The geology and mining industries rely heavily on reliable quantitative data on the elemental composition of various rocks and minerals. The analytical accuracy of the best measurement systems are, however, limited to the accuracy with which the composition of a generally accepted reference sample is known, which serves to calibrate an instrument or validate a method. Thus, there is an established market for well-characterised reference materials which trade internationally as value added commodities. International organisations prepare strict procedures for the preparation and certification of these reference materials. ISO/REMCO is the ISO Committee on Reference Materials that carries out and encourages a broad international effort for the harmonisation and promotion of reference materials, their production and their application. In view of recent developments in ISO/REMCO related to updated guides and changes in definitions, SARM 1 to 6 (the NIMROCs) are in danger of losing their status as certified reference materials (CRMs). Due to the continued popularity of the NIMROCs and the availability of bulk sample, the National Metrology Institute of South Africa (NMISA) embarked on a project to re-certify three materials from the suite of six igneous rock samples, i.e. SARM 2 (Syenite), SARM 3 (Lujavrite) and SARM 4 (Norite). The aim of the re-certification project was to re-certify the materials with a single primary reference measurement procedure in a single laboratory to comply with one of the possible routes to the establishment of metrological traceability as described in ISO Guide 34. Eight elements (Ba, Sr, Cd, Mo, Cu, Ni, Pb and Zn) of SARM 2, SARM 3 and SARM 4 were value assigned during this study to ensure that they comply with the ISO Guide 30 and ISO GUM requirements for traceability and measurement uncertainty. Traceability to the SI units of mass and amount of substance at the highest level of accuracy was established by employing the definitive technique of double isotope dilution ICP-MS, with primary assay standards traceable to the NIST SRM 3100 series and gravimetrically prepared samples. For the first time assigned values with uncertainty statements for these elements in these reference materials were calculated according to the ISO GUM and CITAC/EURACHEM guidelines for expression of the uncertainty of measurement. The uncertainties of the assigned values for all elements were within the target of 5% relative set during the development of the methodology, except for elements in concentrations below 10 mg.kg-1. The ID-ICP-MS results are supported by good comparability with results reported in the literature since 1978, as well as the original certified values published in 1978. The results from this study for all elements in these reference materials have the potential to become new certified values in accordance with the requirements of ISO Guides 34 and 35. This will improve the usefulness of these reference materials to the South African and international geology and mining communities for the purposes of analytical quality control and method validation in exploration and geochemical analysis. Confirmation of the homogeneity and stability of the remaining units of the reference materials is considered necessary to complete the re-certification project. / Thesis (PhD)--University of Pretoria, 2010. / Chemistry / unrestricted

Fish meals (FM) and fish oils (FO) are used extensively as the main protein and lipid sources respectively in industrially compounded salmon feeds, mainly due to their excellent nutritional properties. Nevertheless, several reasons dictate the utilisation of sustainable alternative protein and lipid sources and the subsequent reduction in the reliance on fishery-products in aquafeeds. Soy protein concentrate (SPC) is a very promising alternative to FM Hence, the main objective of the present thesis was to investigate the effects of the increased substitution of FM withSPC, lysine and methionine on the growth performance and immune responses of early and late stage Atlantic salmon parr prior to and after vaccination with commercial vaccines (Experiments II and V presented in Chapters 4 and 6). Furthermore the effects of increasing dietary levels of SPC with consistent and/or increasing dietary supplementation of phosphorus on the Atlantic salmon parr’ body proximate and mineral composition or the skeletal mineral composition respectively, prior and post-vaccination with commercial vaccines; under continuous light or under 12 hours light: 12 hours dark photoperiod (Experiments I and V presented in Chapters 3 and 5 respectively). Lastly the impact of FM-, FO- and fishery-free diets on the growth, carcass proximate composition and immune status of Atlantic salmon post-smolts was investigated (Experiment III presented in Chapter 7). In the latter experiment six diets were tested including: two commercially applied marine based diets, one with partial inclusion of vegetable proteins (VPs) and oils (VOs) according to the EU standards (2011-12) (MBE) and one with partial inclusion of VPs, VOs and land animal-by product (ABP) proteins according to the non-EU standards (MBABP); a fully vegetable protein (VP) diet; a fully algal and vegetable oil (VO) diet; a marine-free VP and VO and algal oil diet (VP/VO) diet; and a marine-free diet with a mix of VPs and land ABP proteins and lipid from VOs and algal oils (MFABP). The results of the Experiments I and II (Chapters 3 and 4) show that late Atlantic salmon parr can grow efficiently on SPC80 diets, however, they require longer periods to adapt to these diets compared to fish fed diets containing lower levels of SPC as a protein source. Decreased mineralisation of body cross-section was observed for salmon fed increasing dietary SPC. Vaccination improved mineralisation for the high dietary SPC salmon groups. However, continuous light exposure promoting fast growth appeared to be detrimental for Atlantic salmon body cross ash, Ca, Mg, Mn, P and Zn. Moreover, it was demonstrated that substitution of up to 50% of high quality FM protein with SPC and constantly added P has the minimum possible impact on late salmon parr growth, whereas it stimulates several immune parameters prior to immunisation. Immunostimulatory effects were also shown for the diets with higher dietary SPC levels. It is not clear if these results were an effect of increased FM replacement with SPC or not properly balanced levels of dietary P. The Experiments III and IV (Chapters 5 and 6) illustrated that early stage Atlantic salmon parr can accept diets with up to 58% protein from SPC without serious effects on body growth. However, higher levels can severely affect salmon growth performance. Moreover, it was shown that long-term feeding of salmon with increasing dietary SPC combined with increasing phosphate supplementation, alone or in combination with vaccination can actually be beneficial for Atlantic salmon parr bone mineralisation. However, mineralisation in vaccinated fish was higher than in PBS-injected fish. This could be linked to the slower growth of vaccinated salmon allowing their developing bones to mineralise properly. Changes in the modulation of the different components of the complement activity was revealed in Atlantic salmon fed increasing dietary levels of SPC. The modulation of complement activity was demonstrated at both studies utilising increasing dietary SPC concentrations, indicating that complement componenets are among the most prominent immunological markers upon dietary FM replacement with SPC. However, overall no differences in total complement activity and therefore the immune capacity and resistance against Aeromonas salmonicida were observed among the salmon groups receiving increasing levels of SPC. Lastly in Experiment V (Chapter 7) higher growth performance indices (weight gain, SGR and TGC) were evident in the MBE salmon compared to the MBABP group, salmon fed diets with complete eleimintion of FM or FO (VP and VO respectively) and fish fed two diets with total substitution of both marine derived feed ingredients, three months after the start of the feeding trial. Higher feed intake was demonstrated for both MBE and VP salmon compared to the other groups for the duration of the first period. The above results could have been influenced by discrepancies in the size of the fish at the start ofthe trial, revealing flaws in the experimental design. Both MBE and VP salmon groups also presented the highest feed conversion ratios, revealing the lowest efficiency in dietary nutrient utilisation in comparison to the rest of salmon which exhibited no differences in feed efficiency, revealing an overall better performance of the MBABP and diets with low levels of marine feedstuffs. Improved FI compared to the values of the first period and higher SGR and TGC values were demonstrated for salmon from the latter treatments compared to MBE and VP salmon, during the second part of the study, revealing compensatory growth for these groups. VP salmon demonstrated the highest and VO salmon the lowest condition factor values. The former finding might possibly be related with higher fat accumulation in the viscero-hepatic tissues. No differences were observed in carcass moisture, protein, fat and ash concentrations among the dietary groups of fish. Furthermore, no differences were demonstrated in terms of total and differential leucocyte counts, plasma haemolytic activity, plasma protein and total IgM levels, stimulated and non-stimulated HKM burst activity among the different dietary groups. However, lower haematocrit values were observed in the MB and VO-fed groups compared to the MFABP and VP/VO groups. Furthermore, decreased lysozyme activity was observed for all diets in contrast to the control groups, whereas FM-free diets promoted plasma anti-protease activity. The former result could have been an effect of either immune or stress induction, whereas the second is regarded as an immunostimulatory effect. The results suggest that marine-oil, marine-protein and marine-free diets could be satisfactorily used for Atlantic salmon post-smolts without severe reductions in their innate immune responses, although longer adaptation periods might be required for the fish to fully accept these diets.

Neste trabalho foi feita uma caracterização do material particulado coletado no Centro de Capacitação e Pesquisa em Meio Ambiente (CEPEMA) localizado na cidade de Cubatão, na Baixada Santista. As coletas ocorreram entre março de 2009 e novembro de 2010, utilizando amostradores de material particulado fino, grosso e inalável (Mini-Vol) e um impactador em cascata (MOUDI) para as várias frações do material particulado, durante oito campanhas experimentais. Foi realizada uma caracterização climatológica com os dados de temperatura, pressão atmosférica, umidade relativa, velocidade e direção do vento das estações da CETESB em Cubatão: Centro (10 anos), Vila Parisi (10 anos) e Vale do Mogi (4 anos). Os dados de chuva foram obtidos da Defesa Civil para a cidade de Santos. A maior parte das coletas de 2009 ocorreu em períodos em que houve precipitação, ao passo que as coletas de 2010 foram amostradas em períodos mais secos. O material particulado fino (MPF) teve concentrações médias de: 15,7 e 18,8 g m-3 em 2009 e 2010, respectivamente, quando coletado pelo MOUDI; e 15,8 e 23,6 g m-3, quando coletado pelo Mini-Vol. O material particulado grosso (MPG) teve concentrações médias de: 11,4 e 14,1 g m-3 em 2009 e 2010, respectivamente, quando coletado pelo MOUDI; e 18,9 e 13,4 g m-3, quando coletado pelo Mini-Vol. As análises de refletância mostraram que o Black Carbon está quase totalmente no MPF, chegando a 15% (20%) da massa do MPF quando coletado pelo MOUDI (Mini-Vol). Os íons dominantes são sulfato (SO42), nitrato (NO3), sódio (Na+), amônio (NH4+) e cálcio (Ca2+) e os elementos dominantes são enxofre (S), silício (Si) e ferro (Fe). As distribuições de tamanho mostram uma moda de nucleação bastante pronunciada para o S, K, Cl e P, indicando a contribuição de fontes antropogênicas e formação secundária do aerossol. As maiores concentrações de Si, Cl, Ca, Fe, Ca2+, NO3 e Na+ se encontram no MPG. Para o Cl e Na+, foram encontradas maiores concentrações nas amostras diurnas com vento do quadrante sul-sudoeste na estação do Centro, demonstrando a contribuição marinha. / This work evaluated the particulate matter (PM) collected at the Environmental Research and Training Center (CEPEMA) located in Cubatão City. Sampling was made between 2009, March and 2010, November for fine, coarse and inhalable aerosol (Mini-Vol) and for the various fractions of PM with a cascade impactor (MOUDI) during eight experimental campaigns. A climatological study was performed for temperature, pressure, relative humidity, wind speed and direction using data from CETESB stations: Centro (10 years), Vila Parisi (10 years) and Vale do Mogi (4 years). Precipitation data was obtained from the Civil Defense for the city of Santos. Most samplings made during 2009 were concomitant with rainy days, whereas 2010 samplings were made in drier periods. Fine particulate matter (FPM) had average concentrations of: 15.7 and 18.8 g m-3 in 2009 and 2010, respectively, with MOUDI and 15.8 and 23.6 g m-3, with Mini-Vol. Coarse Particulate Matter (CPM) had average concentrations of: 11.4 and 14.1 g m-3 in 2009 and 2010, respectively, with MOUDI, and 18.9 and 13.4 g m-3, with Mini-Vol. Reflectance analysis showed that the Black Carbon is almost completely in the FPM, reaching up to 15 % (20 %) of the FPM mass when sampled with MOUDI (Mini-Vol). Dominant ions are sulfate (SO42-), nitrate (NO3-), sodium (Na+), ammonium (NH4+) and calcium (Ca2+) and the dominant elements are sulfur (S), silicon (Si) and iron (Fe). The size distributions shows a very pronounced nucleation mode for the S, K, P and Cl, indicating the contribution of anthropogenic sources and secondary aerosol formation. The highest concentrations of Si, Cl, Ca, Fe, Ca2+, NO3- and Na+ are in CPM. For Cl- and Na+, major concentrations were found in samples with diurnal south-southwest wind indicating marine aerosol contribution.

O diabetes mellitus é uma doença que afeta o metabolismo de carboidratos, gorduras e proteínas e tem como aspectos característicos a hiperglicemia e a excreção da glicose pela urina. Estima-se que o número de casos da doença aumentará muito nos próximos anos, o que a torna preocupante para o sistema público de saúde dos países mais afetados. Além do uso de medicamentos alopáticos, tratamentos complementares como o uso de plantas medicinais pode contribuir para melhorar a qualidade de vida do paciente. Entre as ervas utilizadas, tanto no Brasil quanto em outras partes do mundo, encontram-se Bidens pilosa e Salvia officinalis. Os mecanismos responsáveis pela atividade antidiabética das plantas, geralmente estão associados aos seus metabólitos secundários, no entanto, a influência de micronutrientes não deve ser descartada. Estudos mostram que há uma correlação entre a concentração destes elementos com a presença e o desenvolvimento da doença. O objetivo deste trabalho foi estudar os elementos Cr, Fe, Mg, Mn, V e Zn em Bidens pilosa (picão) e Salvia officinalis (sálvia) cultivadas com tratamento normal (substrato comercial) e com adição dos elementos acima mencionados, e verificar a influência destes elementos na produção de metabólitos secundários que podem atuar como agentes hipoglicêmicos. A determinação e quantificação elementar foram feitas por meio da técnica de Análise por Ativação Neutrônica Instrumental, e para análise dos metabólitos secundários utilizou-se a técnica de Cromatografia Líquida de Alta Eficiência. O resultados indicaram que B. pilosa e S. officinalis podem ser usadas como fontes de Cr, Fe Mg, Mn, V e Zn. Foi observado que a B. pilosa absorveu maior quantidade de Fe no grupo tratamento, e que a S. officinalis foi capaz de acumular Zn nas folhas independente de ter ou não sido tratada. Quanto aos compostos do metabolismo secundário, os resultados indicaram que sua produção pelas plantas aparentemente não foi alterada pela adição da solução dos nutrientes. / Diabetes mellitus is a disease that affects the carbohydrates, lipids and proteins metabolism characterized by hyperglycemia and glucose excretion by urine. It is estimated that the number of cases of this disease will increase in the coming years, worrying the public health system of the most affected countries. Besides the use of allopathic medicine, complementary treatments such as the use of medicinal plants can contribute to improving the pacients quality of life. Among the herbs used, both in Brazil and in other countries, are Bidens pilosa and Salvia officinalis. The mechanisms responsible for antidiabetic activity of the plants, are usually associated with secondary metabolites, however, the influence of micronutrient content should not be discarded. Studies have shown that there is a correlation between the concentration of these elements and the presence and development of the disease. The objective of this work was to study the elements Cr, Fe, Mg, Mn, V and Zn concentration in Bidens pilosa (beggarticks) and Salvia officinalis (sage) cultivated with normal treatment (commercial substrate) and, with the addition of these elements, to verify their influence in the production of secondary metabolites that can act as hypoglycemic agents. The elemental determination and quantification were performed by means of Instrumental Neutron Activation Analysis technique. For the secondary metabolites analysis Liquid Chromatography High Performance technique was used. The results indicated that B. pilosa and S. officinalis may be used as sources of Cr, Fe, Mg, Mn, V and Zn. It was observed that B. pilosa absorbed a larger amount of Fe in the treatment group, and S. officinalis was able to accumulate Zn its in leaves whether treated or not. Considering the secondary metabolism compounds, the results indicated that its production by plants was apparently not altered by the addition of the nutrient solution.

O diabetes mellitus é uma doença que afeta o metabolismo de carboidratos, gorduras e proteínas e tem como aspectos característicos a hiperglicemia e a excreção da glicose pela urina. Estima-se que o número de casos da doença aumentará muito nos próximos anos, o que a torna preocupante para o sistema público de saúde dos países mais afetados. Além do uso de medicamentos alopáticos, tratamentos complementares como o uso de plantas medicinais pode contribuir para melhorar a qualidade de vida do paciente. Entre as ervas utilizadas, tanto no Brasil quanto em outras partes do mundo, encontram-se Bidens pilosa e Salvia officinalis. Os mecanismos responsáveis pela atividade antidiabética das plantas, geralmente estão associados aos seus metabólitos secundários, no entanto, a influência de micronutrientes não deve ser descartada. Estudos mostram que há uma correlação entre a concentração destes elementos com a presença e o desenvolvimento da doença. O objetivo deste trabalho foi estudar os elementos Cr, Fe, Mg, Mn, V e Zn em Bidens pilosa (picão) e Salvia officinalis (sálvia) cultivadas com tratamento normal (substrato comercial) e com adição dos elementos acima mencionados, e verificar a influência destes elementos na produção de metabólitos secundários que podem atuar como agentes hipoglicêmicos. A determinação e quantificação elementar foram feitas por meio da técnica de Análise por Ativação Neutrônica Instrumental, e para análise dos metabólitos secundários utilizou-se a técnica de Cromatografia Líquida de Alta Eficiência. O resultados indicaram que B. pilosa e S. officinalis podem ser usadas como fontes de Cr, Fe Mg, Mn, V e Zn. Foi observado que a B. pilosa absorveu maior quantidade de Fe no grupo tratamento, e que a S. officinalis foi capaz de acumular Zn nas folhas independente de ter ou não sido tratada. Quanto aos compostos do metabolismo secundário, os resultados indicaram que sua produção pelas plantas aparentemente não foi alterada pela adição da solução dos nutrientes. / Diabetes mellitus is a disease that affects the carbohydrates, lipids and proteins metabolism characterized by hyperglycemia and glucose excretion by urine. It is estimated that the number of cases of this disease will increase in the coming years, worrying the public health system of the most affected countries. Besides the use of allopathic medicine, complementary treatments such as the use of medicinal plants can contribute to improving the pacients quality of life. Among the herbs used, both in Brazil and in other countries, are Bidens pilosa and Salvia officinalis. The mechanisms responsible for antidiabetic activity of the plants, are usually associated with secondary metabolites, however, the influence of micronutrient content should not be discarded. Studies have shown that there is a correlation between the concentration of these elements and the presence and development of the disease. The objective of this work was to study the elements Cr, Fe, Mg, Mn, V and Zn concentration in Bidens pilosa (beggarticks) and Salvia officinalis (sage) cultivated with normal treatment (commercial substrate) and, with the addition of these elements, to verify their influence in the production of secondary metabolites that can act as hypoglycemic agents. The elemental determination and quantification were performed by means of Instrumental Neutron Activation Analysis technique. For the secondary metabolites analysis Liquid Chromatography High Performance technique was used. The results indicated that B. pilosa and S. officinalis may be used as sources of Cr, Fe, Mg, Mn, V and Zn. It was observed that B. pilosa absorbed a larger amount of Fe in the treatment group, and S. officinalis was able to accumulate Zn its in leaves whether treated or not. Considering the secondary metabolism compounds, the results indicated that its production by plants was apparently not altered by the addition of the nutrient solution.

Orientador: Mary Rosa Rodrigues de Marchi / Banca: Christine Laure Marie Bourote / Banca: Annibal Duarte Pereira Netto / Banca: Nilva Ré Poppi / Banca: Roma Tauler / Resumo: No Brasil, a queima da cana de açúcar é utilizada para facilitar a colheita, mas este procedimento causa grande poluição ambiental devido a quantidade de fuligem lançada na atmosfera. O material particulado (MP) emitido contém inúmeros contaminantes, tais como: hidrocarbonetos policíclicos aromáticos (HPAs) e elementos. A cidade de Araraquara/SP possui cerca de 200.000 habitantes e é cercada por plantações de cana de açúcar, sendo que a prática de queimada é constante no período da safra (abril-novembro, todos os anos). Neste trabalho, determinou-se a concentração elementar e de HPAs em MP na cidade de Araraquara durante o período da safra (S) e da entre safra (E) da cana de açúcar. Foram coletadas 60 amostras (E) e 220 amostras (S) para a análise de HPAs, e 10 amostras (E) e 10 amostras (S) para a análise elementar. As amostras foram coletadas utilizando um amostrador dicotômico (vazão: 10 L min-1, 24 h) com filtros de PTFE (37 mm, 2 μm de tamanho de poro). Para a análise de HPAs, dez filtros de PTFE contendo o MP foram extraídos em banho de ultrassom com acetona/n-hexano (1:1 v/v), sendo que as análises foram efetuadas por HPLC/FLD. A análise elementar foi efetuada por fluorescência de raios X por energia dispersiva (EDXRF), sem tratamento prévio das amostras. A concentração mediana de HPAs totais foi de 1,9 ng m-3 (E) e 6,2 ng m-3 (S). A concentração mediana de benzo[a]pireno, HPA considerado carcinogênico, foi de 0,026 ng m-3 e 0,15 ng m-3 para os períodos de E e S, respectivamente. O risco potencial de câncer associado à exposição a HPAs por inalação, foi estimado com base na concentração de benzo[a]pireno equivalente (BaPeq), onde a toxicidade de uma mistura de HPAs é definida pela concentração de cada substância multiplicada pelo seu fator de equivalência de toxicidade relativa (FET). Os valores medianos encontrados para... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: In Brazil, the sugar cane crops are burned to facilitate the harvesting, this procedure causes environmental pollution from the large amounts of soot that are released into the atmosphere. This particulate matter (MP) contains numerous contaminants such as polycyclic aromatic hydrocarbons (PAHs) and metals. The city of Araraquara, located at central area from São Paulo State, has around 200,000 inhabitants and is surrounded by sugarcane plantations (46,994 ha of total cultivated area, in the harvest 2008/2009). In this study, PAHs concentrations and elemental composition in the MP were determined in Araraquara city during the sugarcane harvesting (HV) and non-harvesting (NHV) seasons. 60 samples were collected during the NHV and 220 samples during the HV seasons for the analysis of PAHs. 10 samples were collected during the NHV and 10 samples during the HV season for the analysis of Si, K, Ca, Ti, V, Fe, Sr, Cr, Ni, Mn, Cu, Zn, As, Cd, Pb, Sb, Al, S and Cl. The samples were collected using a dichotomous sampler (10 L min-1, 24 h) with PTFE filters. Ten filters sets were extracted (ultrasonic bath with hexane/acetone (1:1 v/v)) and analyzed by HPLC/FLD for the analysis of PAHs. Information concerning the bulk elemental concentration was provided by energy-dispersive x-ray fluorescence (EDXRF). The median concentration for total PAHs was 1.9 ng m-3 (NHV) and 6.2 ng m-3 (HV). Benzo[a]pyrene median concentration was 0.026 ng m-3 and 0.15 ng m-3 for the NHV and HV seasons, respectively. The potential cancer risk associated to inhalation exposure was estimated based on the benzo[a]pyrene toxic equivalence (BaPeq), where the overall toxicity of a PAH mixture is defined by the concentration of each compound multiplied... (Complete abstract click electronic access below) / Doutor

Submitted by Ana Hilda Fonseca (anahilda@ufba.br) on 2014-10-27T17:17:05Z No. of bitstreams: 1 ElecyTese corrigida 30 07 14.pdf: 1118101 bytes, checksum: fcfaf3d2c9511c09fdcaefb24555ec74 (MD5) / Approved for entry into archive by Ana Hilda Fonseca (anahilda@ufba.br) on 2014-10-29T15:53:07Z (GMT) No. of bitstreams: 1 ElecyTese corrigida 30 07 14.pdf: 1118101 bytes, checksum: fcfaf3d2c9511c09fdcaefb24555ec74 (MD5) / Made available in DSpace on 2014-10-29T15:53:08Z (GMT). No. of bitstreams: 1 ElecyTese corrigida 30 07 14.pdf: 1118101 bytes, checksum: fcfaf3d2c9511c09fdcaefb24555ec74 (MD5) / FAPESB / A mandioca ( Manihot esculenta Crantz) é uma plan ta de origem da América do Sul, tendo como produto principal a farinha de mandioca, que é um alimento rico em carboidratos, fibras, proteína, Ca, P, Na, K e Fe , entre outros. A prod ução de farinha corresponde a 22 % da produção nacional de mandioca e é pro duzida por pequenos produtores. Sendo assim, é oportuno o desenvolvimento de estudos que visam à caracterização da farinha de mandioca quanto à sua composição para se ter um controle de qualidade adequado para consumo. O objetivo deste trabalho foi propor estratégias para a caracterização da farinha de mandioca produzida no E stado da Bahia em função das concentrações de Al, As, Ba, Br, Ca, Cd, Cl, Cu, Fe, I, K, Mg, Mn, Na, Ni, P, Pb e Zn. Em uma primeira etapa foram comparados três procedimentos para o prep aro das amostras : (1) por via úmida com aquecimen to condutivo em bloco digestor, (2) assistido por radiação micro - ondas e (3) por via seca. Os elementos foram determinados por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Fo i recomendado o procedimento assistido por radiação micro - ondas para determinação da composição elementar nas 24 amostras de farinha de mandioca adquiridas em diferentes localidades do estado da Bahia devido a sua maior eficiência e menor possibilidade de contaminação. Na segunda etapa foi proposto um procedimento para determinação de As, Pb, Cd e Se empregando espectrometria de absorção atômica com atomização eletrotérmica e detecção simultânea, utilizando a mistura de W e Rh como modificador. Foi possível determinar Pb e Cd em todas as amostras e os resultados obtidos indicaram para concentrações abaixo dos limites estabelecidos pela legislação. Na etapa final foram desenvolvidos estudos preliminares para a determinação de Cl, Br e I por ICP OES. / Cassava (Manihot esculenta Crantz) is a plant of South America, with the main product of cassava flour, which is a food rich in carbohyd rates, fiber, protein, Ca, P, Na, K and Fe. The production flour corresponds 22.1% of national production of cassava and is produced by small producers. Thus, it is desirable to develop studies aimed at characterization of cassava flour in their compositio n to have a quality control suitable for consumption. The objective of this study was to propose strategies for the characterization of cassava flour produced in the state of Bahia in the concentrations of Al, As, Ba, Br, Ca, Cd, Cl, Cu, Fe, I, K, Mg, Mn,N a, Ni, P, Pb and Zn. In a first step we compared three procedures for the preparation: (1) procedures using acids with heat conductive in block digester and (2) assisted by microwave and (3) procedure by calcination. The elements were determined by optical emission spectrometry with inductively coupled plasma (ICP OES). It was recommended the procedure assisted by microwave radiation to determine the elemental composition in 24 samples of cassava flour acquired in different localities of Bahia state conside ring its greater efficiency and less chance of contamination. In the second step was proposed a procedure for determination of As, Pb, Cd and Se using atomic absorption spectrometry with electrothermal atomization and simultaneous detection using a mixture of Rh and W as chemistry modifier. Lead was determined in all samples and the results indicated concentrations below the limits established by law. In the final stage preliminary studies have been developed for the determination of Cl, Br and I by ICP OES . Further studies should be developed to a greater number of samples in order to establish a more complete profile and contribute to the Table of Food Composition at the regional level

Neste trabalho foi feita uma caracterização do material particulado coletado no Centro de Capacitação e Pesquisa em Meio Ambiente (CEPEMA) localizado na cidade de Cubatão, na Baixada Santista. As coletas ocorreram entre março de 2009 e novembro de 2010, utilizando amostradores de material particulado fino, grosso e inalável (Mini-Vol) e um impactador em cascata (MOUDI) para as várias frações do material particulado, durante oito campanhas experimentais. Foi realizada uma caracterização climatológica com os dados de temperatura, pressão atmosférica, umidade relativa, velocidade e direção do vento das estações da CETESB em Cubatão: Centro (10 anos), Vila Parisi (10 anos) e Vale do Mogi (4 anos). Os dados de chuva foram obtidos da Defesa Civil para a cidade de Santos. A maior parte das coletas de 2009 ocorreu em períodos em que houve precipitação, ao passo que as coletas de 2010 foram amostradas em períodos mais secos. O material particulado fino (MPF) teve concentrações médias de: 15,7 e 18,8 g m-3 em 2009 e 2010, respectivamente, quando coletado pelo MOUDI; e 15,8 e 23,6 g m-3, quando coletado pelo Mini-Vol. O material particulado grosso (MPG) teve concentrações médias de: 11,4 e 14,1 g m-3 em 2009 e 2010, respectivamente, quando coletado pelo MOUDI; e 18,9 e 13,4 g m-3, quando coletado pelo Mini-Vol. As análises de refletância mostraram que o Black Carbon está quase totalmente no MPF, chegando a 15% (20%) da massa do MPF quando coletado pelo MOUDI (Mini-Vol). Os íons dominantes são sulfato (SO42), nitrato (NO3), sódio (Na+), amônio (NH4+) e cálcio (Ca2+) e os elementos dominantes são enxofre (S), silício (Si) e ferro (Fe). As distribuições de tamanho mostram uma moda de nucleação bastante pronunciada para o S, K, Cl e P, indicando a contribuição de fontes antropogênicas e formação secundária do aerossol. As maiores concentrações de Si, Cl, Ca, Fe, Ca2+, NO3 e Na+ se encontram no MPG. Para o Cl e Na+, foram encontradas maiores concentrações nas amostras diurnas com vento do quadrante sul-sudoeste na estação do Centro, demonstrando a contribuição marinha. / This work evaluated the particulate matter (PM) collected at the Environmental Research and Training Center (CEPEMA) located in Cubatão City. Sampling was made between 2009, March and 2010, November for fine, coarse and inhalable aerosol (Mini-Vol) and for the various fractions of PM with a cascade impactor (MOUDI) during eight experimental campaigns. A climatological study was performed for temperature, pressure, relative humidity, wind speed and direction using data from CETESB stations: Centro (10 years), Vila Parisi (10 years) and Vale do Mogi (4 years). Precipitation data was obtained from the Civil Defense for the city of Santos. Most samplings made during 2009 were concomitant with rainy days, whereas 2010 samplings were made in drier periods. Fine particulate matter (FPM) had average concentrations of: 15.7 and 18.8 g m-3 in 2009 and 2010, respectively, with MOUDI and 15.8 and 23.6 g m-3, with Mini-Vol. Coarse Particulate Matter (CPM) had average concentrations of: 11.4 and 14.1 g m-3 in 2009 and 2010, respectively, with MOUDI, and 18.9 and 13.4 g m-3, with Mini-Vol. Reflectance analysis showed that the Black Carbon is almost completely in the FPM, reaching up to 15 % (20 %) of the FPM mass when sampled with MOUDI (Mini-Vol). Dominant ions are sulfate (SO42-), nitrate (NO3-), sodium (Na+), ammonium (NH4+) and calcium (Ca2+) and the dominant elements are sulfur (S), silicon (Si) and iron (Fe). The size distributions shows a very pronounced nucleation mode for the S, K, P and Cl, indicating the contribution of anthropogenic sources and secondary aerosol formation. The highest concentrations of Si, Cl, Ca, Fe, Ca2+, NO3- and Na+ are in CPM. For Cl- and Na+, major concentrations were found in samples with diurnal south-southwest wind indicating marine aerosol contribution.

For years considered pristine, glacial ecosystems are attracting more attention of biologists from various branches in last decades. Moreover, they are currently considered to be ecosystems forming the coldest biome on the Earth. The life on glaciers ranges from viruses and bacteria to highest consumers such as few groups of microinvertebrates. The most common are tardigrades (phylum Tardigrada) and rotifers (phylum Rotifera) which inhabit cryoconite holes on the glacial surface. Several studies highlight the importance of the role of these consumers. However, due to the dominance of prokaryotes on the glacial surface, these microinvertebrates are usually out of the major scope of most studies aiming at biological processes. The present study shows pioneering results on the isotopic composition of tardigrades and rotifers, which are the top consumers in cryoconite ecosystems, and is a foundation for the exploration of trophic pathways and interactions within cryoconite holes using elemental and stable isotopic analyses. It also presents information about the species composition of tardigrades and rotifers on different glaciers and in different parts of the ablation zone. We identified 5 species of tardigrades (Hypsibius sp., Hypsibius cf. dujardini, Pilatobius sp., Isohypsibius sp. and Cryoconicus...

Made available in DSpace on 2014-06-11T19:35:06Z (GMT). No. of bitstreams: 0 Previous issue date: 2011-02-25Bitstream added on 2014-06-13T18:46:16Z : No. of bitstreams: 1 silva_fs_dr_araiq.pdf: 2849421 bytes, checksum: 9c4094e5d741a2f65f25f770fedc84be (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / No Brasil, a queima da cana de açúcar é utilizada para facilitar a colheita, mas este procedimento causa grande poluição ambiental devido a quantidade de fuligem lançada na atmosfera. O material particulado (MP) emitido contém inúmeros contaminantes, tais como: hidrocarbonetos policíclicos aromáticos (HPAs) e elementos. A cidade de Araraquara/SP possui cerca de 200.000 habitantes e é cercada por plantações de cana de açúcar, sendo que a prática de queimada é constante no período da safra (abril-novembro, todos os anos). Neste trabalho, determinou-se a concentração elementar e de HPAs em MP na cidade de Araraquara durante o período da safra (S) e da entre safra (E) da cana de açúcar. Foram coletadas 60 amostras (E) e 220 amostras (S) para a análise de HPAs, e 10 amostras (E) e 10 amostras (S) para a análise elementar. As amostras foram coletadas utilizando um amostrador dicotômico (vazão: 10 L min-1, 24 h) com filtros de PTFE (37 mm, 2 μm de tamanho de poro). Para a análise de HPAs, dez filtros de PTFE contendo o MP foram extraídos em banho de ultrassom com acetona/n-hexano (1:1 v/v), sendo que as análises foram efetuadas por HPLC/FLD. A análise elementar foi efetuada por fluorescência de raios X por energia dispersiva (EDXRF), sem tratamento prévio das amostras. A concentração mediana de HPAs totais foi de 1,9 ng m-3 (E) e 6,2 ng m-3 (S). A concentração mediana de benzo[a]pireno, HPA considerado carcinogênico, foi de 0,026 ng m-3 e 0,15 ng m-3 para os períodos de E e S, respectivamente. O risco potencial de câncer associado à exposição a HPAs por inalação, foi estimado com base na concentração de benzo[a]pireno equivalente (BaPeq), onde a toxicidade de uma mistura de HPAs é definida pela concentração de cada substância multiplicada pelo seu fator de equivalência de toxicidade relativa (FET). Os valores medianos encontrados para... / In Brazil, the sugar cane crops are burned to facilitate the harvesting, this procedure causes environmental pollution from the large amounts of soot that are released into the atmosphere. This particulate matter (MP) contains numerous contaminants such as polycyclic aromatic hydrocarbons (PAHs) and metals. The city of Araraquara, located at central area from São Paulo State, has around 200,000 inhabitants and is surrounded by sugarcane plantations (46,994 ha of total cultivated area, in the harvest 2008/2009). In this study, PAHs concentrations and elemental composition in the MP were determined in Araraquara city during the sugarcane harvesting (HV) and non-harvesting (NHV) seasons. 60 samples were collected during the NHV and 220 samples during the HV seasons for the analysis of PAHs. 10 samples were collected during the NHV and 10 samples during the HV season for the analysis of Si, K, Ca, Ti, V, Fe, Sr, Cr, Ni, Mn, Cu, Zn, As, Cd, Pb, Sb, Al, S and Cl. The samples were collected using a dichotomous sampler (10 L min-1, 24 h) with PTFE filters. Ten filters sets were extracted (ultrasonic bath with hexane/acetone (1:1 v/v)) and analyzed by HPLC/FLD for the analysis of PAHs. Information concerning the bulk elemental concentration was provided by energy-dispersive x-ray fluorescence (EDXRF). The median concentration for total PAHs was 1.9 ng m-3 (NHV) and 6.2 ng m-3 (HV). Benzo[a]pyrene median concentration was 0.026 ng m-3 and 0.15 ng m-3 for the NHV and HV seasons, respectively. The potential cancer risk associated to inhalation exposure was estimated based on the benzo[a]pyrene toxic equivalence (BaPeq), where the overall toxicity of a PAH mixture is defined by the concentration of each compound multiplied... (Complete abstract click electronic access below)