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  • Author or Editor: Jing Zhang x
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Abstract

Non-isothermal crystallization of isotactic poly(4-methyl-pentene-1) (P4MP1) is studied by differential scanning calorimeter (DSC), and kinetic parameters such as the Avrami exponent and the kinetic crystallization rate (Z c) are determined. From the cooling and melting curves of P4MP1 at different cooling rates, the crystalline enthalpy increases with the increasing cooling rate, but the degree of crystalline by DSC measurement shows not much variation. Degree of crystalline of P4MP1 calculated by wide angle X-ray diffraction pattern shows the same tendency with crystalline enthalpy, indicating that re-crystallization occurs when samples heated above the second glass transition temperature of P4MP1. By Jeziorny analysis, n 1 value suggests that mainly spherulites’ growth at 2.5 K min−1 transforms into a mixture mode of three-dimensional and two-dimensional space extensions with further increasing cooling rate. In the secondary crystallization process, n 2 values indicate that the secondary crystallization is mainly the two-dimensional extension of the lamellar crystals formed during the primary crystallization process. The rates of the crystallization, Z c and t 1/2 both increase obviously with the increase of cooling rate, especially at the primary crystallization stage. By Mo's method, higher cooling rate should be required in order to obtain a higher degree of crystallinity at unit crystallization time.

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Abstract  

Proficiency testing is one of methods for regularly assessing the accuracy of the analytical data produced by laboratories for particular measurements. In 2008 and 2010, we participated in the IAEA 2008 and 2010 worldwide open proficiency tests on the determination of natural radionuclides in water spiked with 226Ra, 234U and 238U for activity analysis and with 90Sr and 230Th for gross alpha/beta analysis. Feedback statistics from the IAEA final report showed that the radioactivities of all of the samples fell within an acceptable range according to the IAEA. For 226Ra analysis, our result showed that 229Th–225Ra is suitable as a chemical tracer, although there are doubts that different co-precipitation efficient between parent 229Th and its daughter nuclide 225Ra in published literature. The impact factors of the analysis results, such as the lower limit of detection, standard substances, the background and efficiency for daily determination, are discussed in detail.

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Abstract  

To simplify TRPO process, a novel ligand, N,N’-dimethyl-3-oxa-glutaramic acid (DMOGA), was synthesized and used for stripping of An(III, IV) from 30% TRPO-kerosene. The distribution ratios for transuranium elements, including Np(IV), Pu(IV), Am(III), and some fission products, including Eu(III), Fe and Zr between 30% TRPO-kerosene and various HNO3-DMOGA solutions were measured. An(III, IV) and Ln(III) extracted to TRPO from simulated high level liquid waste could be recovered with an efficiency of 99.9% above in one stream with a 3-stage crosscurrent strip experiment with 0.2M DMOGA in HNO3 solution. Using this new agent, the back extraction of TRU elements from loaded TRPO phase becomes more simple and practical. Therefore, the original TRPO process could be simplified.

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A new high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous estimation of astragaloside IV and formononetin in Radix Astragali. Samples were employed to degrease the materials by petroleum ether (boiling point: 60–90°C) and extracted by methanol, and then were alkalized and extracted with n-butanol saturated with water. Separation was achieved on HPTLC plates using petroleum ether (boiling point: 60–90°C) and n-butanol saturated with water-glacial acetic acid as the mobile phase, the results of which were compared with HPLC. The well-resolved peaks for astragaloside IV and formononetin were observed at R F values 0.43 ± 0.02 and 0.75 ± 0.02, respectively. The calibration curves were found linear with a wide range of concentration 1.01–10.10 μg μL−1 with good correlation coefficient for astragaloside IV and formononetin. The method was validated for linearity, precision, reproducibility, accuracy, and limits of detection and quantification. This simple, rapid, sensitive, economic, and reliable HPTLC method is suitable for the routine quantitative analysis and quality control of traditional Chinese medicines (TCMs) such as Radix Astragali, which can be applied for the quality control of saponins and flavonoids in other plants or extracts.

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Abstract

The heat release behaviors of several chemical compounds were detected with C80 calorimeter. Furthermore, the thermodynamic and kinetic parameters of the chemicals were obtained based on the experimental data. Chemical thermal risk was simultaneously graded with combined use of instantaneous power density and the classification standard of thermal instability which was offered by the standard system for the identification of the hazards of materials for emergency response (NFPA704). The results show that the grading standard of thermal risk based on NFPA704 was reasonable and can be used as a preliminary thermal risk assessment for reaction hazards.

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Abstract

The thermal behavior and decomposition of kaolinite–potassium acetate intercalation complex was investigated through a combination of thermogravimetric analysis and infrared emission spectroscopy. Three main changes were observed at 48, 280, 323, and 460 °C which were attributed to (a) the loss of adsorbed water, (b) loss of the water coordinated to acetate ion in the layer of kaolinite, (c) loss of potassium acetate in the complex, and (d) water through dehydroxylation. It is proposed that the potassium acetate intercalation complex is stability except heating at above 300 °C. The infrared emission spectra clearly show the decomposition and dehydroxylation of the kaolinite intercalation complex when the temperature is raised. The dehydration of the intercalation complex is followed by the loss of intensity of the stretching vibration bands at region 3600–3200 cm−1. Dehydroxylation is followed by the decrease in intensity in the bands between 3695 and 3620 cm−1. Dehydration is completed by 400 °C and partial dehydroxylation by 650 °C. The inner hydroxyl group remained until around 700 °C.

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Abstract  

The study demonstrates the advantages of an innovative list-mode multispectral data acquisition system that allows simultaneous creation of several different single, summed, coincident and anticoincident spectra with a single measurement. One of the consequences of list-mode data file offline processing is a reconstructed spectrum with Compton continuum suppression and without any full-energy peak efficiency deduction owing to true coincidence summing. The spectrometer is designed to read out analogue signal from preamplifier of gamma-ray detectors and to digitalize it using DGF/Pixie-4 software and card package (XIA LLC). This is realized by converting an Ortec Compton suppression data acquisition system into an all-digital spectrometer. Instead of using its timing electronic chain to determine the coincidence event, the analog signals from primary and guard detectors were connected directly into the Pixie-4 card for pulse height and time coincident measurement by individually logging and time stamping each electronic pulse. The data acquired in list-mode included coincidence and anticoincidence events consisting of records of energy and timestamp from primary and guard detectors. Every event was stored in a text file for offline processing and spectral reconstruction. A sophisticated computer simulation was also created with the goals of obtaining a better understanding of the experimental results and calculating efficiency.

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Abstract  

This study characterized the removal of strontium from an aqueous solution via co-precipitation followed by microfiltration (CPMF) on a lab-scale. Sodium carbonate was used as the precipitating agent. Ferric chloride was added to a settler at a dosage of 20 mg/L to improve strontium removal, and it was added to a membrane separator at a dosage of 10 mg/L to reduce membrane fouling. The concentration of strontium in the raw water used in this study was about 5 mg/L. In two intermittent tests, where dosages of sodium carbonate were 2000 mg/L and 1000 mg/L, the mean decontamination factors (DFs) were 237 and 158 and the mean concentration factors (CFs) were 288 and 462, respectively. Although the mean DF value was lower when the sodium carbonate dosage was 1000 mg/L instead of 2000 mg/L, the rate at which the specific flux (SF) of the membrane declined decreased as the amount of the effluent treated increased. The problem of strontium release at the beginning of the operation was controlled by a continuous test in which the dosage of sodium carbonate still was 1000 mg/L and the other parameters were the same as in the other tests. The results showed that the mean DF and CF were 157 and 480, respectively.

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The newly emerged chromatographic fngerprint analysis represents a rational approach assessment of Traditional Chinese Medicine (TCM) and its preparations. In the present paper, a quick and reliable analytical method was developed for the quality assessment of QiYi capsules (QY) using high-performance thin-layer chromatography (HPTLC) with the reference of Tripterygium wilfordii. The unique properties of the HPTLC fngerprint were validated by analyzing 10 batches of QY samples. The 9 common peaks of the HPTLC images of QY and the different RF and peak area ratios of the chemical distribution could directly discern the stability by comparison of 10 samples, and also, the 9 common peaks were selected to evaluate the similarities of QY; the similarities of 10 batches of QY were more than 0.960, which indicated a standardized consistency and reliable quality of QY. Therefore, the newly developed HPTLC fngerprint method provided an easy way for sample characterization and differentiation; it allowed for the quality assessment of QY capsules with the reference of T. wilfordii.

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Abstract  

Non-isothermal crystallization kinetics and subsequent melting behavior for three kinds of ethylene-acrylic acid copolymer (EAA) are investigated via differential scanning calorimetry (DSC). From the Jeziorny method, the crystallization rate of the primary stage is significantly influenced by the competitive mobility of chains. While the crystallization rate in the secondary stage decreases in order of acrylic acid (AA) content in copolymers. Mo’s method can also provide a good fitting. Difference between the Jeziorny method and Mo’s method analysis is because of a higher effect of non-crystallizable chain ends. The effective activation energy is also determined via Kissinger’s method.

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