Otimização da análise isotópica de UF6 utilizando-se a técnica de espectrometria de massas por quadrupolo

A procedure for determining of the isotope ratio 235U/238U in UF6 samples was established using a quadrupole mass spectrometer with ionization by electron impact. The following items were optimized in the spectrometer: the parameters in the ion source that provided the most intense peak, with good shape, for the most abundant isotope; the resolution that reduced the non linear effects and the number of analytical cycles that reduced the uncertainty in the results. The measurement process was characterized with respect to the effects of mass discrimination, linearity and memory effect.

Espectrometria de absorção atômica: o caminho para determinações multi-elementares

This paper present an overview of way covered for the spectrometry of atomic absorption (AAS), tracing a line of the historical events in its development and its establishment as a multielement technique. Additionally, the efforts carried by through several researchers in the search for the instrumental evolution, the advances, advantages, limitations, and trends of this approach are related. Several works focusing its analytical applications are cited employing simultaneous multielement determination by flame (FAAS) and/or graphite furnace (GF AAS), and fast sequential multielement determination using FAAS are reported in the present review.

Determinação de isotiocianato de benzila em Carica papaya utilizando cromatografia gasosa com detectores seletivos

In the present work, a method was developed and validated for the quantification of benzyl isothiocyanate (BITC) in the fruits of Carica papaya. The quantification of this compound was carried out by gas chromatography (GC) with selective detectors - nitrogen phosphorus detector (NPD) and flame photometric detector (FPD). The performance of these detectors showed a higher sensitivity of the NPD with a broader linear range of detection. The LOD/LOQ were 0.038/0.100 µg/mL for NPD and 5.78/19.29 µg/mL for FPD. The recovery of the method for BITC was 90,64%. An average value of BITC concentration in all the analyzed samples was 16,23 µg BITC/g.

Sintesis de poliuretanos a partir de polioles obtenidos a partir del aceite de higuerilla modificado por transesterificación con pentaeritritol

Castor oil was reacted by transesterification with various percentages in mass of pentaerythritol to obtain different esters of pentaerythritol. Alternatively, glycerol was also used instead of pentaerythritol for the same reaction in order to establish comparative reference products. The products of the reactions were characterized by matrix-assisted laser desorption/ionization time-of-flight mass spectroscopy in order to detect and quantify (in terms of the molecular mass and structural information) the components of the products obtained. Analysis for hydroxyl value, acid value, viscosity and specific gravity were used to complete the characterization of the polyols obtained and also of the original castor oil. The polymer characterization was accomplished by tensile stress-strain tests, Shore A hardness, thermogravimetric analysis and chemical resistance to solvents.

Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

CE-MS has been increasingly used for analysis of a vast array of compounds. This article reviews the different electrophoretic modes, interfaces and mass analyzers that are commonly used in the CE-MS coupling, as well as the technique advantages and performance characteristics. A large compilation of CE-MS applications is also presented. Therefore, this review is both a guide for beginners and a collection of key references for people who are familiar to the technique. Furthermore, this is the first CE-MS review published in a Brazilian journal and marks the installation of the first two commercial CE-MS units in Sao Paulo State.

Termogravimetria: um novo enfoque para a clássica determinação de cálcio em cascas de ovos

The use of thermoanalytical data in sample preparation is described as a tool to catch the students' attention to some details that can simplify both the analysis and the analytical procedure. In this case, the thermal decomposition of eggshells was first investigated by thermogravimetry (TGA). Although the classical procedures suggest long exposure to high temperatures, the TGA data showed that the decomposition of organic matter takes place immediately when the sample is heated up to 800 °C under air atmosphere. After decomposition, the calcium content was determined by flame atomic emission photometry and compared with the results obtained using classical volumetric titration with EDTA.

Temperature measurements by oh lif and chemiluminescence kinetic modeling for ethanol flames

OH LIF-thermometry was applied to premixed ethanol flames at atmospheric pressure in a burner for three flame conditions. Flame temperatures were simulated from energy equation with PREMIX code of CHEMKIN software package for comparison. A kinetic modeling based on a model validated through chemiluminescence measurements and on a set of reactions for nitrogen chemistry was evaluated. Marinov's mechanism was also tested. Sensitivity analysis was performed for fuel-rich flame condition with Φ = 1.34. Simulated temperatures from both reaction mechanisms evaluated were higher than experimental values. However, the proposed kinetic modeling resulted in temperature profiles qualitatively very close to the experimental.

Especiação de cromo em cimentos e derivados de cimento brasileiros

A method for determination of Cr(III) and Cr(VI) in cement and cement-related materials was studied. Molecular absorption spectrophotometry based on 1,5-diphenylcarbazide as chromogenic reagent was used for determination of Cr(VI) after alkaline extraction. The total chromium concentration was determined using flame atomic absorption spectrometry (FAAS) after complete sample decomposition by fusion. The quantification of Cr(III) was accomplished by subtracting the Cr(VI) concentration from the total chromium concentration. The concentration of Cr(III) in the samples ranged from 10.9 to 88.0 mg kg-1, whereas only in few samples the Cr(VI) concentration was higher than the value established by the European Community to this type of sample [2 mg kg-1 Cr(VI)].

Parâmetros r e R obtidos de programa interlaboratorial: como usá-los

Intralaboratorial and interlaboratorial variabilities can be obtained by conducting an specially designed interlaboratory program. Using the analysis of variance technique one can calculate the r (repeatability) and R (reproducibility) indexes that can help participant laboratories to monitor their routine quality control procedures. An example is described using data obtained from an interlaboratory program where twelve laboratories determined total iron content in silicon metal sample by using flame atomic absorption spectrometry.

Determinação direta de Ca, Mg, Mn e Zn em amostras de leite de búfala da Ilha de Marajó por espectrometria de absorção atômica com chama (FAAS)

This work proposes an analytical procedure for direct determination of calcium, magnesium, manganese and zinc in buffalo milk by flame atomic absorption spectrometry (FAAS). Samples were diluted with a solution containing 10% (v/v) of water-soluble tertiary amines (CFA-C) at pH 8. For comparison, buffalo milk samples were digested with HNO3 and H2O2. According to a paired t-test, the results obtained in the determination of Ca, Mg, Mn and Zn in digested samples and in 10% (v/v) CFA-C medium were in agreement at a 95% confidence level. The developed procedure is simple, rapid, decrease the possibility of contamination and can be applied for the routine determination of Ca, Mg, Mn and Zn in buffalo milk samples without any difficulty caused by matrix constituents, such as fat content, and particle size distribution in the milk emulsion.

Development of a flotation method for preconcentration-separation of trace amounts of some metal ions in plant tissues prior to their FAAS determinations

An efficient flotation method based on the combination of flame atomic absorption spectrometry (FAAS) and separation and preconcentration step for determination of Cr3+, Cu 2+, Co2+, Ni2+, Zn2+, Cd 2+, Fe3+ and Pb2+ ions in various real samples by the possibility of applying bis(2-hydroxyacetophenone)-1,4-butanediimine (BHABDI) as a new collector was studied. The influence of pH, amount of BHABDI as collector, sample matrix, type and amount of eluting agent, type and amount of surfactant as floating agent, ionic strength and air flow rates i.e. variables affecting the efficiency of the extraction system was evaluated. It is ascertained that metal ions such as iron can be separated simultaneously from matrix in the presence of 0.012 mM ligand, 0.025% (w/v) of CTAB to a test sample of 750 mL at pH 6.5. These ions can be eluted quantitatively with 6 mL of 1.0 mol L-1 HNO3 in methanol which lead to the enrichment factor of 125. The detection limits for analyte ions were in the range of 1.3-2.4 ng mL-1. The method has been successfully applied for determination of trace amounts of ions in various real samples.

Removal of copper(II) from sugar-cane spirits employing chitosan

A method employing chitosan as complexant agent in the removal of copper(II) ions generally present in the Brazilian cachaça samples is herein proposed. The efficiency of this method is attributed to its high capacity of metal cations adsorption, mainly due to presence of hydroxyl and amine groups that can serve as chelating sites. The removal of copper(II) ions from this alcoholic beverage was efficient employing either in column and batch system. The analysis were carried out employing the flame atomic absorption spectrometry and the remaining copper(II) concentrations in the treated cachaça were lower than LOD of FAAS technique.

Avaliação do desempenho de surfactantes para a solubilização de fases líquidas não aquosas em meio aquoso

The presence of non-aqueous phase liquids (NAPLs) in the subsurface is a threat to public health as well as a serious environmental issue. NAPLs may remain adsorbed or form lenses floating on aquifers causing long-term contaminations. Surfactants may increase NAPLs solubility, enhancing the pump-and-treatment performance. Size, shape, hydration and ionization degree of the micelles define the affinity and the space available for the solubilization of a particular contaminating agent. The tests carried out at laboratory scale, taking into account the NAPL to be removed and the medium characteristics were useful to select surfactants and evaluate their efficiency as NAPLs solubilizers.

Caracterização de contaminantes presentes em sistemas de tratamento de esgotos, por cromatografia líquida acoplada à espectrometria de massas tandem em alta resolução

This work shows results on the characterization, by liquid chromatography coupled to high resolution tandem mass spectrometry (LC-IT-TOF-MS) with electrospray ionization, of organic compounds present in raw and treated effluents from a combined sewage treatment systems (upflow anaerobic sludge blanket-trickling filter). The sewage samples were prepared by C18 solid phase extraction and the spectra obtained from the various extracts were submitted to principal component analysis to evaluate their pattern and identify the major deprotonated species. Some target compounds were submitted to semiquantitative analysis, using phenolphtalein as internal standard. The results showed the anaerobic step had little impact on the removal of anionic surfactants (LAS), fatty acids, and some contaminantes such as bisphenol A and bezafibrate, whereas the aerobic post-treatment was very efficient in removing these organics.

Caracterização físico-química e microestrutural de conchas de moluscos bivalves provenientes de cultivos da região litorânea da ilha de Santa Catarina

Samples of shells of oysters and mussels from sea farm around the Santa Catarina Island in south Brazil were collected and analyzed by DRX, FRX, SEM, CHN-S, FTIR, TG, AAS/Flame and AAS /GF. The results showed that the crystalline structure of mussel's shells is mainly formed by aragonite and the oyster's shells by calcite. The calcium percentage in both shells species was in the range of 33 to 35% and also 850 and 1200 mg/kg of strontium was detected in the shells of oysters and mussels, respectively. The content of organic matter was larger in the mussel's shells and the thermal degradation of both shells species occurred by three events at different temperatures from 250 to 830 ºC.