Bartlomiej Prusisz

Fractionation of calcium and magnesium in honeys, juices and tea infusions by ion exchange and flame atomic absorption spectrometry.

An analytical procedure was proposed to study the operational fractionation of Ca and Mg in bee honeys, fruit juices and tea infusions. The protocol devised was based on the solid phase extraction of distinct metal fractions on different sorbents, namely strong acidic cation exchanger Dowex 50W x 4, weak acidic cation exchanger Diaion WT01S and strong basic anion exchange resin Dowex 1 x 4. For the evaluation of the amounts of the metal fractions distinguished, a flame atomic absorption spectrometry was used off-line prior to the determination of Ca and Mg concentrations in the effluents obtained. It was established that Ca and Mg are mostly present in the analysed samples in the form of cationic species (96-100%). The accuracy of the entire fractionation scheme and sample preparation procedures involved was verified by the performance of the recovery tests.

Determination of Ca, Mg, Fe and Zn partitioning in UHT cow milks by two-column ion exchange and flame atomic absorption spectrometry detection

An operationally defined fractionation protocol was developed to study the partitioning of Ca, Mg, Fe and Zn in UHT cow milks. The method was based on sorption of distinct metal species by two ion exchange columns, namely strong cation exchanger Dowex 50Wx4 and strong anion exchanger Dowex 1x4, connected in a series. The evaluation of the donation of metal species classes distinguished, that is cationic and anionic fractions, was made after splitting the columns and elution of metal groupings with a 2.0mol l(-1)HCl solution, followed by the determination of metal concentrations in the resulting eluates. The amount of third, inert fraction was assessed by measuring metal contents in the effluents obtained after passage of the samples through the columns. The results achieved utilizing two-column ion exchange based procedure were compared with those obtained for the approach in which the columns were considered separately. The fractionation pattern for each metal studied was thoroughly discussed in light of available knowledge relating to the composition of milk.

Fractionation analysis of manganese and zinc in beers by means of two sorbent column system and flame atomic absorption spectrometry.

In the present article, a method of operational fractionation of Mn and Zn in beer using flame atomic absorption spectrometry was developed. The proposed fractionation scheme was based on use of a hydrophobic adsorbing resin Amberlite XAD7 (first column, 2g resin bed) connected in a series with a strong cation exchanger Dowex 50Wx4 (second column, 1g resin bed). After passing the samples of beers through the columns, distinct groupings of Mn and Zn species retained on the sorbents, i.e., hydrophobic fraction of polyphenols bound metal species and cationic metal species fraction, respectively, were determined in respective eluates obtained after complete recovery of Mn and Zn species with 10ml of 2.0moll(-1) HNO(3) (first column) and 10ml of 4.0moll(-1) HCl (second column). In addition, the effluents collected were analyzed prior to the evaluation of the third, residual fraction, presumably attributed to any hydrophilic anionic and inert metal species. The established fractionation patterns for Mn and Zn were discussed in reference to likely associations of metals with endogenous food bioligands and possible availability of the distinguished metal species classes. The quality of the results was proved by the recovery experiments.

Application of Metalfix Chelamine prior to the determination of noble metals by the inductively coupled plasma atomic emission spectrometry

Metalfix Chelamine chelating resins of two different bead sizes (150-300 and 40-80mum) were examined and compared regarding their application for sorption of Au, Ir, Pd, Pt, Rh and Ru ions from medium of HCl, HNO(3) and mixtures of HCl and HNO(3). The quantitative enrichment of Au, Ir, Pd and Pt was established for the resin of 150-300mum particle size and for solutions acidified with HCl and HNO(3) (3:1) up to the concentration of 0.50moll(-1). In the case of Rh and Ru, the uptake of these metals by the resin was lower than 50%. For the elution, solutions of different reagents, i.e. HCl, HNO(3), KCN, KI, KSCN and (NH(2))(2)CS, were studied with respect to the complete release of the analytes retained by the resin. In addition, influence of various base metals, i.e. Al, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and Zn, on the retention of the noble metals was investigated. Under the selected conditions for the retention and elution of Au, Ir, Pd and Pt, the analytical performance of the proposed pre-concentration procedure was evaluated and it was applied to the determination of these noble metals in anodic sludge sample.

Application of tandem column solid phase extraction and flame atomic absorption spectrometry for the determination of inorganic and organically bound forms of iron in wine.

A tandem column solid phase extraction (SPE) procedure has been devised to examine the fractionation of Fe in wine. Wine was filtered through a 0.45 microm filter and then, the filtrate was driven through an adsorbing Amberlite XAD-7HP column followed by a cation exchange Dowex 50 W-x8-200 column. Three different Fe groupings are discriminated and assessed, including hydrophobic species of Fe bound to phenolic substances and related species (phenolic fraction), cationic species comprising simple Fe ions and labile Fe forms (cationic fraction), in addition to anionic and/or neutral Fe complexes with organic acids (residual fraction). The suitability of the procedure has been evaluated analyzing four bottled red wines. The results obtained were verified using another tandem column assemblage in which an adsorbing Amberlite XAD-16 column was exchanged by the Amberlite XAD-7HP column. The fractionation pattern ascertained for Fe in analyzed wines is discussed in reference to previously published works. In addition, a conditioning treatment and preparation of Amberlite XAD resins have been revised.

Simple and versatile operational fractionation of Fe and Zn in dietary products by solid phase extraction on ion exchange resins

A simple and versatile protocol, based on use of solid phase extraction on strong ion exchangers and off-line detection by flame atomic absorption spectrometry, was devised to fractionate iron and zinc in common dietary food and beverages products, i.e., bee honeys, fruit juices and tea infusions. In the procedure proposed, cation exchanger Dowex 50Wx4 and anion exchanger Dowex 1x4 were used separately for distinguishing broadly meant the cationic metal fraction and the fraction of stable anionic metal complexes, respectively, after retention of metal species and their exhaustive elution by means of a 4.0moll(-1) HCl solution. The third fraction, referred to the residual metal species, was retrieved by difference between total soluble metal contents and sum of metal quantities in separated cationic and anionic fractions. The fractionation pattern observed for both metals was described and discussed.

Ion-exchange column chromatography-an attempt to speciate arsenic

This article presents different strategies for separation and pre-concentration of arsenic species based on classical ion-exchange column chromatography by means of the strong cation or anion-exchange resins used in the analytical atomic spectrometry in the last 30 years. In addition, some aspects of sample pre-treatment, including preservation and extraction of arsenic species, are highlighted.

Interferences elimination in ion chromatography by inclusion of the interfering ion into the mobile phase—Analysis of fluoride in chloride rich dietary samples

New approach to the chloride interferences elimination by addition of the interfering ion to the mobile phase is proposed and evaluated. Different eluents for the non-suppressed ion chromatographic analysis of fluorides in chlorides rich samples were tested and compared with eluent recommended by the column manufacturer. The limit of detection, linearity range and resistance to matrix effects caused by chlorides were the comparison criteria. The applicability of the selected eluent was demonstrated through the analysis of the edible salts and various tea samples. The employment of the proposed eluent shorten the time of the analysis since the only required preparation steps for edible salts were the dissolution and appropriate dilution of the samples. The recovery test was employed to verify the obtained results.