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Studies of thermokinetics in an adiabatic calorimeter

I. Design and testing of an adiabatic automatic calorimeter

Journal of Thermal Analysis and Calorimetry
Authors: S. Zhan, J. Liu, Z. Qin, and Y. Deng

Abstract  

An adiabatic calorimeter in which automation of the control of the adiabatic condition and the thermogram recording is achieved in a simple way has been designed for studies of both thermochemistry and thermokinetics. A new method for specific heat measurements has been proposed and specific heats ofn-heptane were measured to test the reliability of this calorimeter.

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Abstract  

This paper presents several applications of the PHI-TEC II that are not commonly associated with adiabatic calorimeters but which have proved to be extremely valuable. These include simulation of a deep oil well for enhanced oil recovery, isothermal calorimetry of a semibatch reaction, catalyst research using flow through reactors (both plug flow and CSTR) with controlled feeds of high pressure liquid and gas.

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Abstract  

A computerized adiabatic calorimeter for heat capacity measurements in the temperature range 80–400 K has been constructed. The sample cell of the calorimeter, which is about 50 cm3 in internal volume, is equipped with a platinum resistance thermometer and surrounded by an adiabatic shield and a guard shield. Two sets of 6-junction chromel-copel thermocouples are mounted between the cell and the shields to indicate the temperature differences between them. The adiabatic conditions of the cell are automatically controlled by two sets of temperature controller. The reliability of the calorimeter was verified through heat capacity measurements on the standard reference material α-Al2O3. The results agreed well with those of the National Bureau of Standards (NBS): within 0.2% throughout the whole temperature region. The heat capacities of high-purity graphite and polystyrene were precisely measured in the interval 260–370 K by using the above-mentioned calorimeter. The results were tabulated and plotted and the thermal behavior of the two materials was discussed in detail. Polynomial expressions for calculation of the heat capacities of the two substances are presented.

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Abstract  

A fully automated adiabatic calorimeter controlled on line by a computer used for heat capacity measurements in the temperature range from 80 to 400 K was constructed. The hardware of the calorimetric system consisted of a Data Acquisition/Switch Unit, 34970A Agilent, a 7 1/2 Digit Nano Volt /Micro Ohm Meter, 34420A Agilent, and a P4 computer. The software was developed according to modern controlling theory. The adiabatic calorimeter consisted mainly of a sample cell equipped with a miniature platinum resistance thermometer and an electric heater, two (inner and outer) adiabatic shields, two sets of six junction differential thermocouple piles and a high vacuum can. A Lake Shore 340 Temperature Controller and the two sets of differential thermocouples were used to control the adiabatic conditions between the cell and its surroundings. The reliability of the calorimeter was verified by measuring the heat capacities of synthetic sapphire (α-Al2O3), Standard Reference Material 720. The deviation of the data obtained by this calorimeter from those published by NIST was within ±0.1% in the temperature range from 80 to 400 K.

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Abstract  

An automatic pressure tracking adiabatic calorimeter (APTAC) has been developed to obtain the thermokinetic and vapor pressure data during runaway reactions. The heat onset temperature is important data for estimating the thermal hazardous materials. DTBP(di-tert-butyl peroxide)/toluene was chosen for evaluating the measurement values and the thermokinetic parameters. The relationships between the sample mass and the heat onset temperature in the addition to the maximum temperature were investigated to explain the heat of reaction measured by the APTAC. The apparatus properties and the reliability of the data obtained by the APTAC were examined on the basis of the experimental data.

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Studies of thermokinetics in an adiabatic calorimeter

II. Calorimetric curve analysis methods for irreversible and reversible reactions

Journal of Thermal Analysis and Calorimetry
Authors: S. Zhan, J. Liu, Z. Qin, and Y. Deng
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Journal of Thermal Analysis and Calorimetry
Authors: X.-C. Lv, Z.-C. Tan, Z.-A. Li, Y.-S. Li, J. Xing, Q. Shi, and L.-X. Sun

Abstract  

The (R)-BINOL-menthyl dicarbonates, one of the most important compounds in catalytic asymmetric synthesis, was synthesized by a convenient method. The molar heat capacities C p,m of the compound were measured over the temperature range from 80 to 378 K with a small sample automated adiabatic calorimeter. Thermodynamic functions [H TH 298.15] and [S TS 298.15] were derived in the above temperature range with a temperature interval of 5 K. The thermal stability of the substance was investigated by differential scanning calorimeter (DSC) and a thermogravimetric (TG) technique.

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Heat capacities of structure I and II trimethylene oxide (TMO) clathrate hydrates doped with small amount of potassium hydroxide (x=1.8×10−4 to water) were measured by an adiabatic calorimeter in the temperature range 11–300 K. In the str. I hydrate (TMO·7.67H2O), a glass transition and a higher order phase transition were observed at 60 K and 107.9 K, respectively. The glass transition was considered to be due to the freezing of the reorientation of the host water molecules, which occurred around 85 K in the pure sample and was lowered owing to the acceleration effect of KOH. The relaxation time of the water reorientation and its distribution were estimated and compared with those of other clathrate hydrates. The phase transition was due to the orientational ordering of the guest TMO molecules accommodated in the cages formed by water molecules. The transition was of the higher order and the transition entropy was 1.88 J·K−1(TMO-mol)−1, which indicated that at least 75% of orientational disorder was remaining in the low temperature phase. In the str. II hydrates (TMO·17H2O), only one first-order phase transition appeared at 34.5 K. This transition was considered to be related to the orientational ordering of the water molecules as in the case of the KOH-doped acetone and tetrahydrofuran (THF) hydrates. The transition entropy was 2.36 JK−1(H2O-mol)−1, which is similar to those observed in the acetone and THF hydrates. The relations of the transition temperature and entropy to the guest properties (size and dipole moment) were discussed.

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Abstract  

The highly reactive and unstable exothermal features of methyl ethyl ketone peroxide (MEKPO) have led to a large number of thermal explosions and runaway reaction accidents in the manufacturing process. To evaluate the self-accelerating decomposition temperature (SADT) of MEKPO in various storage vessels, we used differential scanning calorimetry (DSC) and vent sizing package 2 (VSP2). The thermokinetic parameters were, in turn, used to calculate the SADT from theoretical equations based on the Semenov model. This study aimed at the SADT prediction value of various storage vessels in Taiwan compared with the UN 25 kg package and UN 0.51 L Dewar vessel. An important index, such as SADT, temperature of no return (T NR) and adiabatic time maximum rate (TMRad), was necessary and useful to ensure safe storage or transportation for self-reactive substances in the process industries.

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of thermodynamic property for this substance is necessary. In this study, the low-temperature heat capacities of this compound over the temperature range from 78 to 350 K were measured by an automated adiabatic calorimeter. The thermodynamic functions

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