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Abstract  

A novel method that spent nuclear fuel is converted into nitrates with N2O4, and then nitrates are extracted with TBP in supercritical CO2 (SC-CO2), has been developed for reprocessing of spent nuclear fuel, which has a potential prospect because of its potential to decrease generation of the secondary liquid waste. In this paper, conversion of Nd2O3 with N2O4 into its nitrate under various conditions and extraction of the conversion product with TBP in SC-CO2 were investigated. When temperature was 60–120 °C, the molar ratio of H2O to Nd2O3 was from 1 to 6, and molar ratio of N2O4 to Nd2O3 was above 8, complete conversion of Nd2O3 into its nitrate was achieved. The conversion product was characterized by thermal analysis (TG-DTA), X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FT-IR) and Raman spectroscopy. Quantitative extraction of the conversion product with TBP in supercritical CO2 was also achieved under experimental conditions.

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Abstract  

The thermal decomposition of strontium acetate hemihydrate has been studied by TG-DTA/DSC and TG coupled with Fourier transform infrared spectroscopy (FTIR) under non-isothermal conditions in nitrogen gas from ambient temperature to 600°C. The TG-DTA/DSC experiments indicate the decomposition goes mainly through two steps: the dehydration and the subsequent decomposition of anhydrous strontium acetate into strontium carbonate. TG-FTIR analysis of the evolved products from the non-oxidative thermal degradation indicates mainly the release of water, acetone and carbon dioxide. The model-free isoconversional methods are employed to calculate the E a of both steps at different conversion α from 0.1 to 0.9 with increment of 0.05. The relative constant apparent E a values during dehydration (0.5<α<0.9) of strontium acetate hemihydrate and decomposition of anhydrous strontium acetate (0.5<α<0.9) suggest that the simplex reactions involved in the corresponding thermal events. The most probable kinetic models during dehydration and decomposition have been estimated by means of the master plots method.

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Summary

Radix Isatidis has widely useful activities including anti-virus, anti-bacterial. Tryptanthrin, indigo, and indirubin are active ingredients in R. Isatidis. Response surface methodology (RSM)-optimized infrared-assisted extraction (IRAE) was developed and combined with HPLC for simultaneous determination of tryptanthrin, indigo, and indirubin from R. Isatidis. IRAE were investigated through extraction yields of the three components and optimized by RSM. The optimum conditions were as follows: infrared power of 129 W, solid/liquid ratio of 1:40 g/mL, and irradiation time of 22.5 min. IRAE conditions obtained by RSM were not only accurate, but also had practical value reflecting the expected optimization. Subsequently, this novel IRAE method was evaluated by extraction yield of the components of R. Isatidis samples from different regions. Compared with common extraction methods including maceration extraction (ME), reflux extraction (RE), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), IRAE showed higher yield with advantages of no limitation of solvent selection, low cost, convenience under optimum extraction conditions. These results suggested the potential of RSM-optimized IRAE for extraction and analysis of the water-/fat-soluble compositions of Chinese herbal medicine. A simple chromatographic separation for simultaneous determination of tryptanthrin, indigo, and indirubin from Chinese herbal medicine R. Isatidis was performed on a C18 column (Diamonsil 150 mm × 4.6 mm i.d., 5 μm) with a mobile phase isocratic consisting of methanol and water at a flow-rate of 0.8 mL min−1. The retention times of tryptanthrin, indigo, and indirubin were 15.4, 31.9, and 58.6 min, respectively. The linear equations were obtained as follows: y = −3094.5744 + 21208.792x for tryptanthrin (R = 0.9998, 0.9–18.0 μg mL−1), y = 4730.0448 + 30180.567x for indigo (R = 0.9997, 0.5–10.0 μg mL−1) and y = −6582.9045 + 67069.312x for indirubin (R = 0.9997, 0.4–8.0 μg mL−1). The result showed that RSM-optimized IRAE was a simple, efficient pretreatment method for the analysis of complex matrix.

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Abstract  

New complexes of the non-natural amino acid (p-iodo-phenylalanine) with divalent cobalt and nickel ions have been synthesized. The composition of the complexes is [M(IC6H4CH2CHNH2COO)2]2.5H2O (M=Co, Ni) and the crystal structure belongs to orthorhombic system. Infrared spectra indicate the nature of bonding in the complex. The first stage in the thermal decomposition process of the complex shows the presence of crystal water. The thermal decomposition process of cobalt complex differs from that of nickel. The intermediate and final residues in the thermal decomposition process have been analyzed to check the pyrolysis reactions. Thermal analysis indicates that the iodine atom of the ligand may coordinate to the metal ion in the lattice.

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Summary

A preparative high-speed countercurrent chromatograph (HSCCC) method for the isolation and purification of C6-C2 natural alcohol and benzyl ethanol from Forsythia suspensa was successfully established. Cornoside, forsythenside F, forsythiaside, and acteoside were rapidly obtained for the first time by HSCCC with a two-phase solvent system ethyl acetate-n-butanol-methanol-water (5:1:0.5:5, υ/υ) in one-step separation. The purities of them were all above 97% as determined by high-performance liquid chromatography, and the combination of ESI-MS and NMR analysis confirmed the chemical structures of the four compounds.

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Influence of different maturity stages and treatments of ethephon, exogenous ABA, and fluridone on the ripening and hormone level of ‘Zhonghuashoutao’ peach during development and post-harvest storage were investigated. The accumulation of endogenous ABA appeared at the onset of ripening and peaked at two weeks before harvest. Fruit firmness decreased, while ethylene release and SSC/TA increased sharply after a maximum peak of ABA, which have triggered the initiation of the fruit ripening. The fruits, harvested at 170 d when fruits have ripened and stored at 20 °C, showed an ethylene climacteric peak, and the pulp started softening normally, and the SSC/TA value increased. Compared with them, the immature green fruits harvested at other dates, could not mature normally due to the lack of normal reciprocity between ABA and ethylene. The ethylene release was promoted by the treatment of exogenous ABA and ethephon during ripening until the endogenous ABA reached a maximum value. However, fluridone treatment showed an inhibitory effect. The above-mentioned changes occurred again in the peach fruits after harvest. The results indicated that both ABA and ethylene play important roles in peach ripening, and their action depended on the ripening stage of peach.

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A method was developed for the preparative separation of two alkaloids from the crude extract of the radix of Rauvolfia verticillata (Lour.) Baill. in a single run. The two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–water (5:5:2:8, v/v), where triethylamine (40 mmol/L) was added to the upper organic phase as the stationary phase and hydrochloric acid (10 mmol/L) was added to the lower aqueous phase as the mobile phase, was selected for this separation by pH-zone-refining counter-current chromatography (PZRCCC). For the preparative separation, the apparatus was rotated at a speed 850 rpm, while the mobile phase was pumped into the column at 2 mL/min. As a result, 112 mg of reserpine and 21 mg of yohimbine were obtained from 3 g of crude extract in a single run. The analysis of the isolated compounds was determined by high-performance liquid chromatography (HPLC) at 230 nm with purities of over 91.0%, and the chemical identification was carried out by the data of electrospray ionization–mass spectrometry (ESI–MS) and nuclear magnetic resonance (NMR) spectroscopy. The technique introduced in this paper is an efficient method for preparative separation of reserpine and yohimbine from devil pepper radix. It will be beneficial to utilize medicinal materials and also useful for the separation, purification, and pharmacological study of Chinese herbal ingredients.

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Summary

An efficient and robust method for analyzing constituents of a well-known traditional Chinese medicine (TCM) formula SiWu decoction (SWD) contains Angelicae Sinensis Radix (ASR), Chuanxiong Rhizoma (CR), Paeoniae Radix Alba (PRA), and Rehmanniae Radix Praeparata (RRP) by ultra high-performance liquid chromatography (UHPLC)/time-of-flight mass spectrometry (TOF-MS) was established. The method efficiently applied to the separation of 75 compounds, including organic acids, phthalides, phenylpropanoid glycosides, iridoid glycosides, monoterpene glycosides, and galloyl glycosides in the complex prescription, 52 compounds in this study can be unambiguously identified or tentatively characterized. The separation was achieved within 20 min at the optimized chromatographic conditions. Our study provided a reliable and high-efficient method for the understanding of the chemical basis of SWD.

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Recently, super rice has gained much importance due to its high yield potential while exogenous application of plant growth regulators (PGRs) is an important aspect in plant development and defense responses under stress conditions. In this study we conducted two pot experiments. Firstly, four super rice cultivars, viz. Peizataifeng, Huayou 213, Yuxiangyouzhan and Huahang 31 were subjected to a series of five chilling temperatures, i.e. 11 °C, 12 °C, 13 °C, 14 °C and 15 °C (day/night) for about 25–27 days. Secondly, seeds of Peizataifeng (super rice) and Yuejingsimiao 2 (non-super rice) were then treated with different combinations of salicylic acid (SA), brassinolide (BR), calcium chloride (CaCl2) and fulvic acid (FA) and then exposed to chilling stress at 13 °C for four days. Resultantly, Peizataifen (super rice) was found with the lowest seedling survival rate at all chilling temperatures among all four super rice cultivars, however, it was still found more resistant when compared with Yuejingsimiao 2 (non-super rice) in the second experiment. Furthermore synergistic effect of all PGRs alleviated low temperature stress in both rice cultivars by improving seedling survival rates, leaf area, seedling dry weight, seedling height, root morphology and by modulating antioxidant enzymes, improving proline content and lowering lipid peroxidation.

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