation, were identified and quantified by DSC. As indicated by the sol-gel analysis, the mechanism of degradation of chain scission seems to be predominant over crosslinking. The modifications induced by irradiation reflect in a greater capacity of water absorption.

Features of the Valorization of Single and Double Based Powders for Codetonation in Emulsion Explosives

Science.gov (United States)

Ribeiro, Jose; Mendes, Ricardo; Tavares, Bruno; Louro, Cristina

2013-06-01

In this work, features of the thermal and detonation behavior of compositions resulting from the mixture of single and double based gun powder within ammonium nitrate (AN) based emulsion explosives are shown. That includes results of thermodynamic-equilibrium calculations of the detonation velocity, the chemical compatibility assessment through differential scanning calorimetry [DSC] and thermo gravimetric analysis [TGA], the experimental determination of the detonation velocity and a comparative evaluation of the shock sensitivity using a modified version of the ``gap-test''. DSC/TGA results for the compositions and for the individual components overlap until the beginning of the thermal decomposition which is an indication of the absence of formation of any new chemical specimens and so of the capability of the composition components. After the beginning of the thermal decomposition it can be seen that the rate of mass loss is much higher for the compositions with gun powder than for the sole emulsion explosive. Both, theoretical and experimental, values of the detonation velocity have shown to be higher for the powdered compositions than for the pure emulsion explosive. Shock sensitivity assessment have ended-up with a slightly bigger sensitivity for the compositions with double based gun powder when compared to the single based compositions or to the pure emulsion.

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

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.

Benchmark thermodynamic properties of methylanisoles: Experimental and theoretical study

International Nuclear Information System (INIS)

Emel’yanenko, Vladimir N.; Zaitseva, Ksenia V.; Agapito, Filipe; Martinho Simões, José A.; Verevkin, Sergey P.

2015-01-01

Highlights: • Thermochemistry of 2-, 3-, and 4-methylanisoles was studied. • Liquid state enthalpies of formation were measured by calorimetry. • Vaporisation enthalpies were derived from by transpiration method. • Ab initio enthalpies of formation are in excellent agreement with experiment. • A new paradigm for obtaining thermochemistry of liquid compounds was suggested. - Abstract: Accurate standard molar enthalpy of formation values in the liquid phase can be obtained by combining high-level quantum chemistry values of gas-phase enthalpies of formation with experimentally determined enthalpies of vaporisation. The procedure is illustrated for 2-, 3-, and 4-methyl-anisoles. Using the W1-F12 and G4 quantum-chemical methods, the gas-phase enthalpies of formation of these compounds at T = 298.15 K were computed. Molar enthalpies of vaporisation for these isomers were measured by the transpiration method. Combining the experimental and the high-level ab initio values, the standard molar enthalpies of formation in the liquid phase for all three isomers were derived and compared with those determined for 2- and 4-methyl-anisoles by using combustion calorimetry

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)

Microstructural response of an Al-modified Ni-Cr-Fe ternary alloy during thermal processing

Energy Technology Data Exchange (ETDEWEB)

Akinlade, D.A. [Department of Mechanical and Manufacturing Engineering, University of Manitoba, Winnipeg, MB (Canada)], E-mail: dotun172@yahoo.co.uk; Caley, W.F. [Department of Process Engineering and Applied Science, Dalhousie University, Halifax, NS (Canada); Richards, N.L.; Chaturvedi, M.C. [Department of Mechanical and Manufacturing Engineering, University of Manitoba, Winnipeg, MB (Canada)

2008-07-15

A thermodynamic package was used to predict the phase transformations that occurred during thermal processing of a superalloy based on the composition of a ternary Ni-Cr-Fe alloy. The effect of the addition of 6 w/o Al on phase transformation in the material sintered were estimated and compared with results obtained experimentally by X-ray diffraction and metallography, while the transformation temperature of the modified alloy was corroborated by differential scanning calorimetry (DSC). Mechanical property of the alloy was estimated in terms of Vickers hardness. These results suggest that despite potential problems encountered in high-temperature powder processing of superalloys that often tend to influence the feasibility of using thermodynamic predictions to model such alloy systems, the software and predictions used in this study offer a way to simulate both design and characterisation of the experimental alloy.

Thermal, magnetic, and structural properties of soft magnetic FeCrNbCuSiB alloy ribbons

International Nuclear Information System (INIS)

Rosales-Rivera, A.; Valencia, V.H.; Quintero, D.L.; Pineda-Gomez, P.; Gomez, M.

2006-01-01

The thermal, magnetic and structural properties of amorphous magnetic Fe 73.5-x Cr x Nb 3 Cu 1 Si 13.5 B 9 alloy ribbons, with x=0, 2, 4, 6, 8, and 10, were studied by using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), magneto-impedance measurements and X-ray diffraction (XRD). The ribbons exhibit ultrasoft magnetic behavior, especially giant magneto-impedance effect, GMI. A three-peak behavior was observed in GMI curves. Particular attention has been given to observation of crystallization kinetics via DSC and TGA. The primary crystallization T pcr , and Curie T c , temperatures were determined from DSC and TGA data, respectively. The effect of partial substitution of iron by Cr on the thermal and magnetic properties is discussed

Preparation of continuous alumina gel fibres by aqueous sol–gel ...

Indian Academy of Sciences (India)

Abstract. Continuous alumina gel fibres were prepared by sol–gel method. The spinning sol was prepared by mixing aluminum nitrate, lactic acid and polyvinylpyrrolidone with a mass ratio of 10:3:1·5. Thermogravimetry– differential scanning calorimetry (TG–DSC), Fourier transform infrared (FTIR) spectra, X-ray diffraction ...

Modulation of gephyrin-glycine receptor affinity by multivalency

DEFF Research Database (Denmark)

Maric, Hans-Michael; Kasaragod, Vikram Babu; Schindelin, Hermann

2014-01-01

. A 2 Å crystal structure of the C-terminal domain of gephyrin (GephE) in complex with a 15-residue peptide derived from the GlyR β-subunit defined the core binding site, which we targeted with the dimeric peptide. Biophysical analyses via differential scanning calorimetry (DSC), thermofluor...

Preparation and Characterization of Sugar Cane Wax Microspheres ...

African Journals Online (AJOL)

HP

scanning calorimetry (DSC) as well as for drug loading, and in vitro and in vivo release in albino sheeps. Results: SEM images .... Rolex, India), and the sphericity factor (S) was calculated using ... using a fully validated high performance liquid ... Pharmacokinetic and data analysis ... microspheres exerts an influence on the.