Projection designs for mixture experiments in orthogonal blocks

Mixture experiments are often carried out in the presence of process variables, such as days of the week or different machines in a manufacturing process, or different ovens in bread and cake making. In such experiments it is particularly useful to be able to arrange the design in orthogonal blocks, so that the model in tue mixture vanauies may ue iitteu inucpenuentiy or tne UIOCK enects mtrouuceu to take account of the changes in the process variables. It is possible in some situations that some of the ingredients in the mixture, such as additives or flavourings, are present in soian quantities, pernaps as iuw a.s 5% ur even !%, resulting in the design space being restricted to only part of the mixture simplex. Hau and Box (1990) discussed the construction of experimental designs for situations where constraints are placed on the design variables. They considered projecting standard response surface designs, including factorial designs and central composite designs, into the restricted design space, and showed that the desirable property of block orthogonality is preserved by the projections considered. Here we present a number of examples of projection designs and illustrate their use when some of the ingredients are restricted to small values, such that the design space is restricted to a sub-region within the usual simplex in the mixture variables.     

Efficient designs for constrained mixture experiments

Many practical experiments on mixtures (where the components sum to one) include additional lower or upper bounds on components, or on linear combinations of them. Usually theory cannot be used to obtain a good design, and algorithmic methods are necessary. Some of the available methods are discussed. Their performance is evaluated on some examples, and the form of the optimal design is investigated.     

Optimization of a product performance using mixture experiments including process variables

This article presents a case study of a chemical compound used in the delay mechanism to start a rocket engine. The compound consists in a three-component mixture. Besides the components proportions, two process variables are considered. The aim of the study is to investigate the mix components proportions and the levels of process variables that set the expected delay time as close as possible to the target value and, at the same time, minimize the width of prediction interval for the response. A linear regression model with normal responses was fitted. Through the model developed, the optimal components proportions and the levels of the process variables were determined. For the model selection, the use of the backward method with an information criterion proved to be efficient in the case under study.     

A-optimal designs for mixture central polynomial model with qualitative factors

Mixture central polynomial models with qualitative factors are widely applied in many fields of research. In this paper, a method of finding A-optimal design for two degree mixture central polynomial model with qualitative factors will be proposed. The variance function will be given for getting the support points of the design. The A-optimality is confirmed by the equivalence theorem. In addition, this method also works effectively with higher degree models.     

Optimal designs for additive mixture model with heteroscedastic errors

This paper presents a study of D- and A-optimality of direct sum designs for additive mixture models when the errors are heteroscedastic. Sufficient conditions are given so that D- and A-optimal designs for additive mixture models can be constructed from the D- and A-optimal designs for homogeneous models in sub-mixture systems.     

Restricted region designs for multifactor mixture experiments

Designs for multifactor mixture experiments in which the component proportions are restricted by some specified lower and upper limits, are called restricted region designs (RRD) for multifactor mixture experiments. In this paper (i) a method of construction of designs for multifactor mixture experiments and (ii) two methods of constructing RRD for multifactor mixture experiments are described. Examples to illustrate the methods of construction have been given.     

Design and analysis of mixture experiments with process variable

A mixture experiment is an experiment in which the response is assumed to depend on the relative proportions of the ingredients present in the mixture and not on the total amount of the mixture. In such experiment process, variables do not form any portion of the mixture but the levels changed could affect the blending properties of the ingredients. Sometimes, the mixture experiments are costly and the experiments are to be conducted in less number of runs. Here, a general method for construction of efficient mixture experiments in a minimum number of runs by the method for projection of efficient response surface design onto the constrained region is obtained. The efficient designs with a less number of runs have been constructed for 3rd, 4th, and 5th component of mixture experiments with one process variable.     

Optimal designs for experiments with mixtures: a survey

This is a survey article on known results about analytic solutions and numerical solutions of optimal designs for various regression models for experiments with mixtures. The regression models include polynomial models, models containing homogeneous functions, models containing inverse terms and ratios, log contrast models, models with quantitative variables, and mod els containing the amount of mixture, Optimality criteria considered include D-, A-, E-,φ_p- and I_λ-Optimalities. Uniform design and uniform optimal design for mixture components, and efficiencies of the {q,2} simplex-controid design are briefly discussed.     

Mixture experiments with process variables: d-optimal orthogonal experimental designs

Blending experiments with mixture in the presence of process variables are considered. We present an experimental design for quadratic (or linear) blending. The design in two orthogonal blocks is D-optimized in the case where there are no restrictions on the blending in two orthogonal blocks is presented when there are arbitrary restrictions on the blending components. The pair of orthogonal blocks can be used with and arbitrary number of process variables. The number of design points needed when different orthogonal blocks are used is usually smaller than when a single block is repeated at the various process variables levels.     

Construction of uniform designs for mixture experiments with complex constraints

Abstract

Mixture experiments have attracted increasingly attention due to their great practical value in production and living, while uniform designs over irregular experimental regions have become a hot topic in the area of experimental designs in the past two decades. Noting that the experimental region of a mixture experiment with q components under some constraints is in fact a (q ? 1)-dimensional geometry, this article proposes a new method for searching nearly uniform designs for mixture experiments with any complex constraints. Two examples with some tables and figures are given to illustrate this method.     

Nearly optimal orthogonally blocked desings for a quadratic mixture model with q components

In experiments with mixtures involving process variables, orthogonal block designs may be used to allow estimation of the parameters of the mixture components independently of estimation of the parameters of the process variables. In the class of orthogonally blocked designs based on pairs of suitably chosen Latin squares, the optimal designs consist primarily of binary blends of the mixture components, regardless of how many ingredients are available for the mixture. This paper considers ways of modifying these optimal designs so that some or all of the runs used in the experiment include a minimum proportion of each mixture ingredient. The designs considered are nearly optimal in the sense that the experimental points are chosen to follow ridges of maxima in the optimality criteria. Specific designs are discussed for mixtures involving three and four components and distinctions are identified for different designs with the same optimality properties. The ideas presented for these specific designs are readily extended to mixtures with q>4 components.     

Experimental designs for mixture systems with multicomponent constraints

In an earlier paper it was recommended that an experimental design for the study of a mixture system in which the components had lower and upper limits should consist of a subset of the vertices and centroids of the region defined by the limitson the components. This paper extends this methodology to the situation where linear combinations of two or more components (e.g., liquid content=x₃+x₄+≦0.35) are subject to lower and upper constraints. The CONSIM algorithm, developed by R. E. Wheeler, is recommended for computing the vertices of the resulting experimental region. Procedures for developing linear and quadratic mixture model designs are discussed. A five-component example which has two multiple-component constraints is included to illustrate the proposed methods of mixture experimentation.     

Orthogonal blocking of response surface split-plot designs

When all experimental runs cannot be performed under homogeneous conditions, blocking can be used to increase the power for testing the treatment effects. Orthogonal blocking provides the same estimator of the polynomial effects as the one that would be obtained by ignoring the blocks. In many real-life design scenarios, there is at least one factor that is hard to change, leading to a split-plot structure. This paper shows that for a balanced ordinary least square–generalized least square equivalent split-plot design, orthogonal blocking can be achieved. Orthogonally blocked split-plot central composite designs are constructed and a catalog is provided.     

Symmetry in mixture experiments

Two types of symmetry can arise when the proportions of mixture components are constrained by upper and lower bounds. These two types of symmetry are shown to be useful for blocking first-order designs, as well as for finding the centroid of the experimental region. Orthogonal blocking of first-order mixture designs provides a method of including process variables in the mixture experiment, with the mixture terms orthogonal to the process factors. Symmetric regions are used to develop spherical and rotatable response surface designs for mixtures. The central composite design and designs based on the icosahedron and the dodecahedron are given for four-component mixtures. The uniform shell designs are three-level designs when applied to mixture experiments.     

A catalogue of designs for partial profiles in paired comparison experiments with three groups of factors

A common strategy for avoiding information overload in multi-factor paired comparison experiments is to employ pairs of options which have different levels for only some of the factors in a study. For the practically important case where the factors fall into three groups such that all factors within a group have the same number of levels and where one is only interested in estimating the main effects, a comprehensive catalogue of D-optimal approximate designs is presented. These optimal designs use at most three different types of pairs and have a block diagonal information matrix.     

Bayesian two-stage optimal design for mixture models

In this paper, a Bayesian two-stage D–D optimal design for mixture experimental models under model uncertainty is developed. A Bayesian D-optimality criterion is used in the first stage to minimize the determinant of the posterior variances of the parameters. The second stage design is then generated according to an optimalityprocedure that collaborates with the improved model from the first stage data. The results show that a Bayesian two-stage D–D-optimal design for mixture experiments under model uncertainty is more efficient than both the Bayesian one-stage D-optimal design and the non-Bayesian one-stage D-optimal design in most situations. Furthermore, simulations are used to obtain a reasonable ratio of the sample sizes between the two stages.     

A graphical method for evaluating mixture designs with respect to the slope

Good estimation of the slopes of the mixture response function may be important as well as estimation of mean mixture response. It is possible to evaluate and compare several mixture designs with respect to the slope. A graphical method is proposed that allows us to evaluate a given design's support for the fitted model in terms of slope variance. We can plot variances of slopes along Cox direction or axial direction according to existence of restriction of simplex region or not when comparing several different mixture designs.     

Mixture and mixture–process variable experiments for pharmaceutical applications

Many experiments in research and development in the pharmaceutical industry involve mixture components. These are experiments in which the experimental factors are the ingredients of a mixture and the response variable is a function of the relative proportion of each ingredient, not its absolute amount. Thus the mixture ingredients cannot be varied independently. A common variation of the mixture experiment occurs when there are also one or more process factors that can be varied independently of each other and of the mixture components, leading to a mixture–process variable experiment. We discuss the design and analysis of these types of experiments, using tablet formulation as an example. Our objective is to encourage greater utilization of these techniques in pharmaceutical research and development. Copyright © 2004 John Wiley & Sons Ltd.