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

Microchimica Acta

Texto completo: acesso restrito. p. 183-189A system has been developed for online preconcentration and determination of Cd using thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS). It is based on the solid-phase extraction of Cd in an Amberlite XAD-2 minicolumn loaded with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM), and the metal ion is eluted with 1 mol L−1 hydrochloridric acid, followed by its determination. The online system allows determining Cd with a detection limit of 8.0 ng L−1 and a quantification limit of 25.0 ng L−1. The precision (repeatability), calculated as the relative standard deviation (% RSD) in sample solutions containing 0.5 and 3.0 µg L−1 of Cd, was 6.1 and 4.5%, respectively. The preconcentration factor obtained was 24. The system’s accuracy was confirmed by analyzing the following certified reference materials (CRMs): Rice flour NIES 10b, Apple leaves NIST 1515 and Orchard leaves NBS 1571. This procedure was applied to the determination of Cd in cabbage and powdered guarana samples

Talanta

Trabalho completo: acesso restrito, p. 960–964In the present paper, a simultaneous pre-concentration procedure for the sequential determination of cadmium and lead in table salt samples using flame atomic absorption spectrometry is proposed. This method is based on the liquid–liquid extraction of cadmium(II) and lead(II) ions as dithizone complexes and direct aspiration of the organic phase for the spectrometer. The sequential determination of cadmium and lead is possible using a computer program. The optimization step was performed by a two-level fractional factorial design involving the variables: pH, dithizone mass, shaking time after addition of dithizone and shaking time after addition of solvent. In the studied levels these variables are not significant. The experimental conditions established propose a sample volume of 250 mL and the extraction process using 4.0 mL of methyl isobutyl ketone. This way, the procedure allows determination of cadmium and lead in table salt samples with a pre-concentration factor higher than 80, and detection limits of 0.3 ng g−1 for cadmium and 4.2 ng g−1 for lead. The precision expressed as relative standard deviation (n = 10) were 5.6 and 2.6% for cadmium concentration of 2 and 20 ng g−1, respectively, and of 3.2 and 1.1% for lead concentration of 20 and 200 ng g−1, respectively. Recoveries of cadmium and lead in several samples, measured by standard addition technique, proved also that this procedure is not affected by the matrix and can be applied satisfactorily for the determination of cadmium and lead in saline samples. The method was applied for the evaluation of the concentration of cadmium and lead in table salt samples consumed in Salvador City, Bahia, Brazil

Journal of Hazardous Materials

Acesso restrito: Texto completo. p. 613-619In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L−1 (Zn) for 60 s preconcentration time, at a sample flow rate of 7.0mLmin−1. Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials. © 2008 Elsevier B.V. All rights reserved

AIDS Research and Human Retroviruses

Texto completo: acesso restrito. p. 1451-1454The risk of HIV-1 mother-to-child transmission (MTCT) is clearly correlated with the maternal HIV cell-free viral load (VL) at delivery. Preventing MTCT in late-presenting (after 28 weeks) HIV-infected pregnant women remains a clinical challenge, and ensuring a rapid decrease of maternal VL is an important preventive strategy. Raltegravir (RGV) has a higher first and second phase viral decay rate, has a high placental transfer, with a potential preloading effect for neonate, and demonstrates effective accumulation in cervicovaginal secretions. We report 14 cases in which RGV was used late in pregnancy for HIV-1 MTCT prophylaxis. All women were RGV naive and the prophylaxis regimens included RGV plus at least two other antiretroviral agents. At RGV initiation, the median gestational age was 36 weeks (range 34–38) and the median maternal plasma HIV-1 RNA viral load was 35,364 copies/ml (range 636–391,535). At delivery, the median gestational age was 38 weeks (range 37–40). The median exposure time to RGV was 17 days (range 7–32), with a mean maternal VL decay of 2.6 log. At delivery, seven women had undetectable (<50 copies/ml) VL, four had between 64 and 457 copies/ml, and in three VL was not available. All but one infant's HIV-RNA tests were negative at 1 and 3 months (one case of in utero MTCT). Raltegravir-containing antiretroviral regimens induced a rapid HIV-RNA decline in maternal VL at delivery, and were safe and effective in preventing MTCT for late-presenting, HIV-infected women

Química Nova

p. 1784-1790.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.São Paul

Revista Atlântica

p.107-121Nutrientes inorgânicos dissolvidos, nitrogênio total (NT) e fósforo total (PT), clorofila-a e salinidade foram analisados no estuário do Rio Cachoeira antes e depois da operação de uma estação de tratamento de esgoto (ETE). As concentrações de nutrientes inorgânicos dissolvidos apresentaram grande variação, com valores desde abaixo do limite de detecção a > 45 μM para silicato, > 30 para o nitrogênio amoniacal e > 28 μM para o nitrito. As concentrações de nitrato foram baixas. A clorofila-a variou desde abaixo do limite de detecção a > 60 μg . L-1. A razão molar de nitrogênio e fósforo inorgânico dissolvido (NID:PID)foi maior que a de Redfield (N:P = 16:1) antes e depois da operação da ETE, decrescendo nos meses seguintes. A razão média SiD:NID foram < 1:1. A SiD:PID foi geralmente < 16:1, indicando que o silicato pode estar limitando a produtividade primária. As concentrações de NT foram altas (56,6 - 310 μM). O PT variou de 2,07 a 3,54 μM. As concentrações de nutrientes e clorofila-a encontradas neste estudo são características de ecossistemas eutrofizados. A ETE e outras fontes pontuais contribuem com uma elevada carga de nutrientes para este estuário, levando a eutrofização desse sistema

Journal of the Brazilian Chemical Society

p. 1566-1570Dois métodos para determinação de vanádio em óleo combustível são propostos utilizando GF AAS. O primeiro é baseado na preparação de uma microemulsão da amostra que é diretamente injetada no tubo de grafite. As temperaturas de pirólise e atomização, 1500 e 2700 ºC, respectivamente, foram otimizadas a partir das curvas de temperatura. Para este procedimento obteve-se um limite de detecção de 0,10 mg g-1 e uma massa característica de 87 pg. O outro método utiliza digestão da amostra com ácido sulfúrico, ácido nítrico e peróxido de hidrogênio. As temperaturas de pirólise e atomização, otimizadas, foram 1000 e 2700 ºC, respectivamente. Para este procedimento, obteve-se um limite de detecção de 0,25 µg g-1 e uma massa característica de 63 pg. A exatidão de ambos os métodos foi confirmada pela análise do material de referência certificado NIST SRM 1634c-trace metals in fuel oil.São Paul