The proton nuclear magnetic resonance spectroscopy （1H-NMR）, the synchronous fluorescence spectrometry （SFS） and the ruthenium ions catalyzed oxidation （RICO） method were used to determine the chemical structure...The proton nuclear magnetic resonance spectroscopy （1H-NMR）, the synchronous fluorescence spectrometry （SFS） and the ruthenium ions catalyzed oxidation （RICO） method were used to determine the chemical structure of polyaromatic nucleus in Oman residue fractions. The results of 1H-NMR analyses showed that the average numbers of aromatic rings in the aromatics, resins and asphaltenes units were 3.2, 5.6 and 8.2, respectively. SFS was used to investigate the distribution of aromatic rings in residue fractions, the main distribution range of aromatic rings in aromatics, resins and asphaltenes were 3 4 rings, 3--5 rings and more than 5 rings, respectively. The aromatic network in residue fractions was oxidized to produce numerous carboxylic acids. The types and content of benzenepolycarboxylic acids, such as phthalic acid, benzenetricarboxylic acids, benzenetetracarboxylic acids, benzenepentacarboxylic acid and benzenehexacarboxylic acid disclosed the condensed types of aromatic nuclei in the core. The biphenyl fraction （BIPH）, the cata-condensed fraction （CATA）, the peri-condensed fraction （PERI） and the condensed index （BCI） were calculated based on the benzenepolycarboxylic acids formed. The results implied that there was less biphenyl type structures in all residue fractions. The aromatics fraction was almost composed of the cata-condensed type system, and the asphaltenes fraction was wholly composed of the peri-condensed type system, while in the resins fraction co-existed the two types, herein the peri-con- densed type was predominant over the cata-condensed type. Based on the analytical results obtained in the study, the components --aromatics, resins and asphaltenes -- were given the likely structural models.展开更多
In this study, the main factors influencing the measurements by means of the off-line low-field 1H NMR in the lab were discussed base on a robust calibration model established by the PLS algorithm using 255 crude oil ...In this study, the main factors influencing the measurements by means of the off-line low-field 1H NMR in the lab were discussed base on a robust calibration model established by the PLS algorithm using 255 crude oil samples. The preheating temperature had a great influence on the viscosity of oil samples and the resolution of spectral analysis. The repeatability of spectral measurements was impacted by the metal and wax content of the oil samples. For the case of high wax content oils, the wax species began to crystallize in the course of determination that could affect the repeatability of spectral measurements. These factors have evidenced why the preheating devices and filter unit are necessary when low field NMR system is used in the online analysis process. The investigation is very important for the on-line application of the low field NMR.展开更多
This paper presents the neutron energy spectrum in the central position of a neutron flux trap assembled in the core center of the research nuclear reactor IPEN/MB-01, obtained by an unfolding method. To this end, we ...This paper presents the neutron energy spectrum in the central position of a neutron flux trap assembled in the core center of the research nuclear reactor IPEN/MB-01, obtained by an unfolding method. To this end, we have used several different types of activation foils （Au, Sc, Ti, Ni, and plates） which have been irradiated in the central position of the reactor core （setting number 203） at a reactor power level （64.57±2.91 watts）. The activation foils were counted by solid-state detector HPGe （high pure germanium detector） （gamma spectrometry）. The experimental data of nuclear reaction rates （saturated activity per target nucleus） and a neutron spectrum estimated by a reactor physics computer code are the main input data to get the most suitable neutron spectrum in the irradiation position obtained through SANDBP （spectrum analysis neutron detection code-version Budapest University） code： a neutron spectra unfolding code that uses an iterative adjustment method. the integral neutron flux, （2.41 ± 0.01） × 10^9 n·cm^-2·s^-1 for the thermal The adjustment resulted in （3.85 ± 0.14） × 10^9 n·cm^-2·s^-1 for neutron flux, （1.09 ±0.02） × 10^9n·cm^-2·s^-1 for intermediate neutron flux and （3.41 ± 0.02） × 10^8 n·cm^-2·s^-1 for the fast neutrons flux. These results can be used to verify and validate the nuclear reactor codes and its associated nuclear data libraries, besides, show how much effective it can be that the use of a neutron flux trap in the nuclear reactor core to increase the thermal neutron flux without increase the operation reactor power level. The thermal neutral flux increased 4.04 ± 0.21 times compared with the standard configuration of the reactor core.展开更多
Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum....Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.展开更多
文摘The proton nuclear magnetic resonance spectroscopy （1H-NMR）, the synchronous fluorescence spectrometry （SFS） and the ruthenium ions catalyzed oxidation （RICO） method were used to determine the chemical structure of polyaromatic nucleus in Oman residue fractions. The results of 1H-NMR analyses showed that the average numbers of aromatic rings in the aromatics, resins and asphaltenes units were 3.2, 5.6 and 8.2, respectively. SFS was used to investigate the distribution of aromatic rings in residue fractions, the main distribution range of aromatic rings in aromatics, resins and asphaltenes were 3 4 rings, 3--5 rings and more than 5 rings, respectively. The aromatic network in residue fractions was oxidized to produce numerous carboxylic acids. The types and content of benzenepolycarboxylic acids, such as phthalic acid, benzenetricarboxylic acids, benzenetetracarboxylic acids, benzenepentacarboxylic acid and benzenehexacarboxylic acid disclosed the condensed types of aromatic nuclei in the core. The biphenyl fraction （BIPH）, the cata-condensed fraction （CATA）, the peri-condensed fraction （PERI） and the condensed index （BCI） were calculated based on the benzenepolycarboxylic acids formed. The results implied that there was less biphenyl type structures in all residue fractions. The aromatics fraction was almost composed of the cata-condensed type system, and the asphaltenes fraction was wholly composed of the peri-condensed type system, while in the resins fraction co-existed the two types, herein the peri-con- densed type was predominant over the cata-condensed type. Based on the analytical results obtained in the study, the components --aromatics, resins and asphaltenes -- were given the likely structural models.
基金the financial support from the SINOPEC (ST 13028)
文摘In this study, the main factors influencing the measurements by means of the off-line low-field 1H NMR in the lab were discussed base on a robust calibration model established by the PLS algorithm using 255 crude oil samples. The preheating temperature had a great influence on the viscosity of oil samples and the resolution of spectral analysis. The repeatability of spectral measurements was impacted by the metal and wax content of the oil samples. For the case of high wax content oils, the wax species began to crystallize in the course of determination that could affect the repeatability of spectral measurements. These factors have evidenced why the preheating devices and filter unit are necessary when low field NMR system is used in the online analysis process. The investigation is very important for the on-line application of the low field NMR.
文摘This paper presents the neutron energy spectrum in the central position of a neutron flux trap assembled in the core center of the research nuclear reactor IPEN/MB-01, obtained by an unfolding method. To this end, we have used several different types of activation foils （Au, Sc, Ti, Ni, and plates） which have been irradiated in the central position of the reactor core （setting number 203） at a reactor power level （64.57±2.91 watts）. The activation foils were counted by solid-state detector HPGe （high pure germanium detector） （gamma spectrometry）. The experimental data of nuclear reaction rates （saturated activity per target nucleus） and a neutron spectrum estimated by a reactor physics computer code are the main input data to get the most suitable neutron spectrum in the irradiation position obtained through SANDBP （spectrum analysis neutron detection code-version Budapest University） code： a neutron spectra unfolding code that uses an iterative adjustment method. the integral neutron flux, （2.41 ± 0.01） × 10^9 n·cm^-2·s^-1 for the thermal The adjustment resulted in （3.85 ± 0.14） × 10^9 n·cm^-2·s^-1 for neutron flux, （1.09 ±0.02） × 10^9n·cm^-2·s^-1 for intermediate neutron flux and （3.41 ± 0.02） × 10^8 n·cm^-2·s^-1 for the fast neutrons flux. These results can be used to verify and validate the nuclear reactor codes and its associated nuclear data libraries, besides, show how much effective it can be that the use of a neutron flux trap in the nuclear reactor core to increase the thermal neutron flux without increase the operation reactor power level. The thermal neutral flux increased 4.04 ± 0.21 times compared with the standard configuration of the reactor core.
基金Science and Technology Project of Yunnan Provincial Department of Science and Technology(Grant No.2018FD081)Yunnan Local Colleges Applied Basic Research Projects[Grant Nos.2019FH001-(109),2017FH001-092,2017FH001-094 and 2018FH001-019]Youth Research Foundation of Qujing Normal University in 2019(Grant No.2019QN004)。
文摘Cynanchum paniculatum(Bunge) Kitagawa is usually used as an herbal medicine for treating many diseases. Paeonol is the main active component, and its content is the key indicator for quality control of C. paniculatum. In the present study, we developed a rapid, accurate and precise method for quantitation of paeonol in C. paniculatum using 1 H NMR spectra. The deuterated solvent of methanol-d4 enabled satisfactory separation of the signals to be integrated in 1 H NMR spectrum. H-6(δ 7.78) of 1 H NMR spectrum of C. paniculatum was selected as the feature signal for quantitation, and trimesic acid(TMA) was selected as an internal standard. Validation of the quantitative method was performed in terms of linearity, specificity, repeatability and stability. This is the first time to report quantitative 1 H NMR(qHNMR) applied to determine the content of paeonol in C. paniculatum and showed a wider linearity range than the reported quantitation of paeonol in others. The simple extraction of paeonol from C. paniculatum was rapid and will prompt the application of the developed method. This work implied that qHNMR represented a feasible alternative to HPLC-based methods for quantitation of paeonol in C. paniculatum, and it was suitable for the quality control of C. paniculatum.
