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1.
Sample pretreatment for the capillary electrophoretic determination of organic acids in chromium(III) plating baths 下载免费PDF全文
Lukáš Taraba Tomáš Křížek Anna Kubíčková Pavel Coufal 《Journal of separation science》2015,38(24):4255-4261
This work deals with the development and optimization of the sample pretreatment and consequent electrophoretic analysis of two modern plating baths containing chromium(III) and either citric acid or oxalic acid. Some model mixtures containing known amounts of components of industrial baths have been prepared to simulate simplified bath matrices. Prior to analysis, a sample pretreatment consisting of the addition of some agents that could release acid from the stable chromium complex was tested. Determination of organic anions was accomplished by indirect UV detection. The best results were achieved by precipitation of chromium(III) hydroxide. The content of oxalate and citrate in real samples was calculated as 96.5% (SD 2.3%) and 97.3% (SD 0.8%), respectively, of the declared amount. Very good robustness of the method and satisfactory repeatability of migration time and peak area were obtained. This simple inexpensive method is suitable for routine determination of citric and oxalic acid in chromium(III)‐based plating baths. 相似文献
2.
A. A. Massaoud H. A. Hanafi T. Siyam Z. A. Saleh F. A. Ali 《Central European Journal of Chemistry》2008,6(1):39-45
Poly (acrylamide-acrylic acid-dimethylaminoethylmethacrylate), p(AM-AA-DMAEM) and Poly(acrylamide-acrylic acid)-ethylenediaminetetracetic
acid disodium, p(AM-AA)-EDTANa2 were prepared by gamma radiation-induced template polymerization technique and used for the separation of Ga (III) from Cu
(II), Ni (II), and Zn (II) in aqueous media. The effect of pH and contact time on the separation process was studied. The
optimum pH value for the separation process is 3–3.5. The result shows that Ga (III) is first extracted while Cu (II), Ni
(II) and Zn(II) are slightly extracted at this pH value. The recovery of metals using HCl, HNO3 and H2SO4 has been studied. The resins may be regenerated using 2M HCl solutions.
相似文献
3.
R. Hernández-Molina I. Kalinina P. Esparza M. Sokolov J. Gonzalez-Platas A. Estévez-Braun E. Pérez-Sacau 《Polyhedron》2007
Complexes of naturally occurring hydroxynaphtho-quinone, lapachol (2-hydroxy-3(3-methyl-2-buthenyl)-1,4-naphthoquinone = HL) with Co(II), Ni(II) and Cu(II) have been prepared by reaction of the corresponding acetates with the ligand (HL) in ethanol. The molecular and crystal structures were determined for [CoL2(EtOH)2] (1), [NiL2(EtOH)2] (2), and [CuL2(py)2] (3). In all cases the deprotonated lapachol behaves as chelating bidentate ligand. The complexes were also characterized by elemental analyses, cyclic voltammetry, and FAB-MS. 相似文献
4.
In the presented work, copper(II) and chromium(III) complexes chemically bonded to silica surface were prepared and used in gas chromatography. Chlorides of these metals were bonded to the silica surface by the use of the ketoimine group originally from 2-(3-triethoxysililpropylimino)-3-(n-butyl)-pentanone-4. Packings obtained in such way were investigated to evaluate their usefulness in the analysis of aliphatic and aromatic halogenated hydrocarbons as well as ethers, thioethers and ketones. Moreover, packings were subjected to elemental analysis and differential scanning calorimetry (DSC), thus some retention parameters were determined to characterize specific interactions between bonded metal and adsorbate molecules. Attempts were also made to separate some mixtures of the nucleophilic compounds. 相似文献
5.
Krassimir Vassilev Warren T. Ford 《Journal of polymer science. Part A, Polymer chemistry》1999,37(15):2727-2736
Poly(propylene imine) dendrimers having 8, 32, and 64 primary amine end groups form diamino Cu(II), diamino Zn(II), and tetramino Co(III) complexes that are identified spectrophotometrically and titrimetrically. The dendrimer–metal ion complexes catalyze the hydrolysis of p-nitrophenyl diphenyl phosphate in zwitterionic buffer solutions at pH ≤ 8.1 with relative activities Cu(II) > Zn(II) > Co(III). The rates of hydrolysis are faster with sodium perchlorate than with sodium chloride to control ionic strength. In sodium perchlorate solutions with Cu(II) the rates increase with increasing size of the dendrimer. In sodium chloride solutions with Cu(II) the rates decrease with increasing size of the dendrimer. Rate constants in buffered sodium chloride solutions of dendrimers and 1.0mM Cu(II) are 1.3–6.3 times faster than in the absence of Cu(II). The fastest hydrolyses occurred at a dendrimer primary amine to Cu(II) ratio NH2/Cu ≤ 2. At NH2/Cu = 4 and with the 1,4,7,10-tetraazacyclodecane complex of Cu(II) hydrolysis rates were much slower. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 2727–2736, 1999 相似文献
6.
《印度化学会志》2023,100(8):101058
The kinetics of Cu(II) accelerated L-valine (Val) oxidation by hexacyanoferrate(III) in CTAB micellar medium were investigated by measuring the decline in absorbance at 420 nm. By adjusting one variable at a time, the progression of the reaction has been inspected as a function of [OH−], ionic strength, [CTAB], [Cu(II)], [Val], [Fe(CN)63−], and temperature using the pseudo-first-order condition. The results show that [CTAB] is the critical parameter with a discernible influence on reaction rate. [Fe(CN)6]3- interacts with Val in a 2:1 ratio, and this reaction exhibits first-order dependency with regard to [Fe(CN)63−]. In the investigated concentration ranges of Cu(II), [OH−], and [Val], the reaction demonstrates fractional-first-order kinetics. The linear increase in reaction rate with added electrolyte is indicative of a positive salt effect. CTAB significantly catalyzes the process, and once at a maximum, the rate remains almost constant as [CTAB] increases. Reduced repulsion between surfactant molecules' positive charge heads brought on by the negatively charged [Fe(CN)6]3-, OH−, and [Cu(OH)4]2- molecules may be responsible for the observed drop in CMC of CTAB. 相似文献
7.
Yan-Tuan Li Zong-Hui Jiang Dai-Zeng Liao Shi-Ping Yan Shu-Lin Ma Gen-Lin Wang 《中国化学》1994,12(5):414-418
Six novel μ-oxamido binuclear complexes, namely Cu(axpn)Ln(L)2(ClO4)3 (Ln: Eu, Gd, Tb, Nd, Ho, Er), where oxpn is N,N'-bis(3-aminopropyl) oxamido, L denotes 5-nitro,10-phenanthroline (abbreviated as NO2-phen), have been synthesized and characterised. The magnetic susceptibility of complexes Cu(oxpn)Gd(NO2-phen)2(ClO4)3.2H2O was measured over the 4–300 K and the observed data were successfully simulated by equation based on spin Hamiltonian operator (H = -2J1 · S2), giving the exchange integral J(Cu-Gd)=-1.62 cm?1. This indicates a weak antiferromagnetic interaction between the Cu(II) and Gd(III) ions. 相似文献
8.
Four μ- oxamido heterodinuclear complexes, [Cu (oxae) Cr (L)2 ] (NO3) 3, where oxae denotes the N, N'bis (2-aminoethyl) oxamido dianion and L represents 1,10-phenanthroline (phen); 5-nitro-1,10-phenanthroline (NO2-phen); 5-methyl-1, 10-phenanthroline (Me-phen) and 2, 2′-bipyridine (bpy), have been synthesized and characterized by elemental analyses, magnetic moments (at room temperature) and molar conductivity measurements and spectroscopy. It is proposed that these complexes have extended oxamido-bridged structures consisting of a copper (II) ion and a chromium (III) ion, which have a square planar environment and octahedral environment, respectively. The cryomagnetic properties of the [Cu(oxae)Cr(bpy)2(NO3)3(1) and [Cu(oxae)Cr(phen)2](NO3)3(2) complexes have been measured over the range of 4.2–300 K. The leastsquares fit of the experimental data based on the spin Hamiltonian, ? = - 2J?1·?2, the exchange integrals (J) were evaluated as +36.9 cm?1 for 1 and +35.8 cm?1 for 2. The reds have connived that the spin coupling between the adjacent copper (II) and chromium (III) ions through oxamido-bridge in both 1 and 2 is ferromagnetic. 相似文献
9.
《Electroanalysis》2005,17(14):1325-1330
Interference by Cu(II) causes serious problems in the detection of As(III) using anodic stripping voltammetry at gold electrodes. The behavior of Cu(II) and As(III) were examined at both a gold macro electrode and two kinds of gold nanoparticle modified electrodes, one where gold particles are deposited on glassy carbon (GC) and the other where basal plane pyrolytic graphite (BPPG) is the substrate. The sensitivity of As(III) detection was higher on gold nanoparticle modified electrodes than those on a macro gold electrode by up to an order of magnitude. In addition, the stripping peak of As(III) was narrower and more symmetric on a gold nanoparticle‐modified GC electrode, leading to analytical data with a lower limit of detection. At a macro gold electrode, the peak currents of Cu(II) were higher than those on gold nanoparticle modified electrodes. Accordingly, through the use of gold nanoparticle modified electrodes, the effect of copper interference to the arsenic detection can be reduced. 相似文献
10.
《Journal of Coordination Chemistry》2012,65(8):1212-1220
An asymmetric bidentate Schiff-base ligand (2-hydroxybenzyl-2-furylmethyl)imine (L–OH) was prepared. Three complexes derived from L–OH were synthesized by treating an ethanolic solution of the appropriate ligand with an equimolar amount of metallic salt. Three complexes, Cu2(L–O?)2Cl2 (1), Ni(L–O?)2 (2) and Co(L–O?)3 (3), have been structurally characterized through elemental analysis, IR, UV spectra and thermogravimetric analysis. Single crystal X-ray diffraction shows metal ions and ligands reacted with different proportions 1?:?1, 1?:?2 and 1?:?3, respectively, so copper(II), nickel(II), and cobalt(III) have different geometries. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(21):3544-3551
New Schiff bases, N,N′-bis(salicylidene)-4-aminobenzylamine (H2L1), N,N′-bis(3-methoxysalicylidene)-4-aminobenzylamine (H2L2), and N,N′-bis(4-hydroxysalicylidene)-4-aminobenzylamine (H2L3), with their nickel(II), cobalt(II), and copper(II) complexes have been synthesized and characterized by elemental analyses, electronic absorption, FT-IR, magnetic susceptibility, and conductance measurements. For the ligands, 1H and 13C NMR and mass spectra were obtained. The tetradentate ligands coordinate to the metal ions through the phenolic oxygen and azomethine nitrogens. The keto-enol tautomeric forms of the Schiff bases H2L1, H2L2, and H2L3 have been investigated in polar and apolar solvents. All compounds were non-electrolytes in DMSO (~10?3 M) according to the conductance measurements. Antimicrobial activities of the Schiff bases and their complexes have been tested against Acinobacter baumannii, Pseudomonas aeruginosa, Micrococcus luteus, Bacillus megaterium, Corynebacterium xerosis, Staphylococcus aureus, Escherichia coli, Candida albicans, Rhodotorula rubra, and Kluyveromyces marxianus by the disc diffusion method; biological activity increases on complexation. 相似文献
12.
Summary The substitution reduction waves of copper(II)-EGTA and copper(II)-EDTA chelates were investigated with differential pulse and tast polarographic methods. The reduction wave of copper(II)-EGTA chelate shifts to more positive potential in the presence of lanthanum(III) and a new differential pulse peak appears. The peak height increases linearly with increasing concentration of lanthanum(III) between 5 and 25 M. When the copper(II)-EDTA chelate is reduced in a supporting electrolyte containing no buffer solution, lanthanum(III) gives a substitution reduction peak, but in acetate buffer solution the lanthanum(III) peak disappears.
Differential-Puls-Polarographisches Verhalten des Kupfer(II)-Ethylenglykol-bis-(2-aminoethylether)-tetraacetat-Chelats und des Kupfer(II)-Ethylendiamintetraacetat-Chelats in Gegenwart von Lanthan(III)
Zusammenfassung Die Substitutionsreduktionswellen des Kupfer(II)-EGTE- und des Kupfer(II)-EDTE-Chelats wurden mit Hilfe der Differential-Puls- und der Tast-Polarographie untersucht. Die Reduktionswelle des Kupfer(II)-EGTE-Chelats verschiebt sich in Gegenwart von Lanthan(III) zu positiverem Potential und ein neuer Differential-Puls-Peak erscheint. Die Peakhöhe nimmt mit steigender Lanthanionkonzentration zwischen 5 und 25 M linear zu. Wenn Kupfer(II)-EDTE-Chelat im pufferfreien Leitelektrolyt reduziert wird, gibt Lanthan(III) einen Substitutionsreduktions-Peak, in Acetat-Pufferlösung jedoch verschwindet der Lanthan(III)-Peak.相似文献
13.
En-Qing Gao Guang-Ming Yang Jin-Kui Tang Dai-Zheng Liao Zong-Hui Jiang Shi-Ping Yan 《Polyhedron》1999,18(27):648-3646
Four novel tetranuclear macrocyclic complexes of the formula [(CuLi)3Fe](ClO4)3·3H2O (i=1–4, Li are the dianions of the [14]N4 and [15]N4 macrocyclic oxamides, namely 2,3-dioxo-5,6:13,14-dibenzo-7,12-bis(ethoxycarbonyl)-1,4,8,11-tetraazacyclotetradeca-7,11-diene, 2,3-dioxo-5,6:13,14-dibenzo-9-methyl-7,12-bis(ethoxycarbonyl)-1,4,8,11-tetraazacyclotetradeca-7,11-diene and 2,3-dioxo-5,6:14,15-dibenzo-7,13-bis(ethoxycarbonyl)-1,4,8,12-tetraazacyclotetradeca-7,12-diene] have been prepared and characterized. These complexes are the first examples of oxamido-bridged Cu(II)–Fe(III) heterometallic species. Cryomagnetic studies on [(CuL1)3Fe](ClO4)3·3H2O (1) and [(CuL3)3Fe](ClO4)3·3H2O (3) (77–300 K) revealed that the Cu(II) and Fe(III) ions interact antiferromagnetically through the oxamido bridge, with the exchange integral J=−30.8 cm−1 for 1 and J=−28.7 cm−1 for 3 based on
. The interaction parameters have been compared with that of the related [Cu3Mn] compound. 相似文献
14.
The new complexes [Co(ecpzdtc)3] (2) [Zn(ecpzdtc)2(py)] (3) and [Cd(ecpzdtc)2(py)]·H2O (4) have been synthesized from sodium 1-ethoxycarbonyl-piperazine-4-carbodithioate [(Na+(ecpzdtc)−]. The ligand and the complexes have been characterized by elemental analyses, IR, magnetic susceptibility and single crystal X-ray data. The [Zn(ecpzdtc)2(py)] and [Cd(ecpzdtc)2(py)]·H2O complexes contain pyridine as the co-ligand. [Co(ecpzdtc)3] (2) crystallizes in the monoclinic system, whereas [Zn(ecpzdtc)2(py)] (3) and [Cd(ecpzdtc)2(py)]·H2O (4) crystallize in the triclinic system. The sulfur donor sites of the bidentate ligand chelate the metal center, forming a four-membered CS2M ring. The cobalt complex has a distorted octahedral geometry, the zinc complex is almost between trigonal bipyramidal and square pyramidal, whereas the cadmium complex is square pyramidal. The crystal structures of all the complexes are stabilized by various types of inter and intramolecular hydrogen bonding. 相似文献
15.
Six novel μ-oxamido heterobinuclear complexes, namely Cu(oxae)Ln(Me2bpy)2-(ClO4)3 (Ln? La, Nd, Gd, Tb, Ho, Er), where oxae denotes N, N'-bis(2-aminoethyl)oxamido dianion, Me2bpy is 4,4'-dimethyl-2,2'-bipyridyl, have been synthesized and characterised by elemental analyses, IR, conductivity measurements and electronic spectra. The temperature dependence of the magnetic susceptibility of Cu(oxae)Gd(Me2bpy)2(ClO4)3 has been measured over the range 4–300 K. The least-squares fit of the experimental susceptibilities yielded J = 1.87 cm?1. The observed Gd(III)-Cu(II) coupling is ferromagnetic. One plausible mechanism that can cause a ferromagnetic coupling between Gd(III) and Cu(II) is discussed in terms of spin-polarization. 相似文献
16.
Eugenijus Norkus Algirdas Vaškelis Irena Stalnioniene 《Journal of Solid State Electrochemistry》2000,4(6):337-341
The surface area (nanoscale roughness) of copper coatings deposited from electroless plating solutions containing Quadrol,
L(+)- and DL(∓)-tartrate as Cu(II) ion ligands was measured using underpotential deposition thallium monolayer formation.
Surface roughness of Cu coatings depends on the plating solution pH and the Cu(II) ligand, and varies over a wide range. In
L(+)-tartrate and Quadrol solutions (pH 12.5–13.3) the roughness factor R
f is low and is equal to 2–3 and 4–6, respectively (substrate: electrodeposited Cu; R
f=2.2). Cu coatings of higher surface area are obtained in DL(∓)-tartrate (pH 12.3–12.7) and Quadrol (pH 12.0) solutions: R
f reaches 20–30. The correlation between R
f and Cu deposition rate was found in L(+)-tartrate solution. The Cu surface area changes are discussed in terms of partial
electrochemical reactions of the autocatalytic Cu deposition process, and the decisive role of cathodic Cu(II) reduction from
adsorbed Cu(II) complex species.
Received: 2 November 1999 / Accepted: 22 February 2000 相似文献
17.
Newton L. Dias Filho 《Mikrochimica acta》1999,130(4):233-240
The isotherms of adsorption of MeX2 (Me = Cu2+, Co2+; X = Cl–, Br–, ClO
4
–
) by silica gel chemically modified with 2-mercaptoimidazole (SiMI) were studied in acetone and ethanol solutions, at 25 °C. Covalently attached 2-mercaptoimidazole molecule to silica gel surface adsorbs MeX2 from solvent by forming a surface complex. The metal is bonded to the surface through the nitrogen atom of attached 2-mercaptoimidazole. At low loading, the electronic and ESR spectral parameters indicated that the Cu2+ complexes are in a distorted-tetragonal symmetry field. The d-d electronic transition spectra showed that for Cu(ClO4)2 complex, the peak of absorption did not change for any degree of metal loading and for Cl– and Br– complexes, the peak maxima shifted to higher energy with lower metal loading. The CoX2(X = Cl–, Br–, ClO
4
–
) analogues possess a distorted-tetrahedral field. 相似文献
18.
The synthesis and characterization of new transition metal complexes of Mn(II), Co(II), Ni(II), Cu(II) and Zn(II) with 3‐(2‐hydroxynaph‐1‐ylazo)‐1,2,4‐triazole ( HL1 ) and 3‐(2‐hydroxy‐3‐carboxynaph‐1‐ylazo)‐1,2,4‐triazole ( HL2 ) have been carried out. Their structures were confirmed by elemental analyses, thermal analyses, spectral and magnetic data. The IR and 1H NMR spectra indicated that HL1 and HL2 coordinated to the metal ions as bidentate monobasic ligands via the hydroxyl O and azo N atoms. The UV‐Vis, ESR spectra and magnetic moment data revealed the formation of octahedral complexes [Mn L1 (AcO)(H2O)3] ( 1 ), [Co L1 (AcO)(H2O)3]·H2O ( 2 ), [Mn L2 (AcO)(H2O)3] ( 6 ) and [Co L2 (AcO)(H2O)3] ( 7 ), [Ni L1 (AcO)(H2O)] ( 3 ), [Zn L1 (AcO)(H2O)]·H2O ( 5 ), [Ni L2 (AcO)(H2O)] ( 8 ), [Zn L2 (AcO)(H2O)]·10H2O ( 10 ) have tetrahedral geometry, whereas [Cu L1 (AcO)(H2O)2] ( 4 ) and [Cu L2 (AcO)(H2O)2]·5H2O ( 9 ) have square pyramidal geometry.. The mass spectra of the complexes under EI‐con‐ ditions showed the highest peaks corresponding to their molecular weights, based on the atomic weights of 55Mn, 59Co, 58Ni, 63Cu and 64Zn isotopes; besides, other peaks containing other isotopes distribution of the metal. Kinetic and thermodynamic parameters of the thermal decomposition stages were computed from the thermal data using Coats‐Redfern method. HL2 and complexes 6 – 10 were found to have moderate antimicrobial activities against Staphylococcus aureus (gram positive), Escherichia coli (gram negative) and Salmonella sp bacteria, and antifungal activity against Fusarium oxysporum, Aspergillus niger and Candida albicans. Also, in most cases, metallation increased the activity compared with the free ligand. 相似文献
19.
The electroanalytical determination of isoprenaline in pharmaceutical preparations of a homemade carbon paste electrode modified with copper(II) hexacyanoferrate(III) (CuHCF) was studied by cyclic voltammetry. Several parameters were studied for the optimization of the sensor such as electrode composition, electrolytic solution, pH effect, potential scan rate and interferences in potential. The optimum conditions were found in an electrode composition (in mass) of 15% CuHCF, 60% graphite and 25% mineral oil in 0.5 mol l−1 acetate buffer solution at pH 6.0. The analytical curve for isoprenaline was linear in the concentration range from 1.96×10−4 to 1.07×10−3 mol l−1 with a detection limit of 8.0×10−5 mol l−1. The relative standard deviation was 1.2% for 1.96×10−4 mol l−1 isoprenaline solution (n=5). The procedure was successfully applied to the determination of isoprenaline in pharmaceutical preparations; the CuHCF modified carbon paste electrode gave comparable results to those results obtained using a UV spectrophotometric method. 相似文献
20.
Stepan J. Chundak Vukadin M. Leovac Luka J. Bjelica 《Monatshefte für Chemie / Chemical Monthly》1987,118(8-9):923-930
The reaction of aquo-ethanolic solutions of Co(II), Ni(II) and Cu(II) salts and ethanolic solution of capric acid hydrazide (L) yielded paramagnetic, high-spin bis- and tris(ligand) chelate complexes. The tris(ligand) complexes, [ML
3]X
2·nH2O [M=Co(II), Ni(II);X=NO
3
–
, ClO
4
–
, 1/2SO
4
2–
], have an octahedral structure formed on account of the bidentate (NO) coordination of three neutral hydrazide molecules. In the bis(ligand) complexes,ML
2(NCS)2 [M=Co(II), Ni(II)] and CuL
2
X
2·nH2O (X=NO
3
–
, ClO
4
–
and 1/2SO
4
2–
), the oxoanions and NCS– take also part in coordination. The complexes have been characterized by elemental analysis, IR spectra, magnetic measurements, molar conductivity and TG analysis.
Caprinsäurehydrazid-Komplexe von Co(II), Ni(II) und Cu(II)
Zusammenfassung Durch die Reaktion von wäßrig-ethanolischen Lösungen von Co(II)-, Ni(II)-und Cu(II)-Salzen mit einer ethanolischen Lösung von Caprinsäurehydrazid (L) wurden paramagnetische high-spin Bis- und Tris-Ligand-Chelatkomplexe erhalten. Tris-Ligand-Komplexe des Typs [ML 3 X 2·nH2O [M=Co(II), Ni(II);X=NO 3 – , ClO 4 – , 1/2SO 4 2– ], die eine oktaedrische Struktur besitzen, entstehen durch die Koordination von drei neutralen zweizähnigen (NO)-Hydrazidmolekülen. Bei den Bis-Ligand-KomplexenML 2(NCS)2 [M=Co(II), Ni(II)], sowie bei den Bis-Ligand-Komplexen CuL 2 X 2·nH2O (X=NO 3 – , ClO 4 – , 1/2SO 4 2– ) nehmen bei der Koordination außer Hydrazid auch die Säurereste teil. Die Komplexe wurden durch Elementaranalyse, IR-Spektren, magnetische Messungen, molare Leitfähigkeit und TG-Analysen charakterisiert.相似文献