Spectrophotometric determination of traces of metallic ions and their mixtures with 3-methyl-1,2-cyclopentanodione dithiosemicarbazone: I. Zinc,cadmium, and mercury

The properties of zinc, cadmium, and mercury complexes of 3-methyl-1,2-cyclopentanodione dithiosemicarbazone and the optimal conditions for their formation are described. The complexes were used with success in the photometric determination of traces of zinc, cadmium, and mercury. Seven procedures are proposed for the accurate analysis of Zn(II)-Cd(II), Zn(II)-Hg(II), Zn(II)-Bi(III), Cd(II)-Hg(II), Cd(II)-Bi(III), Hg(II)-Bi(III), and Zn(II)-Cd(II)-Hg(II) mixtures. Satisfactory results were obtained.     

Determination of arsenic in wheat flour by electrothermal atomic absorption spectrometry using a continuous precipitation-dissolution flow system

A precise, accurate automatic preconcentration method for the determination of total arsenic at the ng g(-1) level in wheat flour is proposed. The sensitivity of the method can be increased by a factor of 20 by precipitating As(V) from 10 ml of digested sample using a weakly acid silver solution. The Ag(3)AsO(4) precipitate is dissolved with 0.5 ml of 6 M ammonia and the resulting solution is collected in an autosampler cup of the ETAAS instrument. The limit of detection achieved in the determination of total arsenic using Pd(NO(3))(2) as modifier is 0.3 ng ml(-1). The proposed method avoids spectral interferences from cations as they do not precipitate with silver cation; anions, which are coprecipitated with silver, are tolerated at concentrations up to about 10 000 times that of As(V). The need to determine As at very low levels in wheat samples, where chloride and phosphate can occur at concentrations 50 000 and 300 000 times higher, respectively, that of arsenic, requires additional steps to suppress the interference of both anions.     

Stopped-flow injection determination of copper(II) at the ng ml−1 level

A stopped-flow injection method for the determination of copper(II) in the range 0.2–300 ng ml^?1 is proposed, based on the catalytic effect of this ion on the 2,2'-dipyridylketone hydrazone/hydrogen peroxide reaction. The oxidation product shows an intense blue fluorescence that is monitored at λ_ex = 350 nm, λ_em = 427 nm. The sampling rate (72 h^?1), r.s.d. (1.4%) and the lack of interference from most foreign ions, allowed application of the method to the determination of copper in foods and blood serum.     

Analysis of gaseous samples by flow injection

A flow-injection configuration based on the repeated change of the flow direction is proposed for the direct analysis of gaseous samples. The sample is injected into a liquid carrier-reagent stream and the repeat passage of the liquid zone close to the gas-liquid interface nearest to the detector is monitored to obtain an absorbance-time multi-peak recording. The system has been applied to the determination of nitrogen dioxide in gaseous samples for the range 0.5–100 μl ml^?1, with a relative standard deviation of 4–5% and a sampling frequency of 60 h^?1. A modification of the injection system allows preconcentration steps to be implemented.     

Flow injection spectrophotometric determination of lactic acid in skimmed milk based on a photochemical reaction

A spectrophotometric method for the determination of lactic acid in milk samples based on the use of a photochemical reaction carried out in a Flow Injection System is proposed. Determination is based on the reaction between lactic acid and Fe(III), which is reduced to Fe(II) in the presence of UV light, being the latter made to react with o-phenanthroline. The complex formed between Fe(II) and o-phenanthroline, Fe(o-phen)(3)(2+) (ferroin) is a coloured compound and it can be spectrophotometrically monitored at 512 nm. The method shows a linear range between 0.5 and 50 mug ml(-1) with a limit of detection of 0.16 mug ml(-1). The precision was +/-2.15 expressed as relative standard deviation (n=11) and the sample throughput of 30 samples h(-1). Also non-linear adjustments have been made and validated by ANOVA. The proposed method has been applied to the determination of lactic acid in both synthetic and milk samples.     

A practical approach to metrology in chemistry and biology

 The inherent difficulties of measurement in chemistry and biology have made it necessary to open discussion forums solely devoted to bench level work. This contribution summarises the conclusions of the Standards, Measurements and Testing Project (SMT4-CT96-6505) of the European Commission, devoted to the application of metrology in chemistry and biology. The objective of this project was to provide orientations and some recommendations which could partially satisfy end-users needs in the near future. Received: 29 September 1998 · Accepted: 21 December 1998     

Experimental characterization of domain walls dynamics in a photorefractive oscillator

We report on the experimental characterization of domain wall dynamics in a photorefractive resonator in a degenerate four-wave mixing configuration. We show how the non-flat profile of the emitted field affects the velocity of domain walls as well as the variations of intensity and phase gradient during their motion. We find a clear correlation between these two last quantities that allows the experimental determination of the chirality that governs the domain walls’ dynamics. PACS 42.65.Sf; 47.54.+r; 42.65.Hw