A new selective and sensitive kinetic method for determination of trace amounts of vanadium(Ⅴ) (0.5～40ng/ml) based on its catalytic effect on the oxidation of azomethine H by bromate at pH 4.2 and 25 ℃ was rep...A new selective and sensitive kinetic method for determination of trace amounts of vanadium(Ⅴ) (0.5～40ng/ml) based on its catalytic effect on the oxidation of azomethine H by bromate at pH 4.2 and 25 ℃ was reported and its reaction mechanism was studied.The reaction was monitored spectrophotometrically by measuring the increase in absorbance of oxidation product of azomethine H at 436 nm after a fixed time ( 5 min ).The detection limit of the method is down to 2.0×10 -10 g/ml and the relative standard deviation (RSD) for 30 ng/ml of V(Ⅴ) is 0.26 % ( n =6). The effect of foreign ions on V(Ⅴ) determination was also discussed,and the method is mostly free from interferences of other ions.The proposed method was successfully applied to the determination of trace amounts of vanadium in water samples.展开更多
A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by C...A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.展开更多
There are abundant vanadium ores in the Cambrian strata in southern Shaanxi,China.Many years of mining activities and surface leaching have polluted the surface water to a certain extent,but the researches on the wate...There are abundant vanadium ores in the Cambrian strata in southern Shaanxi,China.Many years of mining activities and surface leaching have polluted the surface water to a certain extent,but the researches on the water quality characteristics and pollution degree are relatively weak.This contribution was organized to investigate the surface water quality by general parameters,including TDS,Eh,pH,DO,TOC,COD,and EC,in the vanadium ore belt(Yinhua River basin).Major ions were determined to detect the water type and natural chemical weathering,while trace elements were used to illustrate their geochemical characteristics and ecological risk assessment of heavy metals.The study found that the surface water was weakly alkaline and mainly dominated from normal to pool grade.The particle size with1000–10,000 nm of suspended particles was the main carrier of organic matter.The concentration of HCO_(3)^(-)and SO_(4)^(2-)in the anions and Ca^(2+)and Mg^(2+)ions in the cations were relatively high,and the water type was Ca-Mg-HCO_(3)-SO_(4) type.Rock weathering had a great influence on surface water,and the weathering products were mainly silicate and carbonate.Compared with the Type river,the contents of V elements showed an obvious positive anomaly,which may be affected by mining activities of vanadium ore and the annual leaching of the tailings pond.As and Cd in the surface water was polluted seriously.The integrated pollution index suggested that the surface water pollution was serious,and the main stream was more serious with the increasing tailings ponds.展开更多
Divanadium（Ⅴ） complex [VO（aptch）（μ-OCH3）]2（1） and two monovanadium（Ⅴ） complexes [VO（apfah））（OEt）]（2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyaceto...Divanadium（Ⅴ） complex [VO（aptch）（μ-OCH3）]2（1） and two monovanadium（Ⅴ） complexes [VO（apfah））（OEt）]（2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone） have been synthesized and characterized.Single-crystal X-ray diffraction studies reveal that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms.Complex 1 crystallizes in the monoclinic crystal system,space groups P21/c with a = 7.4825（4）,b = 17.0928（11）,c = 11.6961（7） ,β = 98.172（4）o,Z = 2,F（000） = 728,μ = 0.829 mm-1,the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I 〉 2（I）.The vanadium（V） is coordinated to the tridentate ligand,ethanol molecule to form a distorted square-pyramidal geometry,complexes 2a and 2b.Although 2a and 2b have the same asymmetric unit,they belong to different space groups.Complex 2a crystallizes in the monoclinic crystal system,space groups P21/n with a = 10.2293（2）,b = 15.6660（3）,c = 10.6298（2） ,β = 116.259（1）o,Z = 4,μ = 0.676 mm-1;complex 2b crystallizes in the triclinic crystal system,space groups P with a = 8.2808（4）,b = 9.4704（5）,c = 10.0819（5） ,α = 86.133（3）,= 81.956（3）,γ = 80.248（3）o,Z = 2 and μ = 0.670 mm-1.The hydrogen bonds are found to exist in 2b only.The crystal structure is stabilized by intermolecular hydrogen bonds of C-H···O.展开更多
The adsorption properties of nanometer-size TiO2 for V（Ⅴ ） were studied. The adsorption rate could reach above 99~ when the pH values were at the range of 4 10. The adsorption balance time was 10 min , the saturati...The adsorption properties of nanometer-size TiO2 for V（Ⅴ ） were studied. The adsorption rate could reach above 99~ when the pH values were at the range of 4 10. The adsorption balance time was 10 min , the saturation capacity of adsorption of nanometer-size TiO2 to V（Ⅴ） was 6.43 mg per gram. Using 2 mL 1.5 mol · L^-1 NaOH as elution, we found the elution rate could reach 95%. A novel method of extreme-trace V（Ⅴ ） preconeentration with nanometer-size titanium dioxide and determination by graphite furnace atomic absorption spectroscopy （GFAAS） was advanced. The detection limit（3σ）of the method was 0.61μg ·L^-1 , and the relative standard deviation was 8.1% （n=6） of 2.5μg ·L-^1 V（Ⅴ）. Environmental samples experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 91.2% and 102.0%.展开更多
文摘A new selective and sensitive kinetic method for determination of trace amounts of vanadium(Ⅴ) (0.5～40ng/ml) based on its catalytic effect on the oxidation of azomethine H by bromate at pH 4.2 and 25 ℃ was reported and its reaction mechanism was studied.The reaction was monitored spectrophotometrically by measuring the increase in absorbance of oxidation product of azomethine H at 436 nm after a fixed time ( 5 min ).The detection limit of the method is down to 2.0×10 -10 g/ml and the relative standard deviation (RSD) for 30 ng/ml of V(Ⅴ) is 0.26 % ( n =6). The effect of foreign ions on V(Ⅴ) determination was also discussed,and the method is mostly free from interferences of other ions.The proposed method was successfully applied to the determination of trace amounts of vanadium in water samples.
文摘A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol·L -1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0 -12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg·L -1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.
基金supported by National Natural Science Foundation of China(No.4210021463)Natural Science Basic Research Program of Shaanxi Province(No.2020JQ-744)+2 种基金China Postdoctoral Science Foundation(No.2020M673443)Shaanxi Provincial Education Department general special project(No.21JK0775)Public Welfare Geology Project of Shaanxi Province(No.201907)。
文摘There are abundant vanadium ores in the Cambrian strata in southern Shaanxi,China.Many years of mining activities and surface leaching have polluted the surface water to a certain extent,but the researches on the water quality characteristics and pollution degree are relatively weak.This contribution was organized to investigate the surface water quality by general parameters,including TDS,Eh,pH,DO,TOC,COD,and EC,in the vanadium ore belt(Yinhua River basin).Major ions were determined to detect the water type and natural chemical weathering,while trace elements were used to illustrate their geochemical characteristics and ecological risk assessment of heavy metals.The study found that the surface water was weakly alkaline and mainly dominated from normal to pool grade.The particle size with1000–10,000 nm of suspended particles was the main carrier of organic matter.The concentration of HCO_(3)^(-)and SO_(4)^(2-)in the anions and Ca^(2+)and Mg^(2+)ions in the cations were relatively high,and the water type was Ca-Mg-HCO_(3)-SO_(4) type.Rock weathering had a great influence on surface water,and the weathering products were mainly silicate and carbonate.Compared with the Type river,the contents of V elements showed an obvious positive anomaly,which may be affected by mining activities of vanadium ore and the annual leaching of the tailings pond.As and Cd in the surface water was polluted seriously.The integrated pollution index suggested that the surface water pollution was serious,and the main stream was more serious with the increasing tailings ponds.
基金supported by the Scientific Research Common Program of Beijing Municipal Commission of Education,PRC (KM200910028011)
文摘Divanadium（Ⅴ） complex [VO（aptch）（μ-OCH3）]2（1） and two monovanadium（Ⅴ） complexes [VO（apfah））（OEt）]（2a and 2b,H2aptch = 2-hydroxyacetophenone thiophene-2-car-boxylic hydrazone,H2apfah = 2-hydroxyacetophenone 2-furoic acid hydrazone） have been synthesized and characterized.Single-crystal X-ray diffraction studies reveal that 1 is a cen-trosymmetric dimer bridged by two methoxido O-atoms.Complex 1 crystallizes in the monoclinic crystal system,space groups P21/c with a = 7.4825（4）,b = 17.0928（11）,c = 11.6961（7） ,β = 98.172（4）o,Z = 2,F（000） = 728,μ = 0.829 mm-1,the final R = 0.0457 and wR = 0.1137 for 2654 observed reflections with I 〉 2（I）.The vanadium（V） is coordinated to the tridentate ligand,ethanol molecule to form a distorted square-pyramidal geometry,complexes 2a and 2b.Although 2a and 2b have the same asymmetric unit,they belong to different space groups.Complex 2a crystallizes in the monoclinic crystal system,space groups P21/n with a = 10.2293（2）,b = 15.6660（3）,c = 10.6298（2） ,β = 116.259（1）o,Z = 4,μ = 0.676 mm-1;complex 2b crystallizes in the triclinic crystal system,space groups P with a = 8.2808（4）,b = 9.4704（5）,c = 10.0819（5） ,α = 86.133（3）,= 81.956（3）,γ = 80.248（3）o,Z = 2 and μ = 0.670 mm-1.The hydrogen bonds are found to exist in 2b only.The crystal structure is stabilized by intermolecular hydrogen bonds of C-H···O.
文摘The adsorption properties of nanometer-size TiO2 for V（Ⅴ ） were studied. The adsorption rate could reach above 99~ when the pH values were at the range of 4 10. The adsorption balance time was 10 min , the saturation capacity of adsorption of nanometer-size TiO2 to V（Ⅴ） was 6.43 mg per gram. Using 2 mL 1.5 mol · L^-1 NaOH as elution, we found the elution rate could reach 95%. A novel method of extreme-trace V（Ⅴ ） preconeentration with nanometer-size titanium dioxide and determination by graphite furnace atomic absorption spectroscopy （GFAAS） was advanced. The detection limit（3σ）of the method was 0.61μg ·L^-1 , and the relative standard deviation was 8.1% （n=6） of 2.5μg ·L-^1 V（Ⅴ）. Environmental samples experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 91.2% and 102.0%.
