Comparação de dois tipos de amostragem de chuva: deposição total e deposição apenas úmida em àrea costeira tropical

In a tropical coastal area. During 6 months the composition of rain samples collected simultaneously over 24h with an open collector and with an automatic opened collector (KFA - J¸lich Type) at 500m of the Atlantic coastline of Salvador were compared. All average concentrations were higher for the "total" samples than for the "wet only" samples, except for hydrogen ions, nitrate and ammonium.

Separação de espectros simulados e de luminescência total através do método generalizado de anulação do posto (GRAM)

A multivariate curve resolution method, "GENERALIZED RANK ANNIHILATION METHOD (GRAM)", is discussed and tested with simulated and experimental data. The analysis of simulated data provides general guidelines concerning the condition for uniqueness of a solution for a given problem. The second-order emission-excitation spectra of human and animal dental calculus deposits were used as an experimental data to estimate the performance of the above method. Three porphyrinic spectral profiles, for both human and cat, were obtained by the use of GRAM.

Sistema automático para determinação seqüencial de cianeto livre e total empregando eletrodo tubular íon-seletivo de membrana homogênea

This study presents an automated system for potentiometric determination of free and total cyanide which employs a homogeneous membrane tubular ion-selective electrode. After the electrode is assembled, it is connected to a system composed of 3 three-way solenoid valves, sample line, carrier line, acid stream, and gas diffusion chamber. A Turbo Pascal® computer program, developed specifically for this task, automatically performs all the steps involved in data acquisition and processing. The proposed analytical procedure offers operational simplicity, since detection is performed by a tubular electrode, whose assembly is fast and easy. The system has shown reproducibility (r.s.d. < 0.5%, n=6) and high speed (30 readings/hour); it is efficient for determination of free and total cyanide in waste waters of starch processing plants. The detection limit was 1.2x10-5 and 1.5x10-5 mol L-1, for determination of free and total cyanide, respectively. The linear response range was between 1.2x10-5 and 1.0x10-2 mol L-1 for free cyanide and between 1.5x10-5 and 1.0x10-2 for total cyanide.

Gota suspensa para avaliação de aldeído total no ar interno e externo do ambiente

A sensitive and simple system was proposed for the in situ measurement of total aldehyde in outdoor or indoor ambient. The method is based on the use of a reagent drop as an useful interface to preconcentrate the sample prior to determination of total aldehyde as formaldehyde. The drop is formed at the tip of a cylindrical tube that contains two optical fibers placed on opposite sides and in contact with the reagent solution. One optical fiber carries the red light to the drop form a light emitting diode (LED). The transmitted light is measured by a second optical fiber/photodiode system. The analytical signal is read and converted into absorbance. The reagent solution of 3-methyl-2-benzothiazoline hydrazone (MBTH) forms a blue cation during reaction with formaldehyde that can be measured at 660 nm. Some aspects of kinetics reaction formation of dye were reevaluated. The formaldehyde reacts with MBTH and forms the azine in about 12 min. The oxidation of MBTH by Fe (III) and the formation of dye requires 3 min. The absorbance of the reagent drop is proportional to the sampling time and to the analyte concentration. The absorbance signal increases with increased sample gas flow until a maximum is reached then decreases until it forms a plateau. The proposed method was evaluated using both outdoor and indoor samples, and it was shown to viable provide an accurate measure of total aldehyde.

Espectrofotometría de absorción atómica con tubo en la llama: aplicación en la determinación total de cadmio, plomo y zinc en aguas frescas, agua de mar y sedimentos marinos

Thermospray flame furnace Atomic Absorption Spectrometry (TS-FF-AAS) was used for the total determination of Cd, Pb and Zn in fresh water and seawater samples at µg L-1 levels, and in marine sediment samples at µg g-1 levels. Using a sample loop of 50 µL and a peristaltic pump the samples were transported into the metallic tube placed over an air/acetylene flame, through a ceramic capillary (o.d. = 3.2 mm) containing two parallel internal orifices (i.d = 0.5 mm). The detection limits determined for Cd, Pb and Zn using a synthetic water matrix (2.5% m/v NaCl, 0.5% m/v MgCl2 and 0.8% m/v CaCl2) were 0.32 µg L-1; 2.6 µg L-1 and 0.21 µg L-1 respectively. The methodology by TS-FF-AAS was validated by determination of Cd, Pb and Zn in certified reference materials of water and marine sediment, and the t-test for differences between means was applied. No statistically significant differences were established in fresh water and seawater (p>0.05), whereas differences became apparent in marine sediment (p<0.03).

Determinação das formas de nitrogênio e nitrogênio total em rochas-reservatório de petróleo por destilação com arraste de vapor e método do indofenol

Several extraction procedures are described for the determination of exchangeable and fixed ammonium, nitrate + nitrite, total exchangeable nitrogen and total nitrogen in certified reference soils and petroleum reservoir rock samples by steam distillation and indophenol method. After improvement of the original distillation system, an increase in worker safety, a reduction in time consumption, a decrease of 73% in blank value and an analysis without ammonia loss, which could possibly occur, were achieved. The precision (RSD < 8%, n = 3) and the detection limit (9 mg kg-1 NH4+-N) are better than those of published procedures.

Decolorization and toxicity of municipal waste by horseradish (Cochlearia armoracia)

The Municipal Station of Americana, SP, Brazil, treats a volume of 400 l s-1 of effluent, of domestic and textile origin, and produces about 20 t of sludge per day. The plant horseradish, which contains high amount of peroxidases, was able to decolorize this effluent in 2 h and the solid waste in 2 days, at concentrations of 10 and 50%, respectively. However, there was an increase in the toxicity for the bioassays with Hydra attenuatta, Selenastrum capricornutum and lettuce seeds, indicating formation of more toxic substances. Since horseradish showed the ability to decolorize these residues, it can be used as pre-treatment resulting in a sludge of less complex composition.

Determinação de açúcar total em café cru por espectroscopia no infravermelho próximo e regressão por mínimos quadrados parciais

In this work a fast method for the determination of the total sugar levels in samples of raw coffee was developed using the near infrared spectroscopy technique and multivariate regression. The sugar levels were initially obtained using gravimety as the reference method. Later on, the regression models were built from the near infrared spectra of the coffee samples. The original spectra were pre-treated according to the Kubelka-Munk transformation and multiplicative signal correction. The proposed analytical method made possible the direct determination of the total sugar levels in the samples with an error lower by 8% with respect to the conventional methodology.

Mercúrio total em solos de manguezais da Baixada Santista e Ilha do Cardoso, estado de São Paulo

Total Hg content in soils of Baixada Santista, affected by different sources of pollution, and Cardoso Island, which is almost free of anthropogenic activities, were determined by CVAAS. To explain the fate of Hg in the ecosystem, pH, Eh, AVS, Stotal and Total Organic Carbon were also obtained throughout the soil profiles. With the exception of two sampling sites the average content of Hg in samples obtained for Baixada Santista was 0.34 ± 0.20 mg kg-1, which was close to the average data at Cardoso Island (0.30 ± 0.21 mg kg-1). Both of them were below the limit established by CETESB - 0.50 mg kg-1.

Estudo da oxidação total do etanol usando óxidos tipo perovskita LaBO3 (B= Mn, Ni, Fe)

The present work investigated the effect of coprecipitation-oxidant synthesis on the specific surface area of perovskite-type oxides LaBO3 (B= Mn, Ni, Fe) for total oxidation of ethanol. The perovskite-type oxides were characterized by X-ray diffraction, nitrogen adsorption (BET method), thermogravimetric analysis (TGA-DTA), TPR and X-ray photoelectron spectroscopy (XPS). Through method involving the coprecipitation-oxidant was possible to obtain catalysts with different BET specific surface areas, of 33-51 m²/g. The results of the catalytic test confirmed that all oxides investigated in this work have specific catalytic activity for total oxidation of ethanol, though the temperatures for total conversion change for each transition metal.

Diagnóstico espaço-temporal da ocorrência de herbicidas nas águas superficiais e sedimentos do Rio Corumbataí e principais afluentes

Residues of herbicides from sugarcane were monitored in waters and sediments of Corumbataí River and tributaries. Ametryne, atrazine, simazine, hexazinone, glyphosate, and clomazone were detected in water samples, with negligible levels of ametryne and glyphosate in sediment samples. The area of recharge of the Guarani aquifer presented the highest triazine and clomazone levels. The triazines were detected at higher levels, with atrazine above Brazil's potability and quality standards. Total herbicide levels at some sampling points were 13 times higher than the European Community potability limit. There is no Brazilian standard for ametryne, although the risk is larger due to ametryne's higher toxicity for the aquatic biota.

Determinação não destrutiva do nitrogênio total em plantas por espectroscopia de reflectância difusa no infravermelho próximo

Diffuse reflectance near-infrared (DR-NIR) spectroscopy associated with partial least squares (PLS) multivariate calibration is proposed for a direct, non-destructive, determination of total nitrogen in wheat leaves. The procedure was developed for an Analytical Instrumental Analysis course, carried out at the Institute of Chemistry of the State University of Campinas. The DR-NIR results are in good agreement with those obtained by the Kjeldhal standard procedure, with a relative error of less than ± 3% and the method may be used for teaching purposes as well as for routine analysis.

First secondary metabolites from Herissantia crispa L (Brizicky) and the toxicity activity against Artemia salina Leach

The phytochemical investigation of Herissantia crispa led to the isolation of seven compounds, identified as: sitosterol 3-O-β-D-glucopyranoside, stigmasterol 3-O-β-D-glucopyranoside, 3,5,7,4'-tetrahydroxyflavone (kaempferol), 3,5,7,3',4'-pentahydroxyflavone (quercetin), unpublished in the genus Herissantia, besides β-sitosterol, kaempferol 3-O-β-D-(6''-E-p-coumaroil) (tiliroside) glucopyranoside and kaempferol 3,7-di-O-α-L-ramnopyranoside (lespedin), described for the first time in the species. The structural determination of the compounds was made by means of spectroscopy methods such as Infrared Spectroscopy, ¹H and 13C Nuclear Magnetic Resonance, with the aid of two dimensional techniques, and by comparison with literature data. The toxicity activity of the MeOH extract and lespedin on Artemia salina Leach. was also carried out.

Volatile compounds of Nectandra salicina (lauraceae) from Costa Rica and their cytotoxic activity on cell lines

The chemical composition of the volatiles of Nectandra salicina growing wild in Costa Rica was determined by capillary GC/FID and GC/MS. Thirty-seven and forty-two compounds were identified in the leaf and branch oils respectively corresponding to about 92.6 and 86.2% of the total amount of the oils. The major components of the leaf oil were: atractylone (14.6%), viridiflorene (10.1%), α-pinene (9.4%), β-caryophyllene (7.2%), α-humulene (7.0%), δ-cadinene (6.1%), β-pinene (6.0%) and germacrene D (5.8%). The major components of the branch oil were: atractylone (21.1%), germacrene D (10.7%), viridiflorene (7.9%) and 7-epi-α-selinene (5.0%). When the oils were tested on different cell lines, all the LD50 values were higher than 150 µg/mL, with values very similar for the leaf and branch oils. Low toxicity could be explained by antagonistic effects among the main compounds present in the oils.

Estudo da especiação de arsênio inorgânico e determinação de arsênio total no monitoramento ambiental da qualidade de águas subterrâneas

This work reports an alternative, fast and robust method, for the determination of total As, As(III) and As(V) by HG-AAS without the use of prereductants. The method is based on the different rates of arsine formation of the inorganic As species and the effect of As(III) in the signal obtained for total As. Groundwater and mineral spiked waters were used to sample preservation evaluation. The method was validated by the determination of As in SRM 1640 and used in the determination of total As and its inorganic species in groundwater samples collected from mines in the Iron Quadrangle - MG.