Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studi...Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol （Ben-2）, which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.展开更多
A type of home-made reduced activation martensitic steel, high silicon （SIMP） steel, is homogeneously irradiated with energetic Fe ions to the doses of 0.1, 0.25 and 1 displacement per atom （dpa）, respectively, at...A type of home-made reduced activation martensitic steel, high silicon （SIMP） steel, is homogeneously irradiated with energetic Fe ions to the doses of 0.1, 0.25 and 1 displacement per atom （dpa）, respectively, at 300℃ and i dpa, at 400℃. MicrostructurM changes are investigated in detail by transmission electron microscopy with cross-section technique. Interstitial defects and defect dusters induced by Fe-ion irradiation are observed in ali the specimens under different conditions. It is found that with increasing irradiation temperature, size of defect clusters increases while the density drops quickly. The results of element chemical mapping from the STEM images indicate that the Si element enrichment and Ta element depletion occur inside the precipitates in the matrix of SIMP steel irradiated to a dose of 1 dpa at 300℃. Correlations between the microstructure and irradiation conditions are briefly discussed.展开更多
Six representative parent rocks of sand, including limestone, quartzite, gneisses, granite, Basalt and Marble were selected to conduct a systematical research on the effects of various lithologies of manufactured sand...Six representative parent rocks of sand, including limestone, quartzite, gneisses, granite, Basalt and Marble were selected to conduct a systematical research on the effects of various lithologies of manufactured sand on the workability, mechanism properties, volume stability and durability of manufacturedsand concrete. The experimental results show that the strength of manufactured-sand concrete is slightly higher than that of natural-sand concrete. Furthermore, substituting 15% cement of the concrete mixture with equal quantity of the six different lithology stone powder respectively, the data indicated that they can improve the concrete’s workability, postpone the plastic cracking time, enhance the anti-cracking grade, and have no obvious effect on the properties of antifreeze and sulfate attack resistance but reduce the capability to resist chloride ion penetration. Moreover, the differences in concrete’s workability, mechanism properties, volume stability and durability caused by various lithologies of manufactured sand and stone powder were not significant and the influence of lithology variety on the macro properties of concrete could be neglected eventually.展开更多
The formation mechanism of intragranular ferrites with acicular morphology was discussed.The ferrites were characterized by scanning electron microscopy.The results showed that the ferrites had an acicular structure w...The formation mechanism of intragranular ferrites with acicular morphology was discussed.The ferrites were characterized by scanning electron microscopy.The results showed that the ferrites had an acicular structure with radial,symmetrical,and acicular laths,and that the inclusions were the nucleation sites of the intragranular acicular ferrites.Transmission electron microscopy（TEM）was used to characterize the inclusions.The results of TEM with energy dispersive spectroscopy and TEM-selected area electron diffraction indicated that the complex inclusions consisted of Ti-Al complex oxides and MnS.The jagged edges of the complex inclusions can be ascribed to the effects of the crystal structure.The stabilization energy U of the coordination polyhedron growth units varies with the type of connection according to the calculation results.A larger Ucorresponds to more stable growth units,which induces the preferentially oriented growth of inclusions,at which point acicular ferrites are formed.展开更多
A series of Y zeolites exchanged with different amount of cerium and lanthanum cations were investigated. Comprehensive routine analysis tools including X-ray photoelectron spectroscopy（XPS）, X-ray fluorescence（XRF...A series of Y zeolites exchanged with different amount of cerium and lanthanum cations were investigated. Comprehensive routine analysis tools including X-ray photoelectron spectroscopy（XPS）, X-ray fluorescence（XRF）, X-ray diffraction（XRD） and Py-Fourier transform infrared spectroscopy（Py-FTIR） were used to identify the cation location, and the result was verified via XRD Rietveld study. The results revealed that almost all the RE cations in RE-4, most cations in RE-8 to RE-14 and part of cations in RE-16 were located in the sodalite cage. The Al^（IV）/（Al^V＋Al^（VI）） values revealed by ^（27）Al MAS NMR spectra, the silicon aluminum ratio of the framework（SARF） values deduced from ^（29）Si MAS NMR spectra and XRD, and hydroxyl amount were reasonably in accordance with the location and content of rare earth cations. The hydrothermal stability derived from in situ XRD investigation and catalyst activity provided by micro-activity test manifested that samples RE-8 to RE-14 exhibited better performances than RE-4 and RE-16, among which RE-12 had the best properties. The phenomena were interpreted by the cation location and structural properties.展开更多
Four Cu2＋ complexes of salicylidene-amino acid Schiff base with 1,10-phenanthroline （Phen） or 2,2＇- bipyridine （Bipy） were successfully intercalated in interlayer galleries of Mg/AI-NO3-1ayered double hydroxide ...Four Cu2＋ complexes of salicylidene-amino acid Schiff base with 1,10-phenanthroline （Phen） or 2,2＇- bipyridine （Bipy） were successfully intercalated in interlayer galleries of Mg/AI-NO3-1ayered double hydroxide （LDH） by the swelling-restored method. The hybrids were characterized by elemental analysis, X-ray diffraction, FT-IR spectra, UV-vis DRS, TG-DTA and SEM observation. Good protection of the complexes by LDH in neutral and weak acidic solutions was revealed by UV spectra, cyclic voltammograms and luminescence spectra.展开更多
基金the management of Deva Holding A.S., Istanbul, Turkey, for supporting this workthe Scientific and Technological Research Council of Turkey (TUBITAK-TEYDEB Project no: 3110426) for the financial support
文摘Benidipine hydrochloride, used as an antihypertensive agent and long-acting calcium antagonist, is synthesized for commercial use as a drug substance in highly pure form. During the synthetic process development studies of benidipine, process related impurities were detected. These impurities were identified, synthesized and characterized and mechanisms of their formation were discussed in detail. After all standardization procedures, they were used as reference standards for analytical studies. In addition, a separate HPLC method was developed and validated for detection of residual 1-benzylpi- peridin-3-ol （Ben-2）, which is used during benidipine synthesis and controlled as a potential process related impurity. As complementary of this work, stress-testing studies of benidipine were carried out under specified conditions and a stability-indicating UPLC assay method was developed, validated and used during stability studies of benidipine.
基金Supported by the Young Scientists Fund of the National Natural Science Foundation of China under Grant No 11505246the Major Research Plan of the National Natural Science Foundation of China under Grant No 91426301
文摘A type of home-made reduced activation martensitic steel, high silicon （SIMP） steel, is homogeneously irradiated with energetic Fe ions to the doses of 0.1, 0.25 and 1 displacement per atom （dpa）, respectively, at 300℃ and i dpa, at 400℃. MicrostructurM changes are investigated in detail by transmission electron microscopy with cross-section technique. Interstitial defects and defect dusters induced by Fe-ion irradiation are observed in ali the specimens under different conditions. It is found that with increasing irradiation temperature, size of defect clusters increases while the density drops quickly. The results of element chemical mapping from the STEM images indicate that the Si element enrichment and Ta element depletion occur inside the precipitates in the matrix of SIMP steel irradiated to a dose of 1 dpa at 300℃. Correlations between the microstructure and irradiation conditions are briefly discussed.
基金Funded by the National West Communication Construction Technology Project(No.2013 318 354 190)
文摘Six representative parent rocks of sand, including limestone, quartzite, gneisses, granite, Basalt and Marble were selected to conduct a systematical research on the effects of various lithologies of manufactured sand on the workability, mechanism properties, volume stability and durability of manufacturedsand concrete. The experimental results show that the strength of manufactured-sand concrete is slightly higher than that of natural-sand concrete. Furthermore, substituting 15% cement of the concrete mixture with equal quantity of the six different lithology stone powder respectively, the data indicated that they can improve the concrete’s workability, postpone the plastic cracking time, enhance the anti-cracking grade, and have no obvious effect on the properties of antifreeze and sulfate attack resistance but reduce the capability to resist chloride ion penetration. Moreover, the differences in concrete’s workability, mechanism properties, volume stability and durability caused by various lithologies of manufactured sand and stone powder were not significant and the influence of lithology variety on the macro properties of concrete could be neglected eventually.
基金Item Sponsored by National Natural Science Foundation of China(51574106,51474089)Key Funds of Natural Science Foundation of Hebei Province of China(E2016209396)+1 种基金Natural Science Foundation of Hebei Province of China(E2013209207)Research Science Institute on High-level Personnel of Colleges in Hebei Province of China(GCC20142030)
文摘The formation mechanism of intragranular ferrites with acicular morphology was discussed.The ferrites were characterized by scanning electron microscopy.The results showed that the ferrites had an acicular structure with radial,symmetrical,and acicular laths,and that the inclusions were the nucleation sites of the intragranular acicular ferrites.Transmission electron microscopy（TEM）was used to characterize the inclusions.The results of TEM with energy dispersive spectroscopy and TEM-selected area electron diffraction indicated that the complex inclusions consisted of Ti-Al complex oxides and MnS.The jagged edges of the complex inclusions can be ascribed to the effects of the crystal structure.The stabilization energy U of the coordination polyhedron growth units varies with the type of connection according to the calculation results.A larger Ucorresponds to more stable growth units,which induces the preferentially oriented growth of inclusions,at which point acicular ferrites are formed.
基金Project supported by the Foundation of SINOPEC(111015)
文摘A series of Y zeolites exchanged with different amount of cerium and lanthanum cations were investigated. Comprehensive routine analysis tools including X-ray photoelectron spectroscopy（XPS）, X-ray fluorescence（XRF）, X-ray diffraction（XRD） and Py-Fourier transform infrared spectroscopy（Py-FTIR） were used to identify the cation location, and the result was verified via XRD Rietveld study. The results revealed that almost all the RE cations in RE-4, most cations in RE-8 to RE-14 and part of cations in RE-16 were located in the sodalite cage. The Al^（IV）/（Al^V＋Al^（VI）） values revealed by ^（27）Al MAS NMR spectra, the silicon aluminum ratio of the framework（SARF） values deduced from ^（29）Si MAS NMR spectra and XRD, and hydroxyl amount were reasonably in accordance with the location and content of rare earth cations. The hydrothermal stability derived from in situ XRD investigation and catalyst activity provided by micro-activity test manifested that samples RE-8 to RE-14 exhibited better performances than RE-4 and RE-16, among which RE-12 had the best properties. The phenomena were interpreted by the cation location and structural properties.
基金supported by Beijing Municipal Natural Science Foundation(No.2112022)Key Laboratory of Radiopharmaceuticals of Ministry of Education(College of Chemistry, Beijing Normal University) and Analytical and Testing Center of Beijing Normal University
文摘Four Cu2＋ complexes of salicylidene-amino acid Schiff base with 1,10-phenanthroline （Phen） or 2,2＇- bipyridine （Bipy） were successfully intercalated in interlayer galleries of Mg/AI-NO3-1ayered double hydroxide （LDH） by the swelling-restored method. The hybrids were characterized by elemental analysis, X-ray diffraction, FT-IR spectra, UV-vis DRS, TG-DTA and SEM observation. Good protection of the complexes by LDH in neutral and weak acidic solutions was revealed by UV spectra, cyclic voltammograms and luminescence spectra.
