Direct determination of chromium in empty medicine capsules by tungsten coil atomic emission spectrometry

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

A simple and fast method for assessment of the nitrogen-phosphorus-potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

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

Rugged, Portable Tungsten Coil Atomic Emission Spectrometer

Tungsten coil atomic emission spectrometry is an ideal technique for field applications because of its simplicity, low cost, low power requirement, and independence from cooling systems. A new, portable, compact design is reported here. The tungsten coil is extracted from an inexpensive 24 V, 250 W commercial light bulb. The coil is housed in a small, aluminum cell. The emission signal exits from a small aperture in the cell, while the bulk of the blackbody emission from the tungsten coil is blocked. The resulting spectra exhibit extremely low background signals. The atomization cell, a single lens, and a hand-held charge coupled device (CCD) spectrometer are fixed on a 1 x 6 x 30 cm ceramic base. The resulting system is robust and easily transported. A programmable, miniature 400 W solid-state constant current power supply controls the temperature of the coil. Fifteen elements are determined with the system (Ba, Cs, Li, Rb, Cr, Sr, Eu, Yb, Mn, Fe, Cu, Mg, V, Al, and Ga). The precision ranges from 4.3% to 8.4% relative standard deviation for repetitive measurements of the same solution. Detection limits are in the 0.04 to 1500 mu g/L range. Accuracy is tested using standard reference materials for polluted water, peach leaves, and tomato leaves. For those elements present above the detection limit, recoveries range from 72% to 147%.

Direct determination of calcium in milk by atomic absorption spectrometry using flow-injection analysis

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

Bismuth as a general internal standard for lead in atomic absorption spectrometry

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

Avaliação do método das adições de analito para a determinação de sódio em álcool combustível por espestrometria de emissão atômica em chama

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

Ultrasound-assisted extraction of Na and K from swine feed and its application in a digestibility assay: A green analytical procedure

The study is aimed to evaluate the efficiency of ultrasound-assisted extraction (UAE) as a simple strategy focused on sample preparation for metal determination in biological samples. The extraction of sodium and potassium extraction was carried out from swine feed followed by determination of the concentration of these metals by flame atomic emission spectrometry (FAES). The experiment was performed to cover the study of the variables influencing the extraction process and its optimal conditions (sample mass, particle size, acid concentration, sonication time and ultrasound power); the determination of these analytical characteristics and method validation using certified reference material; and the analysis of pre-starter diets. The optimal conditions established conditions were as follows: mass: 100 mg, particle size:<60 μm, acid concentration: 0.10 mol L-1 HCl, sonication time: 50 s and ultrasound power: 102 W. The proposed method (UAE) was applied in digestibility assays of those nutrients present in different piglet pre-starter feeds and their results proved to be compatible with those obtained from mineralized samples (P < 0.05). The ultrasound extraction method was demonstrated to be an excellent alternative for handless sampling and operational costs and the method also has the advantage of does not generating toxic residues that may negatively affect human health and contaminate the environment. © 2013 Elsevier B.V. All rights reserved.

Sequential Determination of Cd, Cu and Pb in Tea Leaves by Slurry Introduction to Thermospray Flame Furnace Atomic Absorption Spectrometry

A simple procedure for the sequential determination of Cd, Cu and Pb in tea leaves by slurry introduction to thermospray flame furnace atomic absorption spectrometry was developed. Detection limits were 0.05 mg kg-1 for Cd, 2.1 mg kg-1 for Cu and 0.68 mg kg-1 for Pb using 0.67 % (m/v) slurries (100 mg/15 mL). © 2013 Springer Science+Business Media New York.

On-line determination of Sb(III) and total Sb using baker's yeast immobilized on polyurethane foam and hydride generation inductively coupled plasma optical emission spectrometry

The yeast Saccharomyces cerevisiae was immobilized in cubes of polyurethane foam and the ability of this immobilized material to separate Sb(III) and Sb(V) was investigated. A method based on sequential determination of total Sb (after on-line reduction of Sb(V) to Sb(III) with thiourea) and Sb(Ill) (after on-line solid-liquid phase extraction) by hydride generation inductively coupled plasma optical emission spectrometry is proposed. A flow system assembled with solenoid valves was used to manage all stages of the process. The effects of pH, sample loading and elution flow rates on solid-liquid phase extraction of Sb(III) were evaluated. Also, the parameters related to online pre-reduction (reaction coil and flow rates) were optimized. Detection limits of 0.8 and 0.15 mu g L-1 were obtained for total Sb and Sb (III), respectively. The proposed method was applied to the analysis of river water and effluent samples. The results obtained for the determination of total Sb were in agreement with expected values, including the river water Standard Reference Material 1640 certified by the National Institute of Standards and Technology (NIST). Recoveries of Sb(III) and Sb(V) in spiked samples were between 81 19 and I I I 15% when 120 s of sample loading were used. (c) 2006 Elsevier B.V. All rights reserved.

The use of silica-immobilized brown alga (Pilayella littoralis) for metal preconcentration and determination by inductively coupled plasma optical emission spectrometry

The brown alga Pilayella littoralis was used as a new biosorbent in an on-line metal preconcentration procedure in a flow-injection system. Al, Co, Cu and Fe were determined in lake water samples by inductively coupled plasma optical emission spectrometry (ICP-OES) after preconcentration in a silica-immobilized alga column. Like other algae, P. littoralis exhibited strong affinity for these metals proving to be an effective accumulation medium. Metals were bound at pH 5.5 and were displaced at pH < 2 with diluted HCl. The enrichment factors for Cu-II, Fe-III, Al-III and Co-II were 13, 7, 16 and 11, respectively. Metal sorption efficiency ranged from 86 to 90%. The method accuracy was assessed by using drinking water certified reference material and graphite furnace atomic absorption spectrometry (GFAAS) as a comparison technique. The column procedure allowed a less time consuming, easy regeneration of the biomaterial and rigidity of the alga provided by its immobilization on silica gel. (C) 2003 Elsevier B.V. All rights reserved.

Analysis of cement slurries by inductively coupled plasma optical emission spectrometry with axial viewing

The feasibility of Portland cement analysis by introduction of slurries in an inductively coupled plasma optical emission spectrometer (ICP-OES) with axial viewing has been evaluated. After a fast manual grinding of the cement samples, owing to the pulverized state of this material, 0.1% m/v slurries were prepared in 1% v/v HCl. The calibration was performed adopting two strategies: one based on slurries prepared from different masses (50, 75, 100 and 125 mg) of a Portland cement standard reference material (NIST SRM 1881), and the other one based on aqueous reference solutions. A complete analysis of cement for major (Al, Ca, Fe, Mg and Si), minor and trace elements (Mn, P, S, Sr and Ti) was accomplished. Both strategies led to accurate results for commercial Portland cement samples, except for Si and Ti. for which the calibration with aqueous reference solutions resulted in low values. Applying a paired t-test it was shown that most results were in agreement at a 95% confidence level with a conventional fusion decomposition procedure. The ICP-OES with axial viewing and end-on gas configuration for removal of the recombination plasma zone was effective for cement slurry analysis without any undesirable particle deposition in the pre-optics interface and without severe spectral interferences. (C) 2002 Elsevier B.V. B.V. All rights reserved.

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)

Direct determination of Cu, Cd, Ni and Pb in aquatic humic substances by graphite furnace atomic absorption spectrometry

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

Tungsten permanent chemical modifier for fast estimation of Se contents in soil by graphite furnace atomic absorption spectrometry

A tungsten carbide coating on the integrated platform of a transversely heated graphite atomizer was used as a modifier for the direct determination of Se in soil extracts by graphite furnace atomic absorption spectrometry. Diethylenetriaminepentaacetic acid (0.0050 mol L-1) plus ammonium hydrogencarbonate (1.0 mol L-1) extracted predominantly available inorganic selenate from soil. The formation of a large amount of carbonaceous residue inside the atomizer was avoided with a first pyrolysis step at 600 degreesC assisted by air during 30 s. For 20 muL of soil extracts delivered to the atomizer and calibration by matrix matching, an analytical curve (10.0-100 mug of L-1) with good linear correlation (r = 0.999) between integrated absorbance and analyte concentration was established. The characteristic mass was similar to63 pg of Se, and the lifetime of the tube was similar to750 firings. The limit of detection was 1.6 mug L-1, and the relative standard deviations (n = 12) were typically <4% for a soil extract containing 50 mug of L-1. The accuracy of the determination of Se was checked for soil samples by means of addition/recovery tests. Recovery data of Se added to four enriched soil samples varied from 80 to 90% and indicated an accurate method.

Development of a method to determine Ni and Cd in biodiesel by graphite furnace atomic absorption spectrometry

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