Wieslaw Zyrnicki

Application of sequential extraction and the ICP-AES method for study of the partitioning of metals in fly ashes

In this work, the original BCR extraction scheme was modified and applied to study the partitioning of metals in fly ashes. In the first step, the water-soluble fraction was investigated here. The next metal fractions were acid-soluble, reducible, and oxidisable. Two kinds of coal fly ash certified reference materials were analysed. Metal concentrations in the extracts were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). The efficiency of the extraction process for each step was examined. The partitioning of metals between the individual fractions was investigated and is discussed.

Multi-element analysis, bioavailability and fractionation of herbal tea products

Herbal teas (Mentha piperitae folium and mixture Marticaria chamomilla flos with Lavandula officinalis flos) were compared considering the total contents of micro (Al, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Sr, Ti, V) and macro (C, H, N, S, Ca, Mg, P) elements, bioavailability and fractionation. Different methods (inductively coupled plasma optical emission spectrometry (ICP OES), Fourier transform infrared spectroscopy (FTIR) and CHNS elemental analysis) were applied. The microwave-assisted digestion procedure was found to be more effective than the hot-plate heating for the wet acid digestion of tea. The application of the modified BCR (Community Bureau of Reference) sequential extraction procedure exhibited differences in the concentrations of metal bound to reducible and oxidizable fractions. The accuracy of method was verified by analysis of certified reference material INCT-TL-1 Tea Leaves. The daily intake of all elements from the analyzed herbal tea infusion did not exceed the maximum permissible levels and does not constitute health risk.

Analytical features of Au, Pd and Pt chemical vapour generation inductively coupled plasma atomic emission spectrometry

Inductively coupled plasma atomic emission spectrometry with volatile species generation of Au, Pd and Pt, through the reaction with NaBH4 in the medium of HCl, has been investigated from the viewpoint of its analytical features. Interference effects from Cd(II), Co(II), Cu(II), Fe(III) and Ni(II) ions, occurring in the solution during the reaction of volatile species generation, were examined. Masking agents, i.e., KCN, (NH2)2SC and EDTA, added to the samples or to the reduction agent, and increase of HCl concentration in the sample were applied for the reduction of the chemical interferences.

Study of the reaction of Ir, Os, Rh and Ru ions with NaBH4 in the acid medium by the inductively coupled plasma atomic emission spectrometry

Generation of Os, Rh and Ru volatile species performed for the first time by the reaction of the noble metal ions with sodium tetrahydroborate in HCl, HNO3, H2SO4 and a mixture of HCl and HNO3 (3∶1) in the gas–liquid phase separation system was reported.

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.

Investigation of Simultaneous Generation of Arsenic, Bismuth and Antimony Hydrides Using Inductively Coupled Plasma Optical Emission Spectrometry

Hydride generation from solution containing As(III), Bi(III), and Sb(III) by means of different borane reductants and acids using inductively coupled plasma optical emission spectrometry as a detection system was investigated. The As, Bi, Sb, B, C, H, and N lines as well as the OH and CN molecules were recorded. Their intensities in relation to hydride formation conditions were measured. Effects of the HCl, CH3COOH, and C6H8O7 acids as well as the NaBH4, H3B-NH(CH3)2, and H3B-NH2C(CH3)3 reductants on efficiency of the As, Sb, and Bi hydride generation were investigated and discussed. Influence of hydride generation conditions on plasma was studied.

Determination of As, Bi, Sb and Sn in conifer needles from various locations in Poland and Norway by hydride generation inductively coupled plasma atomic emission spectrometry

Hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-AES) in the system with aerosolised sample introduction has been employed for the first time for analysis of conifer needles. Arsenic, bismuth, antimony and tin along with other trace elements were simultaneously determined in pine, spruce, yew and thuja foliage sampled from various locations in Poland and Norway. Quality of the measurements was assured by examination of two attested plant reference materials. The application of different analyte introduction techniques and interference effects from matrix elements, i.e. Na, K, Mg, Ca and transition metals in the analysis of needles are discussed.

Excitation temperatures of atoms and ions in a hollow cathode discharge

Abstract Excitation temperatures have been measured in a hollow cathode discharge from intensities of Ar I, Ar II, Ti I, Ti II, AI I, Mg I, Mg II, Cu I and Pb I lines. The differences between values derived from the species listed are discussed.

Fluorine Determination in a Hollow Cathode Discharge by Monofluoride Emission Spectra

Abstract The applicability of the SiF and InF bands to determination of fluorine in a hollow cathode discharge has been studied. The InF bands have been used for the F determination in solid samples containing from 1% to 1x10−4% F, and in solutions for the F− concentration between 10 and 1000 mg 1−1. The lowest detected amount of fluorine in solid sample was 10 ng (1x10−5%).

Study of the Effectiveness of Arsenic Hydride Generation from Various Arsenic Species with the Use of Some Borane Reducing Agents by Inductively Coupled Plasma Atomic Emission Spectrometry

Abstract The application of H3B–NH(CH3)2,H3B–NH2C(CH3)3 and NaBH4 as derivatizing reagents in hydride generation from As(III), As(V), and As(V)-dimethyl forms was investigated. The effects of hydrochloric, acetic, and citric acids on the As responses were studied by using inductively coupled plasma optical emission spectrometry. Intensities of As, B, and H lines, and the pH of the reaction mixture were recorded. The effectiveness of the hydride generation depended on the arsenic form and changed with reductant type as well as with kind and concentration of the acids. The H line intensities were different from those expected from stechiometric reactions between the reductants and acids.