Influência da adição do NaCl e KCl em sistemas de pastas contendo sílica para poços de petróleo em zonas evaporíticas e carbonáticas

One of the major challenges faced nowadays by oil companies is the exploration of pre-salt basins. Thick salt layers were formed in remote ages as a consequence of the evaporation of sea water containing high concentrations of NaCl and KCl. Deep reservoirs can be found below salt formations that prevent the outflow of oil, thus improving the success in oil prospection. The slurries used in the cement operations of salt layers must be adequate to the properties of those specific formations. At the same time, their resulting properties are highly affected by the contamination of salt in the fresh state. It is t herefore important to address the effects of the presence of salt in the cement slurries in order to assure that the well sheath is able to fulfill its main role to provide zonal isolation and mechanical stability. In this scenario, the objective of the present thesis work was to evaluate the effect of the presence of NaCl and KCl premixed with cement and 40% silica flour on the behavior of cement slurries. Their effect in the presence of CO2 was also investigated. The rheological behavior of slurries containing NaCl and KCl was evaluated along with their mechanical strength. Thermal and microstructural tests were also carried out. The results revealed that the presence of NaCl and KCl affected the pozzolanic activity of silica flour, reducing the strength of the hardened slurries containing salt. Friedel´s salt was formed as a result of the bonding between free Cl- and tricalcium aluminate. The presence of CO2 also contributed to the degradation of the slurries as a result of a process of carbonation/bicarbonataion

Estudo da síntese e propriedade magnética de ferritas de manganês/cobalto dopadas com níquel

For the chemical method of synthesis of co-precipitation were produced ferrite powders manganese-cobalt equal stoichiometric formula Mn (1-x) Co (x) Fe2O4, for 0 < x < 1, first reagent element using as the hydroxide ammonium and second time using sodium hydroxide. The obtained powders were calcined at 400 ° C, 650 ° C, 900 ° C and 1150 ° C in a conventional oven type furnace with an air atmosphere for a period of 240 minutes. Other samples were calcined at a temperature of 900 ° C in a controlled atmosphere of argon, to evaluate the possible influence of the atmosphere on the final results the structure and morphology. The samples were also calcined in a microwave oven at 400 ° C and 650 ° C for a period of 45 minutes possible to evaluate the performance of this type of heat treatment furnace. It was successfully tested the ability of this group include isomorphic ferrite with the inclusion of nickel cations in order to evaluate the occurrence of disorder in the crystalline structures and their changes in magnetic characteristics.To identify the structural, morphological, chemical composition and proportions, as well as their magnetic characteristics were performed characterization tests of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDX), thermogravimetric (TG), vibrating sample magnetometry (MAV) and Mössbauer spectroscopy. These tests revealed the occurrence of distortion in the crystal lattice, changes in magnetic response, occurrence of nanosized particles and superparamagnetism

Desenvolvimento de argamassa para restauração utilizando resíduo do polimento do porcelanato

The coatings mortars are essential elements of building structures because they execute an important role in protecting walls and are particularly exposed to aggressive action responsible for its degradation over time. The importance of wall coverings has been the subject of discussion and analysis in the conservation and rehabilitation of old buildings. Are sometimes removed and replaced with inappropriate solutions of constructive point of view or architecture. The most commonly used coatings on walls of old buildings is based on traditional hydraulic lime mortars. The present study aims at the formulation of new lime- based mortars and aerial fine aggregate, in order to contribute to a better field of conservation and restoration mortar coating of old buildings. Residue was used for polishing porcelain as fine aggregate, replacing the aggregate (sand), in percentages 05-30% by mass. We conducted a thorough evaluation of the mortar properties in fresh and hardened state by comparing the performance of the same with a reference mortar. The residue used was characterized as the density, bulk density, and particle size laser, scanning electron microscopy, X-ray diffraction and X-ray fluorescence. Formulations were produced 7, 6 with residue and one commonly used formulation, which served as a reference. In the formulations of lime mortars air (hydrated lime powder CH-I) has been adopted a stroke volume (1:3) with constant binder, was varied and the water / binder and aggregate and waste. For evaluation of mortars fresh, proceeded to consistency analysis, specific gravity, water retention and air content embedded. In the hardened state assays were performed in specific gravity, water retention, modulus of elasticity, tensile strength in bending, compressive strength, water absorption by capillary action, adhesion, tensile strength, resistance to shrinkage and salts by of crystallization trials with resources chloride solution, nitrate and sulfate all sodium in prismatic at 90 days of age, in addition to the micro structural analysis of mortars. Based on the results we can see that the mortar formulated with 10% content of waste and the reference free retraction feature more stable closer to neutrality. The composition of 10% was obtained better performance against the action of the salt crystallization. The mortar with 15% residue obtained better density, lower air content embedded and high capacity for water retention developing good workability. The replacement of 20% of waste generates a satisfactory utilization of resistance to compression, flexion and traction grip the base. And, finally, it can be seen that the mortar with 10, 15 and 20% residual show, in principle, good suitability as coatings, thus enabling a final result consistent with durability, workability and aesthetics developing therefore a material with better performance to repair or replace existing mortars in old buildings

Estudo de inibidores de corrosão em concreto armado, visando a melhoria na sua durabilidade

This thesis has as objective presents a methodology to evaluate the behavior of the corrosion inhibitors sodium nitrite, sodium dichromate and sodium molybdate, as well as your mixture, the corrosion process for the built-in steel in the reinforced concrete, through different techniques electrochemical, as well as the mechanical properties of that concrete non conventional. The addition of the inhibitors was studied in the concrete in the proportions from 0.5 to 3.5 % regarding the cement mass, isolated or in the mixture, with concrete mixture proportions of 1.0:1.5:2.5 (cement, fine aggregate and coarse aggregate), superplasticizers 2.0 % and 0.40 water/cement ratio. In the modified concrete resistance rehearsals they were accomplished to the compression, consistence and the absorption of water, while to analyze the built-in steel in the concrete the rehearsals of polarization curves they were made. They were also execute, rehearsals of corrosion potential and polarization resistance with intention of diagnose the beginning of the corrosion of the armors inserted in body-of-proof submitted to an accelerated exhibition in immersion cycle and drying to the air. It was concluded, that among the studied inhibitors sodium nitrite , in the proportion of 2.0 % in relation to the mass of the cement, presented the best capacity of protection of the steel through all the studied techniques and that the methodology and the monitoring techniques used in this work, they were shown appropriate to evaluate the behavior and the efficiency of the inhibitors

Influência da substituição de areia natural por pó de pedra no comportamento mecânico, microestrutural e eletroquímico de concretos

The construction industry is one of the largest consumers of natural raw materials, and concrete is considered today the most used material wide. This accentuated consumption of natural resources has generated concern with the preservation of the environment, and has motivated various studies related to the use of resid ues, which can partially or entirely substitute, with satisfactory performance, some materials such as the aggregate, and in so doing, decrease the impact on the environment caused by the produced residues. Research has been done to better understand and improve the microstructure of concrete, as well as to understand the mechanism of corrosion in reinforced steel. In this context, this work was developed aiming at discovering the influence of the substitution of natural sand by artificial sand, with rega rd to mechanical resistance, microstructure, and durability. To obtain the electrochemical parameters, an adaptation was made to the galvanostatic electrochemical method to study the corrosion in reinforced steel. Concretes of categories 20 MPa and 40 MPa were produced, containing natural sand, and concretes of the same categories were produced with artificial sand substituting the natural sand, and with the addition of sodium nitrate and sodium chloride. Due to the use of rock dust reject (artificial sand), an evaluation was made of its environmental risk. The results indicate that the concretes of category 20 MPa present a better performance than the concrete made with natural sand, thus making it a viable substitute. For the category 40 MPa, the better performance is from the concrete containing natural sand. The adaptation of the galvanostatic electrochemical technique to the study of the corrosion of reinforced steel within concrete proved to be valid for obtaining electrochemical parameters with a high degree of reliability, considering the number of degrees of freedom

Estudo de adsorvente obtido de terras diatomáceas para remoção de metais pesados em águas produzidas: processamento, caracterização e dinâmica em leito fixo

The acceleration of industrial growth in recent decades on all continents aroused the interest of the companies to counter the impacts produced on the environment, spurred primarily by major disasters in the petroleum industry. In this context, the water produced is responsible for the largest volume of effluent from the production and extraction of oil and natural gas. This effluent has in its composition some critical components such as inorganic salts, heavy metals (Fe, Cu, Zn, Pb, Cd, ), presence of oil and chemicals added in the various production processes. In response to impact, have been triggered by research alternative adsorbent materials for water treatment and water produced, in order to removing oils and acids and heavy metals. Many surveys of diatomaceous earth (diatomite) in Brazil involve studies on the physico-chemical, mineral deposits, extraction, processing and applications. The official estimated Jazi are around 2.5 million tonnes, the main located in the states of Bahia (44%) and Rio Grande do Norte (37,4%). Moreover, these two states appear as large offshore producers, earning a prominent role in research of adsorbents such as diatomite for treatment of water produced. Its main applications are as an agent of filtration, adsorption of oils and greases, industrial load and thermal insulator. The objective of this work was the processing and characterization of diatomite diatomaceous earth obtained from the municipality of Macaíba-RN (known locally as tabatinga) as a low cost regenerative adsorbent for removal of heavy metals in the application of water produced treatment. In this work we adopted a methodology for batch processing, practiced by small businesses located in producing regions of Brazil. The characterization was made by X-ray diffraction (XRD), scanning electron microscopy (SEM) and specific surface area (BET). Research conducted showed that the improvement process used was effective for small volume production of diatomite concentrated. The diatomite obtained was treated by calcination at temperature of 900 oC for 2 hours, with and without fluxing Na2CO3 (4%), according to optimal results in the literature. Column adsorption experiments were conducted to percolation of the in nature, calcined and calcined fluxing diatomites. Effluent was used as a saline solution containing ions of Cu, Zn, Na, Ca and Mg simulating the composition of produced waters in the state of Rio Grande do Norte, Brazil. The breakthrough curves for simultaneous removal of copper ions and zinc as a result, 84.3% for calcined diatomite and diatomite with 97.3 % for fluxing. The calcined fluxing diatomite was more efficient permeability through the bed and removal of copper and zinc ions. The fresh diatomite had trouble with the permeability through the bed under the conditions tested, compared with the other obtained diatomite. The results are presented as promising for application in the petroleum industry

Adsorção de cobre e cromo utilizando fibra de sisal visando o tratamento da água produzida pela indústria petrolífera

Currently, the oil industry is the biggest cause of environmental pollution. The objective was to reduce the concentration of copper and chromium in the water produced by the oil industry. It was used as adsorbent natural sisal fiber Agave sp treated with nitric acid and sodium hydroxide. All vegetable fibers have physical and morphological properties that enablies the adsorption of pollutants. The basic composition of sisal is cellulose, hemicellulose and lignin. The features are typically found in the characterization of vegetable fibers, except the surface area that was practically zero. In the first stage of adsorption, it was evaluated the effect of temperature and time skeeking to optimize the execution of the factorial design. The results showed that the most feasible fiber was the one treated with acid in five hours (30°C). The second phase was a factorial design, using acid and five hours, this time was it determined in the first phase. The tests were conducted following the experimental design and the results were analyzed by statistical methods in order to optimize the main parameters that influence the process: pH, concentration (mol / L) and fiber mass/ metal solution volume. The volume / mass ratio factor showed significant interference in the adsorption process of chromium and copper. The results obtained after optimization showed that the highest percentages of extraction (98%) were obtained on the following operating conditions: pH: 5-6, Concentration: 100 ppm and mass/ volume: 1 gram of fiber/50mL solution. The results showed that the adsorption process was efficient to remove chromium and copper using sisal fibers, however, requiring further studies to optimize the process.

Efeitos do potencial probiótico Enterococcus faecium 32 e de sua associação com o extrato da alga marinha Caulerpa mexicana no tratamento de colite experimental murina

Ulcerative colitis comprising an inflammatory bowel disease, whose most severe consequence is the development of intestinal neoplasia. The drugs currently used to treat the disease trigger a variety of serious adverse effects and are not effective in many cases. Recent studies demonstrated the effectiveness of natural products for the treatment of inflammatory processes. Seaweed extracts and their purified products have shown protective effects in models of inflammation and the association of traditional therapies with probiotics has significantly improved the clinical symptoms of ulcerative colitis. Therefore, the aims of this study include evaluating the potential effects of the use of probiotic strain Enterococcus faecium 32 (Ef32), the methanolic extract of the green seaweed Caulerpa mexicana (M.E.) and their concomitant administration in a murine model of colitis induced by dextran sodium sulfate (DSS). Accordingly, C57BL /6 mice were pretreated orally with Ef32 (109 CFU/ml) for seven days. In the seven days following, the colitis was induced by administration of 3% DSS (w/v) diluted in the animals drinking water. During this period, animals were treated daily with Ef32 and the M.E. (2.0 mg/kg) every other day by intravenous route. The development of colitis was monitored by the disease activity index (DAI), which takes into account the loss of body weight, consistency and presence of blood in stools. After euthanasia, the colon was removed, its length measured and tissue samples were destined for histological analysis and culture for cytokine quantification. The levels of cytokines in the culture supernatant of the colon were measured by ELISA. The treatments with the probiotic Ef32 or the M.E. alone or the combination of these two substances provoked significant improvement as to weight loss and DAI, and prevented the shortening of the colon in response to DSS. The isolated treatments triggered a slight improvement in intestinal mucosal tissue damage. However, their combination was able to completely repair the injury triggered by DSS. The association was also able to reduce the levels of all the cytokines analyzed (IFN-γ, IL-4, IL-6, IL-12, IL-17A and TNF-α). On the other hand, the treatment with Ef32 did not interfere with the levels of TNF-α, whereas treatment with M.E. did not alter the levels of IL-6. Moreover, the treatment with Ef32 not interferes in TNF-α levels, whereas treatment with M.E. did not alter the levels of IL-6. Therefore, the potential probiotic Ef32 and M.E. and especially when these samples were associated proved promising alternatives in the treatment of ulcerative colitis as demonstrated in an experimental model because of its beneficial effects on morphological and clinical parameters, and by reducing the production of proinflammatory cytokines of Th1, Th2 and Th17

Efeitos do alcalóide indólico caulerpina, obtido de alga do gênero caulerpa, em modelo de colite experimental murina

As doenças inflamatórias intestinais são enfermidades onde a tolerância e homeostase da resposta inflamatória estão comprometidas, gerando lesões teciduais e favorecendo o surgimento de neoplasias. Há dois importantes exemplos de doenças inflamatórias intestinais, a colite ulcerativa, foco do modelo desse estudo, e a doença de Crohn. Os medicamentos utilizados no tratamento dessas doenças desencadeiam diversos efeitos adversos; além disso, em alguns pacientes, eles não são eficazes. Os extratos de algas têm demonstrado várias atividades biológicas, entre elas a atividade anti-inflamatória. Os extratos das algas do gênero Caulerpa foram utilizados em vários estudos, onde modelos inflamatórios foram analisados, entre eles o modelo de colite ulcerativa. A utilização do extrato metanólico da C. mexicana como terapêutica nesse modelo atenuou o quadro clinico desenvolvido pelos animais. Sendo assim, o presente estudo teve como objetivo analisar a ação terapêutica da Caulerpina (CLP), extraída da C. racemosa, no modelo murino de colite ulcerativa. Camundongos C57BL/6 machos foram expostos a uma solução de Dextrana Sulfato de Sódio (DSS) a 3% por sete dias. A partir do primeiro dia de exposição ao DSS os animais foram tratados em dias alternados com a CLP nas doses de 4 e 40 mg/kg e com a dexametasona (3 mg/kg) por via oral. O desenvolvimento da doença foi analisado através do índice de atividade da doença (IAD), que leva em consideração a perda de peso corporal, a consistência e a presença de sangue nas fezes. Após a eutanásia, o cólon foi removido e mensurado, e amostras do tecido colônico foram destinadas a análise histológica e à cultura para dosagem de citocinas. Os níveis de citocinas no sobrenadante da cultura do cólon foram mensurados por ELISA. O tratamento com a CLP (4 mg/kg) desencadeou significativa melhora quanto à perda de peso corporal e ao IAD, e atenuou o encurtamento do cólon em resposta ao DSS. Tal dose foi capaz de reduzir os níveis de citocinas pró-inflamatórias analisadas (TNF-, IFN-, IL-6, IL-17), mas não teve efeito significativo nas citocinas anti-inflamatórias IL-10 e TGF-. O tratamento com a CLP (40 mg/kg) não foi eficaz quanto a perda de peso e ao IAD, além de não ter atenuado a redução do cólon em resposta ao DSS. Essa dose conseguiu reduzir os níveis das citocinas pró-inflamatórias, porém não os níveis de IL-6. O tratamento com a dexametasona obteve melhora discreta quanto à perda de peso corporal e ao IAD, porém não atenuou a redução do cólon em resposta ao DSS. Esse tratamento também conseguiu reduzir todas as citocinas pró-inflamatórias testadas. Deste modo a CLP (4 mg/kg) demonstrou ser uma alternativa promissora no tratamento da colite ulcerativa, em razão dos seus efeitos benéficos sobre parâmetros clínicos, morfológicos e moleculares do modelo em estudo

Comparação de efeitos dos extratos de Hypericum perforatum (Hipérico) e de Mentha crispa (Hortelã) em diferentes modelos experiemtais

Several clinic evaluations have been possible with radiobiocomplexes labeled with technetium-99m (99mTc). Some natural and synthetic drugs are capable of to interfere on the labeling of blood constituents with 99mTc, as well as on the biodistribution of radiobiocomplexes. Authors have also reported about the toxicity of several natural products. The aim of this study was to compare the effects of the Mentha crispa (hortelã) and of the Hypericum perforatum (hipérico) in different experimental models. On the labeling of red blood cells (RBC) and plasma and cellular proteins with 99mTc, both extracts were capable of to decrease the radioactivity percentage on the cellular compartment and on the fixation on plasma and cellular proteins. On the morphometry of the RBC, only the hortelã was capable to alter the shape and the perimeter/area ratio of the RBC. On the biodistribution of the radiobiocomplex sodium pertechnetate (Na99mTcO4), the hortelã increased the Na99mTcO4 distribution in the kidney, spleen, liver and thyroid, meanwhile the hipérico decreased the Na99mTcO4 distribution in the bone, stomach, lungs and thyroid, and increased the Na99mTcO4 distribution in the pancreas. On the bacterial cultures survival, the hipérico was capable of to protect the bacteria against the stannous chloride (SnCl2) effect. The hipérico did not alter the topology of plasmidial DNA and did not protect the plasmidial DNA against the SnCl2 action. Probably, the effects presented by both extracts could be due to chemical compounds of the extracts that could alter the morphology of the RBC and the plasma membrane ions transport, and/or by phytocomplexes that could be formed with different effects dependent on the biological system considered

Avaliação de efeitos de um extrato aquoso de cinnamomum zeylanicum L. na marcação de constituintes sanguíneos com tecnécio-99m e na morfologia das hemácias de ratos wistar

Radiobiocomplexes are used to obtain images in nuclear medicine and employed in basic research. Blood constituents labeled with technetium-99m (99mTc) have also been employed as radiobiocomplexes and used also experimental model for evaluation of the biological effects of natural or synthetic drugs. The analysis of the morphology and the morphometrics parameters (perimeter/área ratio) can be used to evaluate the effects of drugs upon the structure of the membrane of red blood cells. Cinnamomum zeylanicum (cinnamon) is a spice used as herbal medicine to treat diseases. The aim of this study was to evaluate the effect of in vitro and in vivo treatment with an aqueous cinnamon extract on the labeling of blood constituents with 99mTc and on the morphology of red blood cells from Wistar rats. In the in vitro treatment, isolated blood sample from animals were incubated with cinnamon extract. In the in vivo treatment, blood samples were also withdrawn from animals treated with cinnamon extract. In both cases, the radiolabeling of blood constituents was done. The morphological analysis of red blood cells was also done. As control, blood or animals treated with NaCl 0.9%. The data obtained on the labeling of blood constituents with 99mTc experiments indicated that the in vitro treatment with cinnamon extract was capable to decrease signiicantly (p<0.05) the percentage of radioactivity in cellular compartments and on the fixation of cellular and plasma proteins. These effects were not observed on the in vivo treatment. The results obtained for the morphology of red blood cells suggest that the in vitro and in vivo treatments did not alter the morphology and the perimeter/area ratio. The in vitro treatment with aqueous cinnamon extract could affect the membrane structures related with the oxidation status of the stannous ion pertechnetate ion, altering the labeling of blood constituentes with 99mTc. This study was a multidisciplinary experimental research. It was developed with the contribution of the different Departments and Services of the Hospital Universitário Pedro Ernesto of the Universidade do Estado do Rio de Janeiro

Efeito de um extrato de Artemísia Vulgaris L. marcação in vitro de constituintes sanguíneos com tecnécio-99m em ratos wistar

Artemisia vulgaris L..is used in folk medicine and in Traditional Chinese Medicine (TCM). This medicinal plant has been utilized as anticonvulsive, analgesic, antispasmodic effect, rheumatic pains, menstrual dyspepsia, asthenia, epilepsy, hepatitis, fevers, anemia and to expel parasites. In nuclear medicine, blood constituents are labeled with technetium-99m (99mTc) and used as radiopharmaceuticals (radiobiocomplexes). Authors have been described that synthetic and/or natural drugs could modify the labeling of blood constituents with 99mTc. The aim of this work was to evaluate the effects of an aqueous extract of Artemisia vulgaris L. on the labeling of blood constituents with 99mTc. Blood samples withdrawn of Wistar rats were incubated with Artemisia vulgaris L, stannous chloride and 99mTc, as pertechnetate ion. Aliquots of plasma (P) and blood cells (BC) were isolated. Aliquots of P and BC were also precipitated with trichloroacetic acid and soluble (SF) and insoluble (IF) fractions were separated. The radioactivity in each fraction was counted and the percentages of radioactivity (%ATI) were calculated. Artemisia vulgaris L. extract decreased significantly (p<0.05) the %ATI on BC and on IF-BC. The analysis of the results indicates that the extract could have substances that could interfere on the transport of stannous through the erythrocyte membrane altering the labeling of blood cells with 99mTc. Working in this study was a multidisciplinary group, with Phisical therapists, Biomedicals, Physicals, Pharmacists, Biologists, Statistics and Physicians.

Análise in vitro da atividade antifúngica e de toxicidade da anfotericina B pré-aquecida

The aim of this work was to evaluate how an aqueous micellar system containing Amphotericin B (AmB) and sodium deoxycholate (DOC) can be rebuilt after heating treatment. Also a review of the literature about the new physicochemical and biological properties of this new system was carried out. Afterwards, heated (AmB-DOC-H) and unheated (AmB-DOC) micelles were subsequently diluted at four different concentrations (50mg.L-1, 5mg.L-1, 0.5mg.L-1 and 0.05mg.L-1) to perform the physicochemical study and, then, the pharmacotoxicity assay, in which two cell models were used for the in vitro experiments, Red Blood Cells (RBC) from human donors and Candida parapisilosis (Cp). While potassium (K+) and hemoglobin leakage from RBC were the used parameters to evaluate the acute and chronic toxicity, respectively, the efficacy of AmB-DOC and AmB-DOC-H were assessed by K+ leakage and cell survival rate from Cp. The spectral study revealed a slight change on the aggregate peak from 327nm to 323nm for AmB-DOC-H compared to AmB-DOC. Concerning the toxicity, although AmB-DOC and AmB-DOC-H presented different behavior for hemoglobin leakage, AmB-DOC produced higher leakage than AmB-DOC-H at high concentrations (from 5mg.L-1) with values tending to zero. However, concerning K+ leakage, both AmB-DOC and AmB-DOC-H, showed similar profile for both cell models, RBC and Cp (p<0,05). AmB-DOC-H and AmB-DOC also revealed similar profile of activity against Cp with equivalent survival rate. In short, the AmB-DOC-H showed much less toxicity than AmB-DOC, but remained as active as the late one against fungal cell. Therefore, the results highlight the importance of this new procedure as a simple, inexpensive and safe alternative to produce a new kind of micelle system for treatment of systemic fungal infections

Ação da cafeína sobre o rendimento esportivo de ciclistas em condições de calor e umidade

Objetivo: Verificar a ação da cafeína no tempo de rendimento, a taxa de esforço percebido (RPE), os níveis plasmáticos de glicose, sódio e potássio, a temperatura timpânica (Tt), o peso corporal (PC), freqüência cardíaca (FC) e concentração urinária da cafeína com a ingestão de doses de 5 e 9 mg/kg de cafeína e placebo, em provas ciclísticas sob condições de alto risco térmico. Métodos: Foram estudados 8 ciclistas treinados e aclimatizados em 3 provas de 45 km utilizando o modelo experimental e duplo-cego com randomização intra-sujeitos. Resultados: Não foram observadas diferenças significativas entre as variáveis avaliadas, entretanto o tempo de rendimento e a RPE foram menores com as doses de 5 e 9 mg/kg de cafeína que com a dose placebo. Conclusões: Estes dados indicam que as condições de calor e umidade podem ser suficientes para mascarar o benefício ergogênico da cafeína, entretanto deve-se considerar que a cafeína pode exercer influencia sobre a percepção subjetiva de esforço podendo levar à redução dos sinais de fadiga durante o exercício e conseqüente melhora do desempenho esportivo

Avaliação de um método de cromatografia em fase gasosa head space e estudo da estabilidade do etanol em amostras de sangue

The ethanol is the most overused psychoactive drug over the world; this fact makes it one of the main substances required in toxicological exams nowadays. The development of an analytical method, adaptation or implementation of a method known, involves a process of validation that estimates its efficiency in the laboratory routine and credibility of the method. The stability is defined as the ability of the sample of material to keep the initial value of a quantitative measure for a defined period within specific limits when stored under defined conditions. This study aimed to evaluate the method of Gas chromatography and study the stability of ethanol in blood samples, considering the variables time and temperature of storage, and the presence of preservative and, with that check if the conditions of conservation and storage used in this study maintain the quality of the sample and preserve the originally amount of analyte present. Blood samples were collected from 10 volunteers to evaluate the method and to study the stability of ethanol. For the evaluation of the method, part of the samples was added to known concentrations of ethanol. In the study of stability, the other side of the pool of blood was placed in two containers: one containing the preservative sodium fluoride 1% and the anticoagulant heparin and the other only heparin, was added ethanol at a concentration of 0.6 g/L, fractionated in two bottles, one being stored at 4ºC (refrigerator) and another at -20ºC (freezer), the tests were performed on the same day (time zero) and after 1, 3, 7, 14, 30 and 60 days of storage. The assessment found the difference in results during storage in relation to time zero. It used the technique of headspace associated with gas chromatography with the FID and capillary column with stationary phase of polyethylene. The best analysis of chromatographic conditions were: temperature of 50ºC (column), 150ºC (jet) and 250ºC (detector), with retention time for ethanol from 9.107 ± 0.026 and the tercbutanol (internal standard) of 8.170 ± 0.081 minutes, the ethanol being separated properly from acetaldehyde, acetone, methanol and 2-propanol, which are potential interfering in the determination of ethanol. The technique showed linearity in the concentration range of 0.01 and 3.2 g/L (0.8051 x + y = 0.6196; r2 = 0.999). The calibration curve showed the following equation of the line: y = x 0.7542 + 0.6545, with a linear correlation coefficient equal to 0.996. The average recovery was 100.2%, the coefficients of variation of accuracy and inter intra test showed values of up to 7.3%, the limit of detection and quantification was 0.01 g/L and showed coefficient of variation within the allowed. The analytical method evaluated in this study proved to be fast, efficient and practical, given the objective of this work satisfactorily. The study of stability has less than 20% difference in the response obtained under the conditions of storage and stipulated period, compared with the response obtained at time zero and at the significance level of 5%, no statistical difference in the concentration of ethanol was observed between analysis. The results reinforce the reliability of the method of gas chromatography and blood samples in search of ethanol, either in the toxicological, forensic, social or clinic