The extraction behavior of Sm(III), Eu(III) ,Er(III) and Yb(III) with 1- nitroso -2- naphthol (HA) in paraffin has been studied. The composition of extracted complexes has been determined to be LnA3 by slope analysis method. The effect of temperature on extraction system is also investigated and thermodynamic parameters are obtained.
The paraffin wax was used as a diluent for 1-nitroso-2-naphthol(HA) and trioctylphosphine oxide(TOPO) in the extraction of lanthanides at 70℃. The composition of the extracted species was given as LnA3(TOPO)2 by means of the slope analysis. The variation of the synergistic extraction equilibrium constant(Ksex) was investigated at 60～80℃, and the thermodynamic data were calculated. The dependence of separation factors on temperature was also studied.
王艳; 周春山; 段青兵; 陈萍
A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high-purity cobalt oxide by ICP-AES. The matrix effect was eliminated by preci- pitation with 1-nitroso-2-naphthol. The matrix effect of cobalt on the absorptions of trace impurities, the effects of reaction time, pH value, dosage of precipitant on the formation of cobalt-1-nitroso-2-naphthol complex, the effects of hydrochloric acid on the stability of this complex and masking of elements were studied. Recoveries of the impurities in spiked sample are from 90% to 110% with a precision of 1.1%-5.0% RSD. The detection limits of the seven elements are in the range of 0.01-0.24μg/g. The method can be applied to the analysis of high-purity cobalt metal, cobalt oxide and other cobalt compounds.
董学畅; 贾智若; 刘志华; 缪明明; 翁哲慧
Tatyana Samarina; Mikhail Proskurnin
Rapid photometric assessment of iron in blood plasma and serum by a simple procedure after the extraction of iron(II) complex with 1-nitroso-2-naphthol in the micellar phase of a nonionic surfactant at the cloud point upon heating (pH range is 4.5–6.3) is proposed. The procedure trueness was verified using a standard reference protocol using bathophenanthroline. The advantages of the procedure are higher sensitivity than the reference protocol: the limit of detection is 0.03 μg/mL, the limit ...
Full Text Available Rapid photometric assessment of iron in blood plasma and serum by a simple procedure after the extraction of iron(II complex with 1-nitroso-2-naphthol in the micellar phase of a nonionic surfactant at the cloud point upon heating (pH range is 4.5–6.3 is proposed. The procedure trueness was verified using a standard reference protocol using bathophenanthroline. The advantages of the procedure are higher sensitivity than the reference protocol: the limit of detection is 0.03 μg/mL, the limit of quantitation is 0.1 μg/mL, the determination range is 0.1 – 2.8 μg/mL (RSD 0.02–0.10. Copper does not interfere with the iron assessment.
Thyssen, Jacob P.; Menné, Torkil; Johansen, Jeanne D.
Background: It is often difficult to establish clinical relevance of metal exposure in cobalt-allergic patients. Dermatologists and patients may incorrectly assume that many metallic items release cobalt at levels that may cause cobalt dermatitis. Cobalt-allergic patients may be unaware...... that they are exposed to cobalt from handling work items, causing hand dermatitis. Objectives: To present early findings with a newly developed cobalt spot test. Methods and Results: A cobalt spot test based on disodium-1-nitroso-2-naphthol-3,6-disulfonate was able to identify cobalt release at 8.3 ppm. The test may...... also be used as a gel test if combined with an agar preparation. We found no false-positive reactions when testing metals and alloys known not to contain cobalt. However, one cobalt-containing alloy, which elicited cobalt dermatitis in cobalt-allergic patients, was negative upon cobalt gel testing...
Samarina, Tatyana; Proskurnin, Mikhail
Rapid photometric assessment of iron in blood plasma and serum by a simple procedure after the extraction of iron(II) complex with 1-nitroso-2-naphthol in the micellar phase of a nonionic surfactant at the cloud point upon heating (pH range is 4.5-6.3) is proposed. The procedure trueness was verified using a standard reference protocol using bathophenanthroline. The advantages of the procedure are higher sensitivity than the reference protocol: the limit of detection is 0.03 μg/mL, the limit of quantitation is 0.1 μg/mL, the determination range is 0.1 - 2.8 μg/mL (RSD 0.02-0.10). Copper does not interfere with the iron assessment.
Citak, Demirhan; Tuzen, Mustafa
A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.
The method of paper chromatography for the separation and quantitative determination of iron, copper, cobalt and nickel in pyrite and chalcopyrite is described.The three systems of ehromtograpbie solvents for the separation of iron, copper, cobalt and nickel on the 8×25 or 15×26 cm Whatman No. 3, involving acetone-hydrochloric acid-water, butanone-hydrochloric acid-water and acetone-acetylacetone-hydrochloric acid-water have been tested. As a developing system for the separation of this four elements in samples, the mixture of aoetone-acetylacetone-hydroehlorio acid-water is considered to be the best. After developing in a 30×40 cm glass dryer, the paper is dried in air and rendered the zone visible by treatment with 0.1% (W/V) rubeanic acid solution. The R1 values, colour reactions with this spray reagent and the eolour are given. A good paper chromatography of elements has been obtained. The elements are determined by colorimetrie method, with 1-nitroso-2-naphthol for cobalt,1-(2-pyridylozo)-2-naphthol for nickel, oxalic acid bis-cyelohexylidene hydrozide for copper, and sulfosalicylic acid for iron. In addition, iron and copper can also be determined by titration with potassium dichromate solution and iodimetry respectively.
Fe- and Cu-complex formation with artificial ligands investigated by ultra-high resolution Fourier-transform ion cyclotron resonance mass spectrometry (FT-ICR-MS: Implications for natural metal-organic complex studies
Full Text Available In recent years, electrospray-ionization mass spectrometry (ESI-MS has been increasingly used to complement the bulk determination of metal-ligand equilibria, for example via competitive ligand exchange-adsorptive cathodic stripping voltammetry (CLE-ACSV. However, ESI-MS speciation analyses may be impacted by instrumental artefacts such as reduction reactions, fragmentation, and adduct formation at the ESI source, changes in the ionization efficiencies of the detected species in relation to sample matrix, and peak overlaps in response to increasing sample complexity. In our study, equilibria of the known artificial ligands citrate, ethylenediaminetetraacetic acid (EDTA, 1-nitroso-2-naphthol (NN, and salicylaldoxime (SA with iron (Fe and copper (Cu were investigated by ultra-high resolution ESI-MS, Fourier-transform ion cyclotron resonance mass spectrometry (FT-ICR-MS, under a variety of sample matrix and ionization settings. The acquired mass spectra were compared with metal-ligand equilibrium data from the literature as well as an adapted speciation model. Overall, the mass spectra produced representative species mentioned in previous reports and predicted by the speciation calculations, such as Fe(Cit, Cu(Cit2, Fe(EDTA, Cu(EDTA, Fe(NN3, and Cu(SA2. The analyses furthermore revealed new species which had been hypothesized but not measured directly using other methods, for example ternary complexes of citrate with Fe and Cu, Cu(SA monomers, and the dimer Fe(SA2. Finally, parallel measurements of a Cu+SA calibration series and a Cu+SA+EDTA competition series indicated that FT-ICR-MS can produce linear responses and low detection limits analogous to those of ACSV. We propose that ultra-high resolution FT-ICR-MS can be used as a representative tool to study interactions of trace metals with artificial as well as natural, unknown ligands at the molecular level.