Simultaneous catalytic-fluorimetric determination of copper and mercury by flow-injection analysis

Summary A catalytic-fluorimetric method is presented for the simultaneous determination of copper(II) and mercury(II) based on their catalytic effects on the oxidation of dipyridyldiketone phenylhydrazone and 2,2-dipyridylketone hydrazone, respectively, using the FIA/ stopped-flow mode. The errors in the determination of these cations are less than 10%, with a sampling rate of 45 samples per hour and the r.s.d. is 0.91% and 1.6% for Cu(II) and for Hg(II), respectively.

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Simultane katalytisch-fluorimetrische Bestimmung von Kupfer und Quecksilber durch Flow-Injection-Analyse

Zusammenfassung Mit Hilfe der FIA/stopped-flow-Technik wurde eine Simultanbestimmung von Cu(II) und Hg(II) durchgeführt, die auf der katalytischen Wirkung dieser Elemente auf die Oxidation von Dipyridyldiketon-phenylhydrazon bzw. 2,2-Dipyridylketon-hydrazon beruht. Die Fehler sind geringer als 10% mit einem Probendurchsatz von 45 Proben je Stunde. Die relative Standardabweichung beträgt 0,91% für Cu und 1,6% für Hg.

     

Simultaneous determination of iron, cobalt, nickel and copper by UV-visible spectrophotometry with multivariate calibration

A method for the simultaneous spectrophotometric determination of the divalent ions of iron, cobalt, nickel and copper based on the formation of their complexes with 1,5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH) is proposed. The resolution of quaternary mixtures of these metallic ions was accomplished by several chemometric approaches. A comparative study of the results obtained for simultaneous determinations in mixture by using principal component regression (PCR) and partial least-squares regression (PLS-1 and PLS-2) for absorbance, first-derivative and second-derivative data is presented. In general, the best recovery values are obtained by the PLS-2 method for absorbance data. This procedure allows the simultaneous determination of the cited ions in alloys and biological materials Good reliability of the determination was proved.     

电位溶出分析法同时测定锡, 铅, 铜

本文应用电位溶出分析法进行同时测定锡、铅和铜的研究。结果发现在草酸溶液中锡、铅和铜有分离清晰的平台,其溶出讯号与浓度呈线性关系,可用于定量分析。用这一方法测定了某些罐头食品中痕量锡、铅和铜,获得满意的结果。     

Simultaneous determination of copper and iron by second derivative spectrophotometry using mixtures of ligands

A highly sensitive and selective second derivative spectrophotometric method has been developed for the determination of copper and iron in mixtures. The method is based on the separation of the analytes by liquid-liquid extraction as picrate ion pairs. Iron-picrate, reacts in the organic phase of DCE with 5-phenyl-3-(4-phenyl-2-pyridinyl)-1,2,4-triazine (PPT). Similarly the copper-picrate reacts with 2,9-dimethyl-4,7-diphenyl-1,10-phenantroline (bathocuproine). The extracts were evaluated directly by derivative spectrophotometric measurement, using the zero-crossing approach for determination of copper and graphic method for iron. Iron and copper were thus determined in the ranges 8-120 ng ml(-1) and 8-125 ng ml(-1), respectively, in the presence of one another. The detection limits achieved (3sigma) were 2.9 ng ml(-1) of iron and 2.8 ng ml(-1) of copper. The relative standard deviations were in all instances less than 2.1%. The proposed method was applied to the determination of both analytes in river and tap water and the results were consistent with those provided by the AAS standard method.     

Simultaneous determination of free and EDTA-complexed copper ions by flame atomic absorption spectrometry with an ion-exchange flow-injection system

A simple method is described for the simultaneous determination of free and complexed copper ions in a flow-injection system comprising ion-exchange and flame atomic absorption spectrometry. Sampling rates for 400-μl samples were 90 h^?1. Typical relative standard deviations for the simultaneous determinations were 1.6% for the complexed metal (0.50 μg ml^?1) and 1.0% for the free metal (0.20 μg ml^?1).     

Simultaneous determination of antimony,arsenic and copper by neutron activation analysis

A rapid procedure has been developed for the mutual separation of antimony and arsenic using tribenzylamine as the extracting agent. The extraction behaviours of Sb(III), Sb(V), As(III), As(V) and Au(III) have been studied as a function of the acidity of the aqueous phase. Various factors which affect the extraction of these complexes have been studied and optimized. The procedure was then applied to lead base alloy for the simultaneous determination of antimony, arsenic and copper. Chemical recoveries were quantitative and only about one hour is required for the chemical processing of duplicate samples.     

Simultaneous determination of polycarboxylic acids by capillary electrophoresis with a copper electrode

The simultaneous determination of polycarboxylic acids including oxalic acid, citric acid, malonic acid, malic acid, tartaric acid, aspartic acid and glutamic acid was achieved by capillary electrophoresis with a copper disk electrode (d = 200 microm). In the system. 0.2 mmol/l cetylpridinium bromide (CPB) was used as an electroosmotic flow (EOF) modifier to reverse the direction of EOF. The effects of the solution pH and CPB concentration on separation were evaluated to achieve the optimum separation conditions. At the working potential of +0.14 V (vs. saturated calomel electrode), the calibration curves for all polycarboxylic acids studied were linear with 2 approximately 3-orders of magnitude and all the detection limits (S/N = 3) were below 15 fmol except malonic acid. Furthermore, the oxalic and citric acids in urine were successfully separated and determined with high sensitivity.     

Simultaneous determination of cobalt,copper, iron and vanadium in crude petroleum oils by HPLC

Summary A method has been developed for the simultaneous formation and solvent extraction of cobalt (II), copper (II), iron (II) and vanadium (IV) complexes of bis (acetylpivalylmethane)ethylenediamine (H₂APM₂en) in methyl isobutyl ketone. The complexes are eluted from a reversed phase HPLC column with a mixture of methanol:water:acetonitrile and detection was at 260 nm. The method has been applied to the simultaneous determination of cobalt, copper, iron and vanadium in crude petroleum oils at the ng level.     

Simultaneous determination of inorganic cations by capillary ion chromatography with a non-suppressed contactless conductivity detector

A non-suppressed capillary ion chromatographic method with a laboratory-made packed cation-exchange column (100 mm × 0.32 mm i.d.) was developed for the separation and simultaneous determination of five common inorganic cations (sodium, ammonium, potassium, magnesium and calcium). Cation exchangers were prepared by the reaction of the hydroxyl group on the surface of diol-group bonded silica gel with 1,3-propanesultone in methanol. Simultaneous separation of these five common inorganic cations were achieved within 17 min using 1 mM methanesulfonic acid and 0.1 mM 15-crown-5 ether in methanol-water (8:2, v/v) as the eluent. The effects of organic solvents and crown ethers in the eluent on the retention of analytes were investigated. The limits of detection (S/N = 3) of the cations were in the range of 18-124 μg/l, the linear correlation coefficients were 0.9991-0.9998, and the RSD values of retention time and peak height were all smaller than 2.1%. The present analytical method was successfully applied to the rapid and direct determination of inorganic cations in samples of river water and commercial drinks, with satisfactory results.     

Simultaneous third-derivative spectrophotometric determination of copper and nickel in iron alloys and aluminium alloy

A method is proposed for the simultaneous determination of copper and nickel by third-derivative spectrophotometry based on the absorption spectra of their complexes with cyanide ion in the ultraviolet range. The method allows the determination of 0.55-5.8 mug/ml of copper and 0.55-6.8 mug/ml of nickel. The relative standard deviation for 11 determinations of 1.5 mul/ml of copper and nickel were 0.78 and 0.72%, respectively. The detection limits were 0.10,mug/ml for nickel and 0.13 mug/ml for copper. The method has been applied to direct determination of copper and nickel in iron alloys and an aluminium alloy without any separation.     

Simultaneous determination of copper and iron in automotive gasoline by X-ray fluorescence after pre-concentration on cellulose paper

This paper proposes an alternative analytical method using energy dispersive X-ray fluorescence (EDXRF) to determine Fe and Cu in gasoline samples. In the proposed procedure, samples were distilled and the distillation residues were spotted on cellulose paper disk to form a uniform thin film and to produce a homogeneous and reproducible interface to the XRF instrument. The disks were dried at 60 °C for 20 min and copper and iron were determined directly in the solid phase at 6.40 and 8.04 keV, respectively. The calibration curves showed linear response in the 20-800 μg L⁻¹ concentration range of each metal. The precisions (repeatability) calculated from 15 consecutive measurements and defined as the coefficient of variation of solutions containing 100 μg L⁻¹ of Fe and Cu were 7.8 and 8.1%, respectively. The limits of detection (LOD), defined as the analyte concentration that gives a response equivalent to three times the standard deviation of the blank (n = 10), were found to be 10 and 15 μg L⁻¹ for Fe and Cu, respectively. The proposed method was applied to copper and iron determination in gasoline samples collected from different gas stations.     

Simultaneous differential rate determination of iron(II) and iron(III) by flow-injection analysis

Flow-injection procedures for the simultaneous spectrophotometric determination iron(II) and iron(III), relying on the different kinetic-catalytic behaviour of iron(II) and iron(III) in the redox reaction between leucomalachite green and peroxodisulphate with and without the presence of the activator 1,10-phenanthroline, are described. Exploiting the fact that one of the chemical reactions is very rapid whereas the other one is comparatively slower, two experimental procedures are presented. In the first, two individual zones of sample solution are injected simultaneously into separate carrier streams of reagent in a two-line system. Taking advantage of the different residence times of the samples in the manifold lines, the resulting colour formation is measured by a single optical detector with two separate flow cells aligned within the same optical path. The second approach is based on the use of a single-line flow-injection system, exploiting the formation of a double peak as a result of injecting a large sample zone, sandwiched between reagent zones of appropriate composition. In this manner two time-resolved signals for the kinetically governed processes can be obtained and thus used for quantification of the individual species.     

Simultaneous determination of iron,cadmium and lead in zinc by proton activation analysis

Iron, cadmium and lead are determined in zinc by proton activation followed by chemical separation of the indicator radionuclides. The method provides detection limits of 0.03, 0.008 ad 0.1 μg g^?1 for iron, cadmium and lead, respectively. The BCR Unalloyed Zinc reference material 321 was analysed. Concentrations of 2.23, 0.215 and 4.641 μg g^? with 1–7% relative standard deviation were obtained for iron, cadmium and lead, respectively. These results contributed to the provisional certification of the reference material.     

Mixed reagents in multicomponent flow-injection analysis Simultaneous determination of iron and copper in blood serum with mixed bathocuproinedisulphonate and bathophenanthrolinedisulphonate or ferrozine

Mixtures of 0.6mM bathocuproinedisulphonate (BC) and 0.2mM bathophenanthrolinedisulphonate (BP) or 2mM BC and 0.2mM ferrozine (FZ) were used for a rapid determination of iron and copper in deproteinated blood serum in the presence of 0.1M formate buffer (pH 3.5), 10mM ascorbic acid and 0.3M trichloroacetic acid, by two variants of multicomponent FIA with a diode-array detector (MC-FIA). Merging zones MC-FIA is especially suitable for the determination of 0.7-33muM Fe and 0.4-35muMCu, for Cu:Fe concentration ratios from 10:1 to 1:10and with RSD <3 or 2% for Fe or RSD <6 or 5% for Cu in artificial mixtures and deproteinated standard blood sera, respectively, and relative errors of less than 3-5%. The concentrations of both elements were calculated according to a simple computer program (ORTHO) for overdetermined systems (10 or 11 wavelengths), but evaluation at the absorption maxima for the individual chelates (at 2 or 3 wavelengths) also gave satisfactory results.     

Simultaneous determination of dichromate and cupric ions

Summary The stage-wise reaction of titanous chloride with a mixture of dichromate and cupric copper is used as the basis of a rapid method for the determination of the individual components of the mixture cited. Diphenylamine is used as indicator for the first reaction while a few drops of ferrous solution in the presence of excess thiocyanate serve as indicator for the second reaction.     

Qualitative analysis of some alloys and determination of copper and iron by the ring-oven method

Methods for the qualitative analysis of various copper alloys, including ancient Egyptian coins, aluminium alloys and zinc alloys by the ring-oven method, are described. Procedures for the colorimetric determination of copper and iron after separation on the ring oven are given.     

Simultaneous determination of trace-levels of alloying zinc and copper by semi-mercury-free potentiometric stripping analysis with chemometric data treatment

Assays of copper and zinc in brass samples were performed by semi-mercury free potentiometric stripping analysis (S-MF PSA) using a thin-film mercury covered glassy-carbon working electrode and dissolved oxygen as oxidizing agent during the stripping step. The stripping peak transients were resolved by chemometrics, which enabled simultaneous determination of both the copper and the zinc concentrations, thereby eliminating the conventional necessary pretreatment of the sample solution, such as initial addition of Ga(III) or solvent extraction of copper. The brass samples were diluted by factors in the range 2 · 10⁴– 5 · 10⁵ which resulted in quantification of the copper and of zinc contents comparable to the specified values within 10%. On the basis of the chemometric treatment, an empirical expression is deduced relating the stripping time to the recorded potential.     

Simultaneous determination of purine bases, ribonucleosides and ribonucleotides by capillary electrophoresis-electrochemistry with a copper electrode

Simultaneous determination of purine bases, ribonucleosides and ribonucleotides was achieved by coupling capillary electrophoresis (CE) with wall-jet amperometric detection. A 200 μm diameter copper disk electrode was applied at working potential, +0.65 V vs. saturated calomel electrode. The current response of high sensitivity and stability was obtained in strong basic solutions which were suitable for satisfactory CE separations. The calibration curve was linear over 2–3 orders of magnitude and the limits of detection for adenine, guanine, xanthine, uric acid, adenosine, guanosine, adenosine-5′-monophosphate and guanosine-5′-monophosphate were below 9 fmol (S/N=3). The use of this method for the separation and detection of compounds present in human plasma samples was reported.     

Simultaneous determination of trace-levels of alloying zinc and copper by semi-mercury-free potentiometric stripping analysis with chemometric data treatment

Assays of copper and zinc in brass samples were performed by semi-mercury free potentiometric stripping analysis (S-MF PSA) using a thin-film mercury covered glassy-carbon working electrode and dissolved oxygen as oxidizing agent during the stripping step. The stripping peak transients were resolved by chemometrics, which enabled simultaneous determination of both the copper and the zinc concentrations, thereby eliminating the conventional necessary pretreatment of the sample solution, such as initial addition of Ga(III) or solvent extraction of copper. The brass samples were diluted by factors in the range 2 · 10⁴– 5 · 10⁵ which resulted in quantification of the copper and of zinc contents comparable to the specified values within 10%. On the basis of the chemometric treatment, an empirical expression is deduced relating the stripping time to the recorded potential. Received: 23 December 1997 / Revised: 25 February 1998 / Accepted: 28 February 1998