Internal standardization combined with dilute-and-shoot preparation of distilled alcoholic beverages for Cu determination by high-resolution continuum source flame atomic absorption spectrometry

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

Evaluation of Lines of Phosphorus and Potassium by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry for Liquid Fertilizer Analysis

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

Armazenamento refrigerado de pomelos variedades flame e henderson revestidos com cera

Objetivou-se, neste trabalho, estudar a conservação de pomelos (Citrus paradisi Macfad.) varieties 'Flame' e 'Henderson' revestidos com cera Sparcitrus e mantidos sob refrigeração (8º C ± 1º C e 95% ± 5% UR). Para cada variedade estudada, utilizou-se delineamento inteiramente casualizado, disposto em esquema fatorial 2 x 5, com 3 repetições, onde o primeiro fator correspondeu aos tratamentos com e sem a aplicação de cera (controle) e o segundo, ao tempo armazenamento (0, 10, 20, 30 e 40 dias). Cada parcela experimental foi composta por cinco frutos. Foram estudadas as seguintes variáveis: perda de massa, rendimento do suco, pH, sólidos solúveis (SS), acidez titulável (AT), SS/AT, açúcares redutores, açúcares não redutores, açúcares solúveis totais, vitamina C e aparência externa. A aplicação de cera é efetiva na preservação da aparência de pomelos 'Flame' e 'Henderson', não afetando sua qualidade interna.

Determination of butyltin compounds in surface sediments from the São Paulo State coast (Brazil) by gas chromatography-pulsed flame photometric detection

Occurrence and the effects of butyltin compounds (BTs) have been studied for some years, mainly in countries of the Northern Hemisphere. Due to widespread use of tributyltin compounds (TBTs) and considering their deleterious effects, it is necessary to conduct studies on its occurrence, especially in the marine environment because of its excessive use in coatings of ship hulls to prevent fouling. Moreover, it was important to extend the evaluation to areas where there is no current information about their occurrence. The present work reports the occurrence of BTs in marine sediments of São Paulo state, Brazil. Commercial and leisure harbor sampling sites were selected because these areas are potentially exposed to BTs from antifouling paints used on ship hulls. Analytical conditions for organotin analysis in marine sediments were optimized for GC with pulsed flame photometric detection. Detection limits ranged from 8.4 to 66.3 ng g(-1) using a 610-nm filter, and the linearity range was 20-500 ng g(-1). Concentration levels of BTs were highest in Santos harbor (360 ng g(-1) TBT in average) and Guaruja marina (670 ng g(-1) TBT in average), which seems to be related to intensive boat traffic. Lower levels of BTs were observed in Cananeia, where only fishing boats are present (50 ng g(-1) TBT in average). (C) 2002 Elsevier B.V. B.V. All rights reserved.

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.

High current-density anodic electro-dissolution in flow-injection systems for the determination of aluminium, copper and zinc in non-ferroalloys by flame atomic absorption spectrometry

An automatic Procedure with a high current-density anodic electrodissolution unit (HDAE) is proposed for the determination of aluminium, copper and zinc in non-ferroalloys by flame atonic absorption spectrometry, based on the direct solid analysis. It consists of solenoid valve-based commutation in a flow-injection system for on-line sample electro-dissolution and calibration with one multi-element standard, an electrolytic cell equipped with two electrodes (a silver needle acts as cathode, and sample as anode), and an intelligent unit. The latter is assembled in a PC-compatible microcomputer for instrument control, and far data acquisition and processing. General management of the process is achieved by use of software written in Pascal. Electrolyte compositions, flow rates, commutation times, applied current and electrolysis time mere investigated. A 0.5 mol l(-1) HNO3 solution was elected as electrolyte and 300 A/cm(2) as the continuous current pulse. The performance of the proposed system was evaluated by analysing aluminium in Al-allay samples, and copper/zinc in brass and bronze samples, respectively. The system handles about 50 samples per hour. Results are precise (R.S.D < 2%) and in agreement with those obtained by ICP-AES and spectrophotometry at a 95% confidence level.

Solid-phase extraction of sugar cane soot extract for analysis by gas chromatography with flame ionisation and mass spectrometric detection

The incomplete combustion of biomass is one of the most important sources of emissions of organic compounds into the atmosphere, like polycyclic aromatic hydrocarbons (PAHs) which show genotoxic activity. Since environmental samples generally contain interferents and trace amounts of PAHs of interest, concentration and clean-up procedures are usually required prior to the final chromatographic analysis. This paper discusses the performance of Sep-Pak cartridges (silica gel and RP18) on clean-up of sugar cane soot extract. The best results were obtained with a silica Sep-Pak cartridge. The recoveries ranged from 79% (benzo[b]fluoranthene) to 113% (benzo[e]pyrene). (C) 2000 Elsevier B.V. B.V. All rights reserved.

GC analysis of organotin compounds using pulsed flame photometric detection and conventional flame photometric detection

Organotin compounds, largely used as biocides in antifouling paints, are among the most toxic materials introduced into the aquatic environment. Sensitive analytical methods are thus required to characterize their occurrence in environmental and biological matrices. The comparison between two different photometric detectors in terms of analytical performance was carried out for the analysis of organotin compounds. A flame photometric detector (FPD) and a pulsed flame photometric detector (PFPD) were optimized. Their respective sensitivity, linearity range and selectivity were evaluated. Limits of detection obtained for a tributyltin compound (TBT) were 5.0 and 0.9 pg (as Sn) for the FPD and PFPD, respectively, using a 390 nm filter. The PFPD showed higher selectivity, besides reduced gas consumption in the flame, and is very attractive for organotin compound speciation in complex environmental matrices.

Determination of Total Sulfur in Agricultural Samples by High-Resolution Continuum Source Flame Molecular Absorption Spectrometry

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

Determination of cadmium in river water samples by flame AAS after on-line preconcentration in mini-column packed with 2-aminothiazole-modified silica gel

A rapid and sensitive method was developed to determine trace levels of Cd2+ ions in an aqueous medium by flame atomic absorption spectrometry, using on-line preconcentration in a mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT). The Cd2+ ions were sorbed at pH 5.0. The preconcentrated Cd2+ ions were directly eluted from the column to the spectrometer's nebulizer-burner system using 100 μL of 2 mol L-1 hydrochloric acid. A retention efficiency of over 95% was achieved. The enrichment factor (calculated as the ratio of slopes of the calibration graphs) obtained with preconcentrations in a mini-column packed with SiAT (A = -1.3 × 10-3 + 1.8 × 10-3 [Cd2+]) and without preconcentrations (A = 4 × 10-5 + 3.5 × 10-3[Cd2+]), was 51 and the detection limit calculated was 0.38 μg L-1. The preconcentration procedure was applied to determine trace levels of Cd in river water samples. The optimum preconcentration conditions are discussed herein.

Rapid determination of zinc in foods by flow injection analysis with flame AAS using gradient calibration method

A calibration method was developed using flow injection analysis (FI) with a Gradient Calibration Method (GCM). The method allows the rapid determination of zinc In foods (approximately 30 min) after treatment with concentrated sulphuric acid and 30% hydrogen peroxide, and analysis with flame atomic absorption spectrometry (FAAS). The method provides analytical results with a relative standard deviation of about 2% and requires less time than by conventional FI calibration. The electronic selection of different segments along the gradient and monitoring of the technique covers wide concentration ranges while maintaining the inherent high precision of flow injection analysis. Concentrations, flow rates, and flow times of the reagents were optimized in order to obtain best accuracy and precision. Flow rates of 10 mL/min were selected for zinc. In addition, the system enables electronic dilution and calibration where a multipoint curve can be constructed using a single sample injection.

The influence of the flame structure on the combustion oscillations in a cylindrical chamber

An experimental study has been conducted with the objective of investigating the effects of the flame structure in the combustion oscillation conditions into a laboratorial scale cylindrical chamber. The experiments were conducted in a water-jacketed 1-m long by 25-cm internal diameter stainless steel vertical tube. The combustor operated with liquefied petroleum gas (LPG) in both oscillatory and non oscillatory conditions, under the same input conditions. Part of the reactant mixture was excited acoustically, before the burner exit, by a speaker positioned strategically. The burner was aligned with the chamber longitudinal axis and positioned at its bottom. The experiments were conducted for 0.16 g/s of LPG burning in stoichiometric equivalence ratio. To analyze the flame structure the image tomographic reconstruction process were used, and the resultant images were associated to the oscillatory conditions (frequency and amplitude) into the combustion chamber. The main conclusions were: 1) when the flame premixed condition increase, for example 60% of the total air flow rate is premixed with LPG, the region of intense energy released is close to burner exit and strong amplitudes of oscillation (close to 50 mbar) were obtained into the chamber; 2) for long flames, predominantly diffusive flames, just weak amplitudes were detected, in the spite of the speaker exiting the premixed flow; 3) when the energy is released distributed through the combustion chamber, the long flame acts like a baffle. Copyright © 2006 by the American Institute of Aeronautics and Astronautics, Inc. All rights reserved.

Determination of calcium and magnesium in hydroethanolic extracts of propolis by atomic absorption flame spectrophotometry

Propolis is a natural product collected by honeybees and has a large range of pharmacological activity, including antimicrobial, antitumoral, antioxidant and anti-inflammatory. Its use as a popular medicine is increasing all over the world, creating a need for quality control of the commercial products. In this study the levels of calcium and magnesium in commercial hydroalcoholic propolis extracts from varies states of Brazil were determined by atomic absorption flame spectrophotometry and different values were obtained for northern and southern states. This study can be extended to the analysis of metals that are harmful to health. The results showed that the calibration curves were linear over a wide concentration range (0.5-4.0 μg.mL -1 for calcium and 0.05-0.4 μg.mL -1 for magnesium) with good correlation coefficients (0.999 and 0.988, respectively). Good analytical recovery (94%) was obtained. The proposed method showed adequate precision and relative standard deviation lower than 2 %. The method is accurate and precise as well as having advantages such as simplicity and speed.

Determination of copper at wide range concentrations using instrumental features of high-resolution continuum source flame atomic absorption spectrometry

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324. 754 nm, 327. 396 nm, 222. 570 nm, 249. 215 nm and 224. 426 nm were evaluated and main figures of merit established. Absorbance measurements at 324. 754 nm, 249. 215 nm and 224. 426 nm allows the determination of Cu in the 0. 07-5. 0 mg L -1, 5. 0-100 mg L -1 and 100-800 mg L -1 concentration intervals respectively with linear correlation coefficients better than 0. 998. Limits of detection were 21 μg L -1, 310 μg L -1 and 1400 μg L -1 for 324. 754 nm, 249. 215 nm and 224. 426 nm, respectively and relative standard deviations (n = 12) were ≤ 2. 7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.