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1.
Summary Stability constants of copper (II) and nickel (II) oxalates have been determined by paper electrophoresis. Oxalic acid (0.005
mol dm−3) was added to the background electrolyte: 0.1 mol dm−3 HClO4. The proportions of HC2O
4
−
and C2O
4
2−
were varied by changing the pH of the electrolyte, these anions yielding the complex ions MHC2O
4
+
and M(C2O4)
2
2−
, average values of the stability constants for which are 102.4 and 107.6 respectively for Cu(II), and 102.3 and 106.5 for Ni(II) (μ=0.1,30°). 相似文献
2.
Summary A capillary electrophoretic method for the determination of Cu(II) and Co(III) chelates with ethylenediamine in electroless
copper plating baths has been developed. The influence of carrier electrolyte parameters such as nature of counter-ion and
pH were studied and discussed. The optimised separations were carried out in a fused silica capillary (57 cm × 75 μm I.D.)
filled with an ethylenediamine sulfate electrolyte (20 mol L−1 ethylendiamine, pH7.0 with H2SO4; applied voltage, +25 kV) using direct UV detection at 214 nm. The detection limits for a signalto-noise ratio of 3 and 10s
hydrodynamic injection were 5×10−6 mol L−1 for Cu(II) and 1×10−6 mol L−1 for Co(III). The relative standard deviations of the peak areas for Cu(II) and Co(III) were found to be 1.5% and 2.4%, respectively,
with five consecutive injections of standard solution containing 5×10−5 mol L−1 of each metal ion. Application of the method to the speciation of Cu(II) and Co(III) complexes in copper plating bath samples
is also demonstrated. 相似文献
3.
A catalytic adsorptive stripping voltammetric method for the determination of copper(II) on a carbon paste electrode (PCE)
in an alizarin red S (ARS)-K2S2O8 system is proposed. In this method, copper(II) is effectively enriched by both the formation and adsorption of a copper(II)-ARS
complex on the PCE, and is determined by catalytic stripping voltammetry. The catalytic enhancement of the cathodic stripping
current of the Cu(II) in the complex results from a redox cycle consisting of electrochemical reduction of Cu(II) ion in the
complex and subsequent chemical oxidation of the Cu(II) reduction product by persulfate, which reduces the contamination of
the working electrode from Cu deposition and also improves analytical sensitivity. In Britton-Robinson buffer (pH 4.56±0.1)
containing 3.6×10−5 mol L−1 ARS and 1.6×10−3 mol L−1 K2S2O8, with 180 s of accumulation at −0.2 V, the second-order derivative peak current of the catalytic stripping wave was proportional
to the copper(II) concentration in the range of 8.0×10−10 to ∼3.0×10−8 mol L−1. The detection limit was 1.6×10−10 mol L−1. The proposed method was evaluated by analyzing copper in water and soil. 相似文献
4.
N. N. Golovnev A. A. Leshok G. V. Novikova A. I. Petrov 《Russian Journal of Inorganic Chemistry》2010,55(1):130-132
The stability constants of the bismuth(III), indium(III), lead(II), and cadmium,(II) monocomplexes with selenourea (seu) and
thiourea (tu) were determined spectrophotometrically at the ionic strength 1 (0.5 mol/L HClO4 + NaClO4) or 2 (1 mol/L HClO4 + NaClO4) and 276 and 298 K. For all metals, the stability constants (β1) of the complexes with seu were higher than those of the complexes with tu and changed in the series Bi3+ > Cd2+ ≈ In3+ > Pb2+. A correlation between logβ1(S) and logβ1(Se) was established. 相似文献
5.
A new and efficient Hg(II) back-elution method for the desorption of Cd, Cu, and Pb from Chelex-100 chelating resin was developed.
A smaller eluent volume and shorter elution time can be achieved using an Hg(II) containing eluent rather than pure nitric
acid. Owing to the remaining Hg(II) ion in the effluent, a mercury thin-film electrode is formed in-situ during the anodic
stripping voltammetric determination without any further addition of Hg(II). The results indicate that all the analytes in
seawater matrix can be completely adsorbed on Chelex-100 resin from the sample at pH 6.5, and subsequently eluted from the
resin with an acid solution of 5 × 10–4 mol/L Hg2+ + 1 mol/L HClO4. The detection limits obtained from the differential-pulse anodic (μg L–1 to ng L–1) stripping voltammetry are at sub-ppb to ppt (μg L–1 to ng L–1) levels permitting to determine Cd, Cu and Pb traces in seawater. The analytical reliability was confirmed by the analysis
of the certified reference material CASS-II (open ocean seawater).
Received: 22 April 1997 / Revised: 5 August 1997 / Accepted: 7 August 1997 相似文献
6.
The oxidative and reductive electrochemistry of the three isomeric nitroanilines has been studied in neutral (0.1 mol L−1 KClO4) and acidic (0.1 mol L−1 HClO4) aqueous electrolyte solutions by cyclic voltammetry and surface enhanced Raman spectroscopy (SERS). The cyclic voltammograms
recorded for o- and p-nitroanilines with a gold electrode in acidic solution, scanning toward negative potentials, revealed formation of phenylenediamine
not observed in neutral solution. Similar behavior of nitroanilines and phenylenediamines was observed on gold and platinum
electrodes. An oxygen–gold adsorbate stretching mode was detected between 400 and 430 cm−1 in the SER-spectra of the three isomeric nitroanilines in both electrolyte solutions at positive electrode potentials, implying
perpendicular adsorption via the nitro group. 相似文献
7.
De Stefano C Milea D Porcino N Sammartano S 《Analytical and bioanalytical chemistry》2006,386(2):346-356
Interactions between myo-inositol 1,2,3,4,5,6-hexakis(dihydrogen phosphate) (phytic acid) and cadmium(II) were studied by using potentiometry (at
25 °C with the ISE-H+ glass electrode) in different metal to ligand (Phy) ratios (1:1≤Cd2+:Phy≤4:1) in NaClaq at different ionic strengths (0.1≤I/mol L−1≤1). Nine CdiHjPhy(12−2i−j)− species are formed with i=1 and 2 and 4≤j≤7; and trinuclear Cd3H4Phy2−. Dependence of complex formation constants on ionic strength was modeled by using Specific ion Interaction Theory (SIT) equations.
Phytate and cadmium speciation are also dependent on the metal to ligand ratio. Stability of CdiHjPhy(12−2i−j)− species was modeled as a function of both the ligand protonation step (j) and the number of metal cations bound to phytate
(i), and relationships found were used for the prediction of species other than those experimentally determined (mainly di-
and tri-protonated complexes), allowing the possibility of modeling Phy and Cd(II) behavior in natural waters and biological
fluids. A critical evaluation of phytate sequestering ability toward cadmium(II) has been made under several experimental
conditions, and the determination of an empirical parameter has been proposed for an objective “quantification” of this ability.
A thorough analysis of literature data on phytate–cadmium(II) complexes has been performed.
Previous contributions to this series: [1–8] 相似文献
8.
AuCl4− + jOH− + kH2O = AuCl4 − j − k
OH
j
(H2O)
k
k − 1 + (j + k)Cl− equilibria at 20°C were studied spectrophotometrically, and the constants β
jk
in acid aqueous solutions were determined for I = 2.0 mol/L (HClO4). 相似文献
9.
Jinzhang Gao Dongyu Lv Wu Yang Xiaoxia Wei Jie Qu Hua Chen Hongxia Dai Jie Ren 《Central European Journal of Chemistry》2007,5(2):581-589
A convenient and sensitive method for determination of sulfanilamide (SNA) was described based on the Mn(II)-catalyzed oscillating
chemical reaction. Under optimum conditions, a linear relationship existed between the changes of oscillating period or amplitude
and the negative of logarithm of SNA concentration in the range of 4.27 × 10−8 mol ·L−1 ∼ 7.41 × 10−6 mol ·L−1 (RSD, 0.85%) and 9.33 × 10−8 mol ·L−1 ∼ 3.02 × 10−6 mol ·L−1 (RSD, 1.08%), respectively. The lower limit of detection was found to be 2.69 × 10−8 mol ·L−1 and 6.03 × 10−8 mol ·L−1, respectively.
相似文献
10.
de la Escosura-Muñiz A González-García MB Costa-García A 《Analytical and bioanalytical chemistry》2006,384(3):742-750
A new electroactive label has been used to monitor immunoassays in the determination of human serum albumin (HSA) using glassy-carbon
electrodes as supports for the immunological reactions. The label was a gold(I) complex, sodium aurothiomalate, which was
bound to rabbit IgG anti-human serum albumin (anti-HSA-Au). The HSA was adsorbed on the electrode surface and the immunological
reaction with gold-labelled anti-HSA was then performed for one hour by non-competitive or competitive procedures. The gold(I)
bound to the anti-HSA was electrodeposited in 0.1 mol L−1 HCl at −1.00 V for 5 min then oxidised in 0.1 mol L−1 H2SO4 solution at +1.40 V for 1 min. Silver electrodeposition at −0.14 V for 1 min followed by anodic stripping voltammetry were
then performed in aqueous 1.0 mol L−1 NH3–2.0×10−4 mol L−1 AgNO3. For both non-competitive and competitive formats, calibration plots in the ranges 5.0×10−10 to 1.0×10−8 mol L−1 and 1.0×10−10 to 1.0×10−9 mol L−1 HSA, respectively, with estimated detection limits of 1.5×10−10 mol L−1 (10 ng mL−1) and 1.0×10−10 mol L−1 (7 ng mL−1), respectively, were obtained. Levels of HSA in two healthy volunteer urine samples were also evaluated, using both immunoassay
formats. 相似文献
11.
This paper describes the development and validation of a sequential injection (SI) anodic stripping voltammetry (ASV) method
using the hanging mercury drop electrode for accumulation of the heavy metal cations Cu(II), Pb(II) and Cd(II). The method
was applied to wastewater samples after proper acid digestion in open vessels to eliminate matrix effects. For a deposition
time of 90 s at the flow rate of 10 μl s−1, the detection limits of the method were 0.06, 0.09 and 0.16 μmol L−1 for Cd, Pb and Cu, respectively. Under these conditions the linear dynamic range was between 0.20 and 9.0 μmol L−1 and the sampling frequency was 30 analyses per hour. The relative standard deviation of the method was 3%(n=7) at the concentration level of 2.0 μmol L−1. The accuracy of the method was evaluated by spiking the samples with known amounts of the metal cations, and by comparison
with an independent analytical technique, the inductively coupled plasma atomic emission spectroscopy (ICP-AES). Average recoveries
were around of 84%, and the results showed no evidence of systematic errors in comparison to the ICP-AES. 相似文献
12.
Cecylia Wardak 《Central European Journal of Chemistry》2008,6(4):607-612
A new all plastic sensor for Co2+ ions based on 2-amino-5 (hydroxynaphtyloazo-1′)-1,3,4 thiadiazole (ATIDAN) as ionophore was prepared. The electrode exhibits
a low detection limit of 1.5 × 10−6 mol L−1 and almost theoretical Nernstian slope in the activity range 4.0 × 10−6–1 × 10−1 mol L−1 of cobalt ions. The response time of the sensor is less than 10 s and it can be used over a period of 6 months without any
measurable divergence in potential. The proposed sensor shows a fairly good selectivity for Co(II) over other metal ions.
The electrode was successfully applied for determination of Co2+ in real samples and as an indicator electrode in potentiometric titration of Co2+ ions with EDTA.
相似文献
13.
Summary Stoichiometric stability constants of Cu(II), Ni(II), Zn(II), Co(II), UO2(II) and Th(VI) phthalate have been determined by paper electrophoresis. Phthalic acid (0.005 mol dm−3) was added to the background electrolyte: 0.1 mol dm−3 HClO4. The proportions of C6H5C2O
4
−
and C6H4C2O
4
=
were varied by changing the pH of the electrolyte. These anions yielded the complexes, Cu C6H5C2O
4
+
, Cu C6H4C2O4, Zn C6H5C2O
4
+
, Co C6H5C2O
4
+
, Ni C6H5C2O
4
+
, UO2 C6H5C2O
4
+
, UO2 (C6H4C2O4)
2
=
and Th (C6H4C2O4)2 whose stability constants are found to be 103.0, 104.7, 102.6, 102.5, 102.3, 103.5, 1012.6 and 1013.4 respectively (μ=0.1, temp 40°C). 相似文献
14.
A simple and fast flow injection fluorescence quenching method for the determination of iron in water has been developed.
Fluorimetric determination is based on the measurement of the quenching effect of iron on salicylic acid fluorescence. An
emission peak of salicylic acid in aqueous solution occurs at 409 nm with excitation at 299 nm. The carrier solution used
was 2 × 10−6 mol L−1 salicylic acid in 0.1 mol L−1 NH4+/NH3 buffer solution at pH 8.5. Linear calibration was obtained for 5–100 μg L−1 iron(III) and the relative standard deviation was 1.25 % (n = 5) for a 20 μL injection volume iron(III). The limit of detection
was 0.3 μg L−1 and the sampling rate was 60 h−1. The effect of interferences from various metals and anions commonly present in water was also studied. The method was successfully
applied to the determination of low levels of iron in real samples (river, sea, and spring waters). 相似文献
15.
Salih Ilhan Hamdi Temel Salih Paşa İbrahim Teğin 《Russian Journal of Inorganic Chemistry》2010,55(9):1402-1409
Eight new macrocyclic complexes were synthesized by template reaction of 1,4-bis(3-aminopropoxy)butane or (±)-trans-1,2-diaminocyclohexane
with metal nitrate and 1,2-bis(2-formylphenyl)ethane and their structures were proposed on the basis of elemental analysis,
FT-IR, UV-Vis, molar conductivity measurements, 1H NMR and mass spectra. The metals to ligand molar ratios of the complexes were found to be 1: 1. The complexes are 1: 2 electrolytes
for Cd(II), Pb(II) and Zn(II) complexes and 1: 3 electrolytes for La(III) as shown by their molar conductivities (Λm) in DMSO at 10−3 mol L−1. Due to the existence of free ions in these complexes, such complexes are electrically conductive. The configurations of
Cd(II) and Zn(II) complexes were proposed to probably tetrahedral, La(III) complexes are octahedral and Pb(II) complexes are
octahedral geometry in the L1 complex and tetrahedral geometry in the L2 complex. 相似文献
16.
Barbora Drtinová Milan Pospíšil 《Journal of Radioanalytical and Nuclear Chemistry》2010,286(3):631-636
Behavior of cadmium(II) in aqueous solutions irradiated by accelerated electrons was studied. A concentration of 8.8 × 10−4 mol L−1 of cadmium dissolved from Cd(NO3)2 requires dose of 15 kGy to be effectively removed from the system containing 1 × 10−2 mol L−1 of HCOOK as a scavenger of OH radicals. The positive effect of deaeration with N2O or N2 was observed in the range of lower doses. The addition of solid modifiers (bentonite, active carbon, zeolite, Cu2O, NiO, TiO2 and CuO) reduced the effectivity of radiation removal of cadmium. Product of irradiation is CdCO3. On the contrary, in the system with cadmium dissolved from CdCl2 radiation reduction takes place. Systems contained organic complexants (ethylene diamine tetraacetic acid–EDTA, citric acid)
were also studied. The solutions of Cd(NO3)2 containing initial concentration 2.37 × 10−4 mol L−1 of CdII were mixed with 3 × 10−4 mol L−1 EDTA. In this system the efficient degradation proceeds up to 90% at a dose of 45 kGy with addition of 5 × 10−3 mol L−1 carbonate (pH 10.5). The product of irradiation is CdCO3. The presence of 1 × 10−2 mol L−1 of HCOOK in the solution is necessary for radiation removal of cadmium complexed with citric acid (1 × 10−3 mol L−1) at pH 8. With increasing concentration of HCOOK (up to 5 × 10−2 mol L−1) decreases the pH value necessary for the radiation induced precipitation of cadmium. The best result was obtained in the
system containing zeolite as a solid modifier. 相似文献
17.
Mozaffar Asadi Maryam Mohammadikish Khosro Mohammadi 《Central European Journal of Chemistry》2010,8(2):291-299
Four Schiff base ligands, salabza-H2 = N,N′-bis(salicylidene)-2-aminobenzylamine, were synthesized by condensation of one mole of 2-aminobenzylamine and two moles of
salicylaldehyde and/or two moles of substituted salicylaldehyde (5-OMe, 5-Br, 5-NO2). All the four Schiff bases and their Mn(II), Co(II), Cu(II) and Zn(II) complexes are characterized by UV-Vis, FT-IR, 1H NMR spectroscopy, mass spectrometry and elemental analysis. The formation constants and the Gibbs free energies were measured
spectrophotometrically for 1:1 complexes in methanol in constant ionic strength (I = 0.1 mol dm−3 NaClO4) and at 25°C. The data refinement was carried out with the SQUAD program. The trend of formation constants of H2L1 with M(II) follows the order: Mn(II) (3.97) < Zn(II) (4.30) < Co(II) (4.89) < Cu(II) (5.73) 相似文献
18.
Karadjova IB Lampugnani L D'Ulivo A Onor M Tsalev DL 《Analytical and bioanalytical chemistry》2007,388(4):801-807
A rapid, accurate, and precise method is described for the determination of Pb in wine using continuous-flow hydride generation
atomic fluorescence spectrometry (CF-HGAFS). Sample pretreatment consists of ten-fold dilution of wine followed by direct
plumbane generation in the presence of 0.1 mol L−1 HCl and 1% m/v K3[Fe(CN)6] with 1% m/v NaBH4 as reducing agent. An aqueous standard calibration curve is recommended for Pb quantification in wine sample. The method
provides a limit of detection and a limit of quantification of 0.3 μg L−1 and 1 μg L−1, respectively. The relative standard deviation varies between 2–6% (within-run) and 4–11% (between-run) at 3–30 μg L−1 Pb levels in wine. Good agreement has been demonstrated between results obtained by CF-HGAFS and direct electrothermal atomic
absorption spectrometry in analyses of red and white wines within the concentration range of 9.2–25.8 μg L−1 Pb. 相似文献
19.
Kathryn E. Toghill Gregory G. Wildgoose Amir Moshar Chris Mulcahy Richard G. Compton 《Electroanalysis》2008,20(16):1731-1737
We report the simultaneous electroanalytical determination of Pb2+ and Cd2+ by square‐wave anodic stripping voltammetry (SWASV) using a bismuth nanoparticle modified boron doped diamond (Bi‐BDD) electrode. Bi deposition was performed in situ with the analytes, from a solution of 0.1 mM Bi(NO3)3 in 0.1 M HClO4 (pH 1.2), and gave detection limits of 1.9 μg L?1 and 2.3 μg L?1 for Pb(II) and Cd(II) respectively. Pb2+ and Cd2+ could not be detected simultaneously at a bare BDD electrode, whilst on a bulk Bi macro electrode (BiBE) the limits of detection for the simultaneous determination of Pb2+ and Cd2+ were ca. ten times higher. 相似文献
20.
Melchor González-Dávila J. Magdalena Santana-Casiano Frank J. Millero 《Journal of solution chemistry》2006,35(1):95-111
The oxidation rates of nanomolar levels of Fe(II) in seawater (salinity S = 36.2) by mixtures of O2 and H2O2 has been measured as a function of pH (5.8–8.4) and temperature (3–35∘C). A competition exists for the oxidation of Fe(II)
in the presence of both O2 (μ mol⋅L−1 levels) and H2O2 (nmol⋅L−1 levels). A kinetic model has been applied to explain the experimental results that considers the interactions of Fe(II) with
the major ions in seawater. In the presence of both oxidants, the hydrolyzed Fe(II) species dominate the Fe(II) oxidation
process between pH 6 and 8.5. Over pH range 6.2–7.9, the FeOH+ species are the most active, whereas above pH 7.9, the Fe(OH)02 species are the most active at the levels of CO2−3 concentration present in seawater. The predicted Fe(II) oxidation rate at [Fe(II)]0 = 30nmol⋅L−1 and pH = 8.17 in the oxygen-saturated seawater with [H2O2]0 = 50nmol⋅L−1 (log 10 k = −2.24s−1) is in excellent agreement with the experimental value of log 10 k = −2.29s−1 ([H2O2]0 = 55nmol⋅L−1, pH = 8). 相似文献