An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 7...An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 717 resins based on the coordination difference between Zn^(2+)/Cu^(2+)and Cl^(-).The theoretical calculation and spectroscopic analyses suggested that the coordination between Zn^(2+)and Cl^(-)is much stronger than that between Cu^(2+)and Cl^(-),and the Cl-concentration significantly affects Zn(Ⅱ)and Cu(Ⅱ)species.The factors involving Cl-concentration,resin dosage,shaking speed,and temperature were investigated to determine the optimal condition,and the maximum separation factor of Zn/Cu reached as high as 479.2.The results of the adsorption isotherms,adsorption kinetics,SEM,FTIR,and XPS analyses indicated that the process followed the monolayer uniform chemisorption.Through the continuous adsorption experiments,Zn(Ⅱ)and Cu(Ⅱ)in the high-chlorine raffinate were separately recovered,allowing the reuse of residual waste acid and germanium.展开更多
The mixture of fullerene—C_(60) and —C_(70) was successfully separated in larger amount by liquid chromatogra- phy on graphite column.The column was first eluted with a mixture of hexane and toluene,and then with to...The mixture of fullerene—C_(60) and —C_(70) was successfully separated in larger amount by liquid chromatogra- phy on graphite column.The column was first eluted with a mixture of hexane and toluene,and then with toluene.The eluates were monitored by UV/visible absorption spectroscopy.Graphite column shows high perfor- mance for separation.and much larger quantities of pure C_(60) can be easily obtained. The synthesis of fullerenes(C_(60) and C_(70))in macroscopic quantities has stimulated scientists to study on the method for separating C_(60) and C_(70).Because of the poor solubility of fullerenes C_(60)/C_(70) in most organic solvents,the separation of C_(60) and C_(70) proved to be a challenging task.Most attempts at the separation have used silica and alu- mina as the stationary phase and a mixture of hexane and benzene(or toluene)as the mobile phase. Fullerenes,however,have only limited solubility in hexane,these separations are usually only achieved by limit- ing the amount of sample to a few milligrams.The hexane-silica technique using phenylglycine based HPLC columns appears to offer good separation,but only for submilligram amounts. The use of graphite powder as the stationary phase in liquid chromatography is an advanced separation tech- nique for fullerenes C_(60)/C_(70).The technique is based on that the fullerene-C_(60) is different from C_(70) in the de- gree of electron delocalisation,and C_(60) is much less diamagnetic than C_(70).It is expected that the dissimilarity will cause the C_(60)/C_(70) molecules to exhibit different interactions with graphite,and can be separated from each other on this basis.展开更多
High-performance liquid chromatographic systems for the separation of buckminsterfullerene(C_(60)) and related fullerene C_(70) were investigated with methanol/benzene or methanol/toluene (35/65-60/40 in Ⅴ/Ⅴ) as elu...High-performance liquid chromatographic systems for the separation of buckminsterfullerene(C_(60)) and related fullerene C_(70) were investigated with methanol/benzene or methanol/toluene (35/65-60/40 in Ⅴ/Ⅴ) as eluant in C18 reversed phase column. The system is suitable for fast analysis of fullerenes at lower percentage of methanol, and repeatly large scale perparation at higher percentage of methanol.展开更多
Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, s...Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, sample molecular structure and solvent compositions on resolution performance were also discussed.展开更多
A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chir...A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.展开更多
The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 a...The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 and D3 resins as well as the axial dispersion coefficients of the fluid through packed columns are determined by means of the pulse-response experiment technique with an inert substance as a tracer and the chromatography measuring technique. The elution curve calculated from these parameters is good agreement with the experimental elution curve. The sensitivity analysis of these parameters is carried out, and the ressult shows that the elation curves of chromatography separation are more sensitive to the variations Of the Phase equilibrium relationship than to the variation of the axial dispersion as well as the lumped mass transfer coefficients.展开更多
A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performance...A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performances,concentration profiles,start-up methodology as well as influ-ences of pH and ionic strength on the separation process.Mathematical models based on the fluiddynamics of the porous medium are proposed.Experiments indicate that the CACE process has agood commercial potential in protein engineering and fine chemicals purification.展开更多
Glutamine peptides were obtained from defatted soybean meal by enzymatic hydrolysis using a combination of Protamex~? and trypsinase. The results showed that the extent of hydrolysis and the concentration of Gln pepti...Glutamine peptides were obtained from defatted soybean meal by enzymatic hydrolysis using a combination of Protamex~? and trypsinase. The results showed that the extent of hydrolysis and the concentration of Gln peptides in the hydrolysate were 22.02%and 6.05 mmol/L, respectively. The hydrolysates were fractionated by size-exclusion chromatography on a Sephadex G-15 into five major fractions(GelF1–GelF5). The peptide(GelF1) fraction with the highest glutamine peptide content(51.8%) was further evaluated to determine its molecular weight distribution. Most(92.37%) peptides were less than 1 000 Da. Glutamic acid and glutamine were the most abundant amino acids, accounting for up to 12.98% of the total amino acid content. In addition, the total amino acid content in GelF1 was higher than that in GelF2 and GelF3.展开更多
基金financially supported by the Postdoctoral Research Foundation of Central South University,China(No.140050037)。
文摘An anion-exchange-based chromatographic separation approach was developed to selectively recover zinc and copper from the high-chlorine raffinate generated in the process of germanium chlorination distillation using 717 resins based on the coordination difference between Zn^(2+)/Cu^(2+)and Cl^(-).The theoretical calculation and spectroscopic analyses suggested that the coordination between Zn^(2+)and Cl^(-)is much stronger than that between Cu^(2+)and Cl^(-),and the Cl-concentration significantly affects Zn(Ⅱ)and Cu(Ⅱ)species.The factors involving Cl-concentration,resin dosage,shaking speed,and temperature were investigated to determine the optimal condition,and the maximum separation factor of Zn/Cu reached as high as 479.2.The results of the adsorption isotherms,adsorption kinetics,SEM,FTIR,and XPS analyses indicated that the process followed the monolayer uniform chemisorption.Through the continuous adsorption experiments,Zn(Ⅱ)and Cu(Ⅱ)in the high-chlorine raffinate were separately recovered,allowing the reuse of residual waste acid and germanium.
文摘The mixture of fullerene—C_(60) and —C_(70) was successfully separated in larger amount by liquid chromatogra- phy on graphite column.The column was first eluted with a mixture of hexane and toluene,and then with toluene.The eluates were monitored by UV/visible absorption spectroscopy.Graphite column shows high perfor- mance for separation.and much larger quantities of pure C_(60) can be easily obtained. The synthesis of fullerenes(C_(60) and C_(70))in macroscopic quantities has stimulated scientists to study on the method for separating C_(60) and C_(70).Because of the poor solubility of fullerenes C_(60)/C_(70) in most organic solvents,the separation of C_(60) and C_(70) proved to be a challenging task.Most attempts at the separation have used silica and alu- mina as the stationary phase and a mixture of hexane and benzene(or toluene)as the mobile phase. Fullerenes,however,have only limited solubility in hexane,these separations are usually only achieved by limit- ing the amount of sample to a few milligrams.The hexane-silica technique using phenylglycine based HPLC columns appears to offer good separation,but only for submilligram amounts. The use of graphite powder as the stationary phase in liquid chromatography is an advanced separation tech- nique for fullerenes C_(60)/C_(70).The technique is based on that the fullerene-C_(60) is different from C_(70) in the de- gree of electron delocalisation,and C_(60) is much less diamagnetic than C_(70).It is expected that the dissimilarity will cause the C_(60)/C_(70) molecules to exhibit different interactions with graphite,and can be separated from each other on this basis.
文摘High-performance liquid chromatographic systems for the separation of buckminsterfullerene(C_(60)) and related fullerene C_(70) were investigated with methanol/benzene or methanol/toluene (35/65-60/40 in Ⅴ/Ⅴ) as eluant in C18 reversed phase column. The system is suitable for fast analysis of fullerenes at lower percentage of methanol, and repeatly large scale perparation at higher percentage of methanol.
文摘Silica gel thin-layer plates covered with L-arginine and copper acetate were used for the separation of amino acid enantiomers, The chromatographic selectivity and the effects of plate different preparation methods, sample molecular structure and solvent compositions on resolution performance were also discussed.
文摘A β-cyclodextrin derivative, perbenzyl-β-cyclodextrin, was prepared and used as a chiral stationary phase for capillary gas chromatography. Using FID detector and the column temperature between 70 and 80℃, the chiral separations of racemic 3-phenyl-1, 2-epoxyethane and 1-phenyl-1-propanol on a 14m×0.23mm I. D. fused silica column with the β-cyclodextrin derivative were carried out and the optical purities of optically active 1-phenyl-1-propanol samples prepared by asymmetric synthesis were determined.
文摘The parameter identification model of largr scale chromatography separation process is proposed. The Phase equilibrium constants and lumped mass transfer coefficients of sugar and reducing sugar adsorption on D1, D2 and D3 resins as well as the axial dispersion coefficients of the fluid through packed columns are determined by means of the pulse-response experiment technique with an inert substance as a tracer and the chromatography measuring technique. The elution curve calculated from these parameters is good agreement with the experimental elution curve. The sensitivity analysis of these parameters is carried out, and the ressult shows that the elation curves of chromatography separation are more sensitive to the variations Of the Phase equilibrium relationship than to the variation of the axial dispersion as well as the lumped mass transfer coefficients.
基金Supported by National Natural Science Foundation of China
文摘A counteracting chromatographic electrophoresis(CACE)separation device has been success-fully built and tested.Experiments are performed with protein mixtures of BSA,Hg,Mg and Cyto-cto study the separation performances,concentration profiles,start-up methodology as well as influ-ences of pH and ionic strength on the separation process.Mathematical models based on the fluiddynamics of the porous medium are proposed.Experiments indicate that the CACE process has agood commercial potential in protein engineering and fine chemicals purification.
基金Supported by National Key R&D Program of China(2016YFD0400203)
文摘Glutamine peptides were obtained from defatted soybean meal by enzymatic hydrolysis using a combination of Protamex~? and trypsinase. The results showed that the extent of hydrolysis and the concentration of Gln peptides in the hydrolysate were 22.02%and 6.05 mmol/L, respectively. The hydrolysates were fractionated by size-exclusion chromatography on a Sephadex G-15 into five major fractions(GelF1–GelF5). The peptide(GelF1) fraction with the highest glutamine peptide content(51.8%) was further evaluated to determine its molecular weight distribution. Most(92.37%) peptides were less than 1 000 Da. Glutamic acid and glutamine were the most abundant amino acids, accounting for up to 12.98% of the total amino acid content. In addition, the total amino acid content in GelF1 was higher than that in GelF2 and GelF3.
