937 resultados para HPLC-UV-PAD


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AssiDomän tillverkar kartong till förpackningsindustrin. Inom detta område är vitheten på kartongytanen viktig parameter. För att höja intrycket av förpackningen samt skapa en skyddande yta lackas ofta förpackningen med UV-lack efter tryck. Efter lackning kan då otryckta lackade ytor uppfattas som mindre vita. För att ta reda på om bestrykningssammansättningen har betydelse har ett fem olika bestrykningar blandats. Pigmenten som använts i bestrykningarna är karbonat, kaolin och titandioxidi olika kombinationer. Kartong har sedan bestrukits med dessa och därefter lackerats med UV-lack. Lackningen har gjorts i tre olika lackmängder. Mätningar har sedan gjorts gällande framförallt vithet. Den samverkan som sker mellan ljus, materialet och dess struktur är av stor vikt för att skapa en yta med goda optiska egenskaper. Resultaten i detta försök visar att lacken påverkar de optiska egenskaperna och framförallt vitheten. De lackerade ytorna fick en gulton efter lackering vilket kan ha att göra med lackens egenskaper. Vitheten hade en något mindre minskning för den bestrykning som bestod av karbonat och titandioxid. Skillnaden var dock mycket liten då alla bestrykningar fick en sänkning av vitheten med cirka 11-13 procentenheter oberoende av utgångsvärdet i vithet för respektive bestrykning innan lackning. Positivt var att det kunde konstateras att den bestrykning som hade det högsta vithetsvärdet före lackning också hade det efter lackning med ett normalt lackpålägg vilket betyder att en hög vithet är av betydelse även om den bestrukna ytan ska lackas. Den sänkning av vitheten som sker kan ha flera tänkbara orsaker. En tänkbar orsak kan vara att lacken förstör den porösa struktur som ger den viktiga ljusspridningen i bestrykningsskiktet. Resultaten visar också att lackens egenskaper tycks vara av stor betydelse. Den gulton som framträdde efter lackning tyder på en ökad absorption av vissa ljusvåglängder. Något som också pekar på detta är att alla fem bestrykningarna fick en liknande sänkning av vitheten. För att säga exakt vad som är orsaken eller vilken kombination som påverkar vitheten mest krävs ytterliggare tester. Olika UV-lacker kan testas eftersom endast en UV-lack har använts i dessa försök. En närmare studie av gränsyta mellan UV-lacken och bestrykningsskiktet bör också göras för att se hur lacken påverkar bestrykningsskiktets struktur.

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To date there are no analytical techniques designed to exclusively measure bioavailable iron in marine environments. The goal of this research is to develop such a technique by isolating the bioavailable iron using the terrestrial siderophore desferrioxamine B (DFB). This project contained many challenging aspects, but the specific goal of this study was to develop a robust analytical technique for quantification of Fe(III)-DFB complexes at nanomolar concentrations. Past work showed that oxalate (Ox) promotes photodissociation of Fe(III)-DFB to Fe(Il), and we are specifically interested in the mechanism of this process. A model was developed using known thermodynamic constants for Fe(III)-DFB and Fe(III) oxalato complexes and adjusting for ionic strength. The model was confirmed by monitoring the UV-VIS absorbance of the system at a variety of oxalate concentrations and pH. The model did not include ternary complexes. Next., the rate of Fe(1I) production during UV irradiation was examined. The results showed that the rate of Fe(II) production was based entirely on the [Fe(Ox)?]3- speciation, and that reoxidation of Fe(II) occurred via reactive oxygen intermediates. This reoxidation could be avoided by either decreasing the oxygen concentration or by adding a Fe(II) stabilizing reagent, such as ferrozine. Further studies need to be done to confirm that these results apply at sub nanomolar concentrations, and the issue of Fe(II) reoxidation at lower Fe concentrations needs to be addressed.

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Este estudo avaliou as porcentagens de Transmitância direta (Td) das resinas compostas microhíbridas Charisma F, Solitaire II (Heraeus Kulzer ), Intens e Tetric Ceram (Ivoclar Vivadent) e nanoparticuladas Esthet-X (Dentsply De trey) e Filtek Supreme (3M Espe) nas cores Vita A3 (Dentina) e translúcido (Esmalte), ou seus correspondentes. Foram confeccionados três corpos-de-prova para cada material e cor, de formato quadrangular com 12x12 mm de lado e espessura de 1 mm. Após fotoativação, foram realizadas três leituras por corpo-de-prova em espectrofotômetro de UV-visível HP 8453 (Hewlett-Packard), com temperatura e umidade controladas (22±2°C/50±5%). Os ângulos de incidência e leitura em 0° / 0° foram utilizados para os comprimentos de onda de 400 a 700 nm. Os espectros obtidos foram analisados quanto ao percentual médio de Td para todo o espectro, em intervalos de 20 nm, e nos comprimentos de onda de 400, 560 e 700 nm. Através de ANOVA e teste de Tukey (p=0,01) encontrou-se que a resina composta Charisma obteve as maiores porcentagens de Td em todos os espectros, exceto para a cor Esmalte em 700 nm, que ficou abaixo da resina composta Esthet-X cor Esmalte. O teste t-Student demonstrou serem significativamente maiores os percentuais de Td para os espectros das cores Translúcido, exceto para as resinas compostas Supreme, em que não diferiram, e Charisma, com porcentagens de Td significativamente maiores para a cor Dentina. Por meio de teste não paramétrico de Friedman verificou-se que todas as resinas compostas estudadas demonstraram aumento significativo de Td com o aumento do comprimento de onda, com exceção da resina composta Solitaire, cores Dentina e Esmalte, que não demonstrou diferenças significativas nos comprimentos de onda de 560 e 700 nm.

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A malha rodoviária brasileira apresenta-se, em sua maior extensão, em má condições de serventia. Uma das alternativas para se evitar deformações permanentes e trincamentos no pavimento é a adição, a quente e em reatores especiais, de polímeros ao asfalto. Esta prática já é realizada no Brasil há alguns anos, porém ainda não se tem um domínio do assunto, principalmente no caso da modificação de ligantes asfálticos brasileiros. O objetivo deste trabalho é avaliar a influência de algumas propriedades do polímero modificador no envelhecimento do ligante asfáltico modificado. Para tanto se realizou inicialmente um estudo sobre o mecanismo de envelhecimento de ligantes puros, inclusive frente a radiação ultravioleta do sol, e em seguida utilizou-se a mesma metodologia para avaliar o papel do polímero neste processo. Além disso, relacionou-se através de um projeto de experimentos a massa molar e teor de estireno do polímero SBS linear com suas propriedades clássicas, estabilidade, temperatura de transição vítrea e morfologia. Observou-se que a simulação de envelhecimento UV em laboratório, desenvolvida neste estudo, foi extremamente satisfatória. Os processos de foto-oxidação e termooxidação resultam em mecanismos diferentes de envelhecimento. A origem e composição química dos ligantes é de suma importância no mecanismo de envelhecimento UV destes. A massa molar e o teor de estireno do polímero modificador representam propriedades importantes para a estabilidade e durabilidade do ligante asfáltico modificado.

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O vídeo apresenta sugestões de como os alunos podem comprar ou construir um pad de estudos para percussão. O professor apresenta diferentes tipos de pads, que são borrachas utilizadas para a prática com baquetas. Alguns são comprados já prontos, outros podem ser construídos pelos alunos. Feito para alunos que estão estudando percussão, o vídeo visa esclarecer algumas questões fundamentais para a aquisição desse equipamento, bem como explicar sua importância nos estudos de percussão.

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Este item é parte de um conjunto de modelos produzido pela equipe do Laboratório de Objetos de Apredizagem (LOA)/UFSCar para o jogo LabTecA

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This article proposes a simple and sensitive HPLC method with photo-diode array detection for the analysis of organic acids, monomeric polyphenols and furanic compounds in wine samples by direct injection. The chromatographic separation of 8 organic acids, 2 furans and 22 phenolic compounds was carried out with a buffered solution (pH 2.70) and acetonitrile as mobile phases and a difunctionally bonded C18 stationary phase, Atlantis dC18 (250 4.6 mm, 5mm) column. The elution was performed in 12 min for the organic acids and in 60 min for the phenolic compounds, including phenolic acids, stilbenes and flavonoids. Target compounds were detected at 210 nm (organic acids, flavan-3-ols and benzoic acids), 254 nm (ellagic acid), 280 nm (furans and cinnamic acid), 315 nm (hydroxycinnamic acids and trans-resveratrol) and 360 nm (flavonoids). The RSD for the repeatability test (n55) of peak area and retention times were below 3.1 and 0.3%, respectively, for phenolics and below 1.0 and 0.2% for organic acids. The RSDs expressing the reproducibility of the method were higher than for the repeatability results but all below 9.0%. Method accuracy was evaluated by the recovery results, with averaged values between 80 and 104% for polyphenols and 97–105% for organic acids. The calibration curves, obtained by triplicate injection of standard solutions, showed good linearity with regression coefficients higher than 0.9982 for polyphenols and 0.9997 for organic acids. The LOD was in the range of 0.07–0.49 mg/L for polyphenols (cinnamic and gallic acids, respectively) and 0.001–0.046 g/L for organic acids (oxalic and lactic acids, respectively). The method was successfully used to measure and assess the polyphenolic fingerprint and organic acids profile of red, white, rose ´ and fortified wines.

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A RP-HPLC method with photodiode array detection (DAD) was developed to separate, identify and quantify simultaneously the most representative phenolic compounds present in Madeira and Canary Islands wines. The optimized chromatographic method was carefully validated in terms of linearity, precision, accuracy and sensitivity. A high repeatability and a good stability of phenolics retention times (a3%) were obtained, as well as relative peak area. Also high recoveries were achieved, over 80.3%. Polyphenols calibration curves showed a good linearity (r2 A0.994) within test ranges. Detection limits ranged between 0.03 and 11.5 lg/mL for the different polyphenols. A good repeatability was obtained, with intra-day variations less than 7.9%. The described method was successfully applied to quantify several polyphenols in 26 samples of different kinds of wine (red, ros and white wines) from Madeira and Canary Islands. Gallic acid was by far the most predominant acid. It represents more than 65% of all phenolics, followed by p-coumaric and caffeic acids. The major flavonoid found in Madeira wines was trans-resveratrol. In some wines, (–)-epicatechin was also found in highest amount. Canary wines were shown to be rich in gallic, caffeic and p-coumaric acids and quercetin.

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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

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Stress urinary incontinence (SUI) is defined as "involuntary loss of urine" due to several processes that alter the ability of the bladder to hold urine properly, regarded as a social and hygienic problem that adversely affects quality of life. In postmenopausal women, IU is associated with atrophy and weakness of the pelvic floor muscles. The objective this study was investigate, using the onehour pad test, stress urinary leakage (SUI), evaluate and compare their results in postmenopausal and premenopausal women. The survey was characterized as a cross-sectional study. The study consisted of 60 postmenopausal women were divided into GIU - consisting of 34 volunteers complaining of involuntary loss of urine during stress - and GSIU - consisting of 26 volunteers without complaints of loss of urine during stress, and 15 women, during the premenopausal (GPM), and ovulatory with normal menstrual cycle. All volunteers were evaluated clinically, subjected to one-hour pad test, after the biochemical evaluation of blood and sex hormones. Statistical analysis was performed by descriptive analysis, ANOVA, Turkey´s post-test and Pearson correlation. The results showed that 100% of postmenopausal patients had involuntary loss of urine during one hour pad test (GIU: 4.0 g; GSIU: 4.5 g). GPM remained continent after an hour pad test (GPM: 0.4 g). In addition, Pearson showed a strong correlation between urine loss with time since menopause (r = 0.8, p <0.01) and body mass index - BMI (r = 0.7; p = 0.01). These data suggest that the one-hour pad test is a useful test to assess and quantify urinary leakage, including those volunteers who had no previous complaint of SUI

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Kalanchoe brasiliensis Cambess (Crassulaceae), commonly known as saião , coirama branca , folha grossa , is originally from Brazil and commonly found in São Paulo to Bahia, mainly in the coastal zone. Regarding of biological activities, most preclinical studies were found in the literature, mainly about the anti-inflammatory activity of extracts obtained from leaves and / or aerial parts of K. brasiliensis. As regards the chemical constitution, it has been reported mainly the presence of flavonoids in the leaves of the species, but until this moment did not knows which are the active compounds. Although it is a species widely used in traditional medicine in Brazil, there is no monograph about the quality parameters of the plant drug. In this context, this study aims to characterize and quantify the chemical markers of hydroethanolic extract (HE) from the leaves of K. brasiliensis, which can be used in quality control of plant drug and derivatives obtained from this species. The methodology was divided into two parts: i. Phytochemical study: to fractionate, isolate and characterizate of the chemical (s) marker (s) of the HE from the leaves of K. brasiliensis; ii. To Developed validate of analytical method by High Performance Liquid Chromatography (HPLC)-diode array detector (DAD) to quantify the chemical (s) marker (s) of the EH. i. The EH 50% was prepared by turbo extraction method. It was then submitted to liquid-liquid partition, obtaining dichloromethane, n-butanol and ethyl acetate (AcOEt) fractions. The AcOEt fraction was selected to continue the fractionation process, because it has a chemical profile rich in flavonoids. The acOEt fraction was submitted to column chromatography using different systems for obtaining the compound Kb1. To identify this compound, it was submitted to UV analysis ii. For quantitative analysis, the EH was analyzed by HPLC, using different methods. After selecting the most appropriate method, which showed satisfactory resolution and symmetrical peaks, it was validated according to parameters in the RE 899/2003. As result, it was obtained from the AcOEt fraction the compound Kb1 (2.7 mg). Until this moment, the basic nucleus was characterized by UV analysis using shift reagents. The partial chemical structure of the compound Kb1 was identified as a flavonol, containing hydroxyls in 3 , 4 position (ring A), 5 and 7 free (ring B) and a replacement of the C3 hydroxyl by a sugar. As the analysis were performed in the HPLC coupled to a DAD, we observed that the UV spectrum of the major peaks of EH from K. brasiliensis shown similar UV spectrum. According to the literature, it has been reported the presence of patuletin glycosydes derivatives in the leaves of this species. Therefore, it is suggested that the compound Kb1 is glycosylated patuletin derivative. Probably the sugar (s) unit(s) are linked in the C3 in the C ring. . Regarding the development of HPLC analytical method, the system used consists of phase A: water: formic acid (99,7:0,3, v / v) and phase B: methanol: formic acid (99,7:0,3, v / v), elution gradient of 40% B - 58% B in 50 minutes, ccolumn (Hichrom ®) C18 (250x4, 0 mm, 5 μm), flow rate 0.8 mL / min, UV detection at 370 nm, temperature 25 ° C. In the analysis performed with the co-injection of thecompound Kb1 + HE of K. brasiliensis was observed that it is one of the major compounds with a retention time of 12.47 minutes and had a content of 15.3% in EH of leaves from K. brasiliensis. The method proved to be linear, precise, accurate and reproducible. According to these results, it was observed that compound Kb1 can be used as a chemical marker of EH from leaves of K. brasiliensis, to assist in quality control of drug plant and its derivatives

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Caffeine is the legal stimulant consumed most extensively by the human world population and may be found eventually in the urine and/or blood of race horses, the fact that caffeine is in foods led us to determine the highest no-effect dose (HNED) of caffeine on the spontaneous locomotor activity of horses and then to quantify this substance in urine until it disappeared. We built two behavioural stalls equipped with juxtaposed photoelectric sensors that emit infrared beams that divide the stall into nine sectors in a 'tic-tac-toe' fashion. Each time a beam was interrupted by a leg of the horse, a pulse was generated; the pulses were counted at 5-min intervals and stored by a microcomputer. Environmental effects were minimized by installing exhaust fans producing white noise that obscured outside sounds. One-way observation windows prevented the animals from seeing outside. The sensors were turned on 45 min before drug administration (saline control or caffeine), the animals were observed for up to 8 h after i.v. administration of 2.0, 2.5, 3.0 or 5.0 mg caffeine kg(-1). The HNED of caffeine for stimulation of the spontaneous locomotor activity of horses was 2.0 mg kg(-1). The quantification of caffeine in urine and plasma samples was done by gradient HPLC with UV detection. The no-effect threshold should not be greater than 2.0 mug caffeine ml(-1) plasma or 5.0 mug caffeine ml(-1) urine. Copyright (C) 2001 John Wiley & Sons, Ltd.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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The application of composite materials and in particular the fiber-reinforced plastics (FRP) has gradually conquered space from the so called conventional materials. However, challenges have arisen when their application occurs in equipment and mechanical structures which will be exposed to harsh environmental conditions, especially when there is the influence of environmental degradation due to temperature, UV radiation and moisture in the mechanical performance of these structures, causing irreversible structural damage such as loss of dimensional stability, interfacial degradation, loss of mass, loss of structural properties and changes in the damage mechanism. In this context, the objective of this thesis is the development of a process for monitoring and modeling structural degradation, and the study of the physical and mechanical properties in FRP when in the presence of adverse environmental conditions (ageing). The mechanism of ageing is characterized by controlled environmental conditions of heated steam and ultraviolet radiation. For the research, it was necessary to develop three polymer composites. The first was a lamina of polyester resin reinforced with a short glass-E fiber mat (representing the layer exposed to ageing), and the other two were laminates, both of seven layers of reinforcement, one being made up only of short fibers of glass-E, and the other a hybrid type reinforced with fibers of glass-E/ fibers of curaua. It should be noted that the two laminates have the lamina of short glass-E fibers as a layer of the ageing process incidence. The specimens were removed from the composites mentioned and submitted to environmental ageing accelerated by an ageing chamber. To study the monitoring and modeling of degradation, the ageing cycles to which the lamina was exposed were: alternating cycles of UV radiation and heated steam, a cycle only of UV radiation and a cycle only of heated steam, for a period defined by norm. The laminates have already undergone only the alternating cycle of UV and heated steam. At the end of the exposure period the specimens were subjected to a structural stability assessment by means of the developed measurement of thickness variation technique (MTVT) and the measurement of mass variation technique (MMVT). Then they were subjected to the mechanical tests of uniaxial tension for the lamina and all the laminates, besides the bending test on three points for the laminates. This study was followed by characterization of the fracture and the surface degradation. Finally, a model was developed for the composites called Ageing Zone Diagram (AZD) for monitoring and predicting the tensile strength after the ageing processes. From the results it was observed that the process of degradation occurs Abstract Raimundo Nonato Barbosa Felipe xiv differently for each composite studied, although all were affected in certain way and that the most aggressive ageing process was that of UV radiation, and that the hybrid laminated fibers of glass-E/curaua composite was most affected in its mechanical properties