Determination of Copper, Iron, Nickel and Zinc in fuel kerosene by FAAS after adsorption and pre-concentration on 2-aminothiazole-modified silica gel

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Gravimetric determination of soil organic matter

Avaliou-se o método de determinação gravimétrica da matéria orgânica do solo pela perda de massa por incineração a 300ºC e comparou-se com o carbono determinado pelo método Walkley-Black. Os dois métodos foram correlacionados positivamente com a seguinte equação de regressão linear: y = 3,720x + 0,2914. r = 0,937. O coeficiente. 3,720 foi maior do que os encontrados na literatura. que variaram de 1,68 a 2,13. Esta diferença foi atribuída ao maior grau de oxidação da matéria orgânica dos solos das regiões tropicais. O método de incineração é aplicável para determinação do C do solo em rotina. O método não contamina o meio ambiente com metal tóxico (Cr6+) e não oferece riscos aos analistas com o uso de ácido sulfúrico concentrado.

Simultaneous determination of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry using a glassy carbon-mercury-film electrode

A new, versatile, and simple method for quantitative analysis of zinc, copper, lead, and cadmium in fuel ethanol by anodic stripping voltammetry is described. These metals can be quantified by direct dissolution of fuel ethanol in water and subsequent voltammetric measurement after the accumulation step. A maximum limit of 20% (v/v) ethanol in water solution was obtained for voltammetric measurements without loss of sensitivity for metal species. Chemical and operational optimum conditions were analyzed in this study; the values obtained were pH 2.9, a 4.7-mum thickness mercury film, a 1,000-rpm rotation frequency of the working electrode, and a 600-s pre-concentration time. Voltammetric measurements were obtained using linear scan (LSV), differential pulse (DPV), and square wave (SWV) modes and detection limits were in the range 10(-9)-10(-8) mol L-1 for these metal species. The proposed method was compared with a traditional analytical technique, flame atomic absorption spectrometry (FAAS), for quantification of these metal species in commercial fuel ethanol samples.

A new approach for determining stability constants of metal ion complexes in aquatic systems based on flow injection-ion exchange-flame atomic absorption spectrometry coupling

A method based an ion exchange(IE)-atomic absorption spectrometry(AAS) coupled by flow techniques, allowing the determination of formation constants of, at least, the first species of complex systems, in aqueous solution, was developed.The IE-AAS coupling reduces significantly the number of experimental steps in comparison with IE batch methods, resulting in an important increase in analytical rate. The method is simple both from experimental and computational points of view, making possible its utilization by workers without special expertise in the field of complex equilibria in solution. on the other hand, taking into account mainly the amount of hollow cathode lamps available to date, the developed procedure may be applied, within certain limitations, to the study of many systems whose features prevent the use of traditional approaches.

Paper-based diffusive gradients in thin films technique coupled to energy dispersive X-ray fluorescence spectrometry for the determination of labile Mn, Co, Ni, Cu, Zn and Pb in river water

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Selective UV-filter detection with sensors based on stainless steel electrodes modified with polyaniline doped with metal tetrasulfonated phthalocyanine films

This work describes the construction and application of two amperometric sensors for sensitive UV-filter determination. The sensors were prepared using stainless steel electrodes in which polyaniline (PANI) was electrochemically polymerized in the presence of nickel (NiPcTS) or iron (FePcTS) tetrasulfonated phthalocyanines. The sensor surface characterizations were carried out using atomic force microscopy (AFM). The PANI/NiPcTS sensor was selective for the chemical UV-filter p-aminobenzoic acid (PABA) and the PANI/FePcTS sensor was selective for octyldimethyl-PABA (ODP), both in a mixture of tetrahydrofuran (THF) and 0.1 mol L(-1) H(2)SO(4) at a volume ratio of 30 : 70, and with an applied potential of 0.0 mV vs. Ag vertical bar AgCl. A detailed investigation of the selectivity was carried out for both sensors, in order to determine their responses for ten different UV filters. Finally, each sensor was successfully applied to PABA or ODP quantification in sunscreen formulations and water from swimming pools.

Determination of density of states in PPS from space-charge-limited current measurements

Space-charge-limited currents measurements have been carried out on undoped amorphous poly p-phenylene sulfide. The scaling law is checked for different samples with varying thickness, and J-V data analyzed. The position of the quasi-Fermi level and the density of states was obtained.

Filmes de metal-hexacianoferrato: Uma ferramenta em química analítica

Chemically modified electrodes based on hexacyanometalate films are presented as a tool in analytical chemistry. Use of amperometric sensors and/or biosensors based on the metal-hexacyanoferrate films is a tendency. This article reviews some applications of these films for analytical determination of both inorganic (e.g. As3+, S2O3 2-) and organic (e.g. cysteine, hydrazine, ascorbic acid, gluthatione, glucose, etc.) compounds.

Determination of Cu, Ni and Pb in Aqueous Medium by FAAS after Pre-Concentration on 2-Aminothiazole Modified Silica Gel

This work describes the synthesis and characterization of 2-aminothiazole modified silica gel (SiAT), and the results of a study of the adsorption and pre-concentration (in batch and using a flow-injection system coupled to an absorption atomic spectrometer) of Cu(II), Ni(II) and Pb(II) in aqueous medium. The adsorption capacities for each metal ions in mmol g -1 were: Cu(II)= 1.18, Ni(II)= 1.15 and Pb(II)= 1.10. The results obtained in the flow experiments showed a recovery of practically 100% of the metal ions adsorbed in a mini-column packed with 100 mg of SiAT, using 100 μL of 2.0 mol L -1 HCl solution as eluent. The sorption-desorption of the metal ions made possible the application of a flow-injection system for the pre-concentration and quantification by FAAS of metal ions at trace level in natural water samples digested and not digest by an oxidizing UV photolysis.

Preconcentration and determination of mercury(II) at a chemically modified electrode containing 3-(2-thioimidazolyl)propyl silica gel

A mercury-sensitive chemically modified graphite paste electrode was constructed by incorporating modified silica gel into a conventional graphite paste electrode. The functional group attached to the (3-chloropropyl) silica gel surface was 2-mercaptoimidazole, giving a new product denoted by 3-(2-thioimidazolyl)propyl silica gel, which is able to complex mercury ions. Mercury was chemically adsorbed on the modified graphite paste electrode containing 3-(2-thioimidazolyl)propyl silica (TIPSG GPE) by immersion in a Hg(II) solution, and the resultant surface was characterized by cyclic and differential pulse anodic stripping voltammetry. One cathodic peak at 0.1 V and other anodic peak at 0.34 V were observed on scanning the potential from -0.1 to 0.8 V (0.01 M KNO3; ν = 2.0 mV s-1 νs. Ag/AgCl). The anodic peak at 0.34 V show an excellent sensitivity for Hg(II) ions in the presence of several foreign ions. A calibration graph covering the concentration range from 0.02 to 2 mg L-1 was obtained. The detection limit was estimated to be 5 μg L-1. The precision for six determinations of 0.05 and 0.26 mg L-1 Hg(II) was 3.0 and 2.5% (relative standard deviation), respectively. The method can be used to determine the concentration of mercury(II) in natural waters contaminated by this metal. 2005 © The Japan Society for Analytical Chemistry.

Preparation of a silica gel modified with 2-amino-1,3,4-thiadiazole for adsorption of metal ions and electroanalytical application

Silica gel with a specific area of 382 m2 g-1 and an average pore diameter of 60 Å was chemically modified with 2-amino-1,3,4-thiadiazole, for the purpose of selective adsorption of heavy metals ions and possible use as a chemically modified carbon paste electrode (CMCPE). The following properties of this functionalized silica gel are discussed: selective adsorption of heavy metal ions measured by batch and chromatographic column techniques, and utilization as preconcentration agent in a chemically modified carbon paste electrode (CMCPE) for determination of mercury(II). The chemical selectivity of this functional group and the selectivity of voltammetry were combined for preconcentration and determination. ©2006 Sociedade Brasileira de Química.

Direct simultaneous determination of Pb(II) and Cu(II) in biodiesel by anodic stripping voltammetry at a mercury-film electrode using microemulsions

A mercury film electrode was used to determine direct and simultaneously Pb(II) (at -410 mV) and Cu(II) (at -100 mV) in biodiesel by anodic stripping voltammetry. A linear response was obtained for Pb(II) and Cu(II) in the 2.00 × 10-8-1.00 × 10-7 mol L-1 concentration range and detection limits were 2.91 × 10-9 mol L-1 and 4.69 × 10-9 mol L-1 for Pb(II) and Cu(II), respectively, with recovery around of 100.0%. © 2012 Elsevier Ltd. All rights reserved.

A comparison between neutron-fluence measurements using metal-activation monitors and standard glasses calibrated via thin uranium-fission monitors and via ηq method

The two fundamental approaches to fission-track dating involve either an explicit determination of the thermal neutron fluence (φ-method) or a calibration against age standards (ζ-method). The neutron fluence measurements are carried out with metal-activation monitors or with uranium-fission monitors, co-irradiated with the samples. Uranium-fission monitors consist of either a thin mono-atomic) film, or a thick fission source (standard uranium glass) irradiated against a muscovite external track detector. In this work, different techniques for performing neutron-fluence measurements were compared: based on thin-film calibration, based on thick-source calibration, and based on gamma spectrometry of co-irradiated metal monitors (Au, Co). The results suggest that more experiments are needed to make all calibrations consistent, including new measurements of the length of etched induced tracks in mica. Also the standard glass calibration carried out with thin films should be confirmed with a greater number of calibrating irradiations. © 2013 Elsevier Ltd. All rights reserved.

Determination of the force systems produced by different configurations of tear drop orthodontic loops

Objective: To determine the mechanical characteristics of teardrop loop with and without helix fabricated using different metal alloy compositions (stainless steel and beta-titanium), submitted to different intensities of bends preactivation (0° and 40°), and with different cross-sectional dimension of the wire used to build these loops (0.017 x 0.025-in and 0.019 x 0.025-in). Methods: Eighty loops used to close spaces were submitted to mechanical tests. The magnitudes of horizontal force, the moment/force ratio, and the load/deflection ratio produced by the specimens were quantified. Loops were submitted to a total activation of 5.0 mm and the values were registered for each 1.0 mm of activation. For statistic data analysis, a analysis of variance was performed and a Tukey's Multiple Comparison test was used as supplement, considering a 5% level of significance. Results: In general, teardrop loops with helix produced lower magnitudes of horizontal force and load/deflection ratio, and higher moment/force ratio than teardrop loops without helix. Among all analyzed variables, metal alloy composition presented greater influence in the horizontal force and in the load/deflection ratio. The moment/force ratio showed to be more influenced by the preactivation of loops for space closure. © 2013 Dental Press Journal of Orthodontics.

Solid-phase extraction of metal ions from fuel ethanol with a nanostructured adsorbent

This work describes the synthesis and characterization of a new octakis[3-(2,2'-dipyridylamine)propyl]octasilsesquioxane (T8-Pr-DPA), and a study of the metal ion preconcentration in fuel ethanol. Batch and column experiments were conducted to investigate for the removal of heavy metal ions from fuel ethanol. The results showed that the Langmuir allowed to describe the sorption equilibrium data of the metal ions on T8-Pr-DPA in a satisfactory way. The following maximum adsorption capacities (in mmolg-1) were determined: 3.62 for Fe (III), 3.32 for Cr (III), 2.15 for Cu (II), 1.80 for Co (II), 1.62 for Pb (II), 1.32 for Ni (II) and 0.88 for Zn (II). The thermodynamic parameters for the adsorption process such as free energy of adsorption (δG), enthalpy of adsorption (δH) and entropy of adsorption (δS) were calculated. Thermodynamic parameters showed that the system has favorable enthalpic, Gibbs free energy, and entropic values. The sorption-desorption of the metal ions has made possible the development of a preconcentration and determination method of metal ions at trace level in fuel ethanol. The method of quantitative analysis for Fe, Cu, Ni and Zn in fuel ethanol by Flame AAS was validated. Several parameters have been taken into account and evaluated for the validation of method, namely: linearity, limit of detection, limit of quantification, and the relative standard deviation and accuracy. The accuracy of the method was assessed by testing analyte recovery in the fuel ethanol samples. © 2013 Elsevier B.V.