Determination of nickel and cobalt by radiochemical displacement

A radiochemical displacement method has been developed for the determination of nickel and cobalt based on the release of Zn-65 from labelled Zn(PAN)₂ [1-(2-pyridylazo) 2-naphthol] complex in chloroform. The displacement behavior of Zn-65 by nickel and cobalt was studied in the pH range 5–7.5. The effect of various ions on the displacement was also examined. 2–20 g of nickel and cobalt was determined by the aid of calibration plots.     

Spectrophotometric determination of bismuth,cobalt, and nickel after extraction of their xanthates with molten naphthalene

Summary A new method for the spectrophotometric determination of bismuth, cobalt and nickel after extraction of their xanthates into molten naphthalene is described. The optimum pH values are 2.4–4.5 for Bi, 7.5–9.0 for Co, 5.5–7.5 for Ni. The naphthalene containing the metal chelates is dissolved in chloroform, and the absorbance is measured against a reagent blank at 362, 350 and 420 nm for Bi, Co and Ni and respectively. Few ions interfere and the method has been applied successfully for the determination of these metal ions in various complex materials.

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Zusammenfassung Eine neue Methode für die spektrophotometrische Bestimmung von Wismuth, Kobalt und Nickel nach Extraktion ihrer Xanthate mit geschmolzenem Naphthalin wurde beschrieben. Das optimale pH für Wismut beträgt 2,4–4,5, für Kobalt 7,5–9,0 und für Nickel 5,5–7,5. Das die Metallchelate enthaltende Naphthalin wird in Chloroform gelöst und die Extinktion gegen eine Reagens-Leerlösung bei 362, 350 bzw. 420 nm für Bi, Co bzw. Ni gemessen. Nur wenige Ionen stören. Das Verfahren wurde mit Erfolg zur Bestimmung der genannten Ionen in verschiedenen komplexen Gemischen angewandt.

     

The simultaneous spectrophotometric determination of nickel and cobalt in mixtures with 3-hydroxypicolinealdehyde azine

The properties of the nickel complex of 3-hydroxypicolinealdehyde azine are described (λ_max = 480 nm, ? = 4.2· 10⁴ l mol^-1 cm^-1). The optimal conditions for a selective and sensitive spectrophotometric determination of nickel are discussed. The absorption spectra of the nickel and cobalt (II) complexes of 3-hydroxypicolinealdehyde azine are sufficiently different to permit the simultaneous spectrophotometric determination of both ions when the absorbances are measured at 480 nm and 540 nm. Mixtures containing nickel and cobalt in ratios from 0.1 to 10 can be analysed. The method has been applied to process catalysts on alumina supports.     

Determination of cobalt,nickel and copper in steel and in radioactive wastes using desferrioxamine “B”

A simple and sensitive spectrophotometric method for the determination of cobalt, nickel and copper with desferrioxamine-B (desferal) is described. The sensitivity of the colour reactions of cobalt, nickel and copper is increased by introducing desferal. The pH range for the formation of Co II, Ni II or Cu II-desferal. Chelates is 4.5–8.5, 5.5–9, and 6.5–9.5, respectively. The molar absorptivities of the chelates are 1.2·10⁵, 5.6·10⁴ and 4.8·10⁴ at 545 nm, 390 nm and 680 nm, respectively. Beer's law is obeyed up to 10 g/ml of metal ion. The effect of desferal concentration, pH, standing time and interfering ions are discussed. The method was applied to the determination of trace amounts of cobalt, nickel and copper in steel and simulated radioactive wastes.     

Influence of d-Electron Divalent Metal Ions in Complex Formation with L-Tartaric and L-Malic Acids

Binary complexes of α-hydroxy acids (L-Tartaric acid and L-Malic acid) with d-electron metal ions (copper, cobalt, nickel) were investigated. Potentiometric measurements have been performed in aqueous solution with computer analysis of the data for determination of the stability constants of complexes formed in the studied systems. The coordination mode of the complexes was defined using spectroscopic methods: electron paramagnetic resonance (EPR), ultraviolet-visible (UV-Vis), circular dichroism (CD), and infrared (IR). Results of the equilibrium studies have provided evidence for the formation of dimers with copper(II) ions and monomers with cobalt(II) and nickel(II) ions.     

Investigations of Cobalt, Nickel, and Copper Diethyldithiocarbamates Using Thermal Lens Spectrometry

Thermal lens spectrometry was used to study the dissociation kinetics of diethyldithiocarbamate complexes of copper(II), cobalt(III), and nickel(II) as a function of pH in the presence of chloride and sulfate ions. It is shown that, as distinct from conventional spectrophotometric and potentiometric measurements, the reversible dissociation of the test complexes and the irreversible oxidation of the ligand can be studied separately (at a level of n × 10^–8–n × 10^–6 M) using thermal lens spectrometry. Because of work in more dilute solutions and due account of the kinetic features of the systems in question, thermal lens spectrometry provides a higher accuracy of the determination of stability constants for diethyldithiocarbamate complexes of copper(II), cobalt(III), and nickel(II). The adsorption of the diethyldithiocarbamate complexes in question from water–ethanol solutions (1 : 3) on Silasorb C₁₈ silica is studied, and the adsorption constants are determined. The limits of detection of copper(II), cobalt(III), and nickel(II) diethyldithiocarbamates obtained in extraction–thermal-lens determination are n × 10^–8 M.     

Direct spectrophotometric method for the determination of cobalt with indane 1,2,3-trionetrioxime in aqueous medium

A simple, sensitive and selective Spectrophotometric method has been developed for the determination of cobalt using indane 1,2,3-trionetrioxime (ITT): The method is based on the colour reaction between ITT and cobalt(II) in sodium acetate-acetic acid buffer (pH 4.5–7.5) medium. The calibration graph for measurement at 320 nm is linear in the range 1.18–23.60g of cobalt per 25 ml, with molar absorptivity of 5.32×10⁴1mol^–1 cm^–1. The effect of interfering ions has been studied and the method was applied to the determination of cobalt in alloys, with good results.     

Spectrophotometric determination of cobalt in iron-, cobalt- and nickel-base alloys

A spectrophotometric method has been developed for the accurate determination of cobalt at milligram level, based on oxidation of the cobalt(II)-EDTA complex with gold(III) chloride at pH 4.0-6.5 and 100 degrees and measurement of the absorbance of the resultant violet cobalt(III)-EDTA complex at 535 nm. The precision is not affected by the presence of several metal ions; including coloured ones such as Cu(II), Ni(II) and Fe(III). However, chromium(III) interferes since it also forms a violet complex with EDTA, but can be removed by separation with pyridine. Practical application of the method is illustrated by the determination of cobalt in alloys based on iron, cobalt and nickel. Over the cobalt range 8-52% the error ranges from 0.1 to 0.3%.     

Simultaneous spectrophotometric determination of traces of cobalt,nickel and copper with dithio-oxamide

The cobalt, nickel and copper complexes of dithio-oxamidc have been characterized in terms of color, effect of pH, structure in solidion, order of addition of reagents, adherence to Beer's law and sensitivity. The reactivity of the reagent to other ions has been reported. A method for the simultaneous spectrophotometric determination of cobalt, nickel and copper has been developed. the results of the application of this procedure to synthetic samples and to several National Bureau of Standards Samples are given.     

Simultaneous spectrophotometric determination of traces of cobalt,nickel and copper with n,n'-bis(3-dimethylaminopropyl)dithio-oxamide

The cobalt, nickel and copper complexes of N,N'-bis(3-dimethylaminopropyl)dithio-oxamide have been characterized in terms of color, effect of pH, rate of color formation, structure in solution, order of addition of reagents, adherence to Beer's law, and sensitivity. The reactivity of the reagent to other ions has been reported. A method for the simultaneous spectrophotometric determination of cobalt, nickel and copper has been developed. The results of the application of this procedure to synthetic samples and to several National Bureau of Standards samples are given.     

Determination of ultra trace amounts of cobalt and nickel in water samples by inductively coupled plasma-optical emission spectrometry after preconcentration on modified C18-silica extraction disks

A highly sensitive and accurate method for preconcentration and determination of ultra trace amounts of cobalt and nickel ions in water samples is proposed. The preconcentration is achieved using C₁₈-silica extraction disks modified with 5-(6-methoxy-2-benzothiazoleazo)-8-aminoquinoline (MBTAQ). The retained ions on the prepared solid phase was eluted with 10 ml of 0.01 M nitric acid and measured by inductively coupled plasma-optical emission spectrometry (ICP-OES). The influence of the type and amount of eluent used, pH, sample and eluent flow rates, amount of MBTAQ and the effect of other ions on extraction efficiency were investigated. The limits of detection of the method were 0.08 and 0.06 μg l^− 1 for cobalt and nickel, respectively, and provide an enrichment factor of 100. The results obtained on 10 successive extractions and elution cycles revealed relative standard deviations of 1.5 and 1.0% for cobalt and nickel, respectively. The proposed method has been applied to the determination of ultra trace amounts of cobalt and nickel ions in natural and synthetic water samples with satisfactory results.     

Spectrophotometric determination of cadmium(II) using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

The complex of cadmium with the reagent 2-(-5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been studied. The composition, stability constant, and free energy change of formation of the complex have been determined. A sensitive spectrophotometric method for the determination of cadmium has been developed and applied for a range of concentration of 0.4–4.0 μg/ml cadmium using the complex Cd-5-Br-PADAP. The optimum conditions for maximum sensitivity of determination such as standing time, pH, wavelength, and order of addition have been determined. The effect of foreign ions on this method has been also studied.     

Synthesis and properties of disulfonated (2-benzimidazolyl)(phenyl)methanone 5-nitro-2-pyridylhydrazone (S2BINPH) and spectrophotometric determination of trace amounts of nickel with S2BINPH

Disulfonated (2-benzimidazolyl)(phenyl)methanone 5-nitro-2-pyridylhydrazone (S₂BINPH) has been synthesized and its reactivity with metal ions investigated. A sensitive and selective spectrophotometric method for the determination of nickel with this reagent has been developed. S₂BINPH reacts with nickel(II) to form a stable 12 (metal ligand) complex with an absorption maximum at 501 nm. The complex formation is quantitative in the pH range 7.2–8.5. Beer's law is obeyed over the range 60–700 ng ml^–1 of nickel and the apparent molar absorptivity of the complex is 8.86 × 10⁴ mol^–1 1 cm^–1 at 501 nm. The proposed method was applied to the determination of nickel in a standard iron- and -steel sample with satisfactory results. Furthermore, proton dissociation constants of S₂BINPH and the overall formation constant of its nickel complex were also determined spectrophotometrically.     

Trisacetylacetonates of cobalt(II) and nickel(II) with the tetrabutylammonium cation at the outer sphere

Conclusions The trisacetylacetonates of cobalt and nickel with the tetrabutylammonium cation in the outer sphere have been synthesized by the interaction of tetrabutylammonium hydroxide, acetylacetone, and the dihydrates of cobalt and nickel bisacetylacetonates. The nickel complex is thermally more stable than the cobalt complex. When heated in vacuum, both complexes decompose into tetrabutylammonium acetylacetonate and anhydrous acetylacetonates of cobalt(II) and nickel(II).Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 5, pp. 975–978, May, 1986.     

Simultaneous differential kinetic determination of cobalt and nickel based on on-line complex formation and ligand substitution reaction using a stopped-flow FIA system

A differential kinetic method utilizing a stopped-flow FIA system is proposed for the simultaneous determination of cobalt and nickel at sub-ppm levels in mixtures. The method is based on the large difference in the rates of the ligand substitution reaction of the metal complexes of 2-(5-bromo-2-pyridylazo)-5-(N-propyl-N-sulfopropylamino)aniline (PSAA) with nitrilotriacetic acid. The apparent reaction rate for the Ni-PSAA complex is more than 100 times larger than that for Co-PSAA complex. The relative standard deviations in the analysis of binary mixture of 0.50 g/ml cobalt and 0.30 g/ml nickel were 1.9% and 2.1%, respectively (n=7). The sample throughput is about 20 h^–1. The effect of various ions was also studied. The proposed method has satisfactorily been applied to synthetic samples containing different ratios of cobalt and nickel 1/12 to 10/1.     

Voltammetric determination of traces of cobalt(II) with a chemically modified carbon paste electrode

Summary A new preconcentration and voltammetric determination method for cobalt(II) in aqueous solution with a chemically modified electrode is proposed. The accumulation behaviour and voltammetry of cobalt(II) has been investigated with a carbon paste electrode modified with cationexchanger and 1,10-phenanthroline. The electrochemical response is characterized with respect to carbon paste composition, pH, preconcentration time, cobalt(II) concentration and other variables. For a 3-min preconcentration time, the electrode gives good linearity for 1×10^–7 to 4×10^–6 mol/l Co(II), a detection limit of 8×10^–8 mol/l. The response can be reproduced with a 4.0% relative standard deviation. The method is fairly free from many coexisting ions interferences. A rapid and convenient renewal procedure allows the use of a single electrode in multiple analytical determinations over several days. Satisfactory results are obtained for the determination of cobalt in a variety of certified standard reference materials.     

Oscillatory Briggs-Rauscher reactions involving macrocyclic transition-metal complexes

New forms have been observed for oscillatory Briggs-Rauscher reactions catalyzed by macrocyclic nickel complexes. The number of oscillations in the reaction increases in the presence of cobalt complexes. Suggestions are made on how the catalysts act in these systems.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 30, No. 3, pp. 167–171, May–June, 1994.     

New iron-containing antibiotics isolation and properties of viridomycins A, B, and C

Summary 1. New iron-containing antibiotics, viridomycins A, B, and C, have been isolated from the actinomyceteActinomyces viridaris.2. Deferriviridomycin A — the precursor of viridomycin A — possesses the capacity for binding not only iron ions but also cobalt, nickel, and copper ions. The copper, nickel, and cobalt analogs of viridomycin A have been obtained.M. M. Shemyakin Institute of Bioorganic Chemistry, Academy of Sciences of the USSR. Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 490–498, July–August, 1975.     

Synthesis and characterization of cobalt(II), nickel(II), copper(II), palladium(II) and dioxouranium(VI) complexes of the antipyrine Schiff base of 3-formylsalicylic acid

A new Schiff base has been synthesized from 4-aminoantipyrine and 3-formylsalicylic acid. The ligand has a dianionic tetradentate compartmental OONO donor system. The cobalt(II), nickel(II), copper(II) and dioxouranium(VI) complexes exist in phenolato-bridged dinuclear species, while palladium(II) gives a mononuclear complex with free –COOH groups. The complexes have been characterized by elemental analyses, i.r., u.v.-vis, thermal and magnetic measurements.     

胶束介质在速差动力学分析中的应用: 钴、镍的同时测定

研究溴化十六烷基三甲铵表面活性剂对钴(Ⅱ)、镍(Ⅱ)与二甲酚橙配位反应的影响, 测定了反应级数和表观活化能。由于胶束介质的存在, 钴(Ⅱ)、镍(Ⅱ)三元配合物的灵敏度比二元配合物分别提高了4.4和8.6倍, 并扩大了两组分的速率差别, 改善了反应的选择性。基于两组分反应速率的差别, 采用对数外推法计算机处理数据, 建立了速差动力学同时测定钴(Ⅱ)、镍(Ⅱ)的新方法。应用于钴精矿等几种实际样品中钴、镍的同时测定获得了满意结果, 其相对误差和标准偏差分别在4%和3%以内。