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Thermodynamic investigation of several natural polyols

Part III. Heat capacities and thermodynamic properties of erythritol

Journal of Thermal Analysis and Calorimetry
Authors: B. Tong, Z. Tan, J. Zhang, and S. Wang

Abstract  

The low-temperature heat capacity C p,m of erythritol (C4H10O4, CAS 149-32-6) was precisely measured in the temperature range from 80 to 410 K by means of a small sample automated adiabatic calorimeter. A solid-liquid phase transition was found at T=390.254 K from the experimental C p-T curve. The molar enthalpy and entropy of this transition were determined to be 37.92±0.19 kJ mol−1 and 97.17±0.49 J K−1 mol−1, respectively. The thermodynamic functions [H T-H 298.15] and [S T-S 298.15], were derived from the heat capacity data in the temperature range of 80 to 410 K with an interval of 5 K. The standard molar enthalpy of combustion and the standard molar enthalpy of formation of the compound have been determined: Δc H m 0(C4H10O4, cr)= −2102.90±1.56 kJ mol−1 and Δf H m 0(C4H10O4, cr)= − 900.29±0.84 kJ mol−1, by means of a precision oxygen-bomb combustion calorimeter at T=298.15 K. DSC and TG measurements were performed to study the thermostability of the compound. The results were in agreement with those obtained from heat capacity measurements.

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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  

The quality of measurement of heat capacity by differential scanning calorimetry (DSC) is based on the symmetry of the twin calorimeters. This symmetry is of particular importance for the temperature-modulated DSC (TMDSC) since positive and negative deviations from symmetry cannot be distinguished in the most popular analysis methods. Three different DSC instruments capable of modulation have been calibrated for asymmetry using standard non-modulated measurements and a simple method is described that avoids potentially large errors when using the reversing heat capacity as the measured quantity. It consists of overcompensating the temperature-dependent asymmetry by increasing the mass of the sample pan.

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Abstract  

A novel thermokinetic research method for determination of rate constants of simple-order reaction in batch conduction calorimeter under isothermal condition, the characteristic parameter method, is proposed in this paper. Only needing the characteristic time parameter tm obtained from the measured thermoanalytical curve, the kinetic parameters of reactions studied can be calculated conveniently with this method. The saponifications of ethyl propionate and ethyl acetate in aqueous ethanol solvent, the polymerization of acrylamide in aqueous solution, the ring opening reaction of epichlorohydrin with hydrobromic acid have been studied. The experimental results indicate that the characteristic parameter method for simple-order reaction is correct.

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Abstract  

According to the theoretical basis of thermokinetics, the integral and differential thermokinetic equations of opposing reactions have been derived, and a novel thermokinetic research method, the characteristic parameter method for opposing reactions which taking place in a batch conduction calorimeter under isothermal condition, has been proposed in this paper. Only needing the characteristic thermoanalytical data corresponding to tm and 2tm from the same curve, the rate constants of forward and backward reactions and equilibrium constant can be calculated simultaneously with this method. In order to test the validity of this method, the proton-transfer reactions of nitroethane with ammonia at 15 and 25°C, and with trihydroxymethyl aminomethane (Tris) at 15 and 30°C have been studied, respectively. The results of rate constants and equilibrium constants calculated with this method are in agreement with those in the literature. Therefore, the characteristic parameter method for opposing reaction is believed to be correct.

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Abstract  

In this paper the dependence of build-up233U,232U,233Pa and fission products from ThO2 irradiated in HFETR on integral thermal neutron fluxes and neutron spectra have been investigated. The yields of all above nuclides in ThO2 increase with the increase of integral thermal neutron fluxes at different neutron spectra. The values of233U/232Th increase with the increases of th and decreases with the increase of fast/thermal neutron ratios ( f/ th). The values of232U/233U increase with the increase of both th and f/ th ratio. The amount of fission products relative to original irradiated thorium decreases with the increase of f/ th ratios. These results could be used to evaluate the behaviour of thorium-based nuclear fuel in reactor.

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Abstract

By using the critical point theory, the existence of periodic solutions to second order nonlinear p-Laplacian difference equations is obtained. The main approach used is a variational technique and the saddle point theorem. The problem is to solve the existence of periodic solutions of second order nonlinear p-Laplacian difference equations.

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In this study, the cDNA of homocysteine S-methyltransferase was isolated from Aegilops tauschii Coss., with the gene accordingly designated as AetHMT1. Similar to other methyltransferases, AetHMT1 contains a GGCCR consensus sequence for a possible zinc-binding motif near the C-terminal and a conserved cysteine residue upstream of the zinc-binding motif. Analysis of AetHMT1 uncovered no obvious chloroplast or mitochondrial targeting sequences. We functionally expressed AetHMT1 in Escherichia coli and confirmed its biological activity, as evidenced by a positive HMT enzyme activity of 164.516 ± 17.378 nmol min−1 mg−1 protein when catalyzing the transformation of L-homocysteine. Compared with the bacterium containing the empty vector, E. coli harboring the recombinant AetHMT1 plasmid showed much higher tolerance to selenate and selenite. AetHMT1 transcript amounts in different organs were increased by Na2SeO4 treatment, with roots accumulating higher amounts than stems, old leaves and new leaves. We have therefore successfully isolated HMT1 from Ae. tauschii and characterized the biochemical and physiological functions of the corresponding protein.

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Summary

An ultra-performance liquid chromatography-quadrupole time-of-flight mass spectrometry UPLC-QTOF-MS method has been developed for qualitative and quantitative analysis major compounds in Saussurea eopygmaea Hand-Mazz, which has long been used as a traditional Tibetan medicine. This method was validated to be sensitive, precise, and accurate with the limits of detection of compounds 2,3,4,6, and 7 with 0.67–1.90 μg mL−1, the overall intra-day and inter-day variations less than 8.45%, and the overall recovery over 93.8%, respectively. The correlation coefficients (R 2) of the calibration curves were higher than 0.998. In addition, by comparison MS and MS/MS spectra with those of authentic compounds and literatures, a total of 14 main peaks were identified within 6 min. These results demonstrate that this approach has the potential for quality control of S. eopygmaea and other Tibetan herbal medicines.

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Purple pericarp is an interesting and useful trait in Triticum aestivum, but the molecular mechanism behind this phenotype remains unclear. The allelic variation in the MYB transcriptors is associated with the phenotype of pigmented organs in many plants. In this study, a MYB transcription factor gene, TaMYB3, was isolated using homology-based cloning and a differentially expressed gene mining approach, to verify the function of the MYB transcriptor in the purple pericarp. The coding sequence of TaMYB3 in cultivar Gy115 was the same as that in cultivar Opata. TaMYB3 was localized to FL0.62–0.95 on chromosome 4BL. The TaMYB3 protein contains DNA-binding and transcription-activation domains, and clustered on a phylogenetic tree with the MYB proteins that regulates anthocyanin and proanthocyanin biosynthesis. TaMYB3 localized in the nuclei of Arabidopsis thaliana and wheat protoplasts after it was transiently expressed with PEG transformation. TaMYB3 induced anthocyanin synthesis in the pericarp cells of Opata in the dark in collaboration with the basic helix–loop–helix protein ZmR, which is also the function of ZmC1. However, TaMYB3 alone did not induce anthocyanin biosynthesis in the pericarp cells of the white grain wheat cultivar Opata in the light after bombardment, whereas the single protein ZmR did. Light increased the expression of TaMYB3 in the pericarp of Gy115 and Opata, but only induced anthocyanin biosynthesis in the grains of Gy115. Our results extend our understanding of the molecular mechanism of the purple pericarp trait in T. aestivum.

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