Determination of traces of molybdenum in sea water by combined anion-exchange — graphite furnace atomic absorption spectrometry

Summary Traces of molybdenum in sea water have been preconcentrated by anion-exchange from acidified samples in the presence of sodium azide. Molybdenum adsorbs strongly on a column of Bio-Rad AG 1 (Cl^–) and can be stripped easily by elution with 2 mol/l NH₄Cl — 2 mol/l NH₄OH solution. Molybdenum in the effluent is determined by graphite furnace atomic absorption spectrometry. The combined method allows to determine traces of molybdenum in sea water as well as non-saline water on a 100 ml sample basis. The method gives a relative standard deviation of better than 8% at a molybdenum level of 10 g 1^–1 of sea water.

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Bestimmung von Molybdänspuren in Meereswasser mit Hilfe einer Kombination von Anionenaustausch und elektrothermischer Atomabsorptionsspektrometrie

     

Anion-exchange behaviour of various metals on DEAE-cellulose in mixed acetic acid-nitric acid media

A number of nitrato complexes of metals have been found to be adsorbed on DEAE-cellulose from mixed acetic acid-nitric acid media, although none can be adsorbed from aqueous nitric acid solutions. The distribution coefficients of Sc, Mo, La, Sm, W, Re, Bi, Th and U are given as functions of acetic acid and nitric acid concentrations (sometimes in the presence of hydrogen peroxide to prevent hydrolytic precipitation). For 25 other metals column adsorption behaviour is described for a 90% acetic acid-10% 7.6M nitric acid mixture. Favourable differences in the distribution coefficients allow useful separations such as FeMoW and USmMoBiTh, to be achieved.     

Anion-exchange behaviour of a number of metal ions on DEAE-cellulose in hydrobromic and hydriodic acid media

Summary The adsorption behaviour of 48 metal ions on DEAE-cellulose layers has been investigated in aqueous hydrobromic and hydriodic acid media. R_F values are given as a function of the hydrobromic and hydriodic acid concentration over the ranges 0.01–6 mol dm^–3 and 0.01–3 mol dm^–3, respectively, and are compared with those obtained with Avicel SF. R_F spectra are comparatively simple in both media, reflecting the strong affinity of the bromide and iodide ions to the DEAE-cellulose phase. Pd, Pt, Re, Au and Hg are distributed chromatographically in either system, while most other metal ions exhibit rather extreme R_F values of near unity or zero. Therefore, the selectivity of the systems is particularly high for Pd, Pt, Re, Au and Hg, providing the possibility of their excellent selective separations.     

Flow analysis of silicate rocks for zirconium

A flow analysis system involving the on-line configuration of an anion-exchange column has been examined to enrich and determine trace concentrations of zirconium of several ppm to hundred ppm levels in silicate rocks and minerals. About 100 mg of sample is decomposed by fusion with a mixture of boric acid and lithium carbonate and taken up with 1M hydrochloric acid to a total of 100 ml. Depending upon the concentration of zirconium, either a 1- or 4-ml aliquot is introduced into an aqueous carrier stream, merged with sulphuric acid and passed through a small volume anion-exchange column. The enriched zirconium is then back eluted with hydrochloric acid, colour-developed with Arsenazo III, and detected spectrophotometrically at 665 nm.     

Studies on novel cyclodextrans: Inclusion of C60 and C70

Cycloisomalto-heptaose (CI-7) and cycloisomalto-octaose (CI-8) are two novel cyclodextrans. Treatment with C₆₀ or C₇₀ by kneading leads to the formation of four distinct water-soluble inclusion complexes: CI-7/C₆₀ (2: 1), CI-8/C₆₀ (2: 1), CI-7/C₇₀ (2: 1) and CI-8/C₇₀ (2: 1). Their formation and structures have been examined by UV vis spectroscopy, X-ray powder diffraction and fluorescence spectral studies. The reaction is a reversible process.     

Production of a positron microprobe using a transmission remoderator.

A production method for a positron microprobe using a beta+-decay radioisotope (22Na) source has been investigated. When a magnetically guided positron beam was extracted from the magnetic field, the combination of an extraction coil and a magnetic lens enabled us to focus the positron beam by a factor of 10 and to achieve a high transport efficiency (71%). A 150-nm-thick Ni(100) thin film was mounted at the focal point of the magnetic lens and was used as a remoderator for brightness enhancement in a transmission geometry. The remoderated positrons were accelerated by an electrostatic lens and focused on the target by an objective magnetic lens. As a result, a 4-mm-diameter positron beam could be transformed into a microprobe of 60 microm or less with 4.2% total efficiency. The S parameter profile obtained by a single-line scan of a test specimen coincided well with the defect distribution. This technique for a positron microprobe is available to an accelerator-based high-intensity positron source and allows 3-dimensional vacancy-type defect analysis and a positron source for a transmission positron microscope.     

Determination of lead in seawater by flow-injection on-line preconcentration-electrothermal atomic absorption spectrometry after coprecipitation with iron(III) hydroxide.

A flow-injection on-line preconcentration-electrothermal atomic absorption spectrometric (ETAAS) method coupled with a coprecipitation method has been developed for the determination of lead in seawater. The combination of two preconcentration procedures, coprecipitation with iron(II) hydroxide and solid-phase extraction with a lead-selective resin, Pb-Spec, allowed the determination of lead at the ng kg(-1) level. Lead in 250 g of a sample solution was collected by coprecipitation with 10 mg of iron. The precipitate was dissolved in 25 ml of 1 mol l(-1) nitric acid; then, a 4-ml aliquot of the sample solution was introduced into the flow-injection system to preconcentrate and separate lead from iron on a Pb.Spec microcolumn. The sorbed lead was eluted with a 1.0 x 10(-4) mol l(-1) EDTA solution. The 30-microl portion of the eluate corresponding to the highest analyte concentration zone was injected into a graphite furnace. The overall enhancement factor was about 200 for 250 g of the sample. The average and standard deviation of ten blank values obtained were 1.7 ng and 0.38 ng, respectively. The recovery was 93.7 +/- 5.0% for seawater spiked with 20 ng kg(-1) lead. The proposed method is applicable to the analysis of seawater for lead at slightly higher levels.