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.     

Note on a mixture experiment with process variables

The experimental design to model the response of a mixture experiment in three blending components in the presence of process variables is considered. Czitrom (1988) gave an experimental design in two orthogonal blocks of blends that was "possibly" D-Optimal in the case of arbitrary restrictions on the blending component proportions. It will be shown that the design is indeed D-Optimal. The pair of orthogonal D-Optimal blocks of blends can be used with an arbitrary number of process variables and require a reduced number of observations     

Mixture designs for five components in orthogonal blocks

The methods developed by John and Draper et al. of partitioning the blends (runs) of four mixture components into two or more orthogonal blocks when fitting quadratic models are extended to mixtures of five components. The characteristics of Latin squares of side five are used to derive rules for reliably and quickly obtaining designs with specific properties. The designs also produce orthogonal blocks when higher order models are fitted.     

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.     

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.     

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.     

Orthogonally blocked mixture component–amount designs via projections of F-squares

Orthogonal block designs for Scheffé’s quadratic model have been considered previously by Draper et al. (1993), John (1984), Lewis et al. (1994) and Prescott, Draper, Dean, and Lewis (1993). Prescott and Draper (2004) obtained mixture component–amount designs via projections of standard mixture designs, viz., the simplex-lattice, the simplex-centroid and the orthogonally blocked mixture designs based on latin squares. Aggarwal, Singh, Sarin, and Husain (2009) considered the case of components assuming equal volume fractions and obtained mixture designs in orthogonal blocks using F-squares. In this paper, we construct orthogonal blocks of two and three mixture component–amount blends by projecting the class of four component mixture designs presented by Aggarwal et al. (2009).     

Efficient arrangements of two-level orthogonal arrays in two and four blocks

When orthogonal arrays are used in practical applications, it is often difficult to perform all the designed runs of the experiment under homogeneous conditions. The arrangement of factorial runs into blocks is usually an action taken to overcome such obstacles. However, an arbitrary configuration might lead to spurious analysis results. In this work, the nice properties of two-level orthogonal arrays are taken into consideration and an effective method for arranging experimental runs into two and four blocks of the same size is proposed. This method is based on the so-called J-characteristics of the corresponding array. General theoretical results are given for studying up to four experimental factors in two blocks, as well as for studying up to three experimental factors in four blocks. Finally, we provide best blocking arrangements when the number of the factors of interest is larger, by exploiting the known lists of non-isomorphic orthogonal arrays with two levels and various run sizes.     

A class of single replicate orthogonal designs

A simple method is given to calculate the number of degrees of freedom confounded with blocks of a specific factorial effect in a single replicate orthogonal design. Two classes of designs having partial orthogonality are also discussed     

Interpretable dimension reduction

The analysis of high-dimensional data often begins with the identification of lower dimensional subspaces. Principal component analysis is a dimension reduction technique that identifies linear combinations of variables along which most variation occurs or which best “reconstruct” the original variables. For example, many temperature readings may be taken in a production process when in fact there are just a few underlying variables driving the process. A problem with principal components is that the linear combinations can seem quite arbitrary. To make them more interpretable, we introduce two classes of constraints. In the first, coefficients are constrained to equal a small number of values (homogeneity constraint). The second constraint attempts to set as many coefficients to zero as possible (sparsity constraint). The resultant interpretable directions are either calculated to be close to the original principal component directions, or calculated in a stepwise manner that may make the components more orthogonal. A small dataset on characteristics of cars is used to introduce the techniques. A more substantial data mining application is also given, illustrating the ability of the procedure to scale to a very large number of variables.     

Multilevel dimensionality-reduction methods

When data sets are multilevel (group nesting or repeated measures), different sources of variations must be identified. In the framework of unsupervised analyses, multilevel simultaneous component analysis (MSCA) has recently been proposed as the most satisfactory option for analyzing multilevel data. MSCA estimates submodels for the different levels in data and thereby separates the “within”-subject and “between”-subject variations in the variables. Following the principles of MSCA and the strategy of decomposing the available data matrix into orthogonal blocks, and taking into account the between- and the within data structures, we generalize, in a multilevel perspective, multivariate models in which a matrix of response variables can be used to guide the projections (formed by responses predicted by explanatory variables or by a limited number of their combinations/composites) into choices of meaningful directions. To this end, the current paper proposes the multilevel version of the multivariate regression model and dimensionality-reduction methods (used to predict responses with fewer linear composites of explanatory variables). The principle findings of the study are that the minimization of the loss functions related to multivariate regression, principal-component regression, reduced-rank regression, and canonical-correlation regression are equivalent to the separate minimization of the sum of two separate loss functions corresponding to the between and within structures, under some constraints. The paper closes with a case study of an application focusing on the relationships between mental health severity and the intensity of care in the Lombardy region mental health system.     

Blocking in two-level non-regular fractional factorial designs

In this paper we consider screening experiments where a two-level fractional factorial design is to be used to identify significant factors in an experimental process and where the runs in the experiment are to occur in blocks of equal size. A simple method based on the foldover technique is given for constructing resolution IV orthogonal and non-orthogonal blocked designs and examples are given to illustrate the process.     

Effect of missing plots in some response surface designs

The effect of one or more missing observations for response surface designs arranged in blocks are examined in this paper. The resu lts as applied to a central composite design with orthogonal blocking, and an equirdial design with orthogonal blocking, are reported.     

Space-filling orthogonal arrays of strength two

This paper considers the use of orthogonal arrays of strength two as experimental designs for fitting a surrogate model. Contrary to standard space-filling designs or Latin hypercube designs, the points of an orthogonal array of strength two are well distributed when they are projected on the two-dimensional faces of the unit cube. The aim is to determine if this property allows one to fit an accurate surrogate model when the computer response is governed by second-order interactions of some input variables. The first part of the paper is devoted to the construction of orthogonal arrays with space-filling properties. In the second part, orthogonal arrays are compared with standard designs for fitting a Gaussian process model.     

Balanced incomplete Latin square designs

Latin squares have been widely used to design an experiment where the blocking factors and treatment factors have the same number of levels. For some experiments, the size of blocks may be less than the number of treatments. Since not all the treatments can be compared within each block, a new class of designs called balanced incomplete Latin squares (BILS) is proposed. A general method for constructing BILS is proposed by an intelligent selection of certain cells from a complete Latin square via orthogonal Latin squares. The optimality of the proposed BILS designs is investigated. It is shown that the proposed transversal BILS designs are asymptotically optimal for all the row, column and treatment effects. The relative efficiencies of a delete-one-transversal BILS design with respect to the optimal designs for both cases are also derived; it is shown to be close to 100%, as the order becomes large.     

Optimal orthogonal block designs for four-mixture components in two blocks based on F-squares for Becker's models and K-model

Orthogonal block designs in mixture experiments have been extensively studied by various authors. Aggarwal et al. [M.L. Aggarwal, P. Singh, V. Sarin, and B. Husain, Mixture designs in orthogonal blocks using F-squares, METRON – Int. J. Statist. LXVII(2) (2009), pp. 105–128] considered the case of components assuming the same volume fractions and obtained mixture designs in orthogonal blocks using F-squares. In this paper, we have used the class of designs presented by Aggarwal et al. and have obtained D-, A- and E-optimal orthogonal block designs for four components in two blocks for Becker's mixture models and K-model, respectively. Orthogonality conditions for the considered models are also given.     

ADJUSTED ORTHOGONAL NESTED ROW-COLUMN DESIGNS

Adjusted orthogonality in nested row-column designs is defined and a sufficient condition established for its existence. It is shown that the properties of an adjusted orthogonal nested row-column design are directly related to those of its separate row and column component designs. A method for constructing efficient adjusted orthogonal designs involving a single replicate of every treatment in each of two blocks is given.     

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.     

Mixture designs for constrained components in orthogonal blocks

It is often the case in mixture experiments that some of the ingredients, such as additives or flavourings, are included with proportions constrained to lie in a restricted interval, while the majority of the mixture is made up of a particular ingredient used as a filler. The experimental region in such cases is restricted to a parallelepiped in or near one corner of the full simplex region. In this paper, orthogonally blocked designs with two experimental blends on each edge of the constrained region are considered for mixture experiments with three and four ingredients. The optimal symmetric orthogonally blocked designs within this class are determined and it is shown that even better designs are obtained for the asymmetric situation, in which some experimental blends are taken at the vertices of the experimental region. Some examples are given to show how these ideas may be extended to identify good designs in three and four blocks. Finally, an example is included to illustrate how to overcome the problems of collinearity that sometimes occur when fitting quadratic models to experimental data from mixture experiments in which some of the ingredient proportions are restricted to small values.     

ON RESOLVABLE INCOMPLETE BLOCK DESIGNS1

A method of constructing resolvable incomplete block designs for v(=ks, 2 ≤ k ≤ s - 1) treatments in blocks of size k using mutually orthogonal Latin squares is proposed. It has been seen in particular that when the number of replications is s — 1 (or s), which is feasible if s is a prime or a prime power, the method gives PBIB (3) (or semi-regular GD) designs. The analysis of such designs has also been discussed.