A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyr...A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyridylazo ) -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu ( Ⅱ ). This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.展开更多
In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4...In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4-aminobiphenyl in aqueous matrices. After extraction the ionic liquid (IL) phase was injected directly into the high performance liquid chromatography (HPLC) system for determination. Some parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. The limits of detection (LOD, S/N = 3) for the four analytes were in the range of 0.45-2.6 μg L^-1. The relative standard deviations (R.S.D., n = 6) were in the range of 6.2-9.8%. This method was applied for the analysis of the real water samples. The recoveries ranged from 93.4 to 106.4%. The main advantages of the method are high speed, high recovery, good repeatability and volatile organic solvent-free.展开更多
The effect of vanadium addition to Cu/γ-Al2O3 catalyst used in the hydrogenation of CO2 to produce methanol was studied. It was found that the catalytic performance of the Cu-based catalyst improved after V addition....The effect of vanadium addition to Cu/γ-Al2O3 catalyst used in the hydrogenation of CO2 to produce methanol was studied. It was found that the catalytic performance of the Cu-based catalyst improved after V addition. The influence of reaction temperature, space velocity and the molar ratio of H2 to CO2 on the performance of 12%Cu-6%V/γ-Al2O3 catalyst were also studied. The results indicated that the best conditions for reaction were as follows: 240 ℃, 3600 h^-1 and a molar ratio of H2 to 602 of 3:1. The results of XRD and TPR characterization demonstrated that the addition of V enhanced the dispersion of the supported CuO species, which resulted in the enhanced catalytic performance of Cu-V/γ-Al2O3 binary catalyst.展开更多
A novel efficient catalyst for the hydrogenation of carbon dioxide to formic acid ruthenium bisphosphine on functionalized silica was in situ synthesized, affording turnover frequency (TOF) of 1190 h^-1 at 100% sele...A novel efficient catalyst for the hydrogenation of carbon dioxide to formic acid ruthenium bisphosphine on functionalized silica was in situ synthesized, affording turnover frequency (TOF) of 1190 h^-1 at 100% selectivity under 80℃ with total pressure of 16.0 MPa. The catalyst can be separated from the reaction mixture easily and reused with moderate loss of activity.展开更多
A Pt-nanooarticle/carbon nanotube modified graphite electrode immobilized with cholesterol oxidase/sol'-gel layer was developed for monitoring cholesterol.Using this electrode,cholesterol concentration(4.0×10^-...A Pt-nanooarticle/carbon nanotube modified graphite electrode immobilized with cholesterol oxidase/sol'-gel layer was developed for monitoring cholesterol.Using this electrode,cholesterol concentration(4.0×10^-6 tp 1.0×10^-4mol/L)could be determined accurately in the presence of ascorbic or uric acid,and the response time was rapid (〈 20 s). This biosensor has high sensitivity and selectivity.展开更多
Tetrahydrofuran ring can be opened with acyl chlorides or anhydrides catalyzed by gallium triiodides to afford iodo esters under mild conditions in good yields.
Enamines, promoted by the samarium/samarium diiodide mixed reagent, were synthesized via the cross-coupling of thioamides and diarylketones in good yields.
A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All sp...A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolunm derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits (LOD, signal-to-noise ratio of 3) of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations (RSD, n = 10) of formaldehyde sulfoxylate, sulflte, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.展开更多
A new catalyst support, Ce-Mg-O, was prepared in a novel way macromolecule surfactant modified method and was used as a catalyst support for low-temperature methane combustion. The results indicate that the new type o...A new catalyst support, Ce-Mg-O, was prepared in a novel way macromolecule surfactant modified method and was used as a catalyst support for low-temperature methane combustion. The results indicate that the new type of FeOx/Ce- Mg-O catalyst exhibits high activity in low-temperature methane combustion, such that the T90 at which 90% conversion of methane occurs can be obtained at 560 ℃. The structure of the catalyst and the effect of the supporter on catalytic activity were characterized by transmission electronic microscopy (TEM), X-ray diffraction (XRD), and temperature-programmed reduction (TPR). The results indicate that the high catalytic activity of FeOx/Ce-Mg-O over methane combustion is strongly dependent on the particle size, typical crystal phase of the Ce-Mg-O, and the interaction of FeOx and Ce-Mg-O.展开更多
In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-...In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.展开更多
A La^3+-Cu/Pt modified electrode was fabricated by electrodepositing process in CuS04 solution by adding a small amount of lanthium compound, and it was employed for direct current (DC) amperometric detection of sp...A La^3+-Cu/Pt modified electrode was fabricated by electrodepositing process in CuS04 solution by adding a small amount of lanthium compound, and it was employed for direct current (DC) amperometric detection of spectinomycin by anion-exchange chromatography. Without derivatization, this method can simultaneously determine the main component and impurities in spectinomycin pharmaceutical raw material. Ease of preparation, being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor for the determination of spectinomycin.展开更多
A convenient method has been developed toward the stereoselective synthesis of N-substituted benzotriazole derivatives under mild conditions. The good stereolectivity, high yields and the simple procedure make the pre...A convenient method has been developed toward the stereoselective synthesis of N-substituted benzotriazole derivatives under mild conditions. The good stereolectivity, high yields and the simple procedure make the present protocol attractive.展开更多
In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 2...In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine (TDA) which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column (150 mm ×4.0 mm) using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection (LOD, 0.13 μg L^-1) was obtained. Within-day relative standard deviation (R.S.D.) was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.展开更多
In this paper, we give a convergence theorem and error estimates for an iteration method under new Kantorovitch-Ostrowski type condition using the information of higher derivatives at initial points. Compared with the...In this paper, we give a convergence theorem and error estimates for an iteration method under new Kantorovitch-Ostrowski type condition using the information of higher derivatives at initial points. Compared with the corresponding study in [3], the convergence determination is established under one global condition, instead of two, on the function.展开更多
Nanosized orthorhombic LiMnO2 was successfully synthesized using Mn2O3 and LiOH.H2O as starting materials.Not only the reaction temperature was lower, but the reaction time for synthesizing was notably shortened to 1 ...Nanosized orthorhombic LiMnO2 was successfully synthesized using Mn2O3 and LiOH.H2O as starting materials.Not only the reaction temperature was lower, but the reaction time for synthesizing was notably shortened to 1 h.In this hydrothermal process, the cations of the starting materials were capable of mixing and interacting in ionic scale, which resulted in the rapid formation of o-LiMnO2 powders at relatively low temperature. The particle size conformed by transmission electron microscopy is around 50-150 nm. Benefiting from its small particle size and good uniformity, the obtained o-LiMnO2 can reach the maximum discharge capacity of 163 mA-h.g^-1 at 0.1 C rate after several cycles. X-ray diffraction data and electrochemical properties suggested the phase transformation from orthorhombic LiMnO2 to defect-type spinel LiMn204 with minor Li2MnO3, which resulted in the capacity fading during cycling.展开更多
An efficient route to synthesize the heteroaryl-substituted 1,8-naphthyridine derivatives was described. Eight 2-heteroaryl- and 2,7-diheteroaryl-1,8-naphthyridine derivatives were obtained through palladium-catalyzed...An efficient route to synthesize the heteroaryl-substituted 1,8-naphthyridine derivatives was described. Eight 2-heteroaryl- and 2,7-diheteroaryl-1,8-naphthyridine derivatives were obtained through palladium-catalyzed C-N-coupling reactions of chloronaphthyridines with imidazole, benzimidazole, morpholine, 3,5-dimethylpyrazole, and phthalimide in moderate to good yields.展开更多
The diaryldiselenides reacted with titanocene hydried (Cp2TiH) generted from Cp2TiCl2/i-BuMgBr to give arylselenium complexes of titanocene. They reacted readily with diaryliodoiums salt to give unsymmetical diaryls...The diaryldiselenides reacted with titanocene hydried (Cp2TiH) generted from Cp2TiCl2/i-BuMgBr to give arylselenium complexes of titanocene. They reacted readily with diaryliodoiums salt to give unsymmetical diarylselenides.展开更多
基金the Analysis and Testing Foundation of Zhejiang Province(No 04045)
文摘A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry (ETAAS) after cloud point extraction ( CPE ). 1-( 2-Pyridylazo ) -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu ( Ⅱ ). This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.
基金the National Natural Science Foundation of China(Nos.20375035,20527005,20775070)by Zhejiang Provincial Natural Science Foundation of China(Nos.Z404105,Y507252).
文摘In this work, a new microextraction method termed ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) was demonstrated for the extraction of 2-methylaniline, 4-chloroaniline, 1-naphthylamine and 4-aminobiphenyl in aqueous matrices. After extraction the ionic liquid (IL) phase was injected directly into the high performance liquid chromatography (HPLC) system for determination. Some parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. The limits of detection (LOD, S/N = 3) for the four analytes were in the range of 0.45-2.6 μg L^-1. The relative standard deviations (R.S.D., n = 6) were in the range of 6.2-9.8%. This method was applied for the analysis of the real water samples. The recoveries ranged from 93.4 to 106.4%. The main advantages of the method are high speed, high recovery, good repeatability and volatile organic solvent-free.
基金Project Supported by NSFC (10131040)SRFDP (2002335090)
文摘A law of iterated logarithm for R/S statistics with the help of the strong approximations of R/S statistics by functions of a Wiener process is shown.
基金This work is supported by the Natural Science Foundation of Zhejiang Province (No. 405088)
文摘The effect of vanadium addition to Cu/γ-Al2O3 catalyst used in the hydrogenation of CO2 to produce methanol was studied. It was found that the catalytic performance of the Cu-based catalyst improved after V addition. The influence of reaction temperature, space velocity and the molar ratio of H2 to CO2 on the performance of 12%Cu-6%V/γ-Al2O3 catalyst were also studied. The results indicated that the best conditions for reaction were as follows: 240 ℃, 3600 h^-1 and a molar ratio of H2 to 602 of 3:1. The results of XRD and TPR characterization demonstrated that the addition of V enhanced the dispersion of the supported CuO species, which resulted in the enhanced catalytic performance of Cu-V/γ-Al2O3 binary catalyst.
基金the National Natural Science Foundation of China (No.20173048) the Specialized Research Fund for the Doctoral Program of Higher Education (No. 20030335068)+1 种基金 the Scientific Research Fund of Zhcjiang Provincial Education Department (No. 20040320) Zhcjiang Provincial Natural Science Foundation of China (No. Y405088).
文摘A novel efficient catalyst for the hydrogenation of carbon dioxide to formic acid ruthenium bisphosphine on functionalized silica was in situ synthesized, affording turnover frequency (TOF) of 1190 h^-1 at 100% selectivity under 80℃ with total pressure of 16.0 MPa. The catalyst can be separated from the reaction mixture easily and reused with moderate loss of activity.
基金The project is supported by the National Natural Science Foundation of China(29975024,202750-34)Key Project of Science and Technology of Zhejiang Province(2003C21024).The authors acknowledge the Instrumental Analysis Center of Zhejiang University for special measurements.
文摘A Pt-nanooarticle/carbon nanotube modified graphite electrode immobilized with cholesterol oxidase/sol'-gel layer was developed for monitoring cholesterol.Using this electrode,cholesterol concentration(4.0×10^-6 tp 1.0×10^-4mol/L)could be determined accurately in the presence of ascorbic or uric acid,and the response time was rapid (〈 20 s). This biosensor has high sensitivity and selectivity.
基金the National Natural Science Foundation of China !298720I0the NSF of she-hang Provincethe Laboratory of Organometallic Ch
文摘Tetrahydrofuran ring can be opened with acyl chlorides or anhydrides catalyzed by gallium triiodides to afford iodo esters under mild conditions in good yields.
基金the National Natural Science Foundation of China(Project No.20072033)Specialized Research Fund for the Doctoral Program of Higher Education of China.
文摘Enamines, promoted by the samarium/samarium diiodide mixed reagent, were synthesized via the cross-coupling of thioamides and diarylketones in good yields.
基金supported by National Natural Science Foundation of China(No.20775070) Zhejiang Provincial Natural Science Foundation of China(No.Y507252)+1 种基金Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028) Zhejiang Provincial Analysis and Testing Foundation of China(No.2007F70061)
文摘A novel method for determination of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate in foodstuffs by ion chromatography separation with postcolumn derivation and UV detection has been developed. All species are separated at Dionex IonPac AG22A and AS22A with mobile phase of a mixture of 4.5 mmol/L sodium carbonate and 0.8 mmol/L sodium bicarbonate at a flow-rate of 1.0 mL/min. The postcolunm derivation solution was 0.24% iodine in 0.2% phosphate acid and the detection wavelength was set at 288 nm. The detection limits (LOD, signal-to-noise ratio of 3) of formaldehyde sulfoxylate, sulfite, thiocyanate, and thiosulfate were 0.004, 0.006, 0.006, and 0.007 mg/L, respectively. Within-day relative standard deviations (RSD, n = 10) of formaldehyde sulfoxylate, sulflte, thiocyanate, and thiosulfate were 3.24%, 3.76%, 2.68%, and 2.07%, respectively. The recoveries of the four anions were in the range of 67.2-116.5%.
基金Project supported bythe Natural Science Foundation of Zhejiang Province (Y505285)
文摘A new catalyst support, Ce-Mg-O, was prepared in a novel way macromolecule surfactant modified method and was used as a catalyst support for low-temperature methane combustion. The results indicate that the new type of FeOx/Ce- Mg-O catalyst exhibits high activity in low-temperature methane combustion, such that the T90 at which 90% conversion of methane occurs can be obtained at 560 ℃. The structure of the catalyst and the effect of the supporter on catalytic activity were characterized by transmission electronic microscopy (TEM), X-ray diffraction (XRD), and temperature-programmed reduction (TPR). The results indicate that the high catalytic activity of FeOx/Ce-Mg-O over methane combustion is strongly dependent on the particle size, typical crystal phase of the Ce-Mg-O, and the interaction of FeOx and Ce-Mg-O.
基金supported by National Natural Science Foundation of China(No.20775070)by Zhejiang Provincial Natural Science Foundation of China(No.R4080124)Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028).
文摘In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.
基金supported by National Natural Science Foundation of China(No.20775070)Zhejiang Provincial Natural Science Foundation of China(No.Y407153)sponsored by Zhejiang Provincial Assay Foundation of China(No.2007F70017)
文摘A La^3+-Cu/Pt modified electrode was fabricated by electrodepositing process in CuS04 solution by adding a small amount of lanthium compound, and it was employed for direct current (DC) amperometric detection of spectinomycin by anion-exchange chromatography. Without derivatization, this method can simultaneously determine the main component and impurities in spectinomycin pharmaceutical raw material. Ease of preparation, being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor for the determination of spectinomycin.
基金the National Natural Science Foundation of China (No. 20072033)Specialized Research Fund for the Doctoral Program of Higher Education of China.
文摘A convenient method has been developed toward the stereoselective synthesis of N-substituted benzotriazole derivatives under mild conditions. The good stereolectivity, high yields and the simple procedure make the present protocol attractive.
基金supported by the National Natural Science Foundation of China(No.20775070)Zhejiang Provincial Natural Science Foundation of China(No.Y507252).
文摘In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine (TDA) which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column (150 mm ×4.0 mm) using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection (LOD, 0.13 μg L^-1) was obtained. Within-day relative standard deviation (R.S.D.) was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.
文摘In this paper, we give a convergence theorem and error estimates for an iteration method under new Kantorovitch-Ostrowski type condition using the information of higher derivatives at initial points. Compared with the corresponding study in [3], the convergence determination is established under one global condition, instead of two, on the function.
基金supported by the National Natural Science Foundation of China under grant No.50372058.
文摘Nanosized orthorhombic LiMnO2 was successfully synthesized using Mn2O3 and LiOH.H2O as starting materials.Not only the reaction temperature was lower, but the reaction time for synthesizing was notably shortened to 1 h.In this hydrothermal process, the cations of the starting materials were capable of mixing and interacting in ionic scale, which resulted in the rapid formation of o-LiMnO2 powders at relatively low temperature. The particle size conformed by transmission electron microscopy is around 50-150 nm. Benefiting from its small particle size and good uniformity, the obtained o-LiMnO2 can reach the maximum discharge capacity of 163 mA-h.g^-1 at 0.1 C rate after several cycles. X-ray diffraction data and electrochemical properties suggested the phase transformation from orthorhombic LiMnO2 to defect-type spinel LiMn204 with minor Li2MnO3, which resulted in the capacity fading during cycling.
基金the National Natural Science Foundation of China (no. 20572096) the Zhejiang Provincial Science Foundation (Grant R405066).
文摘An efficient route to synthesize the heteroaryl-substituted 1,8-naphthyridine derivatives was described. Eight 2-heteroaryl- and 2,7-diheteroaryl-1,8-naphthyridine derivatives were obtained through palladium-catalyzed C-N-coupling reactions of chloronaphthyridines with imidazole, benzimidazole, morpholine, 3,5-dimethylpyrazole, and phthalimide in moderate to good yields.
基金Project 29672008 was supported by NationalNatural Science Foundation of China.
文摘The diaryldiselenides reacted with titanocene hydried (Cp2TiH) generted from Cp2TiCl2/i-BuMgBr to give arylselenium complexes of titanocene. They reacted readily with diaryliodoiums salt to give unsymmetical diarylselenides.