Microwave-assisted distillation of iodine for the indirect atomic absorption spectrometric determination of iodide in milk samples
To complete these microwave distillation studies, a method for iodide determination in milk-type samples is proposed. The iodide contained in the sample is oxidized to iodine, which is distilled by means of microwave energy and reduced back to iodide. This iodide is combined with Hg(II) and 2,2′-dipyridyl to give an ion pair, which is selectively extracted into IBMK. Mercury is determined in the extract by ETAAS in order to determine iodide. The yield of the distillation process (100%) was evaluated using the Sandell–Kolthoff reaction. In addition, for the solvent extraction, no buffer was needed; 3/5 was the best phase ratio (organic/aqueous); 30 s was the shaking time and the extracts wer…
A smartphone-based innovative approach to discriminate red pigments in roman frescoes mock-ups
The characterization of red pigments in frescoes wall paintings has been of great interest for researchers to better understand raw material procurement dynamics, pigment receipts, stylistic evolution and to assess their conservation state. In this study a non-destructive colorimetric approach implementing a smartphone-based method was developed in order to be able to distinguish between three pigments made from minium, haematite and cinnabar minerals, and also mixed pigments, preparing frescoes mock-ups following the roman receipt described by Vitruvius. Portable FT-IR, Raman spectroscopy, portable XRF and visible reflectance spectra analyses were carried out as reference methods for smart…
Recent advances in on-line solid-phase pre-concentration for inductively-coupled plasma techniques for determination of mineral elements
Abstract We provide a critical survey on recent progress in on-line solid-phase pre-concentration for inductively-coupled plasma (ICP)-based techniques for trace-level determination of metals. We highlight some of the useful solid-phase materials suitable for on-line separation and enrichment prior to ICP determination. We discuss different applications of the methods developed along with their analytical figures of merit. Finally, we sketch out future prospects in this field.
Arsenic content of Spanish cows' milk determined by dry ashing hydride generation atomic absorption spectrometry.
SummaryThe arsenic content of cows' milk consumed in Spain was determined. A procedure using dry ashing hydride generation atomic absorption spectrometry was developed for the purpose. Experimental conditions for the destruction of organic matter were established and an interference study was carried out. The method developed has a detection limit of 0·1 ng/g, a relative SD of 5%, and a recovery (mean ± CSI) of 100 ± 4%. The accuracy of the method was checked by analysis of a certified sample of IAEA milk powder (mean ± CSI: certified, 4·85 ± 0·32 ng/g; found, 5·04 ± 0·81 ng/g). The proposed procedure was used to analyse cows' milk samples. The extremely low arsenic levels found do not pres…
Metal speciation in solid matrices
The literature on metal ion speciation in solid matrices is reviewed, taking into account its applications in the analysis of soil, sediment, biological materials, foodstuff and other solid samples. The pretreatment methods of various solid materials required for carrying out speciation studies have been highlighted. The basis of the methods of separation of different species from matrices, such as sequential extraction, selective extraction, etc. is discussed. The instrumental techniques used for the characterization of different chemical species in solid matrices have been mentioned. The literature survey reveals the analytical details of the developed methodologies, and these have been e…