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1.
双水相体系中Cu(Ⅱ),La(Ⅲ),U(Ⅵ),Ce(Ⅳ)光谱行为及萃取分离   总被引:4,自引:1,他引:3  
利用聚乙二醇2000(PEG)-(NH)2SO4-萃取剂(铜试剂)双水相体系,采用液-液萃取的方法,研究了PEG相、单纯水相中金属离子络合物及萃取剂的光谱行为,探讨了金属离子络合物在PEG相中存在形态及萃取机理。同时实验了在不同酸度,不同盐用量,不同萃取剂用量,以及在不同表面活性剂的影响下,铜、镧、铀、铈的萃取率,通过控制一定条件,实现了Cu(Ⅱ)与La(Ⅲ),Cu(Ⅱ)与Ce(Ⅳ)之间的定量萃取分离。  相似文献   

2.
研究了以碘化钾为络合剂,正丙醇-水体系析相萃取分离和富集铋的行为及与一些金属离子分离的条件。试验结果表明,氯化钠能使正丙醇的水溶液分成两相,在分相过程中,Bi(Ⅲ)与碘化钾生成的BiI_4~-与质子化正丙醇(C_3H_7OH_2~+)形成的缔合物[BiI_4~-][C_3H_7OH_2~+]能被正丙醇相完全萃取。当正丙醇、碘化钾和氯化钠的浓度分别为30%(V/V)、6.0×10~(-3)mol·L~(-1)、0.20g·mL~(-1),pH为2时,Bi(Ⅲ)的萃取率达到99.2%以上,V(Ⅴ),W(Ⅵ)和U(Ⅵ)基本不被萃取,实现了Bi(Ⅲ)与上述金属离子的分离,对合成水样中Bi(Ⅲ)进行分离和测定,结果令人满意。  相似文献   

3.
研究了以碘化钾为络合剂,正丙醇-水体系析相萃取分离和富集铋的行为及与一些金属离子分离的条件.试验结果表明,氯化钠能使正丙醇的水溶液分成两相,在分相过程中,Bi(Ⅲ)与碘化钾生成的BiI4-与质子化正丙醇(C3H7OH+)形成的缔合物[BiI4-][C3H7OH2+]能被正丙醇相完全萃取.当正丙醇、碘化钾和氯化钠的浓度分别为30%(V/V)、6.0×10-3mol·L-1、0.20g·mL-1,pH为2时,Bi(Ⅲ)的萃取率达到99.2%以上,V(Ⅴ),W(Ⅵ)和U(Ⅵ)基本不被萃取,实现了Bi(Ⅲ)与上述金属离子的分离,对合成水样中Bi(Ⅲ)进行分离和测定,结果令人满意.  相似文献   

4.
以电感耦合等离子体原子发射光谱法(ICP-AES)为检测手段,研究了新型吸附剂六钛酸钾晶须对环境样品中Cu(Ⅱ),Pb(Ⅱ),CA(Ⅱ)的分离/富集行为以及解脱的主要因素,并考察了共存离子的干扰影响.在pH值为5.0,振荡时间为5 min,静置时间为30 min时,吸附率可达到95%以上.以3 mol·L-1HNO3作为解脱剂,沸水浴加热40 min,振荡5 win.静置40 win,可将吸附在六钛酸钾晶须上的Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ)定量洗脱.测定Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ)的检出险分别为0.007 1,0.006 8,0.007 1 μg·mL-1,相对标准偏差(RSD)为0.63%,0.61%,0.50%.在优化的实验条件下,将其用于菊花和琵琶叶中Cu(Ⅱ),Pb(Ⅱ),Cd(Ⅱ)含量的测定,加标回收率在900A~102.9%之间.  相似文献   

5.
研究了氯化钠存在下碘化钾 -罗丹明 B-水体系浮选分离铋 ( )的行为及其与常见离子分离的条件。结果表明 ,在 p H 7.0 ,1.0 g Na Cl存在下 ,当 0 .1mol/ L碘化钾溶液和 1.0× 10 -3 mol/ L罗丹明 B溶液的用量均为 0 .5 m L时 ,Bi( )可被定量浮选 ,而 Cu( )、Zn( )、Mn( )、Co( )、Ni( )、Al( )等在此条件下不被浮选 ,实现了 Bi( )与这些常见离子之间的定量分离 ,对合成水样进行的定量浮选分离测定 ,结果令人满意  相似文献   

6.
流动注射-多道检测-催化动力学同时测定铜和铁   总被引:10,自引:0,他引:10  
基于Cu(Ⅱ),Fe(Ⅲ)在pH3~9范围内能同时催化过氧化氢氧化罗丹明B的褪色反应,探讨了最佳反应条件,通过构建流动注射pH梯度,采用CCD-二极管阵列检测器检测吸光度差值,反向传播-人工神经网络(BP-ANN)处理数据,实现了Cu(Ⅱ),Fe(Ⅲ)流动注射-催化动力学光度法的同时测定。Cu(Ⅱ)和Fe(Ⅲ)的检出限分别为0.10和0.21μg·L~(-1),采样频率为10次·h~(-1),本法用于标准参考物质和食品样品中铜、铁的同时测定,结果满意。  相似文献   

7.
在水溶液中,Bi(Ⅲ)与溴化四丁基铵和KI形成不溶于水的三元缔合物BiI-4·TBAB+,此三元缔合物沉淀浮于盐水相上层形成界面清晰的液-固两相。当溶液中溴化四丁基铵和KI的浓度分别为5.0×10-4mol/L和3.0×10-3mol/L,pH=3时,Bi(Ⅲ)可与Zr(Ⅳ)、Ce(Ⅲ)、U(Ⅵ)和Mg(Ⅱ)定量分离,Bi(Ⅲ)的浮选率达到100%。对合成水样中Bi(Ⅲ)的分离和测定,效果良好。该方法具有选择性高,操作简便和不污染环境等特点,在微量铋的分离和富集分析中有一定的实用价值。  相似文献   

8.
采用APDC-MIBK萃取分离铝,电感耦合等离子体质谱(ICP-MS)法同时测定高纯铝中Co,Ni,Cu,Mo,Cd,Pb和Bi.详细地讨论了仪器工作参数,内标元素,分离、富集条件,样品基体的干扰,确定了实验的最佳测定条件.结果表明,方法的检出限为0.011~0.052 μg·L-1,回收率为92.2%~103.0%,相对标准偏差(RSD)小于2.3%.方法准确、快速、简便,应用于高纯铝中Co,Ni,Cu,Mo,Cd,Pb和Bi等杂质元素的测定,结果满意.  相似文献   

9.
采用MIBK萃取/反相萃取分离富集的方法,建立了氢化物无色散原子荧光法测定复杂地质样品中的痕量碲的新方法.实验了HCI-NaBr-MIBK体系萃取Te(Ⅳ)的能力,研究了Te(Ⅳ)在KMnO4-HCI-MIBK体系中的反相萃取行为.当萃取条件为3.6 mol·L-1 HCI-100 g·L-1NaBr时,Te(Ⅳ)可被MIBK完全萃取;用HCI-KMnO4氧化MIBK相中的Te(Ⅳ),水相反相萃取Te(Ⅵ),成功分离了氢化物原子荧光法测定Te的Au,Ag,Pt,Pd,Cu,Pb,Co,Ni,Cd,As,Sb,Bi,Hg,Tl和Se等干扰元素,方法检出限为1.14×10-4μg·g-1,相对标准偏差为6.84%,对国家标准物质样品分析的结果与所给参考值吻合,可用于复杂地质样品中痕量Te的测定.  相似文献   

10.
本文用光度分析法,研究了在聚乙二醇-硫酸钠-萃取剂双水相体系中茜素S、孔雀绿和PAR的萃取行为,提出了萃取剂与聚乙二醇之间水作为中介的氢键作用。探讨了Zr(Ⅳ),Ti(Ⅳ),La(Ⅲ)几种稀有金属离子在聚乙二醇-硫酸钠-茜素S体系中萃取条件,结果表明,在pH 1-3缓冲溶液中,Zr(Ⅳ)几乎完全可被PEG相萃取,La(Ⅲ)离子部分被萃取,而Ti(Ⅳ)离子则不被萃取,通过控制溶液酸度(pH2),实现了Ti(Ⅳ)与Zr(Ⅳ)的萃取分离。  相似文献   

11.
用聚丙烯腈纤维 (PAN)改性制备的偕胺肟纤维 (AOCF)分别与三氯化铁、氯化钴、氯化镍、氯化镉和氯化汞在酸性介质中反应 ,制备偕胺肟 铁 (Ⅲ )、偕胺肟 钴 (Ⅱ )、偕胺肟 镍 (Ⅱ )、偕胺肟 镉 (Ⅱ )和偕胺肟 汞 (Ⅱ ) 5种偕胺肟 重金属配合物 (用通式M AOCF表示 )。用红外分光光度计分别对偕胺肟纤维和 5种配合物在 4 0 0 0~ 4 0 0cm- 1 范围进行傅里叶变换红外吸收 ,对各M AOCF的FTIR主要吸收峰做了经验归属 ,并将各M AOCF的特征吸收峰与AOCF的相应吸收峰作对比分析 ,结果表明 :配合物中C—N ,CN ,N—O等键的吸收峰位置均向高波数方向移动 ,且峰的强度增加。说明纤维材料中的偕胺肟基团与重金属离子在酸性介质中进行了配位反应 ,偕胺肟基团与重金属离子之间形成了配位键。  相似文献   

12.
Co(Ⅱ),Ni(Ⅱ)非有机溶剂液—液萃取行为的研究   总被引:3,自引:0,他引:3  
In PEG-Eriochrome cyanine R-(NH4)2SO4 system the liquid-liquid extraction behaviour of Co(II) and Ni(II) without organic solvents was investigated. We found that Ni(II) was almost extracted by PEG phase while Co(II) was not extracted in the water solutions of NaAc-HAc (pH=5) and (NH4)2SO4. Thus Co(II) was quantitatively separated from mixed solutions of Ni(II) and Co(II) ions.  相似文献   

13.
Co(II), Ni(II), Cu(II), Cd(II), and Fe(II) complexes with Schiff base derived from 2-amino-5-(2-amino-1,3,4-thiadiazolyl)-1,3,4-thiadiazole (1) and salicylaldehyde have been prepared. The ligand and its complexes have been characterized by IR, 1H NMR spectra, elemental analyses, magnetic susceptibility, UV-Vis. and thermogravimetry–differential thermal analysis (TGA-DTA). The analytical data show 1:2 metal-to-ligand ratio for Co(II), Ni(II), Cd(II), and Fe(II) and 2:2 metal-to-ligand ratio for Cu(II) complexes. The suggested structures for the N-[5′-Amino-2,2′-bis(1,3,4-thiadiazole)-5-yl]-2-hydroxybenzaldehyde Imine (HL) complexes of Fe(II), Co(II), and Cd(II) are octahedral, for the Ni(II) complex is tetrahedral, and for the Cu(II) complex is square-planar  相似文献   

14.
Novel Supramolecular fluorescence receptor derived from calix-system i.e. calix[4]resorcinarene bearing dansylchloride as fluorophore was designed and synthesized. The compound was purified by column chromatography and characterized by elemental analysis, NMR and Mass spectroscopy. Tetradansylated calix[4] resorcinarene (TDCR) shows a boat conformation with C2v symmetry. The complexation behaviour of metal cations [Ag(I), Cd(II), Co(II), Fe(III), Hg(II), Cu(II), Pb(II), Zn(II), U(VI) (1?×?10-4?M)] with tetra dansylated calix[4]resorcinarene (1?×?10-6?M) was studied by spectophotometry and spectrofluorometry. Red shift in the absorption spectra led us to conclude that there is strong complexation Fe(III), Co(II) and Cu(II) with TDCR. These metal cations also produce quenching with red shifts in the emission spectra. The maximum quenching in emission intensity was observed in the case of Fe(III) and its binding constant was also found to be significantly higher than that of Co(II) and Cu(II). Quantum yield of metal complexes of Fe(III) was found to be lower in comparison with Co(II) and Cu(II) complexes. Stern Volmer analysis indicates that the mechanism of fluorescence quenching is either purely dynamic, or purely static.  相似文献   

15.
利用二甲酚橙作萃取剂 ,在吐温 80 (NH4 ) 2 SO4 二甲酚橙 (XO)固 液萃取体系中 ,研究了萃取相 (固相 )中金属离子络合物吸收光谱 ,与XO光谱比较 ,Cu(Ⅱ ) ,U(Ⅵ ) ,Ce(Ⅳ )离子吸光度增大 ,最大吸收波长红移 2 0~ 30nm ;La(Ⅲ )离子几乎未变。同时探讨了该体系中不同酸度、不同盐用量、不同萃取剂用量、不同类型表面活性剂 ,对Cu(Ⅱ ) ,La(Ⅲ ) ,U(Ⅵ ) ,Ce(Ⅳ )离子的萃取率的影响 ,在pH 6 0的酸度下 ,实现了La(Ⅲ )与U(Ⅵ )之间的萃取分离。  相似文献   

16.
This paper reports on our study of the pH effect of solutions on the average hydrodynamic diameter (dav) of the particles of the disperse phase and the electrokinetic potential (ζ) of the particles of low-soluble iron subgroup metals compounds using Fe(II, III), Ni(II), and Co(II) compounds as an example. The pH effect of solutions on the efficiency of the electroflotation extraction of metal ions from aqueous solutions containing these ions in individual form or in mixture was studied. The efficiency of the electroflotation extraction of the low-soluble compounds of iron subgroup metals is directly related to the particle size and electrokinetic potential of the particles, which depend on рН. The maximum degree of particle extraction α reached 97–99% at рН values characterized by the maximum hydrodynamic diameter of particles (over 20 μm for Fe(II) and Co(II) compounds and over 50 μm for Fe(III) and Ni(II) compounds) at ζ potentials of up to–10 mV for systems approximated to real wastewater. In the case of the extraction of the disperse phase of the Fe(III)–Ni(II)–Co(II) multicomponent system, the synergic effect was observed: the coextraction of metals was more complete and effective, which may be due to suppressed negative charge. In the range of рН 10–11, the degree of extraction of the Fe(III) disperse phase did not exceed 74%; in the ternary system, it reached 94%.  相似文献   

17.
PEG-Na2SO4-PAR体系中Pd(Ⅱ)、U(Ⅵ)、Mo(Ⅵ)的萃取分离   总被引:5,自引:0,他引:5  
本文研究了在聚乙二醇-2000(PEG)-硫酸钠(Na2SO4)-4-(2-吡啶偶氮)-间苯二酚(PAR)体系中,Pd(Ⅱ)、U(Ⅵ)、La(Ⅲ)、Mo(Ⅵ)的萃取行为。实验结果表明,在pH4.5 ̄7.5溶液中,Pd(Ⅱ)、U(Ⅵ)、可被PEG相几乎完全萃取,La(Ⅲ)部分被萃取,而Mo(Ⅵ)则不被蔺取,从而实现了Mo(Ⅵ)与Pd(Ⅱ)、U(Ⅵ)混合离子间的定量分离,并初步探讨了PEG相的萃取机理  相似文献   

18.
双水相体系中镧与钛的分离及光谱性能   总被引:7,自引:0,他引:7  
在聚乙二醇-硫酸铵-铬天青S双水相体系中,用铬天青S作萃取剂,研究了La(Ⅲ),Ti(Ⅳ),Zr(Ⅳ)的液-液萃取行为,在pH5.5时,实现了体系中La(Ⅲ)与Ti(Ⅳ)的分离,通过加入表面活性剂测定光谱方法,研究了高聚物相中La(Ⅲ)的存在形态。  相似文献   

19.
A series of transition metal complexes of Co(II), Ni(II), Zn(II), Fe(III) and VO(IV) have been synthesized involving the Schiff base, 2,3-dimethyl-1-phenyl-4-(2-hydroxy-3-methoxy benzylideneamino)-pyrazol-5-one(L), obtained by condensation of 4-aminoantipyrine with 3-methoxy salicylaldehyde. Structural features were obtained from their FT-IR, UV–vis, NMR, ESI Mass, elemental analysis, magnetic moments, molar conductivity and thermal analysis studies. The Schiff base acts as a monovalent bidentate ligand, coordinating through the azomethine nitrogen and phenolic oxygen atom. Based on elemental and spectral studies six coordinated geometry is assigned to Co(II), Ni(II), Fe(III) and VO(IV) complexes and four coordinated geometry is assigned to Zn(II) complex. The interaction of metal complexes with Calf thymus DNA were carried out by UV–VIS titrations, fluorescence spectroscopy and viscosity measurements. The binding constants (Kb) of the complexes were determined as 5?×?105 M?1 for Co(II) complex, 1.33?×?104 M?1 for Ni(II) complex, 3.33?×?105 M?1 for Zn(II) complex, 1.25?×?105 M?1 for Fe(III) complex and 8?×?105 M?1 for VO(IV) complex. Quenching studies of the complexes indicate that these complexes strongly bind to DNA. Viscosity measurements indicate the binding mode of complexes with CT DNA by intercalation through groove. The ligand and it’s metal complexes were screened for their antimicrobial activity against bacteria. The results showed the metal complexes to be biologically active, while the ligand to be inactive.  相似文献   

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