Proposta metodológica para otimização experimental de formulações : um estudo de caso no setor alimentício

Esta dissertação de mestrado tem por objetivo apresentar uma metodologia para planejamento e análise de experimentos com formulações, em um contexto de múltiplas variáveis de resposta, para aplicação em indústrias alimentícias de pequeno porte que se caracterizam por utilizar métodos empíricos, ou seja, tentativa e erro, no desenvolvimento de seus produtos. A utilização de Projeto de Experimentos com Formulações, como ferramenta estatística de suporte no desenvolvimento de produtos formulados, tem como objetivo otimizar o planejamento, execução e análise dos experimentos, permitindo que a seqüência de ensaios seja estruturada adequadamente, de forma a traduzir os objetivos a serem atingidos. A metodologia proposta neste trabalho apoia-se nessa ferramenta estatística e põe grande ênfase nas fases de identificação do problema e planejamento, fases nas quais a criatividade do investigador tem uma função muito importante. A metodologia proposta é ilustrada através de um estudo de caso. As etapas do estudo de caso envolvem: identificação do problema; planejamento do experimento; execução do experimento; seleção das melhores rodadas experimentais quanto a características de qualidade sensoriais através de uma análise sensorial comparativa com um produto similar líder de mercado (benchmarking); modelagem individual das variáveis de resposta e definição de uma função objetivo e otimização. A aplicação de Projetos de Experimentos fez-se através da utilização de variáveis independentes, tomando o método adaptável a situações onde há algum tipo de restrição. O desenvolvimento do produto, apresentado no estudo de caso, fez-se em um ambiente de Engenharia Simultânea, propiciado pelas características multifuncionais próprias das empresas em questão, reduzindo substancialmente o tempo de desenvolvimento do novo produto, por meio da realização das várias fases do projeto de forma simultânea.

Desenvolvimento de formulações para produção de grés porcelanato a partir de matérias-primas da região da bacia do Parnaíba

Brazil is a great ceramic raw materials productor because of the its big number of clay deposits, in various areas of the ceramic industry. Although, the majority of the natural reservations are unknown or not studied yet, so there is no scientific technical dates that can guide their usage and industrial application, as well as the racional and optimazed way of usage by the industrial sector. The state of Maranhão has a gigant mineral wealth as esmectite, bentonite, kaolin, clays, feldspates, marine salt, iron and others, but produce only products with small agregated value compared to the porcelanato, one of the most expensives ceramic cover tiles, the reason for that is the low water absorption (lower than 0,5%), beside present amazing tecnicals features, like mechanical resistence. The main objective of the work is to do the characterization of four clays, with the finallity of find an application by the results and develop formulations to produce porcelanato using these raw materials from Timon-MA. For this were made the raw materials characterization using X ray fluorecence; X ray diffraction; Differencial thermal analysis; Dilatometric analysis and Tecnological properties, planing three formulations that were sinterized at six different temperatures: 1150, 1170, 1190, 1210, 1230 and 1250ºC for 7 minutes. After the sinteratization, the samples were submitted to tension resistance analysis. Were attained two formulations with the requested properties to produce porcelanato

Estudo da incorporação de cascalho proveniente da perfuração de poços de petróleo em formulações para tijolos de solo-cimento

The present work is to study the characteristics and technological properties of soil-cement bricks made from binary and ternary mixtures of Portland cement, sand, water, with or without addition of gravel from the drilling of oil wells, which could be used by industry, aiming to improve its performance and reduce cost by using the residue and, consequently, increasing its useful life. The soil-cement bricks are one of the alternatives to masonry construction. These elements, after a short curing period, provide compressive strength similar to that of solid bricks and ceramic blocks, and the higher the resistance the higher the amount of cement used. We used the soil from the city of São José do Mipibu / RN, the banks of the River Baldun, cement CPIIZ-32 and residue of drill cuttings from oil wells drilling onshore wells in the town of Mossley, RN, provided Petrobras. To determine the optimum mix, we studied the inclusion of different residues (100%, 80%, 70%, 60% and 50%) where 15 bodies were made of the test piece. The assessment was made of bricks made from simple compression tests, mass loss by immersion and water absorption. The experimental results proved the efficiency and high utilization of the waste from the drilling of oil wells, making the brick-cement-soil residue with a higher strength and lower water absorption. The best result in terms of mechanical strength and water absorption for the ternary mixture was 10% soil, 14% cement and 80% residue. In terms of binary mixtures, we obtained the best result for the mix-cement residue, which was 14% cement incorporated in the residue

Avaliação da potencialidade dos resíduos de gesso de revestimento incorporados em formulações de massas cerâmicas

In building, during the implementation process of major or even minor works, there is a considerable waste of plaster in the steps of coating, making it is a negative factor because of the loss of these processes constructive remains incorporated into buildings, as component, whose final dimensions are higher than those projected. Another negative factor is the disposal of waste gypsum in inappropriate places, thus contributing to the degradation of environmental quality, due to the leaching of this waste and may trigger the formation of sulfuric acid. Therefore, based on this picture, processing and reuse of waste coating, combined with the ceramics industry, which is a strong potential in the reuse of certain types of waste, promote mutual benefits. Thus the overall objective of this work is to conduct a search with scientific and technological aspects, to determine the effect of the incorporation of the residue of plaster for coating, from the building, the formulation of bodies for red ceramic. The residue of plaster coating was collected and characterized. They were also selected raw materials of two ceramic poles of the state of Rio Grande do Norte and formulations have been made with the intention of obtaining those with the best physical and mechanical properties, the residue was added the percentage of 5%, 10%, 15%, 20%, 25% and 30%, in the best formulation of ceramic industry 1 and, according the properties analyses, 5%, 10% and 15% as the best results of ceramic industry 2. The samples were sintered at temperatures of 850 ºC, 950 °C and 1050 °C, the heating rate of 5 ºC / min with isotherm of two hours. They were submitted to testing technology, such as lineal shrinkage, water absorption, apparent porosity, apparent density and bending resistence. The residue incorporation best results in the formulations of mass in red ceramic, were observed between the temperatures of 850 ºC and 950 ºC, in those formulations that have illite clays and medium plastic in their composition, in the range of 0% to 15% residue incorporated

Efeito da adição de feldspato e/ou resíduo de caulin em formulações à base de argila ilítica

The red pottery industry in Piauí state is well developed and stands out at the national context for the technical quality of its products. The floor and wall tile industry, however, is little developed since the state has only one company that produces red clay-based ceramic tiles. This thesis aims at using the predominantly illitic basic mass of the above mentioned industry, with the addition of feldspar and/or kaolin residue in order to obtain products of higher technical quality. Kaolin residue consists basically of kaolinite, muscovite mica and quartz; the feldspar used was potassic. In this experiment, basic mass (MB) was used for experimental control and fifteen formulations codified as follows: F2, F4, F8, F16, F32, FR2, FR4, FR8, FR16, FR32, R2, R4, R8, R16 and R32. All raw materials were dry-milled, classified, formulated and then humidified to 10% water. Thereafter, test samples were produced by unixial pressing process in a rectangular steel matrix (60.0 x 20.0 x 5.0) mm3 at (25 MPa). They were fired at four temperatures: 1080°C, 1120°C, 1160°C, with a heating rate of 10°C/min during up to 10 min in an electric oven, and the last one in an industrial oven with a peak of 1140°C, aim ing to confirm the results found in laboratory and, finally, technological tests were performed: MEA, RL, AA, PA, TRF and PF. The results revealed that the residue under study can be considered a raw material with large potential in the industry of red clay-based ceramic tiles, since the results found both in laboratory and in the industry have shown that the test samples produced from the formulations with up to 4% feldspar and those produced with up to 8% feldspar and residue permitted a reduction in the water absorption rate and an increase in the mechanical resistance while those samples produced with up to 4% residue had an increase in the mechanical resistance when compared to those produced from the basic mass and that the formulation with 2% feldspar and residue presented the best technological properties, lowering the sintering temperature down to 1120°C

Uso de resíduo e de minerais de pegmatito da região do seridó RN e de argilas portuguesas em formulações de grês porcelanato

In the State Rio Grande do Norte, Brazil, the most significant deposits of minerals in the production of granite and pegmatite are Seridó region. Municipalities of Parelhas and Equador are the main responsible for the production of feldspar, quartz, kaolin and granite. The ceramic industries are always in search of competitiveness by investing in new products or improving existing techniques. The stoneware is a type of pottery that stands in the market because it presents technical and aesthetic characteristics superior to other existing products. Characteristics of the raw materials initially obtained with chemical analysis and mineralogical analysis are crucial in getting a product that satisfies the conditions in a manufacturing process and is, in principle, directly related to the firing cycle. This research aimed at developing new formulations for the mass production of ceramic stoneware. The raw materials initially characterized were feldspar, quartz, kaolin and granite. As part of the research was developed at the University of Aveiro, in Portugal, we used two clays used in the production of Portuguese ceramics. The raw material Brazilian and Portuguese and the final product, both in Portugal and Brazil, were analyzed for X-ray fluorescence, X-ray diffraction, granulometric analysis, dilatometric analysis, thermal analysis and analysis of scanning electron microscopy (MEV). The specimens prepared at the University of Aveiro (DECV) were sintered at 10000C and 12000C and the specimens prepared in UFRN were sintered at 10000C, 10500C, 11000C, 11500C, 12000C, 12500C and 13000C, but the best results and demonstrating the presence of the mineral mullite were at temperatures of 12000C, 12500C and 13000C. The results showed that the granite waste used may be considered raw material of excellent quality for use in the ceramic industry and coating floors and more accurately by the industry of stoneware. Physical and mechanical tests conducted on samples of the formulations F01 and F02 developed in UFRN showed a water absorption and mechanical strength suitable for the stoneware

Momento da chuva após a aplicação e a eficácia dos herbicidas sulfosate e glyphosate aplicados em diferentes formulações

Com o objetivo de estudar a influência da chuva sobre o desempenho dos herbicidas sulfosate e glyphosate em diferentes formulações, foram conduzidos dois experimentos, um no inverno de 2000 e outro no verão de 2001, na Fazenda Experimental de Ensino e Pesquisa da Faculdade de Ciências Agrárias e Veterinárias, Campus de Jaboticabal-SP. Os experimentos foram instalados segundo o delineamento experimental de blocos ao acaso, com quatro repetições, no arranjo fatorial de 4x5+1, ou seja, quatro tratamentos de herbicidas, cinco períodos sem chuva após a aplicação e uma testemunha, que não recebeu chuva. As formulações de glyphosate foram: SAqC (1,0 L ha-1), GrDA (0,5 kg ha-1), SAqC Transorb (0,75 L ha-1), mais o sulfosate SAqC (1,09 L ha¹). Os períodos sem chuva após a aplicação foram de 1, 2, 4, 6 e > 48 horas. Os herbicidas foram aplicados em pós-emergência das plantas daninhas, utilizando-se de um pulverizador costal, à pressão constante (mantida por ar comprimido) de 30 lbf pol-2. A chuva foi simulada com um sistema de irrigação por aspersão. A lâmina de água variou entre 18 e 19 mm. em ambas as épocas, a chuva simulada foi prejudicial à ação dos herbicidas, principalmente quando feita nos menores intervalos após a aplicação. Os sintomas de fitointoxicação apareceram mais rapidamente no verão. A formulação Transorb, comercializada como não sendo afetada pela chuva uma hora após a aplicação, não teve o desempenho esperado, tanto no inverno quanto no verão, para períodos de até seis horas sem chuva após a aplicação. O sulfosate apresentou o melhor controle geral das plantas avaliadas, quando se simulou chuva após seis horas, em ambas as épocas. A formulação GrDA foi a mais afetada pela ação da chuva em ambas as épocas.

Eficácia de diferentes formulações no controle da mosca haematobia irritans em bovinos naturalmente infestados

This study evaluated the effectiveness of cypermethrin (5%) associated to Dichlorvos (45%) and piperonyl butoxide (25%) against Haematobia irritans in naturally infested cattle. 60 Nelore females, aging about 50 months, were separated into four groups with 15animals each. After randomization by the number of flies, the groups were divided in the following treatments: T1 = control, T2 and T4 = treated with the association under study at concentrations of 1: 400 and 1: 800, respectively, T3 = treated with cypermethrin 15% + clorpirivos 25% + citronella 1% (positive control) at a concentration of 1:800. Counst of flies were taken 3, 7, 14 and 21 days post treatment (DPT). In the third DPT, treatments T2, T3 and T4 showed efficacy over 98%. At the seventh day, it was found in animals treated with the compound containing piperonyl butoxide efficacy of 95.61 and 97.3% in the control of flies at dose of 1: 800 and 1: 400, respectively. While cattle in the T3 group demonstrated efficacy of 93.82%. The effectiveness of antiparasitic remained above 95% at 14 degrees DPT in both groups T2 and T4. In the same experimental day, animals of group T3 showed effectiveness of 88.24%. At 21 degrees DPT, only the T2 group, was significantly decreased (P <0.05) in the number of flies when compared to other treatments. Therefore, it was found in this study, the synergistic effect of piperonyl butoxide on the antiparasitic activity of synthetic pyrethroids and organophosphates, representing an effective alternative in the chemotherapy control by the parasitism for horn flies in cattle.

Acúmulo de nutrientes e matéria seca na parte aérea de dois cultivares de soja RR sob efeito de formulações de glyphosate

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

Obtenção de placas cerâmico a partir de formulações de massas triaxiais de resíduos de caulim, chamote de telha e cinza vegetal

The production of red ceramic is an industrial activity that causes an intense impact. The manufacture of its products considerably increases the demand for natural resources, mainly with the extraction of raw material. The ceramic material produced generates waste, such as ash firewood and chamote. The residue from the beneficiation of kaolin is deposited in a poor, degrades the environment and contaminate water sources and soil, constituting in this manner, ecological disasters. The main objective of this work is to develop the formulation of a ceramic product consisting solely of industrial solid wastes, from ceramic tiles, (chamote) residue of kaolin and ash firewood. It is assumed that this product made in the laboratory can be used in coatings, wall and floor. The aim is to facilitate the replacement of the raw material of original composition of a ceramic body, for waste, while the process of production equal to the conventionally used, so that the properties of the product are reproduced. This work is characterized waste as its chemical composition, analysis of particle size, X-ray diffraction and thermal behavior. Several formulations were studied. The mass of waste was prepared by dry process, pressed to 25 MPa, and then burned in muffle type oven to 850, 950, 1050 and 1150 °C. The results showed that it is technically possible to produce porous tiles only with waste. It was found that the formulations of bodies play a key role in the properties of the final product, as well as the sintering temperature and heating rates. RN in the waste of kaolin is estimated at 15,000 t/month, about 3,000 gray t/month and chamote with 10 million pieces/month damaged. The presence of carbonates of calcium and magnesium at 1050 ° C results in an appropriate porosity and mechanical strength. The formulation M3JE, composed of 69% waste of kaolin, 7.7% and 23.3% of chamote of gray, became suitable for porous materials with the strength and absorption within the level of national and international standards

Caracterização de matérias-primas regionais e desenvolvimento de formulações de massas cerâmicas para porcelanato

Initially concentrated in some poles at the South and Southeast regions of Brazil, the ceramic tiles industry became wide during the 80 s decade, with a disconcentration industrial and regional pulverization. The competitiveness in the ceramic tiles internal and external consumers markets, it has debtor the industries to invest in sophisticated products each time more, either in design or the technology, but, mainly, in its final properties. Amongst the diverse types of ceramic coating, the porcelanato if has detached had to its process of technological production and excellent characteristics techniques. The Porcelanato is currently the material for coatings that presents the best technical and aesthetic features when compared with others ceramics found on the market. The chemical composition and the others raw materials characteristics have an importance that must to be ally to the inherent characteristics of fabrication process, essentially those related to the cycle of burning. This work had as purpose to develop formularizations of ceramic mass for production of porcelanato without glass coating, pertaining to the group BIa (text of absorption of water ≤ 0.5%) and with resistance superior mechanics 35MPa from raw materials characterized. The ceramic raw materials selected to the development of this study (A1 and A2 clays, feldspate, talc and quartz) were submitted to the following tests: X-ray fluorescence - chemical analysis determination; X-ray diffraction - Analysis of the stages mineralogics; Laser granulometry - size distribution of particles; and Differential thermal analysis - thermal behavior. Were performed tests of absorption of water, lineal retraction of it burns, apparent specific mass and rupture tension the flexing. The results had evidenced that the formularizations that had the A1 clay and talc on its composition were efficient for the porcelanato production remaining their technological characteristics inside of the intervals of variation desired by the Norms of the ABNT

Estudo da introdução de resíduo de britagem de rocha calcária e cinza de biomassa de cana-de-açúcar em formulações de argamassas colantes

The adhesive mortars are a mixture of cement, sand, and additives to polymers that retain the mixing water and promotes adherence, being used in setting on various ceramic substrates. The sand used in the production of these mortars is from the riverbeds, and with the increasing restriction of these sands extraction by environmental agencies, and often having to be transported over long distances to the consumer center. This work aims to design and physical and mechanical characterization of ecological adhesive mortar with total replacement of natural sand by sand from the crushing of limestone, and the addition of mineral ash biomass of cane sugar in partial replacement cement used in the production of adhesive mortar , aiming compositions that meet the regulatory specifications for use adhesive mortar. Standardized tests to determine the tensile bond strength (NBR 14081-4), determination of open time (NBR 14081-3) and determination of slip (NBR 14081-5) were performed. Were also conducted trials squeeze flow in different formulation, the mortar with addition of 15 % gray biomass of cane sugar for cement mortars as well as the total replacement of natural sand by sand limestone crushing, got the best performance among the mortars studied, it was found that the addition of biomass to replace cement is perfectly feasible due to its pozzolanic activity, which contributed to this reduction in the cement matrix formation of adhesive mortar

Novas formulações de fluidos de corte: otimização, propriedades e recuperação do óleo usado

Cutting fluids are lubricants used in metal-mechanical industries. Their complex composition varies according to the type of operation carried out, also depending on the metals under treatment or investigation. Due to the high amount of mineral oil produced in Northeastern Brazil, we have detected the need to better use this class of material. In this work, two novel formulations have been tested, both based on naphthenic mineral oil and additives, such as: an emulsifying agent (A), an anticorrosion agent (B), a biocide (C) and an antifoam agent (D). Each formulation was prepared by mixing the additives in the mineral oil at a 700-rpm stirring velocity for 10 min, at 25°C, employing a 24 factorial planning. The formulations were characterized by means of density, total acid number (TAN), viscosity, flash point and anticorrosion activity. In a subsequent study, oil-in-water emulsions were prepared from these novel formulations. The emulsions were analyzed in terms of stability, corrosion degree, percentage of foam formation, conductivity, accelerated stability and particle size. The samples were appropriately labeled, and, in special, two of them were selected for featuring emulsion properties which were closer to those of the standards chosen as references (commercial cutting oils). Investigations were undertaken on the ability of NaCl and CaCl2 to destabilize the emulsions, at concentrations of 2%, 5% and 10%, at an 800-rpm stirring velocity for 5 min and temperatures of 25º, 40º, 50º and 60ºC. The recovered oils were chemically altered by reincorporating the same additives used in the original formulations, followed by preparation of emulsions with the same concentrations as those of the initial ones. The purpose was to assess the possibility of reusing the recovered oil. The effluents generated during the emulsion destabilization step were characterized via turbidity index, contents of oil and grease, pH, and contents of anions and cations, observing compliance with the parameters established by the current environmental legislation (Brazil s CONAMA 357/05 resolution). It could be concluded that the formulations presented excellent physicochemical properties as compared to commercial cutting fluids, showing that the quality of the newly-prepared fluids is superior to that of the formulations available in the market, enabling technically and environmentally-safe applications

Análise do comportamento de queima de argilas e formulações para revestimento cerâmico

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