Ján Medved

Utilization of optimized BCR three-step sequential and dilute HCl single extraction procedures for soil-plant metal transfer predictions in contaminated lands.

The prediction of soil metal phytoavailability using the chemical extractions is a conventional approach routinely used in soil testing. The adequacy of such soil tests for this purpose is commonly assessed through a comparison of extraction results with metal contents in relevant plants. In this work, the fractions of selected risk metals (Al, As, Cd, Cu, Fe, Mn, Ni, Pb, Zn) that can be taken up by various plants were obtained by optimized BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and by single 0.5 mol L(-1) HCl extraction. These procedures were validated using five soil and sediment reference materials (SRM 2710, SRM 2711, CRM 483, CRM 701, SRM RTH 912) and applied to significantly different acidified soils for the fractionation of studied metals. The new indicative values of Al, Cd, Cu, Fe, Mn, P, Pb and Zn fractional concentrations for these reference materials were obtained by the dilute HCl single extraction. The influence of various soil genesis, content of essential elements (Ca, Mg, K, P) and different anthropogenic sources of acidification on extraction yields of individual risk metal fractions was investigated. The concentrations of studied elements were determined by atomic spectrometry methods (flame, graphite furnace and hydride generation atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry). It can be concluded that the data of extraction yields from first BCR SEP acid extractable step and soil-plant transfer coefficients can be applied to the prediction of qualitative mobility of selected risk metals in different soil systems.

Determination of lead and cadmium in human hair by atomic absorption spectrometric procedures after solid phase extraction

Abstract A separation and preconcentration procedure for Pb and Cd in human hair by using the chelating ion-exchanger, Iontosorb-Oxin, is described. The sorption yield dependence of Pb and Cd, on pH, time, and on the presence of accompanying elements, was investigated. The hair samples were decomposed by microwave irradiation and the determination of lead and cadmium was by flame and electrothermal atomic absorption spectrometry (F-AAS and ETA-AAS, respectively). The precision and accuracy of this procedure were checked by the use of synthetic and certified reference materials. The limit of determination was 1 μg Pb l −1 and 0.1 μg Cd l −1 , respectively. The procedure was applied to samples of human hair.

Free aluminium extraction from various reference materials and acid soils with relation to plant availability

The single extractions with 15 extractants (agents) (H(2)O, KCl, NH(4)Cl, NH(4)F, CaCl(2), BaCl(2), CuCl(2), LaCl(3), Na(2)S(2)O(4), (NH(4))(2)C(2)O(4), Na(4)P(2)O(7), NTA, EDTA, DTPA, HCl), the optimised BCR (Community Bureau of Reference) three-step sequential extraction procedure (SEP) and the solid phase extraction (SPE) by the chelating ion-exchanger Iontosorb Salicyl (cellulose resin containing covalently bound salicylic acid functional groups) were used for the partitioning of Al in very acid soil samples taken from an area influenced by acid mine solutions. The precision, accuracy and repeatibility for all steps of the optimised BCR SEP were checked on the various reference materials (CRM 483 sewage sludge amended soil, CRM BCR 701 freshwater sediment, SRM 2710 and SRM 2711 Montana soils). Also the new indicative values of the optimised BCR SEP fractional Al concentrations were obtained for these reference materials. The aluminium amounts obtained by the used extraction procedures were valuated and discussed from the aspect of the Al concentration in the plants (grass) growing on the same studied soils. The aluminium toxicity indexes (ATI) calculated for the studied soils, the BaCl(2) and acetic acid soil extracts and the grass stems and roots were used for the assessment of the Al toxicity to the plants. The ATI value was defined as the ratio of the nutrient cations (Ca, Mg, K, Na) concentration sum to the Al concentration. The flame atomic absorption spectrometry (LOQ=0.2mgl(-1)) and the inductively coupled plasma optical emission spectrometry (LOQ=0.03mgl(-1)) were used for the aluminium quantification.

Spectrographic determination of gold in geological materials after preconcentration on Spheron-Thiol

Abstract A spectrographic method for the determination of gold in geological materials after preconcentration on chelating sorbent Spheron-Thiol has been developed. The method involves the decomposition of the samples, preconcentration of Au on Spheron-Thiol, decomposition of the sorbent and spectrographic determination of gold at 267.59 nm. The method is simple, rapid and enables the determination of gold at μg g −1 levels in various types of geological materials with good precision and accuracy. The detection limit is 0.5 μg Au kg −1 . The method has been applied to the determination of Au in a number of certified and other reference materials with accurate results.

Thallium fractionation in polluted environmental samples using a modified BCR three-step sequential extraction procedure and its determination by electrothermal atomic absorption spectrometry

Determination of thallium in polluted environmental samples and their extracts obtained by a modified BCR three-step sequential extraction procedure was used to study thallium distribution and mobility in the monitored polluted area affected by acidification (Šobov, Central Slovakia). The results of fractionation applied to 5 soil certified reference materials and 14 environmental samples show that the vast majority of thallium occurred in the residual fraction. This means that highly toxic thallium is strongly entrapped in the parent rock materials remains immobile and its environmental toxicity is therefore reduced. The limit of detection for thallium in the studied fractions was lower than 0.050 mg kg−1, the precision (RSD) of the ultratrace determination of thallium in the studied fractions was better than 17 % and the accuracy of the used method was verified by analyzing certified reference materials.