984 resultados para Characterization andBiotechnology application
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Elastic properties of potassium and lead phosphotungstate glasses have been investigated using ultrasonic velocity measurements. The composition dependence of elastic moduli in WO3-K2O-P2O5 glasses suggests that at low alkali oxide concentrations the atomic ring size increases by network modification, which results in the decrease of elastic moduli. In the highly modified regime, due to the presence of coulombic interaction, the rate of decrease of elastic moduli is reduced. In the WO3-PbO-P2O5 glasses the behaviour of elastic moduli suggests that PbO behaves both as a network former and network modifier. The incorporation of PbO into the network is quantitatively determined by the concentration of P2O5 in the system. The results are consistent with the structural model proposed earlier, based on characterization studies.
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We investigate the feasibility of developing a comprehensive gate delay and slew models which incorporates output load, input edge slew, supply voltage, temperature, global process variations and local process variations all in the same model. We find that the standard polynomial models cannot handle such a large heterogeneous set of input variables. We instead use neural networks, which are well known for their ability to approximate any arbitrary continuous function. Our initial experiments with a small subset of standard cell gates of an industrial 65 nm library show promising results with error in mean less than 1%, error in standard deviation less than 3% and maximum error less than 11% as compared to SPICE for models covering 0.9- 1.1 V of supply, -40degC to 125degC of temperature, load, slew and global and local process parameters. Enhancing the conventional libraries to be voltage and temperature scalable with similar accuracy requires on an average 4x more SPICE characterization runs.
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We investigate the feasibility of developing a comprehensive gate delay and slew models which incorporates output load, input edge slew, supply voltage, temperature, global process variations and local process variations all in the same model. We find that the standard polynomial models cannot handle such a large heterogeneous set of input variables. We instead use neural networks, which are well known for their ability to approximate any arbitrary continuous function. Our initial experiments with a small subset of standard cell gates of an industrial 65 nm library show promising results with error in mean less than 1%, error in standard deviation less than 3% and maximum error less than 11% as compared to SPICE for models covering 0.9- 1.1 V of supply, -40degC to 125degC of temperature, load, slew and global and local process parameters. Enhancing the conventional libraries to be voltage and temperature scalable with similar accuracy requires on an average 4x more SPICE characterization runs.
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This thesis describes the preparation, characterization, and application of welldefined single-component group ten salicylaldimine complexes for the polymerization of ethylene to high molecular weight materials as well as the copolymerization of ethylene and functionalized olefins. After an initial introduction to the field, Chapter 2 describes the preparation of PPh3 complexes that contain a series of modified salicylaldimine and naphthaldimine ligands. Such complexes were activated for polymerization by the addition of cocatalysts such as Ni(COD)2 or B(C6F5)3. As the steric demand of the ligand set increased-the molecular weight, polymerization activity, and lifetime of the catalyst was observed to increase. In fact, complexes containing "bulky" ligands, such as the [Anthr,HSal] ligand (2.5), were found to be highly-active single component complexes for the polymerization of ethylene. Model hydrido compound were prepared-allowing for a better understanding of both the mechanism of polymerization and one mode of decomposition.
Chapter 3 describes the effect which additives play on neutral NiII polymerization catalysts such as 2.5. The addition of excess ethers, esters, ketones, anhydrides, alcohols, and water do not deactivate the catalysts for polymerization. However, the addition of excess acid, thiols, and phosphines was observed to shut-down catalysis. Since excess phosphine was found to inhibit catalysis, "phosphine-free" complexes, such as the acetonittile complex (3.26), were prepared. The acetonitrile complex was found to be the most active neutral polymerization catalyst prepared to date.
Chapter 4 outlines the use of catalyst 2.5 and 3.26 for the preparation of linear functionalized copolymers containing alcohols, esters, anhydrides, and ethers. Copolymers can be prepared with γ-functionalized-α-olefins, functionalized norbornenes, and functionalized tricyclononenes, with up to 30 mol% comonomer incorporation.
Chapter 5 outlines the preparation of a series of PtII alkyl/olefin salicylaldimine complexes which serve as models for the active species in the NiII-catalyzed polymerization process. Understanding the nature of the M-olefin interaction as a the electronic and steric properties of the salicylaldimine ligand is varied has allowed for a number of predictions about the design of future polymerization systems.
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杂化的纳米尺寸的有机/无机化合物开辟了材料科学的新纪元。作为新型功能材料,杂化的有机/无机杂化材料由于在光学、电子、机械、防护涂层、催化、传感器、生物等方面有潜在的应用前景而在材料科学领域引起广泛关注。杂多酸(POMs)作为一种重要的无机化合物,有特异的纳米尺寸结构,优越的物理化学性质和广泛应用价值,因此多酸化合物功能材料的研究引起人们足够的重视。最近,人们把更多的注意力集中到杂化的有机/无机杂化材料范围内,如何更有序的组装杂多酸,因为它们有着更有趣的电、磁、氧化还原和光学性质。1.在4-氨基苯甲酸修饰的玻碳电极表面,我们用层层组装方法制备了六钒取代的理杂多酸(PW6V6)多层膜。表面等离子(SP)技术和循环伏安(CV)法对多层膜进行了表征。结果表明,多层膜生长均匀,平均厚度为2.8nm,并且研究了多层膜对亚硝酸根伽02一)和浪酸根(BrO3-)的催化还原活性。2.研究了通过静电吸附作用,P2W17Fe和QPvP-Os交替组装多层膜。循环伏安(CV),电化学交流阻抗谱(EIS)和紫外一可见光谱(UV-vis)研究结果表明了这种多层膜是均一稳定的。多层膜对H2O2,BrO3-和NO2-有很高的催化活性。特别是EIS成功地监测多层膜的形成过程。随着层数增长,电子传输阻抗Rc,线性增加,氧化还原电对Fe(CN)63/4的电子传输受到抑制,这进一步证实了多层膜的均一性。3,首次在4-氨基苯甲酸修饰的玻碳电极表面成功地构建了含杂多酸P2W15V3的多层膜。值得注意的是,该多层膜对BrO3-和NO2-的还原有显著的电催化活性,而且由于过渡金属钒在P2W15V3起催化作用而有很低的过电位。另外,多层膜中QPVP-O5聚合物的Os中心在抗坏血酸氧化时的催化活性仍然存在,而且通过最外层的调整,多巴胺和抗坏血酸能被分别检测,所以在多巴胺存在时它可用作检测抗坏血酸的电化学传感器。4.迄今为止,人们把更多的注意力集中在杂多酸多层膜的制备,电化学和电催化活性的研究,对杂多酸多层膜功能材料的研究却很少,我们首次够构造了发光的杂多酸多层膜,紫外可见光谱,循环伏安,电化学阻抗技术和荧光光谱证明多层膜生长均匀,室温下,多层膜的发光性能显示Eu3+的特征发射峰是5D0→7Fj(j=1,2,3,4)的跃迁。电化学阻抗谱被成功得应用于监测多层膜的沉积过程。我们发现随多层膜的逐步形成,半圆直径有规律地长大。而且,电荷迁移电阻Rc,随双层数线性增长。可以认为多层膜在基底电极上以非常均匀规律的方式沉积,Fe(CN)63/4氧化还原电对的氧化还原反应逐步被多层膜抑制。5.我们用层层组装方法成功构造了金纳米粒子多层膜,紫外可见光谱,循环伏安和原子力显微技术表征了多层膜的形成,金纳米粒子粒径大约14nm,表面粗糙度6.43nm。
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In this paper, the characterization and application of a chemically reduced graphene oxide modified glassy carbon (CR-GO/GC) electrode, a novel electrode system, for the preparation of electrochemical sensing and biosensing platform are proposed. Different kinds of important inorganic and organic electroactive compounds (i.e., probe molecule (potassium ferricyanide), free bases of DNA (guanine (G), adenine (A), thymine (T), and cytosine (C)), oxidase/dehydrogenase-related molecules (hydrogen peroxide (H2O2/beta-nicotinamide adenine dinucleotide (NADH)), neurotransmitters (dopamine (DA)), and other biological molecules (ascorbic acid (AA), uric acid (UA), and acetaminophen (APAP)) were employed to study their electrochemical responses at the CR-GO/GC electrode, which shows more favorable electron transfer kinetics than graphite modified glassy carbon (graphite/GC) and glassy carbon (GC) electrodes.
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工业的高速发展使地球上有限的水资源受到日益严重的污染,去除水中的有毒、有害化学物质已成为环保领域的一项重要工作。纳米材料与技术的开发应用为实现高效、低成本的水处理开辟了新的途径。 本课题组开发的纳米-亚纳米功能新材料(生态宝)可用作养殖生态环境改良剂,它对“三氮”、硫化物、CODCr、BOD5、重金属等有害物质具有很好的去除能力。生态宝用于养殖幼参,有显著的促生长、增加成活率的作用。生态宝用于养殖对虾,对虾体内重金属含量有明显降低。 以粉末状P25型纳米TiO2为光催化剂,系统的研究了它对染料AB80的光催化降解。在紫外光照射下,光催化反应75min,染料AB80溶液完全脱色,光催化反应135min,染料溶液完全矿化;AB80的光催化脱色反应遵从准一级反应动力学;催化剂的最佳剂量为1.0g/L。AB80在TiO2颗粒表面的吸附符合Langmuir方程式,随着pH值的增加吸附量迅速减少;pH值在反应中起着重要的作用,碱性溶液中的反应速度比酸性溶液的大,pH=10.0初始反应速度最大;电子捕获剂(H2O2)的加入能够显著的提高反应速率,H2O2浓度为5mmol/L时,反应速度变为原来的2.78倍。 以硅藻土为载体,采用溶胶-凝胶法制备了负载型的纳米TiO2,SEM分析结果表明,TiO2的包覆量对负载光催化剂的形貌有很大影响,TiO2包覆量较低(14.5%)的复合物无团聚现象发生。XRD分析结果表明,所制备的TiO2为锐钛矿和金红石混晶型,平均粒径11nm。FT-IR分析结果表明,TiO2和硅藻土之间没有生成化学键。以染料AB80和B-2BF为模型污染物,利用制备的光催化剂复合物进行了吸附-光催化试验,结果表明,TiO2包覆量为14.5%的复合物具有较高的吸附-光催化活性,对模型污染物的降解效果好于德国Degussa公司的商品纳米P25-TiO2。溶液pH对TiO2/硅藻土复合物光催化活性影响很大,弱酸性条件有利于反应的进行。TiO2/硅藻土对实际印染废水有较好的降解效果,试验条件下,废水光催化反应3.5h,色度去除率为100%。研究了液固多相光催化反应的催化剂失活原因及再生手段,提出TiO2/硅藻土复合物再生的方法为酸洗和高温烧结。对于模拟印染废水来说,光催化剂重复使用对光催化活性几乎没有影响,重复使用15次后,催化活性仅降低了12%。而对实际印染废水来说,重复使用对光催化活性有影响,光催化剂复合物重复使用7次后,催化活性降低了41%。TiO2/硅藻土复合光催化剂成本低,简便易行,光催化效果好,有望在环境污染物治理中得到广泛的应用。 采用CuCl水解法制得了硅藻土负载的纳米Cu2O,并利用XRD、SEM等手段对其进行表征。研究了负载的纳米Cu2O对B-2BF和AB80染料废水的光催化降解,发现纳米Cu2O经过负载后,团聚减少,分散性好,对染料废水的光催化降解效率成倍增长。纳米Cu2O包覆量为31.3%的光催化剂复合物光催化活性最好,其光催化效率是纯的Cu2O的6倍。负载的纳米Cu2O可以有效的利用太阳光进行光催化反应,而且太阳光下纳米Cu2O的光催化活性比纳米TiO2的强。太阳能是取之不尽、用之不竭的清洁能源,利用太阳能来处理染料废水成本低、无污染,是一种非常有发展前景的环境治理新技术。pH 5-pH 7是负载纳米Cu2O光催化降解B-2BF的最佳反应范围。负载的纳米Cu2O光催化剂有较好的稳定性,重复使用8次以后,其脱色率仍能达到75%以上。
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Monografia apresentada à Universidade Fernando Pessoa para obtenção do grau Licenciada em Ciências Farmacêuticas
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Este trabalho teve como objetivos a produção, caracterização e aplicação de microelétrodos (MEs) de diamante como sensores amperométricos e potenciométricos em sistemas de corrosão nos quais a agressividade do meio e a presença de produtos de corrosão, constituem obstáculos que podem diminuir o desempenho, ou inviabilizar a utilização, de outros tipos de sensores. Os microeléctrodos são baseados em filmes finos de diamante dopado com boro (BDD – Boron Doped Diamond) depositados sobre fios de tungsténio afiados, através do método de deposição química a partir da fase vapor, assistida por filamento quente (HFCVD – Hot Filament Chemical Vapor Deposition). A otimização das diversas etapas de fabricação dos MEs deu origem ao desenvolvimento de um novo sistema de afiamento eletroquímico para obtenção destes fios e a várias opções para a obtenção dos filmes de diamante condutor e seu isolamento com resinas para exposição apenas da ponta cilíndrica. A qualidade cristalina dos filmes de diamante foi avaliada por espectroscopia de Raman. Esta informação foi complementada com uma caracterização microestrutural dos filmes de diamante por microscopia eletrónica de varrimento (SEM), em que se fez a identificação da tipologia dos cristais como pertencendo às gamas de diamante nanocristalino ou microcristalino. Os filmes de BDD foram utilizados na sua forma não modificada, com terminações em hidrogénio e também com modificação da superfície através de tratamentos de plasma RF de CF4 e O2 indutores de terminações C-F no primeiro caso e de grupos C=O, C-O-C e C-OH no segundo, tal como determinado por XPS. A caracterização eletroquímica dos MEs não modificados revelou uma resposta voltamétrica com elevada razão sinal/ruído e baixa corrente capacitiva, numa gama de polarização quasi-ideal com extensão de 3 V a 4 V, dependente dos parâmetros de crescimento e pós-tratamentos de superfície. Estudou-se a reversibilidade de algumas reações heterogéneas com os pares redox Fe(CN)6 3-/4- e FcOH0/+ e verificou-se que a constante cinética, k0, é mais elevada em elétrodos com terminações em hidrogénio, nos quais não se procedeu a qualquer modificação da superfície. Estes MEs não modificados foram também testados na deteção de Zn2+ onde se observou, por voltametria cíclica, que a detecção da redução deste ião é linear numa escala log-log na gama de 10-5-10-2 M em 5 mM NaCl. Realizaram-se também estudos em sistemas de corrosão modelares, em que os microeléctrodos foram usados como sensores amperométricos para mapear a distribuição de oxigénio e Zn2+ sobre um par galvânico Zn-Fe, com recurso a um sistema SVET (Scanning Vibrating Electrode Technique). Foi possível detetar, com resolução lateral de 100 μm, um decréscimo da concentração de O2 junto a ambos os metais e produção de catiões de zinco no ânodo. Contudo verificou-se uma significativa deposição de zinco metálico na superfície dos ME utilizados. Os MEs com superfície modificada por plasma de CF4 foram testados como sensores de oxigénio dissolvido. A calibração dos microeléctrodos foi efetuada simultaneamente por voltametria cíclica e medição óptica através de um sensor de oxigénio comercial. Determinou-se uma sensibilidade de ~0.1422 nA/μM, com um limite de deteção de 0.63 μM. Os MEs modificados com CF4 foram também testados como sensores amperométricos com os quais se observou sensibilidade ao oxigénio dissolvido em solução, tendo sido igualmente utilizados durante a corrosão galvânica de pares Zn-Fe. Em alguns casos foi conseguida sensibilidade ao ião Zn2+ sem que o efeito da contaminação superficial com zinco metálico se fizesse sentir. Os microeléctrodos tratados em plasma de CF4 permitem uma boa deteção da distribuição de oxigénio, exibindo uma resposta mais rápida que os não tratados além de maior estabilidade de medição e durabilidade. Nos MEs em que a superfície foi modificada com plasma de O2 foi possível detetar, por cronopotenciometria a corrente nula, uma sensibilidade ao pH de ~51 mV/pH numa gama de pH 2 a pH 12. Este comportamento foi associado à contribuição determinante de grupos C-O e C=O, observados por XPS com uma razão O/C de 0,16. Estes MEs foram igualmente testados durante a corrosão galvânica do par Zn-Fe onde foi possível mapear a distribuição de pH associada ao desenvolvimento de regiões alcalinas causadas pela redução do oxigénio, acima da região catódica, e de regiões ácidas decorrentes da dissolução anódica do ânodo de zinco. Com o par galvânico imerso em 50 mM NaCl registou-se uma variação de pH aproximadamente entre 4,8 acima do ânodo de zinco a 9,3 sobre o cátodo de ferro. A utilização pioneira destes MEs como sensores de pH é uma alternativa promissora aos elétrodos baseados em membranas seletivas.
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Les fichiers additionnels sont les données cristallographiques en format CIF. Voir le site de la Cambridge Crystallographic Data Centre pour un visualiseur: http://www.ccdc.cam.ac.uk
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Biodiesel is an alternative fuel, renewable, biodegradable and nontoxic. The transesterification of vegetable oils or animal fat with alcohol is most common form of production of this fuel. The procedure for production of biodiesel occurs most commonly through the transesterification reaction in which catalysts are used to accelerate and increase their income and may be basic, acid or enzyme. The use of homogeneous catalysis requires specific conditions and purification steps of the reaction products (alkyl ester and glycerol) and removal of the catalyst at the end of the reaction. As an alternative to improve the yield of the transesterification reaction, minimize the cost of production is that many studies are being conducted with the application of heterogeneous catalysis. The use of nano-structured materials as catalysts in the production of biodiesel is a biofuel alternative for a similar to mineral diesel. Although slower, can esterify transesterified triglycerides and free fatty acids and suffer little influence of water, which may be present in the raw material. This study aimed at the synthesis, characterization and application of nano-structured materials as catalysts in the transesterification reaction of soybean oil to produce biodiesel by ethylic route. The type material containing SBA-15 mesoporous lanthanum embedded within rightly Si / La = 50 was used catalyst. Solid samples were characterized by X-ray diffraction, thermogravimetric analysis, infrared spectroscopy, nitrogen adsorption and desorption. For the transesterification process, we used a molar ratio of 20:1 alcohol and oil with 0.250 g of catalyst at 60°C and times of 6 hours of reaction. It was determined the content of ethyl esters by H-NMR analysis and gas chromatography. It was found that the variable of conversion obtained was 80%, showing a good catalytic activity LaSBA-15 in the transesterification of vegetable oils via ethylic route
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The program PROBIODIESEL from the Ministry of Science and Technology has substantially increased glycerine, obtained as a sub-product of biodiesel production process, making it necessary to seek alternatives for the use of this co-product. On the other hand, herbicides although play a role of fundamental importance in the agricultural production system in force, have been under growing concern among the various segments of society because of their potential environmental risk. In this work, we used glycerin in microemulsion systems for application of herbicides, to improve efficiency and lower environmental pollution caused by the loss of those products to the environment. To obtain the systems of microemulsinados were used Unitol L90 NP and Renex 40 as surfactants, butanol as co-surfactant, coconut oil as oil phase and aqueous phase as we used solutions of glycerin + water. Through the determination of phase diagrams, the microemulsion region was found in the system E (L90 Unitol, coconut oil and glycerin + water 1:1). Three points were chosen to the aqueous phase rich in characterization and application in the solubilization of glyphosate and atrazine. Three experiments were performed in Horta, Department of Plant Sciences, Plant Science Sector, UFERSA, Mossoró-RN. The first experiment was conducted in randomized complete blocks with 20 treatments and four replications. The treatments consisted of five doses of the herbicide glyphosate (0.0, 0.45, 0.9, 1.35 and 1.8 L ha-1) diluted with four sauces: C1, C2, C3 (microemulsions) and C4 (water). The phytotoxicity of Brachiaria brizantha was measured at 7, 14, 28 and 60 DAA (days after application). At 60 DAA, we evaluated the biomass of plants. The second experiment was developed in randomized complete blocks with 20 treatments and four repetitions. The treatments consisted of five doses of the herbicide atrazine (0.0, 0.4, 0.8, 1.6 and 2.4 L ha-1) diluted with four sauces: C1, C2, C3 (microemulsions) and C4 (water). The phytotoxicity on Zea mays and Talinum paniculatum was evaluated at 2, 7, 20 DAA. The experiment III was developed in randomized complete blocks with 16 treatments and three repetitions. The treatments consisted of 16 combinations among the constituents of the microemulsion: Unitol L90 surfactant (0.0, 1.66, 5.0, 15 %) and glycerin (0.0, 4.44, 13.33 and 40.0 %). The phytotoxicity on Zea mays was evaluated at 1, 7 and 14 DAA. At 14 DAA, we evaluated the biomass of plants. The control plants using the microemulsions was lower than in the water due to the poisoning caused by the initial microemulsions in the leaves of the plants, a fact that hinders the absorption and translocation of the herbicide. There was no toxicity in Zea mays plants caused by the herbicide, however, were highly intoxicated by microemulsions. T. paniculatum was better controlled in spraying with the microemulsions, regardless of the dose of the herbicide. The glycerine did not cause plant damage. Higher poisoning the plants are caused by tensoactive Unitol L90 and higher rates occur with the use of higher concentrations of surfactant and glycerin, or microemulsion. The microemulsions used hampered the action of glyphosate in controlling B. brizantha and caused severe poisoning in corn, and these poisonings attributed mainly to the action of surfactant
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This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d