Experimento didático de quimiometria para planejamento de experimentos: avaliação das condições experimentais na determinação espectrofotométrica de ferro II com o-fenantrolina. Um tutorial, parte III

The objective of this manuscript is to describe a practical experiment that can be employed for teaching concepts related to design of experiments using Matlab or Octave computing environment to beginners, undergraduate and graduate students. The classical experiment for determination of Fe (II) using o-phenanthroline was selected because it is easy to understand, and all the required materials are readily available in most analytical laboratories. The approach used in this tutorial is divided in two steps: first, the students are introduced to the concept of multivariate effects, how to calculate and interpret them, and the construction and evaluation of a linear model to describe the experimental domain by using a 2³ factorial design. Second, an extension of the factorial design by adding axial points is described, thereby, providing a central composite design. The quadratic model is then introduced and used to build the response surface.

ANÁLISE EXPLORATÓRIA DAS CONCENTRAÇÕES DOS METAIS NA, CA, MG, SR E FE EM EXTRATO AQUOSO DE PETRÓLEO, DETERMINADOS POR ICP OES, APÓS OTIMIZAÇÃO EMPREGANDO PLANEJAMENTO DE EXPERIMENTOS

AbstractThe purpose of this study was to evaluate the best operating conditions of ICP OES for the determination of Na, Ca, Mg, Sr and Fe in aqueous extract of crude oil obtained after hot extraction with organic solvents (ASTM D 6470-99 modified). Thus, the full factorial design and central composite design were used to optimize the best conditions for the flow of nebulization gas, the flow of auxiliary gas, and radio frequency power. After optimization of variables, a study to obtain correct classification of the 18 samples of aqueous extract of crude oils (E1 to E18) from three production and refining fields was carried out. Exploratory analysis of these extracts was performed by principal component analysis (PCA), hierarchical cluster analysis (HCA) and linear discriminant analysis (LDA), using the original variables as the concentration of the metals Na, Ca, Mg, Sr and Fe determined by ICP OES.

Aplicação da metodologia de planejamento de experimentos para formulação de massas cerâmicas para telhas

Rio Grande do Norte State stands out as one great producer of structural clay of the brazilian northeastern. The Valley Assu ceramic tiles production stands out obtained from ilitics ball clays that abound in the region under study. Ceramics formulation and the design of experiments with mixture approach, has been applied for researchers, come as an important aid to decrease the number of experiments necessary to the optimization. In this context, the objective of this work is to evaluate the effects of the formulation, temperature and heating rate in the physical-mechanical properties of the red ceramic body used for roofing tile fabrication of the Valley Assu, using design of mixture experiments. Four clays samples used in two ceramics industry of the region were use as raw material and characterized by X-ray diffraction, chemical composition, differential thermal analysis (DTA), thermogravimetric analysis (TGA), particle size distribution analysis and plasticity techniques. Afterwards, they were defined initial molded bodies and made specimens were then prepared by uniaxial pressing at 25 MPa before firing at 850, 950 and 1050 ºC in a laboratory furnace, with heating rate in the proportions of 5, 10 e 15 ºC/min. The following tecnologicals properties were evaluated: linear firing shrinkage, water absorption and flexural strength. Results show that the temperature 1050 ºC and heating rate of 5 ºC/min was the best condition, therefore presented significance in all physical-mechanical properties. The model was accepted as valid based of the production of three new formulations with fractions mass diferents of the initial molded bodies and heated with temperature at 1050 ºC and heating rate of 5 ºC/min. Considering the formulation, temperature and heating rate as variables of the equations, another model was suggested, where from the aplication of design of experiments with mixtures was possible to get a best formulation, whose experimental error is the minor in relation to the too much formulations

Utilização de técnicas do planejamento de experimentos na otimização de um processo de torneamento da superliga NIMONIC 80A

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Planejamento de experimentos em blocos aplicado às propriedades mecânicas de arames de aço para molas

The purpose of this article is to demonstrate an application of the design of block experiments via analysis and multiple linear regression in the investigation of a steel thermal treatment process with multiple responses. The study aimed to design statistical models to predict the mechanical properties in SAE 9254 draw steel wires, with diameters of 2.00 mm and 6.50 mm, after quench hardening and tempering. For this purpose, process input variables (wire diameter, processing speed, tempering temperature and polymer concentration) were investigated regarding their influence on the material tensile strength, yield point and hardness. The results revealed that the mechanical properties of the steel wire are significantly influenced by the selected variables, and analysis of variance (ANOVA) was employed to validate the design of the statistical models. Multiple linear regression allowed for an appropriate representation of the process, and graphical analysis was found to be very useful in displaying the behavior of the multiple responses.

Uma aplicação do planejamento de experimentos e carta de controle em uma indústria de cosmésticos: ciclo DMAIC

Pós-graduação em Engenharia de Produção - FEB

Determinação por meio de planejamento de experimentos da influência do lixamento nas medidas de dureza com durômetro portátil de método UCI

The hardness has an important role in quality control, in research studies and metallurgical and mechanical specification, selection and comparison of various materials. This property is of extreme importance in the oil industry because it is a determining factor to ascertain the safety of the material used in pressure vessels and pipelines. Due to the inability to stop the equipment while checking the hardness, the hardness testers are widely used portable method UCI, its great advantage is the fact that an essay fast, simple realization and not be considered a non-destructive testing with a good relationship money. The objective is to determine if there is significant difference in hardness measurements between 80 and 1200 sandpaper using a portable hardness tester UCI method, the material applied in gas storage spheres composition ASTM 516 Gr 70. After determining the number of homogeneity, we performed the hardness profile to isolate the major factors influencing the hardness part: cold rolling and segregation of impurities. Factors Cooling and sanding were analyzed using the method of design of experiments (DOE), in which it was demonstrated that neither variables nor their interactions, has significant influence on the hardness measurements by portable MIC 10. This fact will lead to reduction in time and cost for surface preparation

Utilização de técnicas de planejamento de experimentos na análise de viabilidade de alterações no processo de pintura de grades Antracite em uma indústria automotiva

The search for better performance and competitive advantage in the current market scenario has made organizations keep their focus on quality planning and the use of effective techniques aimed at continuous improvement and optimization of processes and resources. The situation is not different for the painting process in the automotive industry, which has a significant amount of variables and influential external factors. This work, developed at General Motors in São José dos Campos, aims to analyze the feasibility of changing the painting process of the pickup S10 railings in the Antracite color located in the main line to the another line located in a Painting Repair Booth at the plant and, therefore, to study the possibility about reducing the window of cure for Antracite’s enamel by using Design of Experiments’ techniques. Applying this method is possible to find the best arrangement among studied factors of Painting Repair Booth that are, in this case, the Temperature, in Celsius degrees, and Skid’s Steps, in seconds, and it’s also possible to get their behavior according to quality requirements specified by GM rules for the Brightness and Paint Adhesion on the part. As a result, it can conclude that is possible to paint the S10 Antracite railings in the painting process’ line of Painting Repair Booth, and with the new configuration obtained by the Design of Experiments for the process variables, there are significant gains related to the parts’ quality, costs reduction and the optimization of production capacity, much in the main line as in the line of the Painting Repair Booth

Aplicação do planejamento de experimentos no processo de desenvolvimento de produtos: pesquisa em uma sorveteria artesanal

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES

Aplicação da metodologia de planejamento de experimentos para formulação de massas cerâmicas para telhas

Rio Grande do Norte State stands out as one great producer of structural clay of the brazilian northeastern. The Valley Assu ceramic tiles production stands out obtained from ilitics ball clays that abound in the region under study. Ceramics formulation and the design of experiments with mixture approach, has been applied for researchers, come as an important aid to decrease the number of experiments necessary to the optimization. In this context, the objective of this work is to evaluate the effects of the formulation, temperature and heating rate in the physical-mechanical properties of the red ceramic body used for roofing tile fabrication of the Valley Assu, using design of mixture experiments. Four clays samples used in two ceramics industry of the region were use as raw material and characterized by X-ray diffraction, chemical composition, differential thermal analysis (DTA), thermogravimetric analysis (TGA), particle size distribution analysis and plasticity techniques. Afterwards, they were defined initial molded bodies and made specimens were then prepared by uniaxial pressing at 25 MPa before firing at 850, 950 and 1050 ºC in a laboratory furnace, with heating rate in the proportions of 5, 10 e 15 ºC/min. The following tecnologicals properties were evaluated: linear firing shrinkage, water absorption and flexural strength. Results show that the temperature 1050 ºC and heating rate of 5 ºC/min was the best condition, therefore presented significance in all physical-mechanical properties. The model was accepted as valid based of the production of three new formulations with fractions mass diferents of the initial molded bodies and heated with temperature at 1050 ºC and heating rate of 5 ºC/min. Considering the formulation, temperature and heating rate as variables of the equations, another model was suggested, where from the aplication of design of experiments with mixtures was possible to get a best formulation, whose experimental error is the minor in relation to the too much formulations

Desenvolvimento e avaliação de uma ferramenta computacional multimeios utilizada no auxílio ao aprendizado de projetos de experimentos básicos

Esta dissertação trata do desenvolvimento e avaliação de uma ferramenta computacional multimeios utilizada no auxílio ao aprendizado de projetos de experimentos básicos. A busca da sociedade por novos produtos e processos, cada vez melhores e de forma mais rápida, determina a necessidade da aplicação de técnicas mais objetivas e eficientes para se alcançar estes desafios. O trabalho de execução visando contemplar o mencionado anteriormente, procedeu-se da seguinte forma: (i) revisão e descrição dos conceitos relativos à Engenharia da Qualidade e ao Planejamento, Projeto e Análise de Experimentos (PPAE); (ii) identificação e descrição de métodos ou regras de planejamento experimental; (iii) investigação e identificação dos projetos e análises de experimentos considerados básicos; (iv) desenvolvimento de uma ferramenta multimeios para o auxílio ao aprendizado de PPAE; (v) avaliação da ferramenta desenvolvida, através de um estudo de caso; (vi) conclusões relacionadas ao trabalho desenvolvido. A abordagem adotada para apresentar a técnica experimental, destacou o planejamento, do projeto e análise, detalhando separadamente os mesmos. Este passo almejou, de forma objetiva, identificar aqueles projetos e análises básicos, iniciais ao aprendizado. A elaboração e posterior avaliação da ferramenta multimeios permitiu perceber a potencialidade da mesma, como um meio instrucional para o tema específico de projetos de experimentos, sendo sua aplicação de relativa facilidade. A avaliação mostrou ainda que existe muito a se avançar nos meios físicos de apresentação/execução deste tipo de ferramenta multimeios.

Spatial pattern detection modeling of thrips (Thrips tabaci) on onion fields

Onion (Allium cepa) is one of the most cultivated and consumed vegetables in Brazil and its importance is due to the large laborforce involved. One of the main pests that affect this crop is the Onion Thrips (Thrips tabaci), but the spatial distribution of this insect, although important, has not been considered in crop management recommendations, experimental planning or sampling procedures. Our purpose here is to consider statistical tools to detect and model spatial patterns of the occurrence of the onion thrips. In order to characterize the spatial distribution pattern of the Onion Thrips a survey was carried out to record the number of insects in each development phase on onion plant leaves, on different dates and sample locations, in four rural properties with neighboring farms under different infestation levels and planting methods. The Mantel randomization test proved to be a useful tool to test for spatial correlation which, when detected, was described by a mixed spatial Poisson model with a geostatistical random component and parameters allowing for a characterization of the spatial pattern, as well as the production of prediction maps of susceptibility to levels of infestation throughout the area.

Proposta de método para estimação de tamanho de parcela para culturas agrícolas

Dentre as formas reconhecidas para redução do erro experimental, destaca-se o tamanho ótimo da parcela experimental para aplicação dos tratamentos, existindo vários métodos para sua estimação, baseados em diferentes princípios. O objetivo deste trabalho é propor um método alternativo para a estimação do tamanho ótimo de parcela, para culturas agrícolas, compará-lo com métodos clássicos para esse fim e identificar com quais parâmetros seus resultados estão correlacionados. Realizou-se a validação dos resultados, utilizando-se dados de quatro experimentos com plantas de pimentão, em que se avaliou a produção de frutos, acumulada nas várias colheitas, cultivado em estufa com cobertura plástica. Os resultados obtidos pelo método proposto, denominado Método da Máxima Distância, são coerentes, mas fracamente associados aos resultados observados pelos demais métodos clássicos. O tamanho ótimo da parcela, estimado pelo Método da Máxima Distância, é fortemente influenciado pelo índice de heterogeneidade da produção, que mede a correlação entre as produções de parcelas contíguas. Há, ainda, as características de ser de fácil aplicação, praticamente invariável à acumulação da produção em diversas colheitas, adequando-se para culturas com duas ou mais colheitas nas mesmas plantas, como em experimentos com culturas olerícolas ou forrageiras.

Variabilidade de propriedades físicas e químicas do solo em um pomar cítrico

Objetivando fornecer subsídios para esquemas de amostragem e planejamento de experimentos com citros, avaliou-se, em 1990, a variabilidade de propriedades físicas e químicas do solo em uma transeção de 50 plantas espaçadas de 4 m, em um pomar de laranja 'Pêra' com doze anos de idade, sob manejo uniforme e implantado em um latossolo amarelo distrófico textura média relevo plano, em Governador Mangabeira (BA). Em cada planta, colheu-se uma amostra de solo em um ponto fixo sob a projeção da copa, em faixa sucessivamente adubada. Os resultados permitiram concluir que apenas fósforo e umidade gravimétrica apresentaram distribuição normal, com as demais propriedades seguindo a lognormal. Os maiores coeficientes de variação foram obtidos para potássio e fósforo e, os menores, para saturação por bases, pH em CaCl2, pH em água e areia total. Com exceção de saturação por bases e alumínio, que apresentaram distribuição aleatória, as demais propriedades mostraram dependência espacial, com alcance variando de 18 m (areia total e argila) a 59 m (matéria orgânica, cálcio, magnésio, Ca + Mg e soma de bases).

Influência das variáveis de processo na alcoólise enzimática de óleo de mamona

O potencial de aplicação de lipases em processos biotecnológicos para a modificação de óleos e gorduras tem sido objeto de grande interesse nos meios científico, econômico e industrial nos últimos anos. Além da atividade de hidrólise de ésteres, as lipases podem catalisar uma grande variedade de reações de esterificação, transesterificação e poliesterificação. A transesterificação inclui acidólise, interesterificação e alcoólise. Neste trabalho reações de alcoólise de óleo de mamona para produção de ésteres de ácidos graxos foram estudadas devido a sua importância na obtenção de, por exemplo, agentes de antifricção, emulsificantes, intermediários para produzir uma numerosa quantidade de oleoquímicos e combustível alternativo ao diesel e/ou aditivo ao diesel de petróleo (biodiesel). Neste contexto, foi estudada a etanólise enzimática de óleo de mamona com lipase comercial (Lipozyme IM) usando n-hexano como solvente. Os experimentos foram realizados variando a temperatura, as concentrações de água e enzima no meio reacional e a razão molar óleo-etanol, de acordo com um planejamento de experimentos pré-estabelecidos. Um modelo empírico foi utilizado para avaliar a influência das variáveis de processo no rendimento e, desta forma, as condições de operação que maximizam a produção de ésteres foram estabelecidas para a enzima utilizada.