Resíduos de pesticidas em águas superficiais de área de nascente do Rio São Lourenço-MT: validação de método por extração em fase sólida e cromatografia líquida

A multiresidue method using HPLC/DAD for the determination of fourteen pesticides in water based on SPE, using SDVB (styrene divynilbenzene copolymer) as adsorbent was validated. Recoveries from 61 to 120%, relative standard deviation between 2 and 15% and detection limits from 0.07 to 0.75 µg L-1 were obtained. It was applied to 66 surface water samples collected in a degraded area at the headwaters of São Lourenço river, Mato Grosso, Brazil. Eight pesticides were detected in concentrations ranging from 0.15 to 35.25 µg L-1. Considering ecotoxicological data, carbendazim and carbofuran may represent a risk to aquatic organisms. These results draw attention to the contamination of this vulnerable degraded area.

Drogas de abuso em águas naturais e residuárias urbanas: ocorrência, determinação e aplicações forenses

Drugs of abuse are commonly used outside medical or legal settings where their production, marketing and consumption are subject to legal summons and/or intervention. Classified as emerging contaminants, these substances have been recently detected in samples of environmental concern, such as waters and wastewaters. This review presents the state-of-the-art on the methodological approaches used in sample preparation, the main techniques applied in analytical determination at trace levels, as well as the use of information related to the drug or its metabolite concentration in sewage samples to empirically estimate the consumption of drugs of abuse in a city or region.

Métodos para análises de HPA e BTEX em águas subterrâneas de postos de revenda de combustíveis: um estudo de caso em Campo Grande, MS, Brasil

Two methods using headspace solid-phase microextraction and gas chromatography - mass spectrometry were developed for the determination of polycyclic aromatic hydrocarbons (PAH) and BTEX. Best results were obtained using DVB/CAR/PDMS fiber, with 10 min extraction at 25 °C and 0.15 min desorption at 260 °C (BTEX), and PDMS/DVB fiber, with 60 min extraction at 90 °C, 10% NaCl and 5 min desorption at 270 °C (PAH). LOD intervals were 3x10-2 - 5x10-2 µg L-1 (BTEX) and 1.6x10-3 - 1.4 µg L-1 (PAH). The methods were applied to forty-five groundwater samples from monitoring wells of gas stations and only benzene level exceeded the limit established by Brazilian regulations.

Análise de fármacos em águas por SPE-UPLC-ESI-MS/MS

A method was developed for the analysis of 31 pharmaceutical compounds in Lisbon's drinking water system, using solid-phase extraction (SPE) and ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). The method was validated through estimation of the linearity range, method detection and quantification limits, matrix effects, precision and accuracy. The method detection and quantification limit ranges were 0.009-10 and 0.03-33 ng/L, respectively. Analytes were quantified in water samples collected from the EPAL (Empresa Portuguesa das Águas Livres S.A.) supply system. Carbamazepine, atenolol, sulfadiazine, sulfamethazine, sulfapyridine, sulfamethoxazole, acetaminophen, caffeine and erythromycin were quantified in the analysed samples.

Avaliação da remoção de fármacos e de desreguladores endócrinos em águas de abastecimento por clarificação em escala de bancada

In this work, the efficiency of clarification treatment (coagulation, flocculation and sedimentation) with polyaluminum chloride (PAC) and aluminum sulfate (SA) as coagulants was evaluated in the removal of 7 microcontaminants (diclofenac - DCF, sulfamethoxazole - SMX, ethinylestradiol - EE2, bisphenol-A - BPA, estradiol - E2, estrone - E1 and estriol - E3) in water of low and high turbidity. The clarification treatment led to poor removal rates (40% at most) for all microcontaminants except SMX which exhibited intermediate removal efficiency (67 to 70%). Overall, PAC application yielded better performance compared to SA.

APLICAÇÃO DE ÓXIDOS DE FERRO NANOESTRUTURADOS COMO ADSORVENTES E FOTOCATALISADORES NA REMOÇÃO DE POLUENTES DE ÁGUAS RESIDUAIS

New techniques for treating wastewater, particularly the removal or degradation of organic pollutants and heavy metals, among other pollutants, have been extensively studied. The use of nanostructured iron oxides as adsorbent and photocatalyst for the removal of these contaminants has proved a promising approach, not only because of their high treatment efficiency, but also for their cost-effectiveness, having the flexibility for in situ and ex situ applications. In this review, we briefly introduced the most used kinds of iron oxide nanoparticles, some synthesis techniques for iron oxide nanostructure formation, their potential benefits in environmental clean-up, and their recent advances and applications in wastewater treatment. These advances range from the direct applications of synthesized nanoparticles as adsorbents for removing toxic contaminants or as catalysts to oxidize and break down noxious contaminants (including bacteria and viruses) in wastewater, to integrating nanoparticles into conventional treatment technologies, such as composite photocatalytic filters (membranes, sand and ceramic) that combine separation technology with photocatalytic activity. Finally, the impact of nanoparticles on the environment and human health is briefly discussed.

VALIDAÇÃO INTRALABORATORIAL DA DETERMINAÇÃO DE METILTESTOSTERONA EM ÁGUAS NATURAIS POR VOLTAMETRIA USANDO ELETRODO DE GOTA PENDENTE DE MERCÚRIO

17α-methyltestosterone (17α-MT) is a hormone used in medicine and aquaculture which can be found in natural waters. It is considered an emerging organic pollutant and its accurate and precise analysis is required. Therefore, this study presents the in-house validation of a new voltammetric methodology for 17α-MT analysis in natural waters. A hanging mercury drop electrode and NaOH 5.0×10-3 mol L-1 solution as the electrolyte were employed in the voltammetric determinations. To confirm the presence of 17α-MT in water samples quantitative analysis was performed by ESI-MS/MS. The methodology exhibited good selectivity, linearity, accuracy (recovery of between 100.4 and 108.8%) and precision (RSDs for repeatability of 2.85% and for intermediate precision of 14.10%, with n = 5, respectively). LOD and LOQ were 3.07 µg L-1 and 10.78 µg L-1, respectively. The methodology was suitable for determination of 17α-MT in natural waters due to low-cost, good performance and no sample pre-treatment required.

Pequisas físicas e químicas do sistema hidrográfico da região lagunar de Cananéia: I - Cursos de águas

The present elaboration is a "previous note" about two watercourses, Maria Rodrigues and Baguaçú, belonging to Hydrografic System of the Cananeas Lagoon Region in the Southern Part of it he Coast of the Estado de São Paulo, Brazil, which is the objete of our physical and chemical researches. It is based on the first results obtained from our contact with that region, ttfie studies of which are being continued and will still have to confirm or not the previous conclusions, which we are presenting in this "provisional paper". We studied the Maria Rodrigues and the Baguacu under the discussion whether they are to be clasified as a river in the poper sense ot the word or waUer-courses of any other origin. For this purpose we established observatory-stations along their whole course where we collected quantities of water to be analised. The data included in the table nº 1 and 2 refer to the physical and chemical properties of these portions of water. These physical and chemical properties were discussed and compared one with the other according to the observatory-stations, at the same moment and the tide predominating on that occasion. The physical and chemical datas were obtained according to the norms recommended by the Conseil International permanent pour l'Exploration de la Mer, Copenhague. We also presented a sketch of both; we described their relations with regard to the Mar de Cananéia; we inserted comprehensible histograms of the distribution of the observatory-stations, each of them with the respective indices, and at last we tried to correlate the occurrence of the "plancton" with the physical and chemical properties of water as well in the Maria Rodrigues as in the Baguacú. From these researches result the following previous conclusions: 1 - By the data obtained up to now nothing could be formulated as to a cyclical or "seasonal" aspect. 2 - By the comparison of the phenomena which present the rivers in the proper sense of the word and those observed in the Maria Rodrigues and the Baguacú, we are convinced that both are water-courses of the classical type "marigot,". 3 - Their channels are maintained open by the effect of the tide and, more perphaps, by the infiltration-water deriving from the underground-water level owing to the type of the soil of that region, which in mean shows an elevation of 2-4 meters over sea-level. 4 - From tables 1 and 2 and histograms 2 and 3 we stated that the water, not only of the Maria Rodrigues but also of the Baguacú, conserve more or less the same physical and chemical properties, provided that: 1) the localities to be compared are the mouths or equidistant points from them in the lower course, and 2) the moment and tide must be the same. Tables 3a and 3b show sufficiently this supposition.

Ocorrência de Pseudocycnus appendiculatus Heller: Copépodo da família Pseudocycnidae, em águas do litoral paulista

During April 9 to 15, 1949, some parasitic copepods have been caught at the northern seashore region of São Paulo State (Brazil), in the Channel of São Sebastião. All copepods belong to the family Pseudocycnidae and to the species Pseudocycnus appendiculatus Heller. The animals were found in the gills of Gymnosarda alleterata (Rafinesque). This paper deals with the geographical distribution of the species, for the first time captured in brazilian waters.

Resultados científicos do cruzeiro do Baependi e do Vega à Ilha da Trindade: oceanografia física - contribuição para o conhecimento das características físicas e químicas das águas

In May 1950 a trip was undertaken by the ships "Baependi" and "Vega" to the Trindade Island - 20º30'S and 29º20'W - Approximately 1200 km off the coast of Espirito Santo State. This scientific expedition was realized by the iniciative of the Minister J. A. Lins de Barros. In this expedition the supervisor of the oceanographic works was Prof. W. Besnard, the director of the São Paulo Oceanographic Institute. He brougth home 42 samples of water for study, collected upon the insular terrace of the island, referring to the 15 established stations - see table I - with depths varying between 0 m and 115 m. The physical and chemical properties of them are to be seen on table II. The results obtained were compared with those of the German Expedition to the South Atlantic, 1925/27 ("Meteor"), observed at the stations 157-158-159-163 of profile VI and 168-169-170 of profile VII. The mean results obtaneid by the boats "Baependi" and "Vega" are represented on table IV. We constructed vertical sections - I to VI - of each group of Stations, showing the slope of the insular shelves and, in a general manner, the distribution of salinity. We made also longitudinal section - E, M, I - involving the island and corresponding, respectively, to the groups of stations, the farthest, nearest and intermediary ones. As the number of samples received is reduced and consequently the data obtained are few, no conclusions could be deduced. We made only a commentary supposing that the predominating waters surrounding the island are the same as those coming from the mentioned stations on Profile VI, marked by the "Meteor". No indication authorizes the supposition that waters of the Brazil Current or those of Profile VII of the "Meteor" reach the Trindade Island. On the contrary, its waters must be warm and salted to which Albert Defant (Die Troposphaere, Wiss. Erg. D. Atl. Exp. "Meteor" Band VI, 1 Tel Lief. 3, Berlin, 1936) has referred, as the island is located very near to the limits of the perspective diagram of warm water circulation pointed out. (Kieler Meeresforschungen, Inst. Meereskunde, Universit. Kiel, Band VII, Heft 1, S 24, 1950).

Contribuição da cidade de Botucatu - SP com nutrientes (fósforo e nitrogênio) na eutrofização da represa de Barra Bonita

As concentrações de nutrientes (fósforo e nitrogênio) na nascente, cidade e foz do ribeirão Lavapés/ Botucatu-SP foram avaliadas e comparadas com as do rio Capivara. O rio Capivara como o ribeirão Lavapés, possui nascente no alto da cuesta e desemboca suas águas na represa de Barra Bonita/ rio Tietê (Figura 1). O rio Capivara possui uma das nascentes próxima a uma do ribeirão Lavapés e, ambos possuem a foz próxima uma da outra na represa de Barra Bonita. O uso e tipo de solo nas margens de ambos cursos d´águas são bastante parecidos, o que implica em uma poluição rural semelhante, assim a grande diferença que afeta a qualidade da água, entre os dois cursos d´águas é a poluição urbana, na cidade de Botucatu (ribeirão Lavapés). Deste modo procurou-se avaliar a contribuição de nutrientes (fósforo e nitrogênio) do ribeirão Lavapés e rio Capivara na represa de Barra Bonita , e estimar a carga retida no lodo do ribeirão Lavapés e a despejada na represa em função dos lançamentos de esgotos sanitários no mesmo, na cidade de Botucatu. O trabalho foi realizado em um período de seca, sem alagamentos, o que permitiu medir as vazões próximas da foz e avaliar a carga diária, no período, de nutrientes lançados na represa. Foram avaliados também, oxigênio dissolvido, demanda química do oxigênio e condutividade Elétrica. Embora os resultados sejam estimativos e variáveis no tempo, podemos concluir que a poluição na cidade de Botucatu por esgoto sanitário além de inviabilizar o uso da água no seu percurso, e causar outros prejuízos, contribui para agravar a eutrofização na represa de Barra Bonita.

Oxigênio dissolvido (OD), demanda bioquímica de oxigênio (DBO) e demanda química de oxigênio (DQO) como parâmetros de poluição no ribeirão Lavapés/Botucatu - SP

Oxigênio dissolvido (OD), demanda bioquímica do oxigênio (DBO) e demanda química do oxigênio (DQO) foram utilizados como parâmetros para se avaliar o grau e capacidade de autodepuração do ribeirão Lavapés, que atravessa a cidade de Botucatu - SP. Avaliou-se o perfil de poluição orgânica e identificadas as zonas de autodepuração, e pontualmente foi realizado uma coleta de 24 horas, de hora em hora, onde foi possível correlacionar a poluição orgânica com as atividades domésticas. A DQO mostrou-se como a melhor técnica para avaliar o perfil de poluição orgânica, identificar as zonas de depuração, e para avaliar a poluição orgânica, neste curso d’água. A relação DQO/DBO foi em média 3,4 caracterizando um esgoto biodegradável, indicando que praticamente não existe adição de efluentes industriais, permitindo assim estimar a DBO através da DQO. Nos trechos de água limpa, nascente e foz, em que a DQO estava abaixo de 5 mg L-1 O2, foram utilizados os valores de oxigênio consumido (método do permanganato), o que não invalidou a identificação das zonas de depuração. No entanto pesquisas para desenvolver o método de DQO (dicromato) para baixas concentrações, abaixo de 5 mg L-1 são necessárias para uma melhor avaliação da recuperação do curso d’água.

Determinação da demanda química de oxigênio em águas por espectrofotometria simultânea dos íons crômio(III) e dicromato

Propõe-se metodologia analítica para a determinação da demanda química de oxigênio(DQO) em águas e efluentes pouco poluídos, pela espectrofotometria simultânea dos íons crômio(III) e dicromato, após a clássica oxidação sulfocrômica das amostras, à quente e catalisada por íons Ag+. Demonstra-se que a inter-relação entre as concentrações de DQO, de crômio(III) formado e de dicromato residual permite simplificar a resolução numérica do sistema - de multicomponente, envolvendo as concentrações desses dois íons, e medidas de absorbância em pelo menos dois comprimentos de onda para monocomponente, envolvendo diretamente a concentração em DQO, e medida de absorbância num único comprimento de onda.