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.     

Using quantile plots of the prediction variance for comparing designs for a constrained mixture region: an application involving a fertilizer experiment

Summary. Vining and co-workers have used plots of the prediction variance trace (PVT) along the so-called prediction rays to compare mixture designs in a constrained region R . In the present paper, we propose a method for describing the distribution of the prediction variance within the region R by using quantile plots. More comprehensive comparisons between mixture designs are possible through the proposed plots than with the PVT plots. The utility of the quantile plots is illustrated with a four-component fertilizer experiment that was initiated in São Paulo, Brazil.     

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.     

Optimum designs for estimation of optimum point under cost constraint

In this paper, we consider the estimation of the optimum factor combination in a response surface model. Assuming that the response function is quadratic concave and there is a linear cost constraint on the factor combination, we attempt to find the optimum design using the trace optimality criterion. As the criterion function involves the unknown parameters, we adopt a pseudo-Bayesian approach to resolve the problem.     

Optimum designs for parameter estimation in a mixture experiment with two correlated responses

In this paper, we investigate a mixture problem with two responses, which are functions of the mixing proportions, and are correlated with known dispersion matrix. We obtain D- and A-optimal designs for estimating the parameters of the response functions, when none or some of the regression coefficients of the two functions are the same. It is shown that when no prior knowledge about the regression coefficients is available, the D-optimal design is independent of the dispersion matrix, while the A-optimal design depends on it, provided the response functions are of different degree. On the other hand, when some of the regression coefficients are known to be the same for both the functions, the D-optimal design depends on the dispersion matrix when the two response functions are not of the same degree.     

Optimum covariate designs in split-plot and strip-plot design set-ups

The problem considered is that of finding optimum covariate designs for estimation of covariate parameters in standard split-plot and strip-plot design set-ups with the levels of the whole-plot factor in r randomised blocks. Also an extended version of a mixed orthogonal array has been introduced, which is used to construct such optimum covariate designs. Hadamard matrices, as usual, play the key role for such construction.     

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.     

Optimum Mixture Design Using Deficiency Criterion

In a mixture experiment the measured response is assumed to depend only on the relative proportion of ingredients or components present in the mixture. Scheffe (1958 Scheffe , H. ( 1958 ). Experiments with mixtures . J. R. Statist. Soc. B 20 : 344 – 360 . [Google Scholar], 1963 Scheffe , H. ( 1963 ). Simplex – centroid design for experiments with mixtures . J. R. Statist. Soc. B 25 : 235 – 263 . [Google Scholar]) first systematically considered this problem and introduced different models and designs suitable in such situations. Optimum designs for the estimation of parameters of different mixture models are available in the literature. The problem of estimating the optimum proportion of mixture components is of great practical importance. Pal and Mandal (2006 Pal , M. , Mandal , N. K. ( 2006 ). Optimum designs for optimum mixtures . Statist. Probab. Lett. 76 ( 13 ): 1369 – 1379 .[Crossref], [Web of Science ®] , [Google Scholar], 2007 Pal , M. , Mandal , N. K. (2007). Optimum mixture design via equivalence theory. communicated. JCISS 32:107–126. [Google Scholar]) attempted to find a solution to this problem by adopting a pseudo-Bayesian approach and using the trace criterion. Subsequently, Pal and Mandal (2008 Pal , M. , Mandal , N. K. ( 2008 ). Minimax designs for optimum mixtures . To appear in Statist. Probab. Lett.  [Google Scholar]) solved the problem using minimax criterion. In this article, the deficiency criterion due to Chatterjee and Mandal (1981 Chatterjee , S. K. , Mandal , N. K. ( 1981 ). Response surface designs for estimating the optimal point . Calcutta Statist. Assoc. Bull. . 30 : 145 – 169 .[Crossref] , [Google Scholar]) has been used as a measure for comparing the performance of competing designs.     

On the construction of optimal designs

Two strategies for specifying additional data to be included with the data of a non-orthogonal design are presented. The additional data increase the magnitude of the information matrix X′X and the orthogonality of the design matrix. Sequentially, the new points are augmented to the original design, such that each new point optimally increases the smallest eigenvalue of X′X. The new runs are created in a predefined spherical region and a rectangular region. Optimum number of additional observations is presented in order to orthogonalize the design matrix X and optimize some functions of the information matrix X′X. Comparisons of the results acquired with the proposed methods versus the most commonly used procedures for data augmentation are carried out. In addition, the advantages of the use of our techniques over the studied methods to solve the augmenting data problems are discussed.     

Optimum mixture designs in a restricted region

In a mixture experiment, the response depends on the proportions of the mixing components. Canonical models of different degrees and also other models have been suggested to represent the mean response. Optimum designs for estimation of the parameters of the models have been investigated by different authors. In most cases, the optimum design includes the vertex points of the simplex as support points of the design, which are not mixture combinations in the true non-trivial sense. In this paper, optimum designs have been obtained when the experimental region is an ellipsoidal subspace of the entire factor space which does not cover the vertex points of the simplex.     

A simple method for constructing confounded designs for mixed factorial experiments

This paper presents the sinplesr procedure that uses wodular aryithmetic for constructing confounded designs for mixed factorial experiments. The present procedure and the classical one for confounding in symmetrical factorial experiments are both at the same mathema.tical level. The present procedure is written for

practitioners and is lllustrared with several examples.     

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.     

Long-term experiments and strip plot designs

In a long-term experiment usually the experimenter needs to know whether the effect of a treatment varies over time. But time usually has both a fixed and a random effects over the output and the difficulty in the analysis depends on the particular design considered and the availability of covariates. Actually, as shown in the paper, the presence of covariates can be very useful to model the random effect of time. In this paper a model to analyze data from a long-term strip plot design with covariates is proposed. Its effectiveness will be tested using both simulated and real data from a crop rotation experiment.     

A-optimal designs for optimum mixture in an additive quadratic mixture model

In the analysis of experiments with mixtures, quadratic models have been widely used. The optimum designs for the estimation of optimum mixing proportions in a quadratic mixture model have been studied by Pal and Mandal [Optimum designs for optimum mixtures. Statist Probab Lett. 2006;76:1369–1379] and Mandal et al. [Optimum mixture designs: a pseudo-Bayesian approach. J Ind Soc Agric Stat. 2008;62(2):174–182; Optimum mixture designs under constraints on mixing components. Statist Appl. 2008;6(1&2) (New Series): 189–205], using a pseudo-Bayesian approach. In this paper, a similar approach has been employed to obtain the A-optimal designs for the estimation of optimum proportions in an additive quadratic mixture model, proposed by Darroch and Waller [Additivity and interaction in three-component experiments with mixture. Biometrika. 1985;72:153–163], when the number of components is 3, 4 and 5. It has been shown that the vertices of the simplex are necessarily the support points of the optimum design, and the other support points include barycentres of depth at most 2.     

Using the chinese remainder theorem in constructing confounded designs for mixed factorial experiments

A procedure for constructing confounded designs for mixed factorial experiments derived from the Chinese Remainder Theorem is presented. The present procedure as well as others, all through use of modular arithmetic, are compared.     

Near-optimal designs for dual channel microarray studies

Summary.  Much biological and medical research employs microarray studies to monitor gene expression levels across a wide range of organisms and under many experimental conditions. Dual channel microarrays are a common platform and allow two samples to be measured simultaneously. A frequently used design uses a common reference sample to make conditions across different arrays comparable. Our aim is to formulate microarray experiments in the experimental design context and to use simulated annealing to search for near-optimal designs. We identify a subclass of designs, the so-called interwoven loop designs, that seems to have good optimality properties compared with the near-optimal designs that are found by simulated annealing. Commonly used reference designs and dye swap designs are shown to be highly inefficient.     

On d- and e- minimax optimal designs for estimating the axial slopes of a second-order response surface over hypercubic regions

Design of experiments for estimating the slopes of a response surface is considered. Design criteria analogous to the traditional ones but based upon the variance-covariance matrix of the estimated slopes along factor axes are proposed. Optimal designs under the proposed criteria are derived for second-order polynomial regression over hypercubic regions. Best de¬signs within some commonly used classes of designs are also obtained and their efficiencies are investigated.     

A likelihood-based constrained algorithm for multivariate normal mixture models

It is well known that the log-likelihood function for samples coming from normal mixture distributions may present spurious maxima and singularities. For this reason here we reformulate some Hathaways results and we propose two constrained estimation procedures for multivariate normal mixture modelling according to the likelihood approach. Their perfomances are illustrated on the grounds of some numerical simulations based on the EM algorithm. A comparison between multivariate normal mixtures and the hot-deck approach in missing data imputation is also considered.Salvatore Ingrassia: S. Ingrassia carried out the research as part of the project Metodi Statistici e Reti Neuronali per lAnalisi di Dati Complessi (PRIN 2000, resp. G. Lunetta).     

On some DS-optimal designs in spherical regions

For polynomial regression over spherical regions the d-th order D_s-optimal designs for the λ-th order models are derived for 1 ≤ λ ≤ d ≤ 4. Efficiencies of these designs with respect to the λ-th order D-optimal designs are obtained. The effects of estimating addtional parameters due to an m-th order model (d ≥ m >>λ) on the efficiencies are investigated.