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Abstract  

The crystal structure, melting range, decomposition temperature, solubilities in aqueous and organic phase, and distribution ratio in biphase system of N,N,N′,N′-tetramethyl diglycolamide (TMDGA) have been studied in the present work. Water-soluble TMDGA with very low solubility in kerosene or 30 % trialkyl phosphine (TRPO)/kerosene meets the primary requirement to act as the stripping agent in TRPO process which has been developed for actinides partitioning from high level waste. Slope analysis, electrospray ionization mass spectrometry (ESI–MS) and spectrophotometric titration indicate that in weak and moderate acidic aqueous solution, up to three TMDGA molecules form complexes with Zr4+, trivalent lanthanides (Ln3+), trivalent actinides (An3+) or tetravalent actinides (An4+). Their complex formation constants determined by liquid–liquid extraction method follow the order predicted by the electrostatic model of 4f and 5f elements and the covalent model of 4d transition elements: Ln3+ ~ An3+ < An4+ ≪ Zr4+. Hydrolysis of actinide cations, especially An4+, in the media of low acidity, reduces the complexation stability. In addition, the effect of aqueous acidity and temperature has been investigated. No obvious influence of temperature on Np4+ complexes has been found. However, the influence on Am3+ and Pu4+, especially on their 1:1 or 1:2 complex species with TMDGA, is relatively considerable. Strong affinity of TMDGA to An3+ and An4+ implies that TMDGA has potential to strip An3+ and An4+ from TRPO.

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Acta Orientalia Academiae Scientiarum Hungaricae
Authors:
Feng Jing
,
Peter Kornicki
,
Anikó Schmidt
,
Gyula Wojtilla
, and
Abdurishid Yakup
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A high-performance thin-layer chromatographic (HPTLC) method for simultaneous analysis of temephos and fenitrothion in green tea has been established and validated. The sample was extracted with ethyl acetate by mechanical vibration at room temperature and the extract was cleaned by use of an SPE tandem column, before elution with dichloromethane. The extract was applied as bands to glassbacked silica gel 60F254 HPTLC plates. The plates were developed with acetone-hexane 3+7 (v/v), in an unsaturated glass twin-trough chamber. The developed HPTLC plates were evaluated densitometrically. The detection limits of temephos (R F 0.55) and fenitrothion (R F 0.69) were 20 and 10 ng, respectively. Recovery from green tea of the two pesticides at levels of 0.2 to 4 mg kg−1 was 80–107% with relative standard deviations of 4.4–20.2%. The precision and accuracy of the method were generally fit for analysis of temephos and fenitrothion residues in green tea.

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Abstract  

This work reports the synthesis and preliminary biodistribution results of [131I]SIB-PEG4-CHC in tumor-bearing mice. The tributylstannyl precursor ATE-PEG4-CHC was synthesized by conjugation of ATE to amino pegylated colchicine NH2-PEG4-CHC. [131I]SIB-PEG4-CHC was radiosynthesized by electrophilic destannylation of the precursor with a yield of ~44%. The radiochemical purity (RCP) appeared to be >95% by a Sep-Pak cartridge purification. [131I]SIB-PEG4-CHC was lipophilic and was stable at room temperature. Biodistribution studies in tumor-bearing mice showed that [131I]SIB-PEG4-CHC cleared from background rapidly, and didn’t deiodinate in vivo. However, the poor tumor localization excluded it from further investigations as a tumor-targeted radiopharmaceuticals.

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A double-development TLC method has been developed for simultaneous qualitative and quantitative analysis of hydrophilic and lipophilic constituents of Salvia miltiorrhiza (Danshen). The optimized mobile phases dichloromethane-ethyl acetate-formic acid 22:24:10 (ν/ν) and petroleum ether-ethyl acetate-cyclohexane 25:11:14 (ν/ν) were used for the double development on nano-silica gel 60F254 plates. Their characteristic TLC profiles were observed under UV light at 254 and 365 nm and the bands were then revealed by reaction with 5% H2SO4 in EtOH. Quantification of twelve compounds was achieved by densitometry at 260 or 290 nm, with reference at 400 nm. Linearity was quite good (R 2 > 0.99) within the ranges tested. This method could be used for quality control of Danshen.

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Abstract  

This paper introduces the analysis method and principle of pulse fast-thermal neutron analysis (PFTNA). A system for the measurement of low caloric power of coal by PFTNA is also presented. The 14 MeV pulse neutron generator and BGO detector and 4096 MCA were applied in this system. A multiple linear regression method applied to the data solved the interferential problem of multiple elements. The error of low caloric power between chemical analysis and experiment was less than 0.4 MJ/kg.

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Abstract  

The sorption of Co(II) on Na-attapulgite as a function of contact time, solid content, pH, ionic strength, foreign ions, fulvic acid (FA) and temperature under ambient conditions was studied. The kinetic of Co(II) sorption on Na-attapulgite was described well by pseudo-second-order model. The sorption of Co(II) on Na-attapulgite was strongly dependent on pH and ionic strength. The sorption of Co(II) was mainly dominated by outer-sphere surface complexation and/or ion exchange at low pH, whereas inner-sphere surface complexation or surface precipitation was the main sorption mechanism at high pH values. The presence of FA did not affect Co(II) sorption obviously at pH <7, and a negative effect was observed at pH >7. The Langmuir and Freundlich models were used to simulate the sorption data at different temperatures, and the results indicated that the Langmuir model simulated the data better than the Freundlich isotherm model. The thermodynamic parameters (∆G°, ∆S°, ∆H°) calculated from the temperature-dependent sorption isotherms indicated that the sorption of Co(II) on Na-attapulgite was an endothermic and spontaneous process. The results suggest that the attapulgite sample is a suitable material in the preconcentration and solidification of radiocobalt from large volumes of aqueous solutions.

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Abstract  

N-dodecanoylpyrrolidine (DOPOD) was synthesized and used for the extraction of nitric acid and uranyl(VI) ions from nitric media in toluene. The effects of nitric acid concentration, extractant concentration, temperature, salting-out agent (LiNO3) have been studied. The main adduct of DOPOD and HNO3 is HNO3·DOPOD. The complex formation of uranyl(VI) ion, nitrate ion and DOPOD (UO2(NO3)2·2DOPOD) as extracted species are further confirmed by IR spectra and the values of thermodynamic parameters have also been calculated.

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Abstract  

A new bifunctional extractant named phenyl-N,N-dibutylcarbamoylmethyl sulfoxide (PCMSO) is synthesized and characterized in order to investigate its selectivity and capability in the extraction from acidic nitrate media in nuclear reprocessing. The extraction of uranium (VI) with PCMSO in toluene has been studied at various concentrations of nitric acid, extractant and salting-out agent (LiNO3). The mechanism of extraction is discussed in the light of the results obtained. The extracted species has also been investigated using FT-IR spectrometry. The related thermodynamic functions were calculated. The IR spectral study was also made of the extracted species.

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A simple, rapid, and sensitive liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the simultaneous quantitation of PA-824 and moxifloxacin in rat plasma using carbamazepine as an internal standard (IS). The sample preparation involved a one-step protein precipitation method with methanol. The separation was performed on Inertsil® ODS3 C18 column (150 mm × 4.6 mm, 5 μm) and maintained at 30 °C. The mobile phase consisted of 0.1% formic acid in acetonitrile–water (90:10 v/v) with fast isocratic elution at a flow rate of 0.6 mL/min and a run time of 10 min. A mass spectrometer was run in the positive ion electrospray ionization (ESI) mode using multiple reaction monitoring (MRM) to monitor the mass transitions. The MRM transitions were chosen to be m/z 360.1 → m/z 175.0 for PA-824, m/z 402.0 → m/z 383.9 for moxifloxacin, and m/z 237.1 → m/z 194.0 for IS. The method was fully validated in terms of selectivity, linearity, accuracy, precision, matrix effect, recovery, and stability, respectively. The method was successfully applied to drug–drug interaction (DDI) study of PA-824 and moxifloxacin in rats. The results show that the main pharmacokinetic parameters of PA-824, namely, T max, t 1/2, and AUC(0–t), increased more in the PA-824 and moxifloxacin group than in the PA-824 group. However, there were little changes in the main pharmacokinetic parameters of moxifloxacin from single and combined groups.

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