Sorption preconcentration in combined methods for the determination of noble metals

Combined methods for the determination of noble metals with the use of sorption preconcentration with complexing, anion-exchange, and other sorbents are reviewed. Characteristics of sorbents, techniques of sorption preconcentration, and techniques for the preparation of a concentrate for determination are considered. Features of instrumental methods for the determination of noble metals in the analysis of different materials are discussed. Examples of the use of sorption preconcentration in combined methods for the determination of noble metals are given from publications between 1996–2005.     

Methods for the determination of local anesthetic agents

The main methods for the determination of local anesthetics are considered, and their advantages and disadvantages are discussed. After the systematization of published data, it was established that the greatest number of works were devoted to the determination of novocaine, lidocaine, and ultracaine; therefore, methods for their determination are considered separately. It was demonstrated that the extraction and sorption preconcentration of local anesthetics as ion associates with chromogenic organic reagents is promising. It was substantiated that the development of combined rapid and sensitive extraction-photometric, sorptionspectroscopic, and colorimetric methods for the determination of novocaine, lidocaine, and ultracaine with chromogenic organic reagents in different test materials is a problem of considerable current interest.     

Flow methods for the determination of elements in solutions based on sorption preconcentration and inductively coupled plasma mass spectrometry

Methods involving an on-line combination of sorption preconcentration with the determination of elements by inductively coupled plasma mass spectrometry (ICP-MS) are considered. The reasons for the effect of the composition of the solution on the analytical signals in the determination of elements, the issues related to recording of nonstationary signals, and the procedures for the sorption preconcentration of elements in the corresponding flow systems are discussed. Some examples of the determination of elements in environmental samples, biological fluids, and other samples are given.     

Flow Sorption–Spectroscopic Analysis

Combinations of the dynamic sorption preconcentration of elements with spectroscopic determination techniques was considered. The use of sorption systems in flow spectroscopic techniques are discussed, and the evaluation of the efficiency of these systems in the preconcentration of elements is described. The application of flow sorption–spectroscopic techniques to the determination of elements in natural water, drinking water, soil, food stuffs, rocks, and ores is surveyed.     

Trends in sorption preconcentration combined with noble metal determination.

Nowadays much attention is being paid to the determination of trace amounts of noble metals in geological, industrial, biological and environmental samples. The most promising techniques, such as inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and electrothermal atomic absorption spectrometry (ETAAS) are characterized by high sensitivity. However, the accurate determination of trace noble metals has been limited by numerous interferences generated from the presence of matrix elements. To decrease, or eliminate, these interferences, the sorption preconcentration of noble metals is often used prior to their instrumental detection. A great number of hyphenated methods of noble metal determination using sorption preconcentration have been developed. This review describes the basic types of available sorbents, preconcentration procedures and preparations of the sorbent to the subsequent determination of noble metals. The specific features of instrumental techniques and examples of ETAAS, FAAS, ICP-AES, ICP-MS determinations after the sorption preconcentration of noble metals are considered. The references cited here were selected mostly from the period 1996 - 2006.     

Preconcentration of gaseous organic pollutants in the atmosphere

Three basic methods of preconcentration of organic atmospheric pollutants, viz. by cold trap, absorption in solutions and adsorption on solids at ambient temperature, and methods of liberating the trapped components, are discussed. Adsorption on solids is becoming more widely employed because of its advantages, and selection of the most appropriate sorbent for a given group of pollutants is of major importance. The characteristics of individual types of sorbents are presented, as well as the basic methods of determination of sorption capacity.     

Amberlite XAD-7 impregnated with Xylenol Orange: a chelating collector for preconcentration of Cd(II), Co(II), Cu(II), Ni(II), Zn(II) and Fe(III) ions prior to their determination by flame AAS

A new chelating resin, Xylenol Orange coated Amberlite XAD-7, was prepared and used for preconcentration of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) prior to their determination by flame atomic absorption spectrophotometry. The optimum pH values for quantitative sorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) are 4.5-5.0, 4.5, 4.0-5.0, 4.0, 5.0 and 5.0-7.0, respectively, and their desorptions by 2 mol L(-1) HCl are instantaneous. The sorption capacity of the resin has been found to be 2.0, 2.6, 1.6, 1.6, 2.6 and 1.8 mg g(-1) of resin for Cd, Co, Cu, Fe, Ni and Zn, respectively. The tolerance limits of electrolytes, NaCl, NaF, NaI, NaNO3, Na2SO4 and of cations, Mg2+ and Ca2+ in the sorption of the six metal ions are reported. The preconcentration factor was between 50 and 200. The t1/2 values for sorption are found to be 5.3, 2.9, 3.2, 3.3, 2.5 and 2.6 min for the six metals, respectively. The recoveries are between 96.0 and 100.0% for the different metals at preconcentration limits between 10 to 40 ng mL(-1). The preconcentration method has been applied to determine the six metal ions in river water samples after destroying the organic matter (if present in very large amount) with concentrated nitric acid (RSD < or = 8%, except for Cd for which it is upto 12.6%) and cobalt content of vitamin tablets with RSD of approximately 3.0%.     

Possibilities for the simultaneous preconcentration and flame atomic absorption spectrometric determination of Cr(III) and Cr(VI) using a C18 column and sorption loop

The sorption loop as a preconcentration unit used so far in the low-pressure flow injection (FI) system was combined with the hydraulic high-pressure nebulizer (HHPN) and a high-pressure liquid chromatographic (HPLC) column. Thus, the sorption preconcentration of Cr(VI) can be coupled to a powerful sample introduction method or preconcentration techniques of Cr(III). The subsequent determination of the Cr(VI) content of the samples was carried out by flame atomic absorption (FAAS).     

Neutron activation analysis of water and waste

The neutron activation method has been applied to the determination of Ag, Cd, Co, Cr, Cu, Fe, Hg, Mo, Se and Zn in waters and wastes. The method involves decomposition of organic substances by ozonation, preconcentration of elements to be determined by coprecipitation with thionalide at pH 9 or sorption on Dowes 1×2 loaded with 8-hydroxyquinoline-5-sulfonic acid at pH 7, irradiation of the concentrate, radiochemical separation of the respective radioisotopes and gamma spectrometric measurement of the activity. Accuracy and precision of the determination have been evaluated.     

Bestimmung organischer Wasserverunreinigungen

Zusammenfassung An Hand von Modellverbindungen (Xylol, Toluol, Kresol, Dichlorphenol, Pyridin) werden Möglichkeiten zur Bestimmung organischer Wasserverunreinigungen gezeigt. Nach Konzentration der Stoffe durch Sorption an einem Styrol-Divinylbenzol-Copolymer und der Überführung in organische Lösung können die Komponenten mittels GC-MS identifiziert werden.

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Determination of organic contaminants in water

By means of model compounds (xylene, toluene, cresol, dichlorophenol, pyridine) possibilities for the determination of organic substances in water are discussed. After a preconcentration by sorption on a styrene-divinylbenzene copolymer and transferring into organic solution analytical determination of the components is achieved by gas chromatography/mass spectrometry.

     

Sorption preconcentration of thallium(I) on polyurethane foam modified with molybdophosphate

Sorption preconcentration of thallium(I) on polyurethane foam modified with molybdophosphate was studied. Optimal conditions for the immobilization of molybdophosphate and the composition of the adsorbed heteropoly complex were determined. A procedure was proposed for the sorption preconcentration of thallium(I) and its subsequent determination by atomic absorption spectrometry in nitric acid desorbates with the determination limit 7.5 μg/500 mL.     

Sorption characteristics of caffeine onto untreated polyurethane foam: application to its determination in human plasma

In the present paper, the sorption properties of caffeine (CAF) onto polyether type polyurethane foam (PUF) as solid phase sorbent were investigated with UV determination at 274.3 nm. Batch and column methods were used to optimize chemical, flow, kinetic and isothermal conditions for preconcentration of CAF. Results indicated quantitative sorption of CAF at pH 8 and 30 min shaking time. The maximum sorption capacity was found to be 4.1 mg g(-1). Column preconcentration was recommended at a flow rate of 1.5 mL min(-1) and desorption with 4 mL from 0.15 mol L(-1) hydrochloric acid. The procedure provided a linear analytical range of 0.05-30 mg L(-1). The detection and quantification limits are 0.016 and 0.047 mg L(-1), respectively. The procedure was applied to determination of CAF in spiked human plasma. The obtained recoveries were 98-101% and RSD values were from 0.05 to 9.5%.     

Amberlite XAD-7 impregnated with Xylenol Orange: a chelating collector for preconcentration of Cd(II), Co(II), Cu(II), Ni(II), Zn(II) and Fe(III) ions prior to their determination by flame AAS

A new chelating resin, Xylenol Orange coated Amberlite XAD-7, was prepared and used for preconcentration of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) prior to their determination by flame atomic absorption spectrophotometry. The optimum pH values for quantitative sorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II) and Zn(II) are 4.5–5.0, 4.5, 4.0–5.0, 4.0, 5.0 and 5.0–7.0, respectively, and their desorptions by 2 mol L^–1 HCl are instantaneous. The sorption capacity of the resin has been found to be 2.0, 2.6, 1.6, 1.6, 2.6 and 1.8 mg g^–1 of resin for Cd, Co, Cu, Fe, Ni and Zn, respectively. The tolerance limits of electrolytes, NaCl, NaF, NaI, NaNO₃, Na₂SO₄ and of cations, Mg²⁺ and Ca²⁺ in the sorption of the six metal ions are reported. The preconcentration factor was between 50 and 200. The t_1/2 values for sorption are found to be 5.3, 2.9, 3.2, 3.3, 2.5 and 2.6 min for the six metals, respectively. The recoveries are between 96.0 and 100.0% for the different metals at preconcentration limits between 10 to 40 ng mL^–1. The preconcentration method has been applied to determine the six metal ions in river water samples after destroying the organic matter (if present in very large amount) with concentrated nitric acid (RSD ≤ 8%, except for Cd for which it is upto 12.6%) and cobalt content of vitamin tablets with RSD of ～ 3.0%.     

Sorption of caffeine and theophylline on hypercrosslinked polystyrene

The sorption of caffeine and theophylline from water solutions on hypercrosslinked polystyrene MN-200 was studied. It is shown that sorption is described by the Langmuir equation. The conditions of the dynamic sorption concentration of caffeine and theophylline on a concentrating column and the conditions of its desorption were found. A procedure for spectrophotometric determination of caffeine and theophylline with a dynamic preconcentration is proposed.     

Sorption Preconcentration and Gas-Chromatographic Determination of Aminazin in Biological Fluids

The sorption characteristics of the drug aminazin on unmodified and chemically modified silicas were examined. The effects of pH and ionic strength on the sorption of aminazin are discussed. Sorption isotherms of aminazin on all of the sorbents were adequately described by the Langmuir equation. The distribution coefficients and the maximum specific adsorption of this compound on the test sorbents were calculated. A highly sensitive and well-reproducible procedure was developed for determining aminazin in biological fluids. This procedure involves sorption preconcentration and gas-chromatographic determination with a thermionic detector.     

Preconcentration of Trace Elements in Water for Speciation Studies

Trace element speciation has recently become one of the most important problems in water analysis. Proper combination of preconcentration techniques with instrumental determination methods is essential to speciation analysis, because sensitivity and selectivity of direct determination methods are generally lacking. The present paper describes such preconcentration techniques as filtration, centrifugation, flotation and sorption, which have been developed in the author's laboratory for the speciation of heavy metals in river and pond waters by electron microscopy, X-ray microanalysis and chemical analysis. The application of freeze concentration to the speciation of silica in high-purity waters is also discussed.     

Preconcentration of Polycyclic Aromatic Hydrocarbons on Polyurethane Foams and Their Determination in Waters with the Use of Luminescence and High-Performance Liquid Chromatography

A technique was developed for the sorption preconcentration of polycyclic aromatic hydrocarbons on polyurethane foams in the batch and dynamic modes providing their simultaneous quantitative extraction. A procedure was proposed for screening waters for polycyclic aromatic hydrocarbons based on the preconcentration of these compounds with polyurethane foam, determination of their total amount by the luminescence method, desorption of adsorbed compounds with acetonitrile, and determination of individual compounds in the eluate by high-performance liquid chromatography with fluorescence detection. The procedure was tested with model and real samples of water.     

Sorption of microamounts of Ce3+, Pm3+, Eu3+, Gd3+ and Yb3+ on aluminium hydroxide

The sorption of microamounts of trivalent lanthanides (Ln³⁺) on freshly precipitated Al(OH)₃ has been measured in dependence on pH and the time of sorption. Also, the influence of organic complexing ligands and inorganic electrolytes on the sorption process has been investigated. The mechanism of sorption is discussed. Freshly precipitated Al(OH)₃ can be used for the preconcentration of microamounts of trivalent lanthanides. However, the preconcentration is not quantitative in the presence of high concentrations of complexing ligands (citrate and similar) which form strong complexes with Ln³⁺ ions.     

Selection of Conditions for the Dynamic Sorption Preconcentration of a 1,1-Dimethylhydrazine Derivative (4-Nitrobenzaldehyde N,N-Dimethylhydrazone) on Hydrophobized Silica

The type of mass transfer in the sorption of 4-nitrobenzaldehyde N,N-dimethylhydrazone (BDH) on silica chemically modified with hexadecyl groups was determined using the linear model of sorption dynamics, and distribution and mass transfer coefficients of hydrazone were calculated. Optimal conditions of the dynamic sorption preconcentration and desorption of BDH and its subsequent determination by reversed-phase high-performance liquid chromatography were proposed. The detection limit of the compound for preconcentration from a sample of 100 mL was 1 g/L.     

High-sensitivity X-ray fluorescence analysis of solutions with the use of a sorption accumulation microsystem

A mass-transfer kinetic model is proposed for an embedded sorption accumulation microsystem based on polycapillary structures to be used in the developed X-ray fluorescence analyzer with preconcentration. The model is used to substantiate a kinetic method for high-sensitivity X-ray fluorescence determination of elements in multicomponent solutions. With the use of this model, experimental data on X-ray fluorescence spectra are analyzed and kinetic and equilibrium parameters are found for the sorption of copper, nickel, manganese, iron, and zinc on the selective DETATA sorbent.