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1.
Reproducible specific heat capacities (C p) of triglycerides can be obtained by using heat-flux DSC under improved operating conditions. The improved operating parameters, such as the scanning rate, the sample mass and the atmosphere within the DSC chamber, were established via statistical analysis of the experimental data with trilaurin as a sample. The specific heat capacity results on trilaurin were compared with the values calculated by using estimation methods. The precision of the specific heat capacity measured for trilaurin under these conditions was within ±1%. 相似文献
2.
D. J. Hourston M. Song H. M. Pollock A. Hammiche 《Journal of Thermal Analysis and Calorimetry》1997,49(1):209-218
Modulated-temperature differential scanning calorimetry was used to measure the glass transition temperature,T
g, the heat capacity relaxation in the glassy state and the increment of heat capacity, Cp, in the glass transition region for several polymers. The differential of heat capacity with respect to temperature was used to analyseT
g and Cp simply and accurately. These measurements are not affected by complex thermal histories. 相似文献
3.
Guoan Zhu Changtai Tian Jimin Zheng 《Journal of Thermal Analysis and Calorimetry》1995,45(1-2):269-273
The specific heat capacity of M·NBA·DEA crystals were measured by differential scanning calorimetry. Both the direct and ratio methods of DSC were used in the determinations. The relative average deviations are 0.08% to 0.18%. The relative average deviations of ratio method are 0.23–0.69%. 相似文献
4.
The heat capacity of fluorinated propane and butane derivatives by differential scanning calorimetry
Sun -Hee Hwang D. D. DesMarteau A. L. Beyerlein N. D. Smith P. Joyner 《Journal of Thermal Analysis and Calorimetry》1992,38(11):2515-2528
The constant pressure liquid-phase heat capacities of 21 hydrogen containing fluorinated propane and butane derivatives and one fluorinated ether (CF3OCF2H) with boiling points ranging from -34.6° to 76.7°C have been measured to 3% accuracy by differential scanning calorimetry at 40°C. The measurements are needed to help identify alternative refrigerants and blowing agents that do not deplete the stratospheric ozone layer. The DSC method has two significant advantages for this purpose, which are:
Mittels DSC bei 40°C wurden die Flüssigphasen-Wärmekapazitäten für konstanten Druck von 21 wasserstoffhaltigen fluorierten Propan- und Butanderivaten und von einem fluorierten Ether (CF3OCF2H) mit Siedenpunkten zwischen -34.6° und 76.7°C gemessen. Diese Messungen dienen der Suche nach alternativen Kühl- und Treibmitteln, welche die Ozonschicht der Stratosphäre nicht mindern. Für diese Aufgabe hat die DSC-Methode zwei eindeutige Vorteile:
This work was supported jointly by the U.S. Environmental Protection Agency's Stratospheric Ozone Protection Branch at Research Triangle Park, North Carolina and the Electric Power Research Institute at Palo Alto, California. 相似文献
(i) | only small samples (less than 100 mg) are required, and |
(ii) | the instruments are available in many laboratories and can be used for the heat capacity measurement of liquids with subambient boiling points without modification or special accessories. |
(i) | es werden nur geringe Probenmengen benötigt (weniger als 100 mg) und |
(ii) | die Geräte sind in vielen Laboratorien zugänglich und können ohne Ånderungen zur Messung von Wärmekapazitäten von Flüssigkeiten mit Siedepunkten unter Umgebungstemperatur verwendet werden. |
This work was supported jointly by the U.S. Environmental Protection Agency's Stratospheric Ozone Protection Branch at Research Triangle Park, North Carolina and the Electric Power Research Institute at Palo Alto, California. 相似文献
5.
《Fluid Phase Equilibria》2006,244(1):68-77
Heat capacities for nine ionic liquids (IL) have been determined with the “three-step” method using two different differential scanning calorimeters (DSC). In addition, the heat capacities of these ionic liquids have been studied by the modulated-temperature differential scanning calorimetry (MDSC™). The measurements cover a temperature range from 315 to 425 K. 相似文献
6.
B. Wunderlich 《Journal of Thermal Analysis and Calorimetry》1997,48(2):207-224
Modulated differential scanning calorimetry (MDSC) uses an abbreviated Fourier transformation ?r the data analysis and separation of the reversing component of the heat flow and temperature signals. In this paper a simple spread-sheet analysis will be presented that can be used to better understand and explore the effects observed in MDSC and their link to actual changes in the instrument and sample. The analysis assumes that instrument lags and other kinetic effects are either avoided or corrected for. 相似文献
7.
Randall K. Weese 《Thermochimica Acta》2005,429(1):119-123
An investigation of the use of modulated differential scanning calorimeter (MDSC) to measure thermal conductivity (κ) of the explosive Tetryl using isothermal and non-isothermal methods. Issues surrounding the use of silicone oil as a heat transfer aid are discussed. Using these methods the calculated isothermal and non-isothermal properties of specific heat capacity were observed to be 0.844 and 0.863 J/(g K) and the calculated thermal conductivity values were found to be 0.165 and 0.186 W/K. Calibration experiments using polystyrene indicate that the non-isothermal method is more reproducible but has a larger offset (35%) from the true value. Our corrected values for Tetryl fall in the middle of the considerable range of values reported in the literature. 相似文献
8.
Christian P. Camirand 《Thermochimica Acta》2004,417(1):1-4
A technique of measurement of thermal conductivity of solid materials by differential scanning calorimetry is presented. It concerns small samples having a diameter less than 8.0 mm, a height less than 2.0 mm and a low thermal conductivity. This method requires many samples with different heights which are heated in such a way that a calibration substance put on their top undergoes a first-order phase transition. The analysis of heat transfer of a such experiment predicts that the slope of the differential power during the transition is proportional to the factor 2 and inversely proportional to the sum of the thermal resistances. A measurement of the thermal conductivity of samples made of polytetrafluoroethylene powder, compressed at the density of 2.10±0.03 g cm−3, has been performed; the value obtained is 0.33±0.02 W m−1 K−1. Measurements of thermal conductivity of small metal hydride pellets are also presented. The precision of the measurements are on average 10%. 相似文献
9.
The quality of measurement of heat capacity by differential scanning calorimetry (DSC) is based on strict symmetry of the twin calorimeter. This symmetry is of particular importance for temperature-modulated DSC (TMDSC) since positive and negative deviations from symmetry cannot be distinguished in the most popular analysis methods. The heat capacities for sapphire-filled and empty aluminum calorimeters (pans) under designed cell imbalance caused by different pan-masses were measured. In addition, the positive and negative signs of asymmetry have been explored by analyzing the phase-shift between temperature and heat flow for sapphire and empty runs. The phase shifts change by more than 180° depending on the sign of the asymmetry. Once the sign of asymmetry is determined, the asymmetry correction for temperature-modulated DSC can be made.On leave from Toray Research Center, Inc., Otsu, Shiga 520, JapanThis work was supported by the Division of Materials Research, National Science Foundation, Polymers Program, Grant # DMR 90-00520 and the Division of Materials Sciences, Office of Basic Energy Sciences, U.S. Department of Energy at Oak Ridge National Laboratory, managed by Lockheed Martin Energy Research Corp. for the U.S. Department of Energy, under contract number DE-AC05-960R22464. 相似文献
10.
Measurement of the sensitization of nitrocompounds by amines using differential scanning calorimetry
We report a new method of making empirical measurements of the sensitization of nitrocompounds by amines based on thermal analysis. The method is sensitive, accurate and reproducible. We have used this method to measure the sensitization of nitromethane, N-methyl-N-(2,4,6-trinitrophenyl) nitramine (tetryl), picric acid and trinitrotoluene (TNT) by a number of aliphatic amines. 相似文献
11.
In temperature-modulated calorimetry, the condition in sample amount, especially thickness, required for high-accuracy heat capacity measurement should be made clear. We propose the condition of maximum thickness of a sample for measuring heat capacity within an accuracy of 1%. The other important factor for high-accuracy heat capacity measurement is thermal contact conductance between a sample and a sample pan and also that between a pan and a base plate of an apparatus. The conditions in these thermal contact conductances required for high-accuracy heat capacity measurement are discussed. Among them, if only thermal contact conductance between a pan and a base plate is significant, there is an ingenious method to measure heat capacity with high accuracy. Furthermore, if the thermal contact conductance between a pan and a base plate is infinite, we offer a simple method to obtain complex heat capacity. 相似文献
12.
Differential scanning calorimetry is well suited to record heat productions of chemical and physical processes as data for the following kinetic analysis. To obtain kinetic parameters of complex reactions, nonlinear optimization methods have to be used. Such complex reaction systems are polymerizations. We tried to evaluate measurements of the epoxy cure and the polymerization of β-propiolactame with simple and complex models. In both cases the simple models did not produce satisfactory results. But by using complex models a successful fitting of the measured data was possible. Our investigation shows that the combination of DSC and modern nonlinear evaluation methods presents a suitable tool for the kinetic investigation of polymerizations. 相似文献
13.
J. C. O.?Santos M. G. O.?Santos J. P.?Dantas Marta M.?Conceio P. F.?Athaide-Filho A. G.?Souza 《Journal of Thermal Analysis and Calorimetry》2005,79(2):283-287
Summary TG and DSC analyses were carried out in this work to evaluate the changes in the denaturation of human hair keratin submitted to different chemical effects. Hair bleaching and chlorinating treatments caused changes in the denaturation temperatures and denaturation enthalpies of hair keratin. Bleached hair and hair kept in a chlorinated solution presented a lower denaturation enthalpy and a higher denaturation temperature compared to the control hair sample. The TG and DSC analyses allowed to quantify the degradation level of hair fibers after the chemical treatments. AFM was also utilized to characterize the morphological alterations in the hair fiber surfaces caused by the chlorinating and bleaching treatments. 相似文献
14.
Thermal analysis of the binary system KCl-LiCl in the composition range 0.368–0.812 mol fraction of LiCl was studied by differential scanning calorimetry (DSC). On the basis of the DSC curves, the experimental data for the phase-diagram, the latent heat of fusion, and the average specific heat in the liquid and solid states are presented as a function of the composition of the mixture. The experimental results compared with literature data. The following empirical correlation between the heat of fusion (H) and of compositions of the mixture in mol fraction of LiCl (x) was obtained: ·GH=26.95–50.20x+43.06x2 with a minimum value of 11.8 kJ(g mol)–1 at the eutectic point of 0.587 mol fraction of LiCl at 354.4°C. These results are required as basic data to develop thermal energy storage materials, based on the phase change of a molten mixture of KCl-LiCI. 相似文献
15.
A procedure is described to determine the limit of detection of DSC instruments by using tiny signals from spontaneous polymorphic transitions of CsCl, K2Cr2O7 and Na2SO4. It is shown how such signals can be found well-resolved in DSC diagrams of powder samples. To distinguish them from the baseline noise they should exhibit a height at least twice that of the baseline width. For the instrument employed the corresponding smallest amount of heat, i.e., the limit of detection, was found to be 0.1 mJ.The authors thank Mr. H. Maltry for technical help and the Deutsche Forschungsgemeinschaft for support. 相似文献
16.
Pascale De Meuter Jo Amelrijckx Hubert Rahier Bruno Van Mele 《Journal of Polymer Science.Polymer Physics》1999,37(20):2881-2892
The slow isothermal crystallization of concentrated amorphous starch systems is measured by Modulated Differential Scanning Calorimetry (MDSC). It can be followed continuously by the evolution (stepwise decrease) of the MDSC heat capacity signal (Cp), as confirmed with data from X-ray diffractometry, Dynamic Mechanical Analysis, Raman spectroscopy, and conventional Differential Scanning Calorimetry. Isothermal MDSC measurements enable a systematic study of the slow crystallization process of a concentrated starch system, such as a pregelatinized waxy corn starch with 24 wt % water and 76 wt % starch. After isothermal crystallization, a broad melting endotherm with a bimodal distribution is observed, starting about 10°C beyond the crystallization temperature. The bulk glass transition temperature (Tg) decreases about 15°C during crystallization. The isothermal crystallization rate goes through a maximum as a function of crystallization time. The maximum rate is characterized by the time at the local extreme in the derivative of Cp (tmax), or by the time to reach half the decrease in Cp (t1/2). Both tmax and t1/2 show a bell-shaped curve as a function of crystallization temperature. The temperature of maximum crystallization rate, for the system studied, lies as high as 75°C. This is approximately 65°C above the initial value of Tg. Normalized Cp curves indicate the temperature dependence of the starch crystallization mechanism. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 2881–2892, 1999 相似文献
17.
W. M. Leung 《Colloid and polymer science》1985,263(10):818-821
Fusion behaviour of solution-grown low molecular weight polyethylene single crystals was studied by differential scanning calorimetry at different heating rates. The results were correlated to the polymer chain conformation in the crystal. It was found that in the molecular weight range studied, crystals of shorter chain length and fewer foldings per chain are less stable and more susceptible to heat annealing. Melting endotherms of the crystals of the lowest molecular weight fraction grown at various temperatures indicate that during crystallization, a fractional stem at the end of a folding chain will be rejected outside the lamellae of the crystal. 相似文献
18.
B. E. I. Abdelrazig S. D. Main D. V. Nowell 《Journal of Thermal Analysis and Calorimetry》1992,38(3):495-504
Thermal methods are used extensively in investigating cements and effects of additives on their hydration behaviour. Calcium chloride is the most effective and widely used accelerator for cement hydration, but the result is largely dependent on the rate at which it is added. In this study the influence of calcium chloride dosage on the hydration behaviour of OPC pastes aged for different periods has been investigated by means of differential scanning calorimetry (DSC), thermogravimetry (TG) and X-ray diffraction (XRD) methods. The results are discussed in relation to the relative amounts of calcium hydroxide and total reaction product formed. Chloroaluminate was a product of hydration in the samples dosed with greater than 1% calcium chloride. XRD was unable of itself to differentiate between monochloroaluminate and the calcium aluminate hydrate C4AH13 when present in small amounts. Thermal methods proved effective in characterising the products of hydration in the presence of chloride.
Zusammenfassung Bei der Untersuchung von Zement und des Einflusses von Additiven auf das Hydratationsverhalten von Zement finden thermoanalytische Methoden eine breite Anwendung. Der effektivste und meistbenutzte Beschleuniger für die Hydratation von Zement ist Calciumchlorid, aber die Ergebnisse hängen stark von der Dosiergeschwindigkeit ab. In vorliegender Studie wird mittels DSC-, TG- und Röntgendiffraktionsmethoden der Einflu\ der Dosierung von Calciumchlorid auf das Hydratationsverhalten von verschieden alten OPC-Zementbreiproben untersucht. Die Ergebnisse wurden in Bezug auf die relativen Mengen Calciumhydroxid und das gebildete Gesamtreaktionsprodukt gewertet.Bei Dosen von mehr als 1% Calciumchlorid konnte als Hydratationsprodukt Chloraluminat festgestellt werden. Sind Monochloraluminat und das Calciumaluminathydrat C4AH13 in geringen Mengen vorhanden, kann man zwischen den beiden mittels Röntgendiffraktion nicht unterscheiden. Thermoanalytische Methoden erwiesen sich als effektives Hilfsmittel bei der Charakterisierung der Produkte der Hydratation in Gegenwart von Chlorid.相似文献
19.
Kinetics
of polyurethane formation between several polyols and isocyanates with dibutyltin
dilaurate (DBTDL) as the curing catalyst, were studied in the bulk state by
differential scanning calorimetry (DSC) using an improved method of interpretation.
The molar enthalpy of urethane formation from secondary hydroxyl groups and
aliphatic isocyanates is 72±3 kJ mol-1
and for aromatic isocyanates it is 55±2 kJ mol-1
. In the case of a single second order reaction for aliphatic isocyanates
reaction, activation energy is 70±5 kJ mol-1
with oxypropylated polyols and 50±3 kJ mol-1
with Castor oil. For aromatic isocyanates and oxypropylated polyols the activation
energy is higher around 77 kJ mol-1 .
In the case of two
parallel reactions (situation for IPDI and TDI 2-4) best fits are observed
considering two different activation energies. 相似文献