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
A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) ...A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography-diode array detector (HPLC-DAD). Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients (r^2) varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection (LODs) (S/N = 3) were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.展开更多
Impact, friction and corrosion from the grinding balls and the grinding medium during the mineral processing result in liner breakage. Liner, made from Hadfield steel or alloyed steel, could not have served in wet gri...Impact, friction and corrosion from the grinding balls and the grinding medium during the mineral processing result in liner breakage. Liner, made from Hadfield steel or alloyed steel, could not have served in wet grinding environment for more than ten months. Composite liner, made from HCWCI (high Cr white cast iron) and carbon steel, has been developed successfully with liquid-liquid composing process based on LFC (lost foam casting). The microstructure of composite was analyzed with optical microscope, SEM (scanning electron microscope)/EDX energy-dispersive X-ray and XRD (X-ray diffraction). According to micrograph, the combination region of two metals was staggered like dogtooth, no mixtures occurred between two liquid metals, and its interface presented excellent metallurgical bonding state. The results of mechanical property test show that, the hardness of HRC, the fracture toughness, and the bending strength are more than 61, 16.5 J/cm2 and 1 600 MPa, respectively. Comparison between liners made from bimetal composite and alloyed steel has also been investigated in industrial hematite ball mill. The results of eight months test in wet grinding environment prove that the service life of bimetal composite liner is three times as long as that of one made from alloyed steel.展开更多
A simple method has been proposed for the determination of clozapine (CLZ) and chlorpromazine (CPZ) in human urine by dispersive liquid-liquid microextraction (DLLME) in combination with high-performance liquid ...A simple method has been proposed for the determination of clozapine (CLZ) and chlorpromazine (CPZ) in human urine by dispersive liquid-liquid microextraction (DLLME) in combination with high-performance liquid chromatography-ultraviolet detector (HPLC-UV). All important variables influencing the extraction efficiency, such as pH, types of the extraction solvent and the disperser solvent and their volume, ionic strength and centrifugation time were investigated and optimized. Under the optimal conditions, the limit of detection (LODs) and quantification (LOQs) of the method were 13 and 39 ng/mL for CLZ, and 2 and 6 ng/mL for CPZ, respectively. The relative standard deviations (RSDs) of the targets were less than 5.1% (C=0.100 μg/mL, n=9). Good linear behaviors over the tested concentration ranges were obtained with the values of R20.999 for the targets. The absolute extraction efficiencies of CLZ and CPZ from the spiked blank urine samples were 98.3% and 97.8%, respectively. The applicability of the technique was validated by analyzing urine samples and the mean recoveries for spiked urine samples ranged from 93.3% to 105.0%. The method was successfully applied for the determination of CLZ and CPZ in real human urine.展开更多
A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floatin...A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop(DLLME-SFO) followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient(r) of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.展开更多
A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by...A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.展开更多
Generally, most soil slope failures are induced by rainfall infiltration, a process that involves interactions between the liquid phase, gas phase,and solid skeleton in an unsaturated soil slope. In this study, a loos...Generally, most soil slope failures are induced by rainfall infiltration, a process that involves interactions between the liquid phase, gas phase,and solid skeleton in an unsaturated soil slope. In this study, a loosely coupled liquid-gas-solid three-phase model, linking two numerical codes,TOUGH2/EOS3, which is used for water-air two-phase flow analysis, and FLAC^(3D), which is used for mechanical analysis, was established. The model was validated through a documented water drainage experiment over a sandy column and a comparison of the results with measured data and simulated results from other researchers. The proposed model was used to investigate the features of water-air two-phase flow and stress fields in an unsaturated soil slope during rainfall infiltration. The slope stability analysis was then performed based on the simulated water-air two-phase seepage and stress fields on a given slip surface. The results show that the safety factor for the given slip surface decreases first, then increases, and later decreases until the rainfall stops. Subsequently, a sudden rise occurs. After that, the safety factor decreases continually and reaches its lowest value, and then increases slowly to a steady value. The lowest value does not occur when the rainfall stops, indicating a delayed effect of the safety factor. The variations of the safety factor for the given slip surface are therefore caused by a combination of pore-air pressure, matric suction, normal stress, and net normal stress.展开更多
The liquid-phase furfural (FAL) hydrogenation to furfuryl alcohol (FOL) and tetrahydrofurfuryl alcohol (THFOL) was investigated using sulfonate group (-SO3H) grafted activated carbon (AC) supported Ni cataly...The liquid-phase furfural (FAL) hydrogenation to furfuryl alcohol (FOL) and tetrahydrofurfuryl alcohol (THFOL) was investigated using sulfonate group (-SO3H) grafted activated carbon (AC) supported Ni catalyst, which was prepared and activated simultaneously by liquid phase reduction method. This functionalized nickel catalyst demonstrated an enhanced catalytic performance for selective hydrogenation of FAL, in which almost 100% FOL (〈80℃) and THFOL (〉100℃) selectivity with complete conversion was obtained, respectively. More importantly, the conversion of transfer hydrogenation of FAL to FOL also can reach almost 100% under optimal conditions (140℃, 4.0h). The effect of -SO3H was evaluated and systematically analyzed by the combination of reaction performance and physico-chemical characterizations. Cycling test proved the prepared catalyst could be recycled and reused for several times without noticeably reducing catalytic activity of hvdrogenation.展开更多
The homogeneous liquid was separated into two phases, (Fe, Co)-rich LI and Cu-rich L2, once the melt was undercooled below a liquid-phase separation temperature Tsep. If the duration from Tsep to Tsl (solidificatio...The homogeneous liquid was separated into two phases, (Fe, Co)-rich LI and Cu-rich L2, once the melt was undercooled below a liquid-phase separation temperature Tsep. If the duration from Tsep to Tsl (solidification temperature of LI phase), termed the liquid-phase separation interval Δt, exceeded a critical value, an eggtype structure was observed. By utilizing differential thermal analyses (DTA), the solidification process of the undercooled Fe-Co-Cu alloys was studied. Additionally, an immiscible boundary was obtained, which was a convex parabola with a symmetrical axis of XCu=0.52. Depending on the relative amounts of LI and L2, the minor phase was nucleated firstly to form liquid droplets and separated from the original liquids at the beginning of liquid-phase separation.展开更多
The kinetics of liquid-phase hydrogenation of toluene catalyzed by MlNi_5 was studied by investigating the influences of the reaction temperature and pressure on the mass transfer-reaction processes inside the slurry....The kinetics of liquid-phase hydrogenation of toluene catalyzed by MlNi_5 was studied by investigating the influences of the reaction temperature and pressure on the mass transfer-reaction processes inside the slurry. The results show that the reaction rate accelerates when the reaction temperature increases, and reaches its maximum at about 490 K, but if temperature is higher than 510 K, the reaction rate decreases rapidly. The whole reaction process is controlled by the reaction at the surface of the catalyst particles. The mass transfer resistance at gas-liquid interface and that from the bulk liquid phase to the surface of the catalyst particle can be neglected. The apparent reaction rate is zero order for toluene concentration and first order for hydrogen concentration in the liquid phase. The kinetic model is obtained. The kinetic model fits the experimental data very well. The apparent activation energy of the hydrogen absorption reaction of MlNi_5-toluene slurry system is 41.01 kJ·mol^(-1).展开更多
Attitude maneuver of liquid-filled spacecraft with an appendage as a cantilever beam by momentum wheel is studied. The dynamic equations are derived by conserva- tion of angular momentum and force equilibrium principl...Attitude maneuver of liquid-filled spacecraft with an appendage as a cantilever beam by momentum wheel is studied. The dynamic equations are derived by conserva- tion of angular momentum and force equilibrium principle. A feedback control strategy of the momentum wheel is ap- plied for the attitude maneuver. The residual nutation of the spacecraft in maneuver process changes with some chosen parameters, such as steady state time, locations of the liq- uid container and the appendage, and appendage parame- ters. The results indicate that locations in the second and fourth quadrants of the body-fixed coordinate system and the second quadrant of the wall of the main body are better choices for.placing the liquid containers and the appendage than other locations if they can be placed randomly. Higher density and thicker cross section are better for lowering the residual nutation if they can be changed. Light appendage can be modeled as a rigid body, which results in a larger residual nutation than a flexible model though. The resid- ual nutation decreases with increasing absolute value of the initial sloshing angular height.展开更多
The atomic behavior of liquid-solid mixed-phase nanofluid flows inside nanochannels is investigated by a molecular dynamics simulation (MDS). The results of visual observation and statistic analysis show that when t...The atomic behavior of liquid-solid mixed-phase nanofluid flows inside nanochannels is investigated by a molecular dynamics simulation (MDS). The results of visual observation and statistic analysis show that when the nanoparticles reach near each other, the strong interatomic force will make them attach together. This aggrega- tion continues until all nanoparticles make a continuous cluster. The effect of altering the external force magnitude causes changes in the agglomeration rate and system enthalpy. The density and velocity profiles are shown for two systems, i.e., argon (Ar)-copper (Cu) nanofluid and simple Ar fluid between two Cu walls. The results show that using nanopar- ticles changes the base fluid particles ordering along the nanochannel and increases the velocity. Moreover, using nanoparticles in simple fluids can increase the slip length and push the near-wall fluid particles into the main flow in the middle of the nanochannel.展开更多
KF or K2CO3 was added into the 1-butanol-water system and two phases were formed: water-rich phase (water phase) and 1-butanol-rich phase (1-butanol phase). The liquid liquid equilibrium (LLE) data for 1-butano...KF or K2CO3 was added into the 1-butanol-water system and two phases were formed: water-rich phase (water phase) and 1-butanol-rich phase (1-butanol phase). The liquid liquid equilibrium (LLE) data for 1-butanol-water-KF and 1-butanol-water-K2CO3 systems were measured at 25℃ and showed that 1-butanol phase contained negligible salt and water phase contained negligible 1-butanol when the concentrations of KF and K2CO3 in the water phase were equal to or higher than 27.11% and 31.68% , respectively. Thus water could be separated efficiently from 1-butanol-water by adding KF or K2CO3 into the system. A theoretical calculation of LLE data was calculated by using the Pitzer theory to get water activity in the water phase, and by the models, such as the Wilson, NRTL or the UNIQUAC for the 1-butanol phase. For 1-hutanol-water-KF system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and Wilson equa tion, while for 1-butanol-water-K2CO3 system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and UNIQUAC eauation.展开更多
In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of c...In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.展开更多
TiO2 nanowire arrays were successfully fabricated by liquid-phase deposition method using porous alumina templates. The obtained TiO2 nanowires were characterized using Raman spectroscopy, X-ray diffraction (XRD), s...TiO2 nanowire arrays were successfully fabricated by liquid-phase deposition method using porous alumina templates. The obtained TiO2 nanowires were characterized using Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FE- SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) analysis. Results of electron microscopic observations indicated that the nanowires were smooth and uniform with a diameter of about 50-80 nm and several micrometers in length. SAED, Raman, and XRD mea- surements showed that TiO2 nanowires were single-crystalline with a pure rutile structure after heating at 800 ~C for 10 h. In this situation, the nanowire constituents grew preferentially along the 〈001〉 direction. Furthermore, the formation process and mechanistic study of the Ti02 nanowire arrays were proposed and discussed in detail. The nanowires are clearly produced by the deposition of TiO2 particles on the inner wall of the template nanochannels.展开更多
A temperature-controlled ionic liquid dispersive liquid-phase microextraction in combination with high performance liquid chromatography was developed for the enrichment and determination of triazine herbicides such a...A temperature-controlled ionic liquid dispersive liquid-phase microextraction in combination with high performance liquid chromatography was developed for the enrichment and determination of triazine herbicides such as cyanazine,simazine,and atrazine in water samples.1-Octyl-3-methylimidazolium hexafluorophosphate([C8MIM][PF6]) was selected as the extraction solvent.Several experimental parameters were optimized.Under the optimal conditions,the linear range for cyanazine was in the concentration range of 0.5–80 mg/L and the linear range for simazine and atrazine was in the range of1.0–100 mg/L.The limit of detection(LOD,S/N = 3) was in the ranges of 0.05–0.06 mg/L,and the intra day and inter day precision(RSDs,n = 6) was in the ranges of 3.2%–6.6% and 4.8%–8.9%,respectively.Four real water samples were analyzed with the developed method,and the experimental results showed that the spiked recoveries were satisfactory.All these exhibited that the developed method was a valuable tool for monitoring such pollutants.展开更多
Nonlinear coupled dynamics of a liquid-filled spherical container in microgravity are investigated. The governing equations of the low-gravity liquid sloshing in a convex axisymmetrical container subjected to lateral ...Nonlinear coupled dynamics of a liquid-filled spherical container in microgravity are investigated. The governing equations of the low-gravity liquid sloshing in a convex axisymmetrical container subjected to lateral excitation is obtained by the variational principle and solved with a modal analysis method. The variational formulas are transformed into a frequency equation in the form of a standard eigenvalue problem by the Galerkin method, in which admissible functions for the velocity potential and the liquid flee surface displacement are determined analytically in terms of the Gaussian hypergeometric series. The coupled dynamic equations of the liquid-filled container are derived using the Lagrange's method and are numerically solved. The time histories of the modal solutions are obtained in numerical simulations.展开更多
Isomeric triterpenic acids of oleanolic acid (OA) and ursolic acid (UA) both have very low ultraviolet absorption and always exist in the same plant, so the separation and simultaneous determination of them have been ...Isomeric triterpenic acids of oleanolic acid (OA) and ursolic acid (UA) both have very low ultraviolet absorption and always exist in the same plant, so the separation and simultaneous determination of them have been a difficult task. In this study, a sensitive method combining dispersive liquid-liquid microextraction (DLLME) with HPLC-UV was developed for the extraction and determination of OA and UA in traditional Chinese medicinal herbs (CMHs). Variables influencing DLLME such as type and volume of extraction solvent, volume of dispersive solvent, ionic strength, aqueous phase pH, extraction time, centrifugation speed and time, and sample volume were investigated and optimized. Under the optimum conditions, both OA and UA attained favorable extraction efficiencies with enrichment factors 1378 and 933, respectively. The linear dynamic ranges of 0.07 - 30.4 μg?mL–1 for OA and 0.08 - 33.6 μg?mL–1 for UA were obtained with square correlation coefficients of 0.9963. The detection limits of OA and UA were both 0.02 μg?mL–1. The method recoveries ranged between 88.2% - 116.2% for OA and 85.7% - 108.2% for UA with the RSDs (n = 5) lower than 8.6%. The proposed method was successfully applied to concentrate and simultaneously determine these two triterpenic acids in Hedyotis diffusa and Eriobotrya japonica samples.展开更多
The main problems with the liquid-phase technology of carbon fiber/aluminum matrix composites include poor wetting of the fiber with liquid aluminum and formation of aluminum carbide on the fibers’surface.This paper ...The main problems with the liquid-phase technology of carbon fiber/aluminum matrix composites include poor wetting of the fiber with liquid aluminum and formation of aluminum carbide on the fibers’surface.This paper aims to solve these problems.The theoretical and experimental dependence of porosity on the applied pressure were determined.The possibility of obtaining a carbon fiber/aluminum matrix composite wire with a strength value of about 1500 MPa was shown.The correlation among the strength of the carbon fiber reinforced aluminum matrix composite,the fracture surface,and the degradation of the carbon fiber surface was discussed.展开更多
Two different solvents had been used to separate benzene from 1-hexene under atmosphere pressure by employing one of the following two solvents, viz.: dimethyl sulfoxide (DMSO) at 298.15 K and 318.15 K, and furfural a...Two different solvents had been used to separate benzene from 1-hexene under atmosphere pressure by employing one of the following two solvents, viz.: dimethyl sulfoxide (DMSO) at 298.15 K and 318.15 K, and furfural at 298.15 K. A series of liquid-liquid equilibrium (LLE) data had been obtained and the distribution coefficient together with the separation factor were calculated from them. Both the NRTL and the UNIQUAC models could fit in with the experimental data quite well.展开更多
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supported both by the Natural Science Foundations of Hebei(No.B2008000210)the Scientific Research Foundation of Agricultural University of Hebei.
文摘A novel method for the determination of five carbamate pesticides (metolcarb, carbofuran, carbaryl, isoprocard and diethofencard) in water samples was developed by dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography-diode array detector (HPLC-DAD). Some experimental parameters that influence the extraction efficiency were studied and optimized to obtain the best extraction results. Under the optimum conditions for the method, the calibration curve was linear in the concentration range from 5 to 1000 ng mL^-1 for all the five carbamate pesticides, with the correlation coefficients (r^2) varying from 0.9984 to 0.9994. Good enrichment factors were achieved ranging from 80 to 177- fold, depending on the compound. The limits of detection (LODs) (S/N = 3) were ranged from 0.1 to 0.5 ng mL^-1. The method has been successfully applied to the analysis of the pesticide residues in environmental water samples.
基金Item Sponsored by National Natural Science Foundation of China (50805109)Fundamental Research Funds for Central Universities of China (2011-1a-023)
文摘Impact, friction and corrosion from the grinding balls and the grinding medium during the mineral processing result in liner breakage. Liner, made from Hadfield steel or alloyed steel, could not have served in wet grinding environment for more than ten months. Composite liner, made from HCWCI (high Cr white cast iron) and carbon steel, has been developed successfully with liquid-liquid composing process based on LFC (lost foam casting). The microstructure of composite was analyzed with optical microscope, SEM (scanning electron microscope)/EDX energy-dispersive X-ray and XRD (X-ray diffraction). According to micrograph, the combination region of two metals was staggered like dogtooth, no mixtures occurred between two liquid metals, and its interface presented excellent metallurgical bonding state. The results of mechanical property test show that, the hardness of HRC, the fracture toughness, and the bending strength are more than 61, 16.5 J/cm2 and 1 600 MPa, respectively. Comparison between liners made from bimetal composite and alloyed steel has also been investigated in industrial hematite ball mill. The results of eight months test in wet grinding environment prove that the service life of bimetal composite liner is three times as long as that of one made from alloyed steel.
基金supported by Science Research Funds of Medical Course, HUST
文摘A simple method has been proposed for the determination of clozapine (CLZ) and chlorpromazine (CPZ) in human urine by dispersive liquid-liquid microextraction (DLLME) in combination with high-performance liquid chromatography-ultraviolet detector (HPLC-UV). All important variables influencing the extraction efficiency, such as pH, types of the extraction solvent and the disperser solvent and their volume, ionic strength and centrifugation time were investigated and optimized. Under the optimal conditions, the limit of detection (LODs) and quantification (LOQs) of the method were 13 and 39 ng/mL for CLZ, and 2 and 6 ng/mL for CPZ, respectively. The relative standard deviations (RSDs) of the targets were less than 5.1% (C=0.100 μg/mL, n=9). Good linear behaviors over the tested concentration ranges were obtained with the values of R20.999 for the targets. The absolute extraction efficiencies of CLZ and CPZ from the spiked blank urine samples were 98.3% and 97.8%, respectively. The applicability of the technique was validated by analyzing urine samples and the mean recoveries for spiked urine samples ranged from 93.3% to 105.0%. The method was successfully applied for the determination of CLZ and CPZ in real human urine.
基金supported by the Natural Science Foundation of Hebei(No.B2010000657)
文摘A novel,simple,rapid,efficient and environment-friendly method for the determination of trace copper in cereal samples was developed by using dispersive liquid-liquid microextraction based on solidification of floating organic drop(DLLME-SFO) followed by flame atomic absorption spectrometry.In the DLLME-SFO,copper was complexed with 8-hydroxy quinoline and extracted into a small volume of 1-dodecanol,which is of low density,low toxicity and proper melting point near room temperature. The experimental parameters affecting the extraction efficiency were investigated and optimized.Under the optimum conditions, the calibration graph exhibited linearity over the range of 0.5—500 ng/mL with the correlation coefficient(r) of 0.9996.The enrichment factor was 122 and the limit of detection was 0.1 ng/mL.The method was applied to the determination of copper in the complex matrix samples such as rice and millet with the recoveries for the spiked samples at 5.0 and 10.0 u,g/g falling in the range of 92.0-98.0%and the relative standard deviation of 3.9-5.7%.
基金The National Science Foundation of China under contract No.40606028the Special Fund from the National Key Basic Research Program of China under contract No.2006CB400601.
文摘A sensitive solvent extraction method for the determination of nonamolar concentrations of silicate in natural waters is developed. According to the traditional aqueous silicate method, silicomolybdenum blue formed by the reaction between silicate and ammoni- um molydate and reduced by metol-sulfite reagent is extracted by methyl isobutyl ketone. The absorbance can be enhanced substantially up to 10-folds. The detection limit of silicate is 8 nmol/dm^3 , which is one tenth smaller than the traditional method, with the precision of 4.0% at a silicate level of 50 nmol/dm^3 and 3.2% at a silicate level of 6 μmol/dm^3. Comparing the calibration curves in the distilled water and seawater, it can be seen that the salt effect also exists in the extraction method. However, the salt effect is a linear function of the salinity and can be corrected by simple calibration. The proposed method is successfully applied to the determination of silicate in natural waters. Natural concentrations of arsenate, arsenite and phosphate cause negligible interference.
基金supported by the National Natural Science Foundation of China(Grants No.51579170 and 51179118)the Science Fund for Creative Research Groups of the National Natural Science Foundation of China(Grant No.51321065)
文摘Generally, most soil slope failures are induced by rainfall infiltration, a process that involves interactions between the liquid phase, gas phase,and solid skeleton in an unsaturated soil slope. In this study, a loosely coupled liquid-gas-solid three-phase model, linking two numerical codes,TOUGH2/EOS3, which is used for water-air two-phase flow analysis, and FLAC^(3D), which is used for mechanical analysis, was established. The model was validated through a documented water drainage experiment over a sandy column and a comparison of the results with measured data and simulated results from other researchers. The proposed model was used to investigate the features of water-air two-phase flow and stress fields in an unsaturated soil slope during rainfall infiltration. The slope stability analysis was then performed based on the simulated water-air two-phase seepage and stress fields on a given slip surface. The results show that the safety factor for the given slip surface decreases first, then increases, and later decreases until the rainfall stops. Subsequently, a sudden rise occurs. After that, the safety factor decreases continually and reaches its lowest value, and then increases slowly to a steady value. The lowest value does not occur when the rainfall stops, indicating a delayed effect of the safety factor. The variations of the safety factor for the given slip surface are therefore caused by a combination of pore-air pressure, matric suction, normal stress, and net normal stress.
基金the National Natural Science Foundation of China (Nos. 51502297, 51372248, and 51432009)Instrument Developing Project of the Chinese Academy of Sciences (No. yz201421)
文摘The liquid-phase furfural (FAL) hydrogenation to furfuryl alcohol (FOL) and tetrahydrofurfuryl alcohol (THFOL) was investigated using sulfonate group (-SO3H) grafted activated carbon (AC) supported Ni catalyst, which was prepared and activated simultaneously by liquid phase reduction method. This functionalized nickel catalyst demonstrated an enhanced catalytic performance for selective hydrogenation of FAL, in which almost 100% FOL (〈80℃) and THFOL (〉100℃) selectivity with complete conversion was obtained, respectively. More importantly, the conversion of transfer hydrogenation of FAL to FOL also can reach almost 100% under optimal conditions (140℃, 4.0h). The effect of -SO3H was evaluated and systematically analyzed by the combination of reaction performance and physico-chemical characterizations. Cycling test proved the prepared catalyst could be recycled and reused for several times without noticeably reducing catalytic activity of hvdrogenation.
基金supported by the Natural Science Foundation of China (Grant No.50771084)the Natural Science Foundation of the Education Department of Jiangsu province,China (Grant No.09KJB430004)
文摘The homogeneous liquid was separated into two phases, (Fe, Co)-rich LI and Cu-rich L2, once the melt was undercooled below a liquid-phase separation temperature Tsep. If the duration from Tsep to Tsl (solidification temperature of LI phase), termed the liquid-phase separation interval Δt, exceeded a critical value, an eggtype structure was observed. By utilizing differential thermal analyses (DTA), the solidification process of the undercooled Fe-Co-Cu alloys was studied. Additionally, an immiscible boundary was obtained, which was a convex parabola with a symmetrical axis of XCu=0.52. Depending on the relative amounts of LI and L2, the minor phase was nucleated firstly to form liquid droplets and separated from the original liquids at the beginning of liquid-phase separation.
文摘The kinetics of liquid-phase hydrogenation of toluene catalyzed by MlNi_5 was studied by investigating the influences of the reaction temperature and pressure on the mass transfer-reaction processes inside the slurry. The results show that the reaction rate accelerates when the reaction temperature increases, and reaches its maximum at about 490 K, but if temperature is higher than 510 K, the reaction rate decreases rapidly. The whole reaction process is controlled by the reaction at the surface of the catalyst particles. The mass transfer resistance at gas-liquid interface and that from the bulk liquid phase to the surface of the catalyst particle can be neglected. The apparent reaction rate is zero order for toluene concentration and first order for hydrogen concentration in the liquid phase. The kinetic model is obtained. The kinetic model fits the experimental data very well. The apparent activation energy of the hydrogen absorption reaction of MlNi_5-toluene slurry system is 41.01 kJ·mol^(-1).
基金supported by the National Natural Science Foundation of China (11072030)
文摘Attitude maneuver of liquid-filled spacecraft with an appendage as a cantilever beam by momentum wheel is studied. The dynamic equations are derived by conserva- tion of angular momentum and force equilibrium principle. A feedback control strategy of the momentum wheel is ap- plied for the attitude maneuver. The residual nutation of the spacecraft in maneuver process changes with some chosen parameters, such as steady state time, locations of the liq- uid container and the appendage, and appendage parame- ters. The results indicate that locations in the second and fourth quadrants of the body-fixed coordinate system and the second quadrant of the wall of the main body are better choices for.placing the liquid containers and the appendage than other locations if they can be placed randomly. Higher density and thicker cross section are better for lowering the residual nutation if they can be changed. Light appendage can be modeled as a rigid body, which results in a larger residual nutation than a flexible model though. The resid- ual nutation decreases with increasing absolute value of the initial sloshing angular height.
文摘The atomic behavior of liquid-solid mixed-phase nanofluid flows inside nanochannels is investigated by a molecular dynamics simulation (MDS). The results of visual observation and statistic analysis show that when the nanoparticles reach near each other, the strong interatomic force will make them attach together. This aggrega- tion continues until all nanoparticles make a continuous cluster. The effect of altering the external force magnitude causes changes in the agglomeration rate and system enthalpy. The density and velocity profiles are shown for two systems, i.e., argon (Ar)-copper (Cu) nanofluid and simple Ar fluid between two Cu walls. The results show that using nanopar- ticles changes the base fluid particles ordering along the nanochannel and increases the velocity. Moreover, using nanoparticles in simple fluids can increase the slip length and push the near-wall fluid particles into the main flow in the middle of the nanochannel.
文摘KF or K2CO3 was added into the 1-butanol-water system and two phases were formed: water-rich phase (water phase) and 1-butanol-rich phase (1-butanol phase). The liquid liquid equilibrium (LLE) data for 1-butanol-water-KF and 1-butanol-water-K2CO3 systems were measured at 25℃ and showed that 1-butanol phase contained negligible salt and water phase contained negligible 1-butanol when the concentrations of KF and K2CO3 in the water phase were equal to or higher than 27.11% and 31.68% , respectively. Thus water could be separated efficiently from 1-butanol-water by adding KF or K2CO3 into the system. A theoretical calculation of LLE data was calculated by using the Pitzer theory to get water activity in the water phase, and by the models, such as the Wilson, NRTL or the UNIQUAC for the 1-butanol phase. For 1-hutanol-water-KF system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and Wilson equa tion, while for 1-butanol-water-K2CO3 system, the experimental data were found in good agreement with the calculated results by using Pitzer theory and UNIQUAC eauation.
文摘In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.
基金supported by the Institute of Science and High Technology and Environmental Sciences(No.1/1859)
文摘TiO2 nanowire arrays were successfully fabricated by liquid-phase deposition method using porous alumina templates. The obtained TiO2 nanowires were characterized using Raman spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FE- SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED) analysis. Results of electron microscopic observations indicated that the nanowires were smooth and uniform with a diameter of about 50-80 nm and several micrometers in length. SAED, Raman, and XRD mea- surements showed that TiO2 nanowires were single-crystalline with a pure rutile structure after heating at 800 ~C for 10 h. In this situation, the nanowire constituents grew preferentially along the 〈001〉 direction. Furthermore, the formation process and mechanistic study of the Ti02 nanowire arrays were proposed and discussed in detail. The nanowires are clearly produced by the deposition of TiO2 particles on the inner wall of the template nanochannels.
基金financially supported by the National Natural Science Foundation of China (No. 21377167)Program for New Century Excellent Talents in University (No. NCET-10-0813)
文摘A temperature-controlled ionic liquid dispersive liquid-phase microextraction in combination with high performance liquid chromatography was developed for the enrichment and determination of triazine herbicides such as cyanazine,simazine,and atrazine in water samples.1-Octyl-3-methylimidazolium hexafluorophosphate([C8MIM][PF6]) was selected as the extraction solvent.Several experimental parameters were optimized.Under the optimal conditions,the linear range for cyanazine was in the concentration range of 0.5–80 mg/L and the linear range for simazine and atrazine was in the range of1.0–100 mg/L.The limit of detection(LOD,S/N = 3) was in the ranges of 0.05–0.06 mg/L,and the intra day and inter day precision(RSDs,n = 6) was in the ranges of 3.2%–6.6% and 4.8%–8.9%,respectively.Four real water samples were analyzed with the developed method,and the experimental results showed that the spiked recoveries were satisfactory.All these exhibited that the developed method was a valuable tool for monitoring such pollutants.
基金the National Natural Science Foundation of China(Nos.10572022,10772026)
文摘Nonlinear coupled dynamics of a liquid-filled spherical container in microgravity are investigated. The governing equations of the low-gravity liquid sloshing in a convex axisymmetrical container subjected to lateral excitation is obtained by the variational principle and solved with a modal analysis method. The variational formulas are transformed into a frequency equation in the form of a standard eigenvalue problem by the Galerkin method, in which admissible functions for the velocity potential and the liquid flee surface displacement are determined analytically in terms of the Gaussian hypergeometric series. The coupled dynamic equations of the liquid-filled container are derived using the Lagrange's method and are numerically solved. The time histories of the modal solutions are obtained in numerical simulations.
文摘Isomeric triterpenic acids of oleanolic acid (OA) and ursolic acid (UA) both have very low ultraviolet absorption and always exist in the same plant, so the separation and simultaneous determination of them have been a difficult task. In this study, a sensitive method combining dispersive liquid-liquid microextraction (DLLME) with HPLC-UV was developed for the extraction and determination of OA and UA in traditional Chinese medicinal herbs (CMHs). Variables influencing DLLME such as type and volume of extraction solvent, volume of dispersive solvent, ionic strength, aqueous phase pH, extraction time, centrifugation speed and time, and sample volume were investigated and optimized. Under the optimum conditions, both OA and UA attained favorable extraction efficiencies with enrichment factors 1378 and 933, respectively. The linear dynamic ranges of 0.07 - 30.4 μg?mL–1 for OA and 0.08 - 33.6 μg?mL–1 for UA were obtained with square correlation coefficients of 0.9963. The detection limits of OA and UA were both 0.02 μg?mL–1. The method recoveries ranged between 88.2% - 116.2% for OA and 85.7% - 108.2% for UA with the RSDs (n = 5) lower than 8.6%. The proposed method was successfully applied to concentrate and simultaneously determine these two triterpenic acids in Hedyotis diffusa and Eriobotrya japonica samples.
基金financially supported by ISSP RAS-Russian Government contracts
文摘The main problems with the liquid-phase technology of carbon fiber/aluminum matrix composites include poor wetting of the fiber with liquid aluminum and formation of aluminum carbide on the fibers’surface.This paper aims to solve these problems.The theoretical and experimental dependence of porosity on the applied pressure were determined.The possibility of obtaining a carbon fiber/aluminum matrix composite wire with a strength value of about 1500 MPa was shown.The correlation among the strength of the carbon fiber reinforced aluminum matrix composite,the fracture surface,and the degradation of the carbon fiber surface was discussed.
基金the financial supports provided by the National Natural Science Foundation of China (No.21177038)
文摘Two different solvents had been used to separate benzene from 1-hexene under atmosphere pressure by employing one of the following two solvents, viz.: dimethyl sulfoxide (DMSO) at 298.15 K and 318.15 K, and furfural at 298.15 K. A series of liquid-liquid equilibrium (LLE) data had been obtained and the distribution coefficient together with the separation factor were calculated from them. Both the NRTL and the UNIQUAC models could fit in with the experimental data quite well.