To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry ...To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.展开更多
A new type of HPLC stationary phase containing thymine derivative was successfully prepared.It was found to give selective separation of nucleic acid bases and several purine derivatives,such as caffeine and theophyll...A new type of HPLC stationary phase containing thymine derivative was successfully prepared.It was found to give selective separation of nucleic acid bases and several purine derivatives,such as caffeine and theophylline.The retention behaviour and elution order of the solutes were interpreted in terms of molecular structure.展开更多
A novel slow-down set waveform is proposed to improve the set performance and a 1 kb phase change random access memory chip fabricated with a 13nm CMOS technology is implemented to investigate the set performance by d...A novel slow-down set waveform is proposed to improve the set performance and a 1 kb phase change random access memory chip fabricated with a 13nm CMOS technology is implemented to investigate the set performance by different set programming strategies based on this new set pulse. The amplitude difference （I1 - I2） of the set pulse is proved to be a crucial parameter for set programming. We observe and analyze the cell characteristics with different I1 - I2 by means of thermal simulations and high-resolution transmission electron microscopy, which reveal that an incomplete set programming will occur when the proposed slow-down pulse is set with an improperly high I1 - I2. This will lead to an amorphous residue in the active region. We also discuss the programming method to avoid the set performance degradations.展开更多
Mg–Zn–Ag alloys have been extensively studied in recent years for potential biodegradable implants due to their unique mechanical properties,biodegradability and biocompatibility.In the present study,Mg–3Zn-x Ag（w...Mg–Zn–Ag alloys have been extensively studied in recent years for potential biodegradable implants due to their unique mechanical properties,biodegradability and biocompatibility.In the present study,Mg–3Zn-x Ag（wt%,x=0.2,0.5 and0.8）alloys with single-phase crystal structure were prepared by backward extrusion at 340°C.The addition of Ag element into Mg–3Zn slightly influences the ultimate tensile strength and microstructure,but the elongation firstly increases from12%to 19.8%and then decreases from 19.8%to 9.9%with the increment of Ag concentration.The tensile yield strength,ultimate tensile strength and elongation of Mg–3Zn–0.2Ag alloy reach up to 142,234 MPa and 19.8%,respectively,which are the best mechanical performance of Mg–Zn–Ag alloys in the present work.The extruded Mg–3Zn–0.2Ag alloy also possesses the best corrosion behavior with the corresponding corrosion rate of 3.2 mm/year in immersion test,which could be explained by the single-phase and uniformly distributed grain structure,and the fewer twinning.展开更多
An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading,...An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading, washing, and eluting） used a flow rate of1.0 m L/min, and dicyandiamide was eluted with 20 m L of a methanol/acetonitrile mixture（V/V = 2：3）, followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy（HPLC–UV）. Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge（with activated carbon）.Separation was achieved on a ZIC-Hydrophilic Interaction Liquid Chromatography（ZIC-HILIC）（50 mm × 2.1 mm, 3.5 μm） chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions（R^2〉 0.999）. Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations（RSDs, n = 3） were below 6.1% with a detection limit of 5.0 ng/m L for stream water samples.展开更多
Si_(3)N_(4)ceramics contain two crystalline phases:a-Si_(3)N_(4)andβ-Si_(3)N_(4),distinguished by their stacking sequences along the c-axis.The equiaxed grains of a-Si_(3)N_(4)with the ABCD stacking sequence show hig...Si_(3)N_(4)ceramics contain two crystalline phases:a-Si_(3)N_(4)andβ-Si_(3)N_(4),distinguished by their stacking sequences along the c-axis.The equiaxed grains of a-Si_(3)N_(4)with the ABCD stacking sequence show high hardness.In contrast,theβ-phase adopts an ABAB stacking pattern and forms elongated columnar grains through preferential growth along the c-axis.展开更多
Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of...Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of parathyroid hormone (PTH) in presence of meta-cresol as a stabilizer in a pharmaceutical formulation.Chromatography was performed with mobile phase containing 0.1% Trifluoroacetic acid (TFA) in MilliQ water and 0.1% TFA in acetonitrile with gradient program and flow rate at 0.3 mL/min for HPLC and 0.4 mL/min for UPLC.Quantification was accomplished with internal reference standard (qualified against innovator product and National Institute for Biological Standards and Control (NIBSC) standard).The methods were validated for linearity (correlation coefficient 0.99),range,accuracy,precision and robustness.Robustness was confirmed by considering three factors;mobile phase composition,column temperature and flow rate/age of mobile phase.Intermediate precision was confirmed on different equipments,different columns and on different days.The relative standard deviation (RSD) (<2% for RP-HPLC and <1% for UPLC,n=30) indicated a good precision.Retention time was found about 17 min and 2 min by HPLC and UPLC methods,respectively.Both methods are simple,highly sensitive,precise and accurate and have the potential of being useful for routine quality control.展开更多
LaMgNi（4-x）Cox（x = 0-0.8） electrode alloys used for MH/Ni batteries were prepared by induction melting. The structures and electrochemical hydrogen storage properties of the alloys were investigated in detail.X-ra...LaMgNi（4-x）Cox（x = 0-0.8） electrode alloys used for MH/Ni batteries were prepared by induction melting. The structures and electrochemical hydrogen storage properties of the alloys were investigated in detail.X-ray diffraction（XRD） and scanning electron microscopy（SEM） analysis show that LaMgNi4 phase and LaNi5 phase are obtained. The lattice parameters of the two phases increase first and then decrease with Co content increasing.The electrochemical properties of the alloy electrodes were measured by means of simulated battery tests. Results show that the addition of Co does not change the discharge voltage plateau of the alloy electrodes. However, the maximum discharge capacity increases from 319.9 mAh·g^-1（x = 0）to 347.5 mAh·g^-1（x = 0.4） and then decreases to331.7 mAh·g^-1（x = 0.8）. The effects of Co content on electrochemical kinetics of the alloy electrodes were also performed. The high rate dischargeability（HRD） first increases and then decreases with Co content increasing and reaches the maximum value（95.0 %） when x = 0.4. Test results of the electrochemical impedance spectra（EIS）,potentiodynamic polarization curves and constant potential step measurements of the alloy electrodes all demonstrate that when Co content is 0.4 at%, the alloy exhibits the best comprehensive electrochemical properties.展开更多
Sixteen indole derivatives have been computed at B3LYP/6-31 IG^＊＊ level using density functional theory （DFF）. Based on linear solvation energy theory, the structural parameters were employed to present correlatio...Sixteen indole derivatives have been computed at B3LYP/6-31 IG^＊＊ level using density functional theory （DFF）. Based on linear solvation energy theory, the structural parameters were employed to present correlation between the parameters of chromatograph capacity factor （CCF） and molecular structural parameters. As a result, the correlation equation of the reversed phased high performance liquid chromatograph capacity factor to the intercept lgk＇w and slope S of CCF were obtained, from which the correlation coefficients of lgk＇w to the structural parameters are r^2 = 0.9596 and q^2 = 0.9262. While the correlation coefficients of the parameter S r^2 q^2 with structures are = 0.9750 and = 0.9252. Moreover, the effect of water as solvent on the present two models was also considered using SCRF method, and the result shows that the predicting capacity of correlation equation of lgkw＇ increases, while that of the model for S decreases slightly. Both two correlation equations achieved in this work are more advantageous than those using theoretical descriptors from molecular connectivity indices.展开更多
基金supported by the Preventive medicine and public health research project of Anhui,China(No.2011Y0103)the Natural Science Foundation of Anhui,China(No.11040606M216)
文摘To establish an analytical method for determination of four bisphenols （BPA, BPB, BPF, and BPS） and two alkylphenols （4-n-OP, 4-n-NP） in water by ultra performance liquid chromatography- tandem mass spectrometry （UPLC/MS/MS）. The water samples were extracted and condensed with solid-phase extraction （SPE） using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%.
文摘A new type of HPLC stationary phase containing thymine derivative was successfully prepared.It was found to give selective separation of nucleic acid bases and several purine derivatives,such as caffeine and theophylline.The retention behaviour and elution order of the solutes were interpreted in terms of molecular structure.
基金Supported by the Strategic Priority Research Program of Chinese Academy of Sciences under Grant No XDA09020402the National Key Basic Research Program of China under Grant Nos 2013CBA01900,2010CB934300,2011CBA00607,and 2011CB932804+2 种基金the National Integrate Circuit Research Program of China under Grant No 2009ZX02023-003the National Natural Science Foundation of China under Grant Nos 61176122,61106001,61261160500,and 61376006the Science and Technology Council of Shanghai under Grant Nos 12nm0503701,13DZ2295700,12QA1403900,and 13ZR1447200
文摘A novel slow-down set waveform is proposed to improve the set performance and a 1 kb phase change random access memory chip fabricated with a 13nm CMOS technology is implemented to investigate the set performance by different set programming strategies based on this new set pulse. The amplitude difference （I1 - I2） of the set pulse is proved to be a crucial parameter for set programming. We observe and analyze the cell characteristics with different I1 - I2 by means of thermal simulations and high-resolution transmission electron microscopy, which reveal that an incomplete set programming will occur when the proposed slow-down pulse is set with an improperly high I1 - I2. This will lead to an amorphous residue in the active region. We also discuss the programming method to avoid the set performance degradations.
基金supported by the National Natural Science Foundation of China (Nos. 51371046 and 51525101)the National Key Research and Development Program of China (No. 2016YFB0701202)the Fundamental Research Funds of the Central Universities (No. N141008001)
文摘Mg–Zn–Ag alloys have been extensively studied in recent years for potential biodegradable implants due to their unique mechanical properties,biodegradability and biocompatibility.In the present study,Mg–3Zn-x Ag（wt%,x=0.2,0.5 and0.8）alloys with single-phase crystal structure were prepared by backward extrusion at 340°C.The addition of Ag element into Mg–3Zn slightly influences the ultimate tensile strength and microstructure,but the elongation firstly increases from12%to 19.8%and then decreases from 19.8%to 9.9%with the increment of Ag concentration.The tensile yield strength,ultimate tensile strength and elongation of Mg–3Zn–0.2Ag alloy reach up to 142,234 MPa and 19.8%,respectively,which are the best mechanical performance of Mg–Zn–Ag alloys in the present work.The extruded Mg–3Zn–0.2Ag alloy also possesses the best corrosion behavior with the corresponding corrosion rate of 3.2 mm/year in immersion test,which could be explained by the single-phase and uniformly distributed grain structure,and the fewer twinning.
基金Department of Chemistry at Mississippi State University for financial support for this project
文摘An improved method for trace level quantification of dicyandiamide in stream water has been developed. This method includes sample pretreatment using solid phase extraction.The extraction procedure（including loading, washing, and eluting） used a flow rate of1.0 m L/min, and dicyandiamide was eluted with 20 m L of a methanol/acetonitrile mixture（V/V = 2：3）, followed by pre-concentration using nitrogen evaporation and analysis with high performance liquid chromatography–ultraviolet spectroscopy（HPLC–UV）. Sample extraction was carried out using a Waters Sep-Pak AC-2 Cartridge（with activated carbon）.Separation was achieved on a ZIC-Hydrophilic Interaction Liquid Chromatography（ZIC-HILIC）（50 mm × 2.1 mm, 3.5 μm） chromatography column and quantification was accomplished based on UV absorbance. A reliable linear relationship was obtained for the calibration curve using standard solutions（R^2〉 0.999）. Recoveries for dicyandiamide ranged from 84.6% to 96.8%, and the relative standard deviations（RSDs, n = 3） were below 6.1% with a detection limit of 5.0 ng/m L for stream water samples.
基金financially supported by the National Natural Science Foundation of China(52322207,92163208,and 52494933)the National Key Research and Development Plan of China(2021YFB3701400)the Independent Innovation Projects of the Hubei Longzhong Laboratory(2022ZZ-11)。
文摘Si_(3)N_(4)ceramics contain two crystalline phases:a-Si_(3)N_(4)andβ-Si_(3)N_(4),distinguished by their stacking sequences along the c-axis.The equiaxed grains of a-Si_(3)N_(4)with the ABCD stacking sequence show high hardness.In contrast,theβ-phase adopts an ABAB stacking pattern and forms elongated columnar grains through preferential growth along the c-axis.
文摘Rapid and sensitive reversed phase high performance liquid chromatography (RP-HPLC) and ultra performance liquid chromatography (RP-UPLC) method with UV detection has been developed and validated for quantification of parathyroid hormone (PTH) in presence of meta-cresol as a stabilizer in a pharmaceutical formulation.Chromatography was performed with mobile phase containing 0.1% Trifluoroacetic acid (TFA) in MilliQ water and 0.1% TFA in acetonitrile with gradient program and flow rate at 0.3 mL/min for HPLC and 0.4 mL/min for UPLC.Quantification was accomplished with internal reference standard (qualified against innovator product and National Institute for Biological Standards and Control (NIBSC) standard).The methods were validated for linearity (correlation coefficient 0.99),range,accuracy,precision and robustness.Robustness was confirmed by considering three factors;mobile phase composition,column temperature and flow rate/age of mobile phase.Intermediate precision was confirmed on different equipments,different columns and on different days.The relative standard deviation (RSD) (<2% for RP-HPLC and <1% for UPLC,n=30) indicated a good precision.Retention time was found about 17 min and 2 min by HPLC and UPLC methods,respectively.Both methods are simple,highly sensitive,precise and accurate and have the potential of being useful for routine quality control.
基金financially supported by the National Natural Science Foundations of China (Nos.51161015,51371094 and 51471054)
文摘LaMgNi（4-x）Cox（x = 0-0.8） electrode alloys used for MH/Ni batteries were prepared by induction melting. The structures and electrochemical hydrogen storage properties of the alloys were investigated in detail.X-ray diffraction（XRD） and scanning electron microscopy（SEM） analysis show that LaMgNi4 phase and LaNi5 phase are obtained. The lattice parameters of the two phases increase first and then decrease with Co content increasing.The electrochemical properties of the alloy electrodes were measured by means of simulated battery tests. Results show that the addition of Co does not change the discharge voltage plateau of the alloy electrodes. However, the maximum discharge capacity increases from 319.9 mAh·g^-1（x = 0）to 347.5 mAh·g^-1（x = 0.4） and then decreases to331.7 mAh·g^-1（x = 0.8）. The effects of Co content on electrochemical kinetics of the alloy electrodes were also performed. The high rate dischargeability（HRD） first increases and then decreases with Co content increasing and reaches the maximum value（95.0 %） when x = 0.4. Test results of the electrochemical impedance spectra（EIS）,potentiodynamic polarization curves and constant potential step measurements of the alloy electrodes all demonstrate that when Co content is 0.4 at%, the alloy exhibits the best comprehensive electrochemical properties.
基金This work was supported by the National Basic Research Program of China (2003CB415002) and the China Postdoctoral Science Foundation (No. 2003033486) and the Natural Science Research Fund of University in Jiangsu (04KJB150149)
文摘Sixteen indole derivatives have been computed at B3LYP/6-31 IG^＊＊ level using density functional theory （DFF）. Based on linear solvation energy theory, the structural parameters were employed to present correlation between the parameters of chromatograph capacity factor （CCF） and molecular structural parameters. As a result, the correlation equation of the reversed phased high performance liquid chromatograph capacity factor to the intercept lgk＇w and slope S of CCF were obtained, from which the correlation coefficients of lgk＇w to the structural parameters are r^2 = 0.9596 and q^2 = 0.9262. While the correlation coefficients of the parameter S r^2 q^2 with structures are = 0.9750 and = 0.9252. Moreover, the effect of water as solvent on the present two models was also considered using SCRF method, and the result shows that the predicting capacity of correlation equation of lgkw＇ increases, while that of the model for S decreases slightly. Both two correlation equations achieved in this work are more advantageous than those using theoretical descriptors from molecular connectivity indices.
