目的对比改良肩关节镜下双纽扣钢板动态固定与锁骨钩钢板切开复位内固定治疗RockwoodⅢ~Ⅴ型肩锁关节脱位的中期疗效。方法回顾性分析2015年1月至2019年12月华中科技大学同济医学院附属同济医院收治的51例RockwoodⅢ~Ⅴ型肩锁关节脱位...目的对比改良肩关节镜下双纽扣钢板动态固定与锁骨钩钢板切开复位内固定治疗RockwoodⅢ~Ⅴ型肩锁关节脱位的中期疗效。方法回顾性分析2015年1月至2019年12月华中科技大学同济医学院附属同济医院收治的51例RockwoodⅢ~Ⅴ型肩锁关节脱位患者资料,其中RockwoodⅢ型19例,Ⅳ型18例,Ⅴ型14例;男32例,女19例;年龄11~65岁,平均(38.6±17.2)岁。21例行改良肩关节镜下双纽扣钢板动态固定术(A组),30例行锁骨钩钢板切开复位内固定术(B组)。比较两组术中及术后住院情况,采用Constant-Murley评分、加利福尼亚大学洛杉矶分校(University of California at Los Angeles,UCLA)评分、疼痛视觉模拟评分(visual analogue scale,VAS)评估肩关节功能。结果患者术后随访24~29个月,平均(24.4±5.2)个月。相较于B组,A组术中出血量更少,住院时间更短,住院总费用更低,但手术时间更长,差异均有统计学意义(P<0.05)。术后3周、6周、12周,A组的Constant-Murley评分、UCLA评分和VAS均优于B组(P<0.05);末次随访时以上3项评价指标组间比较差异均无统计学意义(P>0.05)。两组Constant-Murley评分和UCLA评分术后生存率比较,术后早期A组明显优于B组,末次随访时两组差异无统计学意义。结论对于RockwoodⅢ~Ⅴ型肩锁关节脱位,术后早期(术后3周、6周、12周)关节镜下改良纽扣钢板动态固定更有优势,术后中期(术后24个月)两种方式的治疗效果差异无统计学意义。展开更多
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
A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. ...A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. It crystallizes in a triclinic system with space group P 1, a =0 625 59(8) nm, b =0 639 84(9) nm, c =0 747 19(10) nm, α =78 718(2)°, β =80 099(2)°, γ =77 100(2). The compound contains mixed valence V 4+ /V 5+ vanadium oxide layers constructed from VO 4 tetrahedra, pairs of edge sharing VO 5 square pyramid and methylamine with protonated organic amines occupying the interlayer space.展开更多
The separation and recovery of V from chromium-containing vanadate solution were investigated by a cyclic metallurgical process including selective precipitation of vanadium,vanadium leaching and preparation of vanadi...The separation and recovery of V from chromium-containing vanadate solution were investigated by a cyclic metallurgical process including selective precipitation of vanadium,vanadium leaching and preparation of vanadium pentoxide.By adding Ca(OH)_(2) and ball milling,not only the V in the solution can be selectively precipitated,but also the leaching kinetics of the precipitate is significantly improved.The precipitation efficiency of V is 99.59%by adding Ca(OH)_(2) according to Ca/V molar ratio of 1.75:1 into chromium-containing vanadate solution and ball milling for 60 min at room temperature,while the content of Cr in the precipitate is 0.04%.The leaching rate of V reaches 99.35%by adding NaHCO_(3) into water according to NaHCO_(3)/V molar ratio of 2.74:1 to leach V from the precipitate with L/S ratio of 4:1 mL/g and stirring for 60 min at room temperature.The crystals of NH_(4)VO_(3) are obtained by adjusting the leaching solution pH to be 8.0 with CO2 and then adding NH_(4)HCO_(3) according to NH_(4)HCO_(3)/NaVO_(3) molar ratio of 1:1 and stirring for 8 h at room temperature.After filtration,the crystallized solution containing ammonia is reused to leach the precipitate of calcium vanadates,and the leaching efficiency of V is>99%after stirring for 1 h at room temperature.Finally,the product of V_(2)O_(5) with purity of 99.6%is obtained by calcining the crystals at 560℃ for 2 h.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
A novel mixed valance vanadium phosphate Na 3.6 H 1.4 P 2V 5O 18 ·11H 2O was synthesized by a hydrothermal method and its structure was characterized by X ray diffraction, infrared spectroscopy...A novel mixed valance vanadium phosphate Na 3.6 H 1.4 P 2V 5O 18 ·11H 2O was synthesized by a hydrothermal method and its structure was characterized by X ray diffraction, infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. Na 3.6 H 1.4 P 2V 5O 18 ·11H 2O crystallizes in the cubic system with the cell parameter a =1.601(8) nm. The ratio of V( Ⅳ)/ V(Ⅴ) in the compound is 3.55.展开更多
A novel vanadium（V） oxoperoxo complex [VOO2（APTCH）（CH3OH）] （HAPTCH = 2-acetylpyridine thiophene-2-carboxylic hydrazone） has been synthesized and characterized by IR, TGA and X-ray single-crystal structure dete...A novel vanadium（V） oxoperoxo complex [VOO2（APTCH）（CH3OH）] （HAPTCH = 2-acetylpyridine thiophene-2-carboxylic hydrazone） has been synthesized and characterized by IR, TGA and X-ray single-crystal structure determination. The complex crystallizes in the monoclinic system, space group P21/c with a = 11.232（2）, b = 10.762（2）, c = 112.613（3）, β = 99.44（3）°, V = 1504.1（5）3, Dc = 1.657 g·cm-3, Z = 4, F（000） = 768, μ = 0.827 mm-1, the final R = 0.0392 and wR = 0.1073 for 2266 observed reflections with I 〉 2σ（I）. Single-crystal X-ray diffraction studies reveal that the vanadium（V） is coordinated by a tridentate ligand, methanol molecule and peroxo group to form a pentagonal-bipyramidal geometry. The crystal structure is stabilized by intermolecular hydrogen bonds of O-H···N and C-H···O.展开更多
文摘目的对比改良肩关节镜下双纽扣钢板动态固定与锁骨钩钢板切开复位内固定治疗RockwoodⅢ~Ⅴ型肩锁关节脱位的中期疗效。方法回顾性分析2015年1月至2019年12月华中科技大学同济医学院附属同济医院收治的51例RockwoodⅢ~Ⅴ型肩锁关节脱位患者资料,其中RockwoodⅢ型19例,Ⅳ型18例,Ⅴ型14例;男32例,女19例;年龄11~65岁,平均(38.6±17.2)岁。21例行改良肩关节镜下双纽扣钢板动态固定术(A组),30例行锁骨钩钢板切开复位内固定术(B组)。比较两组术中及术后住院情况,采用Constant-Murley评分、加利福尼亚大学洛杉矶分校(University of California at Los Angeles,UCLA)评分、疼痛视觉模拟评分(visual analogue scale,VAS)评估肩关节功能。结果患者术后随访24~29个月,平均(24.4±5.2)个月。相较于B组,A组术中出血量更少,住院时间更短,住院总费用更低,但手术时间更长,差异均有统计学意义(P<0.05)。术后3周、6周、12周,A组的Constant-Murley评分、UCLA评分和VAS均优于B组(P<0.05);末次随访时以上3项评价指标组间比较差异均无统计学意义(P>0.05)。两组Constant-Murley评分和UCLA评分术后生存率比较,术后早期A组明显优于B组,末次随访时两组差异无统计学意义。结论对于RockwoodⅢ~Ⅴ型肩锁关节脱位,术后早期(术后3周、6周、12周)关节镜下改良纽扣钢板动态固定更有优势,术后中期(术后24个月)两种方式的治疗效果差异无统计学意义。
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 the National Natural Science Foundation of China(No.2 0 1710 10 )
文摘A new layered mixed valence vanadium oxide, [CH 3NH 3] 2[(V ⅣO) 2(V ⅤO 4) 2], which contains interlamellar organic cations was prepared under hydrothermal conditions and its single crystal structure was determined. It crystallizes in a triclinic system with space group P 1, a =0 625 59(8) nm, b =0 639 84(9) nm, c =0 747 19(10) nm, α =78 718(2)°, β =80 099(2)°, γ =77 100(2). The compound contains mixed valence V 4+ /V 5+ vanadium oxide layers constructed from VO 4 tetrahedra, pairs of edge sharing VO 5 square pyramid and methylamine with protonated organic amines occupying the interlayer space.
基金The authors are grateful for the financial supports from the National Natural Science Foundation of China(51974369)the Postgraduate Research Innovation Project of Central South University,China(2019zzts244).
文摘The separation and recovery of V from chromium-containing vanadate solution were investigated by a cyclic metallurgical process including selective precipitation of vanadium,vanadium leaching and preparation of vanadium pentoxide.By adding Ca(OH)_(2) and ball milling,not only the V in the solution can be selectively precipitated,but also the leaching kinetics of the precipitate is significantly improved.The precipitation efficiency of V is 99.59%by adding Ca(OH)_(2) according to Ca/V molar ratio of 1.75:1 into chromium-containing vanadate solution and ball milling for 60 min at room temperature,while the content of Cr in the precipitate is 0.04%.The leaching rate of V reaches 99.35%by adding NaHCO_(3) into water according to NaHCO_(3)/V molar ratio of 2.74:1 to leach V from the precipitate with L/S ratio of 4:1 mL/g and stirring for 60 min at room temperature.The crystals of NH_(4)VO_(3) are obtained by adjusting the leaching solution pH to be 8.0 with CO2 and then adding NH_(4)HCO_(3) according to NH_(4)HCO_(3)/NaVO_(3) molar ratio of 1:1 and stirring for 8 h at room temperature.After filtration,the crystallized solution containing ammonia is reused to leach the precipitate of calcium vanadates,and the leaching efficiency of V is>99%after stirring for 1 h at room temperature.Finally,the product of V_(2)O_(5) with purity of 99.6%is obtained by calcining the crystals at 560℃ for 2 h.
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A novel mixed valance vanadium phosphate Na 3.6 H 1.4 P 2V 5O 18 ·11H 2O was synthesized by a hydrothermal method and its structure was characterized by X ray diffraction, infrared spectroscopy, differential thermal analysis, and thermogravimetric analysis. Na 3.6 H 1.4 P 2V 5O 18 ·11H 2O crystallizes in the cubic system with the cell parameter a =1.601(8) nm. The ratio of V( Ⅳ)/ V(Ⅴ) in the compound is 3.55.
基金supported by the Scientific Research Common Program of Beijing Municipal Commission of Education, PRC (KM200910028011)
文摘A novel vanadium（V） oxoperoxo complex [VOO2（APTCH）（CH3OH）] （HAPTCH = 2-acetylpyridine thiophene-2-carboxylic hydrazone） has been synthesized and characterized by IR, TGA and X-ray single-crystal structure determination. The complex crystallizes in the monoclinic system, space group P21/c with a = 11.232（2）, b = 10.762（2）, c = 112.613（3）, β = 99.44（3）°, V = 1504.1（5）3, Dc = 1.657 g·cm-3, Z = 4, F（000） = 768, μ = 0.827 mm-1, the final R = 0.0392 and wR = 0.1073 for 2266 observed reflections with I 〉 2σ（I）. Single-crystal X-ray diffraction studies reveal that the vanadium（V） is coordinated by a tridentate ligand, methanol molecule and peroxo group to form a pentagonal-bipyramidal geometry. The crystal structure is stabilized by intermolecular hydrogen bonds of O-H···N and C-H···O.
