A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively f...A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively from an aqueous solution using a chelating collector 2-thenoyltrifluoroacetone （TTA） dissolved in heptane at alkaline pH condition, then, chloroform was used for extracting the green powder into organic phase. The red phosphor remains in aqueous phase with potassium sodium tartrate depressant （PST）. Therefore, three phosphors can be separated successfully from their artificial mixtures by liquid/liquid extraction, and grades and recovery of separated products reach respectively as follows： red is 96.9% and 95.2%, blue is 82.7% and 98.8%, green is 94.6% and 82.6%.展开更多
A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separat...A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.展开更多
This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid e...This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.展开更多
Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on...Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on liquid-solid diffusion and reaction is reported in this paper.The extraction process,product microstructure and extraction efficiency were systematically studied.The results show that the extraction rate of RE at 1200℃is about 20%higher than that at 1100℃.The enhanced extraction efficiency at 1200℃results from the fact that the liquid Fe and Fe2 B are not co-soluble with Cu,Reducing the mass ratio of Cu to waste and the size of the waste scraps is also beneficial to enhancing the separation of RE and Fe elements.In addition,the extraction time should be well controlled,for example,less than 2 h at 1100℃,in order to avoid the increased Fe content in the extracted product.Based on optimized process,the RE elements ca n be almost fully extracted from the waste.This work thus provides an effective method to recover the RE elements.展开更多
The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohe...The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohexyl-BTP） as extractant in 1-alkyl-3-methylimidazolium bis（trifluoromethylsufonyl）imide（[Cnmim][NTf2]） ionic liquid. Isohexyl-BTP in ionic liquids exhibited remarkably better extraction performance for lanthanides than that in octanol-dodecane（3：7 v/v） system. Lower HNO3 concentration and short alkyl chain length of [Cnmim]^＋ were more favourable for removal of lanthanides. Besides, it was confirmed that isohexyl-BTP in ILs formed a 1：3 complex [Ln（BTP）3（NO3）n]^（3–n）＋（n=0, 1） by slope analysis. In addition, [C2mim][NTf2] preferred to extract lanthanides via a cation exchange mechanism at lower acidity, which was proved via UV-Vis measurement. It was speculated that extraction mechanism shifted from cation exchange to neutral species extraction with increase in HNO3 concentration and alkyl chain length of [Cnmim]^＋ due to the H^＋ completion, NO3^- inhibition and hydrophobicity of IL.展开更多
diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone ...diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone 5), A new 4 acylpyrazol 5 one derivative (H 2BPMPP) was syntheszed, which contains a heterocyclic ring between two 1 phenyl 3 methyl 4 acylpyrazol 5 one rings. The new compound was characterized by element analyses, UV, IR and 1H NMR spectra. The equilibrium of the keto enol tautomerism was studied. The results show that a lower dielectric constant of solvent favors the enol form which has a higher λ max . Due to special merits of paraffin wax, the solid liquid extraction behavior of Ce(Ⅲ) with molten paraffin wax as a diluent was also investigated at higher temperature. The value of the pH 1/2 was 3.19 and the value of log K ex was 3.467. The chemical composition of the complex was obtained by the slope analysis method.展开更多
Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and ...Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and （3） supported liquid extraction （SLE）. Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring （MRM） in a positive ion mode with ESI. The transitions monitored were m./z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification （LLOQ） was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.展开更多
The extractive desulfurization of a model gaso- line containing several alkyl thiols and aromatic thiophenic compounds was investigated using two imidazolium-based ionic liquids （ILs）, 1-butyl-3-methylimidazolium te...The extractive desulfurization of a model gaso- line containing several alkyl thiols and aromatic thiophenic compounds was investigated using two imidazolium-based ionic liquids （ILs）, 1-butyl-3-methylimidazolium tetrachloroaluminate, and 1-octyl-3-methylimidazolium te- trafluoroborate, as extractants. A fractional factorial design of experiments was employed to evaluate the effects and possible interactions of several process variables. Analysis of variance tests indicated that the number of extraction steps and the IL/gasoline volume ratio were of statistically highly significant, but none of the interactions were significant. The results showed that the desulfurization efficiency of the model gasoline by the ILs could reach 95.2 % under the optimal conditions. The optimized conditions were applied to study the extraction of thiophenic compounds in model gasoline and several real gasoline samples; the following order was observed in their separation： benzothio- phenc 〉 thiophcne 〉 3-methylthiophene 〉 2-methylthiophene, with 96.1% removal efficiency for benzothiophene. The IL extraction was successfully applied as a complementary process to the adsorptive desulfurization with acti- vated Raney nickel and acetonitrile solvent. The results indicated that the adsorptive process combined with IL extraction could provide high efficiency and selectivity, which can be regarded as a promising energy efficient desulfurization strategy for production of low-sulfur gasoline.展开更多
Uniform nanorods of rare earth phosphate(REPO_4, RE = La–Gd) nanocrystals were prepared in a properly designed ionic liquid extraction system by a stripping precipitation method. Rare earth ions were extracted into t...Uniform nanorods of rare earth phosphate(REPO_4, RE = La–Gd) nanocrystals were prepared in a properly designed ionic liquid extraction system by a stripping precipitation method. Rare earth ions were extracted into the organic phase at first; after that, the loaded organic phase was stripped by aqueous solution of PO_4^(3-) under stirring at room temperature within 5 min.The extractant used here is a bifunctional ionic liquid extractant called [A336][cyanex272]. The products are hexagonal phase in crystal structure, and their morphology is nanorods. The diameter of the products is from 30 to 50 nm, and the length increases from 200 nm to 2 μm gradually. Besides, the ionic liquid-absorbed CePO_4:Tb^(3+) nanorods show improved luminescent emitting intensity and lifetime. Based on the results, a possible growth mechanism of the REPO_4(RE = La–Gd) nanorods is proposed, where the extractants here also play roles of structure-directing agents and surfactants during the formation process of nanocrystals.展开更多
In this work, the process simulation of pressure-swing distillation(PSD) and extractive distillation(ED) using ionic liquid(IL) 1-butyl-3-methylimidazolium acetate([bmim][OAc]) as the entrainer for separation of ethyl...In this work, the process simulation of pressure-swing distillation(PSD) and extractive distillation(ED) using ionic liquid(IL) 1-butyl-3-methylimidazolium acetate([bmim][OAc]) as the entrainer for separation of ethyl acetateethanol-water mixture is performed. The design parameters of the two distillation processes are optimized with the minimum total annual cost(TAC) serving as the objective function. The results show that the TAC saving of ED process is 35.27% in comparison with that of PSD process in the case of achieving the same purity and yield of ethyl acetate.In addition, the dynamic controllability of ED process is further studied. The traditional two-point temperature control structure is proposed for the ED process, and it works pretty well while taking into account the disturbances in both feed rate and feed composition.展开更多
Extraction and separation of yttrium in chloride medium using tri-n-octylmethylammonium（2-sec-octylphenoxy） acetate（[N（1888）][SOPAA]） as an extractant were studied in this article. Tri-n-butyl phosphate（TBP） w...Extraction and separation of yttrium in chloride medium using tri-n-octylmethylammonium（2-sec-octylphenoxy） acetate（[N（1888）][SOPAA]） as an extractant were studied in this article. Tri-n-butyl phosphate（TBP） was used as a phase modifier to accelerate phase separation and improve the stability of organic phase. The addition of TBP contributed to shortening phase separation time, increasing extraction capacity of rare earth elements（REEs） and decreasing viscosity of organic phase. The slope analysis method and infrared spectroscopy were conducted to investigate the ion-association extraction mechanisms. Extraction and stripping performances of the different systems were also compared. The article showed that the extraction performance of mixed [N（1888）][SOPAA] and TBP is superior to that of [N（1888）][SOPAA] for heavy rare earth element（HREE）.展开更多
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-l...A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.展开更多
A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS...A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS/MS） with supported liquid extraction（SLE）.lrbesartan（IRB） was used as an internal standard（IS）.The analyte in rat plasma（200 μL） was isolated through SLE using ethyl acetate as the eluting solvent.The chromatographic separation was achieved on Luna-HILIC（250 mm × 4.6 mm,5 μm）column with a mobile phase of 0.1% of formic acid in water：acetonitrile（5：95,v/v）,at a constant flow rate of 1.0mL/min.The MS/MS ion transitions for DRV（548.1→392.0） and IS（429.2→207.1） were monitored on an ion trap mass spectrometer,operating in the multiple reaction monitoring（MRM） mode.The lower limit of quantitation（LLOQ） was 0.2 ng/mL and quantitation range was 0.2-5000 ng/mL.The method was validated for its selectivity,sensitivity,carryover,linearity,precision,accuracy,recovery,matrix effect and stability.The method was successfully applied to pharmacokinetic study in rats.展开更多
Several metal-based ionic liquids（ILs） were synthesized and used as extractants for the desulfurization of dibenzothiophene（DBT） in simulated fuel oil.The effects of several anion and metal ions,n（ILs）/n（metal...Several metal-based ionic liquids（ILs） were synthesized and used as extractants for the desulfurization of dibenzothiophene（DBT） in simulated fuel oil.The effects of several anion and metal ions,n（ILs）/n（metal） as mole ratio,V（IL）/V（oil） and extractive times on the removal ratio of DBT were investigated in detail.The results showed that[BMIM]HSO4/FeCl3（BMIM was short for l-butyl-3-methyl imidazole）was superior to the other ILs for the extractive desulfurization.A total of 100%of DBT was removed at room temperature in 5 min with V[BMIM]HSO4/Fecl3/Voil = 1：1.The extractive activity of[BMIM]HSO4/FeCl3 IL did not change almost after five runs.Extractive desulfurization of different sulfur compounds and commercial diesel fuel oil were also examined.The removal ratios of the sulfur compounds as the reaction substrates were all over 90%and the sulfur content of commercial diesel oil decreased to120 ppm from 12,400 ppm.展开更多
A novel process for separation of red （Y2O3： Eu^3＋）, blue （Sr, Ca, Ba）10（PO4）6Cl2： Eu^2＋ and green （LaPO4： Tb^3＋, Ce^3＋） fine tricolor phosphor powders was established. First, the green phosphor was ext...A novel process for separation of red （Y2O3： Eu^3＋）, blue （Sr, Ca, Ba）10（PO4）6Cl2： Eu^2＋ and green （LaPO4： Tb^3＋, Ce^3＋） fine tricolor phosphor powders was established. First, the green phosphor was extracted and separated from three phosphor mixtures in heptane/DMF（N, N-Dimethylformamide） system using stearylamine or laurylamine （DDA） as the cationic surfactant. Then, after being treated with 99.5% ethanol, the blue and red phosphors could be separated in Heptane/DMF system in presence of 1-octanesulfonic acid sodium salt as the anionic surfactant. Satisfactory separation results have been achieved through two steps extractions with their artificial mixtures. The grades and recovery of separated products reached respectively as follows： red product was 95.3% and 90.9%, blue product was 90.0% and 95.2%, and green product was 92.2% and 91.8%.展开更多
Four ionic liquids （ILs）： 3-（diethoxyphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P（OEt）2][PF6] （IL-1）, 3-（ethoxyphenylphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3...Four ionic liquids （ILs）： 3-（diethoxyphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P（OEt）2][PF6] （IL-1）, 3-（ethoxyphenylphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3PPh（OEt）][PF6] （IL-2）, 3-（diphenylphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P（Ph）2][PF6] （IL-3）, and 3-（diethoxyphosphoryl）propyl triphenylphosphinium bis（trifluoromethanesulfonyl）imide [Ph3PC3P（OEt）2][NTf2] （IL-4） were synthesized and characterized by IR and 31p, 1H, 13C NMR spectroscopy. The liquid-liquid extraction of neodymium（Ⅲ） by these phosphorus functionalized ionic liquids （PFILs） diluted with common room temperature ionic liquid 1-hexyl-3-methylimidazolium bis（trifluoromethylsulfonyl）imide [C6mim][NTf2] was studied. The extraction percentage of Nd（Ⅲ） was measured as a fimction of various parameters, such as the ini- tial pH of aqueous phase, equilibrium time, temperature, and concentration of PFIL extractant. The influence of the nature of diluents and salting-out reagents on extraction was also investigated. The results indicated that the extraction process was exothermical and the extraction percentage of Nd（Ⅲ） by IL-1 was the highest among the PFILs investigated. A possible metal complexation mechanism was proposed for the present PFIL/IL extraction system. And the loaded Nd（Ⅲ） ions by PFIL could be stripped completely from the ionic liquid phase by 1 mol/L nitric acid.展开更多
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
The present study examined the effect of alkali extraction on pit membranes （PMs） and liquid uptake of four conifers. Af- ter alkali extraction, the deposits around the PMs almost dissolved in Cunninghamia lanceolat...The present study examined the effect of alkali extraction on pit membranes （PMs） and liquid uptake of four conifers. Af- ter alkali extraction, the deposits around the PMs almost dissolved in Cunninghamia lanceolata Hook. and Cryptomeriajaponica D. Don wood which showed good liquid uptake. In contrast, in Larix leptolepis Gordon and Pseudotsuga menziesii Franco, although the tori adhered strongly to the pit aperture preventing liquid transportation, the liquid uptake of the woods improved markedly. More- over, the combined treatment of alkali extraction-transverse compression had no synergistic effect in improving liquid uptake. These results demonstrate that alkali extraction is effective in improving the liquid uptake of wood.展开更多
The extraction of copper from acidic medium using Liquid Emulsion Membrane LEM as contactors was studied. b diketone LIX 54 as an extractant ,sesqueoleate which is nonionic surfactant with HLB value 3.7 and 0.1 M H2SO...The extraction of copper from acidic medium using Liquid Emulsion Membrane LEM as contactors was studied. b diketone LIX 54 as an extractant ,sesqueoleate which is nonionic surfactant with HLB value 3.7 and 0.1 M H2SO4 as stripping solution were used. The influence of initial concentration of copper in the aqueous feed phase, pH of external and internal aqueous phase, stirring speed, and concentration of extractant on the extraction rate was examined. The results obtained showed that practically all the copper content was removed from the acidic feed solution. The recovery of copper attained 96–100% and concentration ratios of about 40-fold could be achieved.展开更多
Process intensification using liquid emulsion membranes (LEMs) for extraction of copper has been studied in this work. In LEM process the extraction and stripping processes are combined in one stage. The solubility of...Process intensification using liquid emulsion membranes (LEMs) for extraction of copper has been studied in this work. In LEM process the extraction and stripping processes are combined in one stage. The solubility of the solute or the chemical affinity between the solute and carrier reagent in the membrane results in the separation of the solute from the feed mixture. In this work the membrane phase comprised of LIX 664N as the extractant dissolved in kerosene and Span 80 as surfactant. The stripping phase was sulfuric acid with 180 g/l concentration and feed phase had copper concentration of 3.5 g/l. Effect of various process parameters such as batch contact time, speed of agitation, W:O ratio and treat ratio has been experimentally investigated to get better insight of the process. The maximum enrichment of copper in the internal phase obtained was 11.6 times with batch contact time of 10 minutes, agitation speed of 300 rpm and treat ratio of 6:1.展开更多
基金Funded by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry (ROCS, SEM [2005] No. 383)
文摘A novel process for separation of red （Y2O3：Eu^3＋）, blue（BaMgAl10O17：Eu^2＋） and green （CeMgAl10O17：Tb^3） rare earth fluorescent powders was proposed. At first, the blue powder can be extracted selectively from an aqueous solution using a chelating collector 2-thenoyltrifluoroacetone （TTA） dissolved in heptane at alkaline pH condition, then, chloroform was used for extracting the green powder into organic phase. The red phosphor remains in aqueous phase with potassium sodium tartrate depressant （PST）. Therefore, three phosphors can be separated successfully from their artificial mixtures by liquid/liquid extraction, and grades and recovery of separated products reach respectively as follows： red is 96.9% and 95.2%, blue is 82.7% and 98.8%, green is 94.6% and 82.6%.
基金supported by the National Natural Science Foundation of China (No. 21621003)
文摘A novel on-line system composed of supercritical fluid extraction(SFE), dilution line and reverse phase liquid chromatography/mass spectrometry(RPLC/MS) was constructed for on-line extraction and reverse phase separation of some fat-soluble components in foods. Three columns including a trap column,concentration column and analytical column were used for trapping the fat-soluble components, on-line enrichment and reverse phase separation, respectively. Capsaicinoids were on-line extracted by a CO_2 supercritical fluid, then concentrated and separated by using the C_(18) columns, finally detected by mass spectrometry(MS). Capsaicin eluted at 10.1 min and limit of detection(LOD, S/N=3) for the standard solution is 0.55pg. The linearity was calculated with a value of coefficient of determination(R^2)≥0.998 in the range of 1.1–8.5 ng. Concentrations of capsaicin in the green, yellow, and red bell peppers were determined to be 60.33 ng/g, 31.79 ng/g, 35.38ng/g, respectively.
基金supported by the National Natural Science Foundation of China(41325010)
文摘This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.
基金Project supported by Guangdong Provincial Science and Technology Program(2015B010105008)the Dongguan Innovative Research Team Program(201536000200027)。
文摘Recovery of rare earth(RE)elements from Nd-Fe-B waste is one of the ways to solve the problem of socalled RE-crisis,An alternative approach of extracting RE elements from Nd-Fe-B waste by molten Cu extraction based on liquid-solid diffusion and reaction is reported in this paper.The extraction process,product microstructure and extraction efficiency were systematically studied.The results show that the extraction rate of RE at 1200℃is about 20%higher than that at 1100℃.The enhanced extraction efficiency at 1200℃results from the fact that the liquid Fe and Fe2 B are not co-soluble with Cu,Reducing the mass ratio of Cu to waste and the size of the waste scraps is also beneficial to enhancing the separation of RE and Fe elements.In addition,the extraction time should be well controlled,for example,less than 2 h at 1100℃,in order to avoid the increased Fe content in the extracted product.Based on optimized process,the RE elements ca n be almost fully extracted from the waste.This work thus provides an effective method to recover the RE elements.
基金supported by the National Natural Science Foundation of China(11475112)the Ph.D.Programs of Foundation of Ministry of Education of China(20130073120051)
文摘The extraction behavior of several lanthanides（La^3＋, Eu^3＋, Lu^3＋） from nitric acid（HNO3） solution was studied using a novel extraction system based on 2,6-bis（5,6-dihexyl-1,2,4-triazin-3-yl） pyridine（isohexyl-BTP） as extractant in 1-alkyl-3-methylimidazolium bis（trifluoromethylsufonyl）imide（[Cnmim][NTf2]） ionic liquid. Isohexyl-BTP in ionic liquids exhibited remarkably better extraction performance for lanthanides than that in octanol-dodecane（3：7 v/v） system. Lower HNO3 concentration and short alkyl chain length of [Cnmim]^＋ were more favourable for removal of lanthanides. Besides, it was confirmed that isohexyl-BTP in ILs formed a 1：3 complex [Ln（BTP）3（NO3）n]^（3–n）＋（n=0, 1） by slope analysis. In addition, [C2mim][NTf2] preferred to extract lanthanides via a cation exchange mechanism at lower acidity, which was proved via UV-Vis measurement. It was speculated that extraction mechanism shifted from cation exchange to neutral species extraction with increase in HNO3 concentration and alkyl chain length of [Cnmim]^＋ due to the H^＋ completion, NO3^- inhibition and hydrophobicity of IL.
文摘diketone type chelating ligands have high coordinative activity and selectivity, and are widely applied in analytical chemistry. In order to obtain profounder understanding to the properties of bis(4 acylpyrazolone 5), A new 4 acylpyrazol 5 one derivative (H 2BPMPP) was syntheszed, which contains a heterocyclic ring between two 1 phenyl 3 methyl 4 acylpyrazol 5 one rings. The new compound was characterized by element analyses, UV, IR and 1H NMR spectra. The equilibrium of the keto enol tautomerism was studied. The results show that a lower dielectric constant of solvent favors the enol form which has a higher λ max . Due to special merits of paraffin wax, the solid liquid extraction behavior of Ce(Ⅲ) with molten paraffin wax as a diluent was also investigated at higher temperature. The value of the pH 1/2 was 3.19 and the value of log K ex was 3.467. The chemical composition of the complex was obtained by the slope analysis method.
文摘Three extraction methods were compared for their efficiency to analyze sitagliptin and simvastatin in rat plasma by LC-MS/MS, including （1） liquid-liquid extraction （LLE）, （2） solid phase extraction （SPE） and （3） supported liquid extraction （SLE）. Comparison of recoveries of analytes with different extraction methods revealed that SLE was the best extraction method. The detection was facilitated with ion trap-mass spectrometer by multiple reactions monitoring （MRM） in a positive ion mode with ESI. The transitions monitored were m./z 441.1→325.2 for simvastatin, 408.2→235.1 for sitagliptin and 278.1→260.1 for the IS. The lower limit of quantification （LLOQ） was 0.2 ng/mL for sitagliptin and 0.1 ng/mL for simvastatin. The effective SLE offers enhanced chromatographic selectivity, thus facilitating the potential utility of the method for routine analysis of biological samples along with pharmacokinetic studies.
基金National Iranian Oil Refining & Distribution Company(NIORDC) and Research & Development (R&D) center of this company for their financial support during the completion of this work
文摘The extractive desulfurization of a model gaso- line containing several alkyl thiols and aromatic thiophenic compounds was investigated using two imidazolium-based ionic liquids （ILs）, 1-butyl-3-methylimidazolium tetrachloroaluminate, and 1-octyl-3-methylimidazolium te- trafluoroborate, as extractants. A fractional factorial design of experiments was employed to evaluate the effects and possible interactions of several process variables. Analysis of variance tests indicated that the number of extraction steps and the IL/gasoline volume ratio were of statistically highly significant, but none of the interactions were significant. The results showed that the desulfurization efficiency of the model gasoline by the ILs could reach 95.2 % under the optimal conditions. The optimized conditions were applied to study the extraction of thiophenic compounds in model gasoline and several real gasoline samples; the following order was observed in their separation： benzothio- phenc 〉 thiophcne 〉 3-methylthiophene 〉 2-methylthiophene, with 96.1% removal efficiency for benzothiophene. The IL extraction was successfully applied as a complementary process to the adsorptive desulfurization with acti- vated Raney nickel and acetonitrile solvent. The results indicated that the adsorptive process combined with IL extraction could provide high efficiency and selectivity, which can be regarded as a promising energy efficient desulfurization strategy for production of low-sulfur gasoline.
基金financially supported by the National Natural Science Foundation of China (No. 51174184)the National Basic Research Program of China (No. 2012CBA01202)the Key Research Program of the Chinese Academy of Sciences (No. KGZD-EW-201-1)
文摘Uniform nanorods of rare earth phosphate(REPO_4, RE = La–Gd) nanocrystals were prepared in a properly designed ionic liquid extraction system by a stripping precipitation method. Rare earth ions were extracted into the organic phase at first; after that, the loaded organic phase was stripped by aqueous solution of PO_4^(3-) under stirring at room temperature within 5 min.The extractant used here is a bifunctional ionic liquid extractant called [A336][cyanex272]. The products are hexagonal phase in crystal structure, and their morphology is nanorods. The diameter of the products is from 30 to 50 nm, and the length increases from 200 nm to 2 μm gradually. Besides, the ionic liquid-absorbed CePO_4:Tb^(3+) nanorods show improved luminescent emitting intensity and lifetime. Based on the results, a possible growth mechanism of the REPO_4(RE = La–Gd) nanorods is proposed, where the extractants here also play roles of structure-directing agents and surfactants during the formation process of nanocrystals.
基金supported by the National Natural Science Foundation of China (Grant No. 21676299 and 21476261)
文摘In this work, the process simulation of pressure-swing distillation(PSD) and extractive distillation(ED) using ionic liquid(IL) 1-butyl-3-methylimidazolium acetate([bmim][OAc]) as the entrainer for separation of ethyl acetateethanol-water mixture is performed. The design parameters of the two distillation processes are optimized with the minimum total annual cost(TAC) serving as the objective function. The results show that the TAC saving of ED process is 35.27% in comparison with that of PSD process in the case of achieving the same purity and yield of ethyl acetate.In addition, the dynamic controllability of ED process is further studied. The traditional two-point temperature control structure is proposed for the ED process, and it works pretty well while taking into account the disturbances in both feed rate and feed composition.
基金Project supported by‘Hundreds Talents Program’from Chinese Academy of SciencesNational Natural Science Foundation of China(21571179)+1 种基金Science and Technology Major Project of the Fujian Province,China(2015HZ0101)Xiamen Universities,Research Institutions Jointing Enterprise Projects(3502Z20152009)
文摘Extraction and separation of yttrium in chloride medium using tri-n-octylmethylammonium（2-sec-octylphenoxy） acetate（[N（1888）][SOPAA]） as an extractant were studied in this article. Tri-n-butyl phosphate（TBP） was used as a phase modifier to accelerate phase separation and improve the stability of organic phase. The addition of TBP contributed to shortening phase separation time, increasing extraction capacity of rare earth elements（REEs） and decreasing viscosity of organic phase. The slope analysis method and infrared spectroscopy were conducted to investigate the ion-association extraction mechanisms. Extraction and stripping performances of the different systems were also compared. The article showed that the extraction performance of mixed [N（1888）][SOPAA] and TBP is superior to that of [N（1888）][SOPAA] for heavy rare earth element（HREE）.
基金supported by the Shanghai Pharmaceutical Association
文摘A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.
文摘A novel bioanalytical method was developed and validated for the quantitative determination of darunavir（DRV） in rat plasma by employing hydrophilic interaction chromatography and tandem mass spectrometry（HILIC-MS/MS） with supported liquid extraction（SLE）.lrbesartan（IRB） was used as an internal standard（IS）.The analyte in rat plasma（200 μL） was isolated through SLE using ethyl acetate as the eluting solvent.The chromatographic separation was achieved on Luna-HILIC（250 mm × 4.6 mm,5 μm）column with a mobile phase of 0.1% of formic acid in water：acetonitrile（5：95,v/v）,at a constant flow rate of 1.0mL/min.The MS/MS ion transitions for DRV（548.1→392.0） and IS（429.2→207.1） were monitored on an ion trap mass spectrometer,operating in the multiple reaction monitoring（MRM） mode.The lower limit of quantitation（LLOQ） was 0.2 ng/mL and quantitation range was 0.2-5000 ng/mL.The method was validated for its selectivity,sensitivity,carryover,linearity,precision,accuracy,recovery,matrix effect and stability.The method was successfully applied to pharmacokinetic study in rats.
基金financially supported by the National Natural Science Foundation of China(No.21106032)Hebei University of Science and Technology doctor funding(No.000172)
文摘Several metal-based ionic liquids（ILs） were synthesized and used as extractants for the desulfurization of dibenzothiophene（DBT） in simulated fuel oil.The effects of several anion and metal ions,n（ILs）/n（metal） as mole ratio,V（IL）/V（oil） and extractive times on the removal ratio of DBT were investigated in detail.The results showed that[BMIM]HSO4/FeCl3（BMIM was short for l-butyl-3-methyl imidazole）was superior to the other ILs for the extractive desulfurization.A total of 100%of DBT was removed at room temperature in 5 min with V[BMIM]HSO4/Fecl3/Voil = 1：1.The extractive activity of[BMIM]HSO4/FeCl3 IL did not change almost after five runs.Extractive desulfurization of different sulfur compounds and commercial diesel fuel oil were also examined.The removal ratios of the sulfur compounds as the reaction substrates were all over 90%and the sulfur content of commercial diesel oil decreased to120 ppm from 12,400 ppm.
基金Funded by the Scientific Research Foundation for the Returned Overseas Chinese Scholars, State Education Ministry (ROCS, SEM [2005] No. 383)
文摘A novel process for separation of red （Y2O3： Eu^3＋）, blue （Sr, Ca, Ba）10（PO4）6Cl2： Eu^2＋ and green （LaPO4： Tb^3＋, Ce^3＋） fine tricolor phosphor powders was established. First, the green phosphor was extracted and separated from three phosphor mixtures in heptane/DMF（N, N-Dimethylformamide） system using stearylamine or laurylamine （DDA） as the cationic surfactant. Then, after being treated with 99.5% ethanol, the blue and red phosphors could be separated in Heptane/DMF system in presence of 1-octanesulfonic acid sodium salt as the anionic surfactant. Satisfactory separation results have been achieved through two steps extractions with their artificial mixtures. The grades and recovery of separated products reached respectively as follows： red product was 95.3% and 90.9%, blue product was 90.0% and 95.2%, and green product was 92.2% and 91.8%.
基金supported by Natural Science Foundation of Zhejiang Province(Y4100113)2014 Regional Demonstration Project of Marine Economic Development of Ministry of Finance PRC and State Oceanic Administra tion PRC
文摘Four ionic liquids （ILs）： 3-（diethoxyphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P（OEt）2][PF6] （IL-1）, 3-（ethoxyphenylphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3PPh（OEt）][PF6] （IL-2）, 3-（diphenylphosphoryl）propyl triphenylphosphinium hexafluorophosphate [Ph3PC3P（Ph）2][PF6] （IL-3）, and 3-（diethoxyphosphoryl）propyl triphenylphosphinium bis（trifluoromethanesulfonyl）imide [Ph3PC3P（OEt）2][NTf2] （IL-4） were synthesized and characterized by IR and 31p, 1H, 13C NMR spectroscopy. The liquid-liquid extraction of neodymium（Ⅲ） by these phosphorus functionalized ionic liquids （PFILs） diluted with common room temperature ionic liquid 1-hexyl-3-methylimidazolium bis（trifluoromethylsulfonyl）imide [C6mim][NTf2] was studied. The extraction percentage of Nd（Ⅲ） was measured as a fimction of various parameters, such as the ini- tial pH of aqueous phase, equilibrium time, temperature, and concentration of PFIL extractant. The influence of the nature of diluents and salting-out reagents on extraction was also investigated. The results indicated that the extraction process was exothermical and the extraction percentage of Nd（Ⅲ） by IL-1 was the highest among the PFILs investigated. A possible metal complexation mechanism was proposed for the present PFIL/IL extraction system. And the loaded Nd（Ⅲ） ions by PFIL could be stripped completely from the ionic liquid phase by 1 mol/L nitric acid.
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%.
基金supported by the Mission Project Fund,provided by the Center for Exploratory Research on Humanosphere,Research Institute for Sustainable Humanosphere,Kyoto University,Japan
文摘The present study examined the effect of alkali extraction on pit membranes （PMs） and liquid uptake of four conifers. Af- ter alkali extraction, the deposits around the PMs almost dissolved in Cunninghamia lanceolata Hook. and Cryptomeriajaponica D. Don wood which showed good liquid uptake. In contrast, in Larix leptolepis Gordon and Pseudotsuga menziesii Franco, although the tori adhered strongly to the pit aperture preventing liquid transportation, the liquid uptake of the woods improved markedly. More- over, the combined treatment of alkali extraction-transverse compression had no synergistic effect in improving liquid uptake. These results demonstrate that alkali extraction is effective in improving the liquid uptake of wood.
文摘The extraction of copper from acidic medium using Liquid Emulsion Membrane LEM as contactors was studied. b diketone LIX 54 as an extractant ,sesqueoleate which is nonionic surfactant with HLB value 3.7 and 0.1 M H2SO4 as stripping solution were used. The influence of initial concentration of copper in the aqueous feed phase, pH of external and internal aqueous phase, stirring speed, and concentration of extractant on the extraction rate was examined. The results obtained showed that practically all the copper content was removed from the acidic feed solution. The recovery of copper attained 96–100% and concentration ratios of about 40-fold could be achieved.
文摘Process intensification using liquid emulsion membranes (LEMs) for extraction of copper has been studied in this work. In LEM process the extraction and stripping processes are combined in one stage. The solubility of the solute or the chemical affinity between the solute and carrier reagent in the membrane results in the separation of the solute from the feed mixture. In this work the membrane phase comprised of LIX 664N as the extractant dissolved in kerosene and Span 80 as surfactant. The stripping phase was sulfuric acid with 180 g/l concentration and feed phase had copper concentration of 3.5 g/l. Effect of various process parameters such as batch contact time, speed of agitation, W:O ratio and treat ratio has been experimentally investigated to get better insight of the process. The maximum enrichment of copper in the internal phase obtained was 11.6 times with batch contact time of 10 minutes, agitation speed of 300 rpm and treat ratio of 6:1.
