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Analytical and Bioanalytical Chemistry (v.367, #8)
A systematic approach to optimum working conditions with inductively coupled plasma atomic emission spectrometry by B. Knauthe; M. Otto; F. Martin (pp. 679-685).
Optimum experimental factors were determined for the analytical determination of Al, Cd, Fe, Pb, and Zn by ICP atomic emission spectrometry. Based on systematically determined factor levels, working conditions were found that gave similiar, and sometimes better results compared with the hitherto used levels of factors. All measurements were performed with a sampling time of 150 ms as often used in routine analysis in the laboratory. This optimization resulted in a reduced outer plasma gas flow from 15 L/min argon to 12 L/min without any relevant changes of the achievable detection limits. A serious problem was that only one analytical line of Al could be used. A comparison with the lower limit of application (comparable with the detection limit) from German directive DIN 38406, part 22 ([1]), showed that the detection limits of Al and Fe are superior, whereas for Cd there was only little improvement. The detection limits of Zn and especially Pb are always higher than the lower range of application under these conditions. Therefore, the use of two device-parameter sets for hard and soft lines, respectively, is strongly suggested. Maps with the observed signal-to-noise-ratios were systematically acquired for each element analyzed in connection with different strategies for optimum search.
Indirect fluorescence detection of phenolic compounds by capillary electrophoresis on a glass device by Martin Arundell; Peter D. Whalley; A. Manz (pp. 686-691).
A micromachined capillary electrophoresis system has been fabricated on a glass device for the separation and indirect fluorescence detection of phenols. Using this device two phenols viz., 2,4-dichlorophenol and pentachlorophenol, were separated within 12 s compared to under 19 min on a conventional capillary electrophoresis system using direct ultraviolet detection. The precision of the glass device ranged from 12.7%–16.7% compared to 0.42%–4.9% for the conventional system. Both systems showed good linearity in the concentration range of 0.8– 6.38 mM for the glass device and 5–130 μM for the conventional system. The relationship between temperature and high voltage with baseline drift was also investigated. These results provide a foundation for the development of a miniaturised chemical analysis system for the on-line analysis of phenols in water.
Needle-type glucose microbiosensor based on glucose oxidase immobilised in an overoxidised polypyrrole film (an in-vitro study) by M. Quinto; I. Losito; F. Palmisano; C. G. Zambonin (pp. 692-696).
A fast response, needle-type glucose microbiosensor has been fabricated by a one-step electrochemical immobilisation of glucose oxidase in a polypyrrole film. The sensor shows a remarkable rejection of electroactive interferences, especially paracetamol. The maximum bias observed in the worst situation never exceeded the value of 6%. The fabrication procedure delivered very reproducible devices and the sensitivity of a newly prepared biosensor was typically 650 nAmM–1cm–2. The kinetic parameters, obtained from an existing model, permitted to understand the sensor behaviour.
Applications of a versatile sol-gel derived renewable electrode for capillary electrophoresis by Lin Hua; Swee Ngin Tan (pp. 697-700).
A new electrode has been developed and applied for amperometric detection in capillary electrophoresis (CE), comprised of carbon sol-gel composite material. The versatility of the sol-gel technique permits the flexible configuration of the electrode. The performance of such a sol-gel carbon composite electrode (CCE) is first evaluated in a typical CE application for the detection of purine-based compounds. Application of the CCE is also demonstrated for the detection of phenolic compounds in a micellar system. Separation resolution for non-ionic phenolic compounds can significantly be enhanced by introducing sodium dodecyl sulfate (SDS) at a concentration above its critical micelle concentration (cmc) to the buffer. Another design of the CCE incorporating the electrocatalyst Cu2O is employed for the analysis of sugars and organic acids based on dynamic modification with cetyltrimethylammonium bromide (CTAB). It has been found that the presence of surfactant in the separation buffer does not adversely influence the electrochemical detection using a sol-gel derived carbon electrode.
Soil-modified carbon paste electrode: a useful tool in environmental assessment of heavy metal ion binding interactions by Irena Grabec Švegl; Božidar Ogorevc (pp. 701-706).
Carbon paste electrodes (CPEs) modified with different soils in their native form were prepared to create a soil-like solid phase suitable for application in studies of heavy metal ion uptake and binding interactions. The preparation of CPEs modified with five different soils was examined and their heavy metal ion uptake behavior investigated using a model Cu(II) aqueous solution. Metal ions were accumulated under open circuit conditions and were determined after a medium exchange using differential pulse anodic stripping voltammetry, applying pre-electrolysis at –0.7 V. The soil-modified CPE accumulation behavior, including the linearity of the current response versus Cu(II) concentration, the influence of the pH on the solution, and the uptake kinetics, was thoroughly investigated. The correlation between the soil-modified CPE uptake capability and the standard soil parameters, such as ion exchange capacity, soil pH, organic matter and clay content, were evaluated for all five examined soils. The influence of selected endogenous cations (K(I), Ca(II), Fe(III)) on the transfer of Cu(II) ions from a solution to the simulated soil solid phase was examined and is discussed. Preliminary examinations of the soil-modified CPE uptake behavior with some exogenous heavy metal ions of strong environmental interest (Pb(II), Hg(II), Cd(II) and Ag(I)) are also presented. This work demonstrates some attractive possibilities for the application of a soil-modified CPE in studying soil-heavy metal ion binding interactions, with a further potential use as a new environmental sensor appropriate for fast on-site testing of polluted soils.
Determination of underivatized amino acids by high-performance liquid chromatography and electrochemical detection at an amino acid oxidase immobilized CuPtCl6 modified electrode by Jianhong Pei; Xiao-yuan Li (pp. 707-713).
An amperometric sensor for amino acids based on the immobilization of amino acid oxidase on the surface of a CuPtCl6/GC is described. The amperometric current is due to the oxidation of H2O2 liberated during the enzyme reaction on the surface of the enzyme electrode. The electrode response characteristics as well as kinetic parameters have been evaluated. The enzyme electrode was characterized as an electrochemical biosensor, which was used as detector in high performance liquid chromatography (HPLC) for the determination of a mixture of amino acids with satisfactory results.
Effects of various salts on the determination of arsenic by graphite furnace atomic absorption spectrometry. Direct determination in seawater by Jean Yves Cabon (pp. 714-721).
The effect of Na, Mg, Ca and Sr as their nitrate, chloride and sulfate salts and seasalt, with and without the use of palladium, on the determination of arsenic by electrothermal atomic absorption spectrometry was investigated. In the absence of any stabilizing agent, arsenic was partially lost as molecular species at low temperatures. The effect of salts on the shape of the atomization signal, the integrated absorbance and the stabilizing effect were highly dependent both on their nature and mass. By trapping arsenic, oxide species resulting from the decomposition of nitrate salts induced a high stabilization effect depending on their vaporization temperatures: MgO∼CaO>SrO>Na2O. The stabilization effect of chlorides occurred about 200 °C lower and depended on mass, volatility and hydrolytic properties: SrCl2>CaCl2>MgCl2∼NaCl. The effect of sulfates was mainly dependent on their decomposition/vaporization mechanisms, and in the presence of Na2SO4 or CaSO4 a strong chemical interference effect was observed. Palladium stabilized arsenic in the presence of nitrates, chlorides or even sulfates, leading to a similar delaying effect, signal shape and integrated absorbance. Seasalt induced also important modifications to the atomization signal of As. Moreover, an interference effect was observed, which could probably be attributed to the simultaneous vaporization of sulfate in seasalt. In seawater, Pd suppressed this interference effect and permitted to use a high pyrolysis temperature up to 1400 °C to remove the major part of the seawater matrix before atomization. Under optimized conditions, the detection limit for As obtained in unmodified seawater in the presence of Pd was 0.34 μg L–1 for a 10 μl sample.
Determination of cobalt in sewage sludge using ultrasonic slurry sampling graphite furnace atomic absorption spectrometry by Rosa Ana Conte; M. T. C. de Loos-Vollebregt (pp. 722-726).
Cobalt in sludge of domestic and industrial origin, with high iron contents (> 17 g/kg), was determined by slurry sampling graphite furnace atomic absorption spectrometry (GF-AAS). Slurries prepared by ultrasonic stirring were adequately diluted to cover the variation in cobalt content in the sludge samples. The diluent was 5% HNO3. Standard atomisation conditions for cobalt determination were used and no matrix modifier was applied. Slurry sampling GF-AAS results in the sludge were verified by analysing totally digested samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) and by GF-AAS. The procedure was validated by analysing the certified reference material BCR 146 R, a sewage sludge of industrial origin. Recoveries for cobalt in the spiked slurried sludge samples ranged from 92 to 96%, with a relative standard deviation of 10%. Recoveries in the certified sludge using slurry sampling GF-AAS technique were about 103% for a cobalt content of 7.39 mg/kg.
Rapid determination of lead and cadmium in sewage sludge samples using electrothermal atomic absorption spectrometry with slurry sample introduction by I. López-García; P. Viñas; J. Arroyo-Cortéz; M. Hernández-Córdoba (pp. 727-732).
Lead and cadmium concentrations in sewage sludge samples are determined by suspending the ground samples in a solution containing 10% (v/v) concentrated hydrofluoric acid, 1% (v/v) concentrated nitric acid, 0.5% (m/v) dihydrogen ammonium phosphate and 0.1% (m/v) sodium hexametaphosphate. Aliquots of 20 μL of these suspensions (4 mg/mL) are diluted to 1000 μL with the same solution and then injected into the electrothermal atomizer. The drying stage is performed by programming a 400 °C temperature, a ramp time of 20 s and a hold time of 15 s on the power supply of the atomizer. No ashing step is used. Platform atomization is carried out at 1600 and 1800 °C for Pb and Cd, respectively. Calibration is performed using aqueous standards in the 5–75 and 0.2– 5 μg/L Pb and Cd ranges, respectively. Results obtained for three certified reference materials and four samples demonstrate the reliability of the procedures described.
Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples by O. Zuloaga; Nestor Etxebarria; Luis A. Fernández; Juan M. Madariaga (pp. 733-737).
The microwave-assisted extraction (MAE), accelerated solvent extraction (ASE) and Soxhlet extraction of two isomers of hexachlorocyclohexane, α-HCH and γ-HCH, from a polluted landfill soil have been optimized following different experimental designs. In the case of microwave-assisted extraction, the following variables were considered: pressure, extraction time, microwave power, percentage of acetone in n-hexane mixture and solvent volume. When ASE extraction was studied the variables were pressure, temperature and extraction time. Finally, the percentage of acetone in n-hexane mixture and the extraction time were the only variables studied for Soxhlet extraction. The concentrations obtained by the three extraction techniques were, within their experimental uncertainties, in good agreement. This fact assures the possibility of using both ASE and MAE techniques in the routine determination of lindane in polluted soils and sediments.
Graphite furnace-atomic absorption spectrophotometric determination of palladium in soil by K. S. Patel; P. C. Sharma; P. Hoffmann (pp. 738-741).
A new and sensitive procedure for the graphite furnace-atomic absorption spectrophotometric (GF-AAS) determination of Pd in soil at nanogram level is described. The method is based on prior separation and enrichment of the metal as Pd(II)-SnCl3 –-N-butylacetamide (BAA) complex into 1-pentanol (PN) by solvent extraction method. The value of the molar absorptivity of the complex in three solvents, i.e. ethyl acetate, 1-pentanol, chloroform, lie in the range of (0.70–2.75) × 104 L mol–1 cm–1 at λmax 360–440 nm. The metal could be enriched into organic solvent, i.e. PN, up to 10-folds. The sensitivity (A = 0.0044) of the method in the term of the peak height was 0.5 ng Pd/mL of the aqueous solution at an enrichment factor (EF) of 5. Optimization of analytical variables during enrichment and GF-AAS determination of the metal are discussed. The method has been applied for the analysis of Pd to soil samples derived from roads and highways in Germany.
A DANREF certified reference plastic for measurement of overall migration into the food simulant olive oil by single sided testing by K. H. Lund; L. Lillemark; J. H. Petersen (pp. 742-747).
A reference material for the determination of overall migration from a plastic coextrudate into the fatty food simulant olive oil was produced and certified in an interlaboratory study. The analyses were carried out according to the ENV 1186 standard from the European Committee for Standardization (CEN) [1, 2, 3] with exposure of the coextrudate to olive oil for 10 days at 40 °C. After an initial preliminary interlaboratory study eight laboratories participated in the certification round, and two different methods were used to obtain single sided exposure of the plastic to the oil. The certified value was determined as the mean of laboratory mean values. No outliers were found. A reference value of 8.6 mg/dm2± 1.4 mg/dm2 (± half width of the 95% confidence interval) was obtained which is within the range relevant for the regulatory limit (10 mg/ dm2), making this reference material suitable for laboratories measuring according to the EU overall migration limit [4]. The material has been found stable over 45 months.
Determination of some trace elements in human tooth enamel by Eva Reitznerová; Dula Amarasiriwardena; Marta Kopčáková; R. M. Barnes (pp. 748-754).
Determination of seven elements (Cu, Fe, Mg, Mn, Pb, Sr and Zn) in whole enamel and surface layers of extracted non-carious human teeth by FAAS, ETA AAS, ICP-AES and ICP-MS (Pb) is demonstrated. Techniques are described for obtaining whole enamel and its acid dissolution. Fifty μm width enamel layers from outer enamel surface to a 200 μm depth were successively etched in 1 mL of 3 M HClO4 for 3 min dissolution periods. Enamel samples were analyzed for populations under and over 20 years of age and enamel from Bronze Age teeth. Concentrations of microelements in the whole enamel and in the first surface layer (50 μm depth) were compared. With exception of Sr and Mg, all elements show significantly higher concentrations in the first layer than in whole enamel and higher concentration in teeth of individuals over 20 years, which demonstrate the cumulative effect of these elements. The Cu, Fe, Mn, Pb and Zn concentrations in four layers of erupted and non-erupted teeth decreased while Mg and Sr concentrations increased toward enamel-dentine junction. The concentrations of most elements were almost constant as they approached the 150 μm layer. This concentration gradient may result from interaction between saliva and teeth and supports the hypothesis that the surface de- and re-mineralization process is effective at most to 150 μm from the enamel surface.
The determination of certain major and minor elements in geological samples by inductively coupled plasma atomic emission spectrometry. Some interference problems with the analysis of geological standard reference materials and nutrition supplements by A. Väisänen; Rose Matilainen; Jouni Tummavuori (pp. 755-760).
Direct ICP-AES measurements of the digested geological standard reference material samples yielded the wrong information about their composition. The differences between certified and measured concentrations of the samples were due to the complicated sample matrix. The measured concentrations can be successfully corrected by using a multiple linear regression technique. The correction is based on the multiple regression line calculated from the analytical results at synthetic mixtures of matrix elements, where concentrations varied on five levels. There were no significant (P = 0.05) differences between certified and measured concentrations in standard reference materials after the correction. The same method was used in the analysis of nutrition supplements.
How faster and cheaper to determine chromium by adsorptive cathodic stripping voltammetry in the presence of DTPA and nitrate by M. Korolczuk (pp. 761-762).
A modification of the voltammetric procedure for the determination of chromium in the presence of DTPA and nitrates was proposed. Morpholinoethanesulfonic (MES) acid and its sodium salt were used for stabilisation of pH instead of acetate buffer. In the presence of MES the determination of chromium can be carried out in the presence of dissolved oxygen without decrease of sensitivity of the measurements. Elimination of the purge step decreases total analysis time and saves gas.
Analytical control of silica glass production. Voltammetric determination of titanium and iron in raw materials and silica glass samples by M. Gawryś; J. Golimowski (pp. 763-765).
Adsorptive stripping voltammetric (AdSV) methods are presented for the determination of titanium and iron in quartz and silica glass samples obtained after pressure decomposition. Mandelic acid and catechol were used as complexing agents for titanium and iron, respectively. The method for titanium determination is based on the catalytic effect of chlorate ions. An insoluble residue remaining after decomposition of quartz and silica glass samples in HF+H2SO4 mixture was checked by energy-dispersive X-ray analyses. ET-AAS was applied as a reference method to AdSV measurements.