Augmented Box-Behnken Designs for Fitting Third-Order Response Surfaces

Box-Behnken designs are popular with experimenters who wish to estimate a second-order model, due to their having three levels, their simplicity and their high efficiency for the second-order model. However, there are situations in which the model is inadequate due to lack of fit caused by higher-order terms. These designs have little ability to estimate third-order terms. Using combinations of factorial points, axial points, and complementary design points, we augment these designs and develop catalogues of third-order designs for 3–12 factors. These augmented designs can be used to estimate the parameters of a third-order response surface model. Since the aim is to make the most of a situation in which the experiment was designed for an inadequate model, the designs are clearly suboptimal and not rotatable for the third-order model, but can still provide useful information.     

Some new augmented fractional Box–Behnken designs

The augmented Box–Behnken designs are used in the situations in which Box–Behnken designs (BBDs) could not estimate the response surface model due to the presence of third-order terms in the response surface models. These designs are too large for experimental use. Usually experimenters prefer small response surface designs in order to save time, cost, and resources; therefore, using combinations of fractional BBD points, factorial design points, axial design points, and complementary design points, we augment these designs and develop new third-order response surface designs known as augmented fractional BBDs (AFBBDs). These AFBBDs have less design points and are more efficient than augmented BBDs.     

Sequential asymmetric third order rotatable designs (SATORDs)

Rotatable designs that are available for process/ product optimization trials are mostly symmetric in nature. In many practical situations, response surface designs (RSDs) with mixed factor (unequal) levels are more suitable as these designs explore more regions in the design space but it is hard to get rotatable designs with a given level of asymmetry. When experimenting with unequal factor levels via asymmetric second order rotatable design (ASORDs), the lack of fit of the model may become significant which ultimately leads to the estimation of parameters based on a higher (or third) order model. Experimenting with a new third order rotatable design (TORD) in such a situation would be expensive as the responses observed from the first stage runs would be kept underutilized. In this paper, we propose a method of constructing asymmetric TORD by sequentially augmenting some additional points to the ASORDs without discarding the runs in the first stage. The proposed designs will be more economical to obtain the optimum response as the design in the first stage can be used to fit the second order model and with some additional runs, third order model can be fitted without discarding the initial design.KEYWORDS: Response surface methodology, rotatability, orthogonal transformation, asymmetric, sequential experimentation, third order designs     

A simpler way of obtaining non-sIngularity conditions of rotatability

In response surface designs, it is not usually easy to handle the moment matrix X'X, especially for higher orders. This paper presents a method in which the moment matrix of a response surface of any order can be standardized, i.e., X'X splits into a diagonal matrix consisting of sub-matrices of lower order. This eases the calculation of the determinant and the inverse of X'X. The method has been illustrated with applications to second, third and fourth order response surfaces.     

On group divisible response surface (GDRS) designs

In this paper some experimental situations are identified corresponding to which suitable response surface designs do not exist. A class of response surface designs is introduced to cope with these situations. Their analysis with and without blocking and methods of construction is discussed.     

Designs for approximately linear regression: Maximizing the minimum coverage probability of confidence ellipsoids

The classical D-optimality principle in regression design may be motivated by a desire to maximize the coverage probability of a fixed-volume confidence ellipsoid on the regression parameters. When the fitted model is exactly correct, this amounts to minimizing the determinant of the covariance matrix of the estimators. We consider an analogue of this problem, under the approximately linear model E[y|x] = θ^Tz(x) + f(x). The nonlinear disturbance f(x) is essentially unknown, and the experimenter fits only to the linear part of the response. The resulting bias affects the coverage probability of the confidence ellipsoid on θ. We study the construction of designs which maximize the minimum coverage probability as f varies over a certain class. Explicit designs are given in the case that the fitted response surface is a plane.     

Fourth order rotatability

Fourth order rotatable designs are discussed. A general k, design moment inequality is given. The variance function for two-factor designs is derived, and plotted for a specific design. A minimum point set requirement for two-factor designs is established, thus enabling one to form an infinity of such designs. Some difficulties in obtaining deLigns for k>2 are described. Some questions are posed for future work.     

Response Surface Designs Where Levels of Some Factors are Difficult to Change

This article considers response surface designs in which the number of levels of some of the factors are constrained. Two general types of designs are examined: CUBE designs and STAR designs. The specific factor levels are chosen to give variance contours with a high level of sphericity, thus providing designs that are close to rotatable.     

Minimax designs for estimating slopes in a trigonometric regression model

Abstract

Designs for the first order trigonometric regression model over an interval on the real line are considered for the situation where estimation of the slope of the response surface at various points in the factor space is of primary interest. Minimization of the variance of the estimated slope at a point maximized over all points in the region of interest is taken as the design criterion. Optimal designs under the minimax criterion are derived for the situation where the design region and the region of interest are identical and a symmetric “partial cycle”. Some comparisons of the minimax designs with the traditional D- and A-optimal designs are provided. Efficiencies of some exact designs under the minimax criterion are also investigated.     

Computer-Generated Neighbor Designs

Neighbor designs are useful to remove the neighbor effects. In this article, an algorithm is developed and is coded in Visual C + +to generate the initial block for possible first, second,…, and all order neighbor designs. To get the required design, a block (0, 1, 2,…, k ? 1) is then augmented with (v ? 1) blocks obtained by developing the initial block cyclically mod (v ? 1).     

Orthogonally Blocked Mixture Experiments in Ellipsoidal Restricted Regions

In practical situations involving mixtures formed from several ingredients, interest is sometimes centered on the response in an ellipsoidal neighborhood around a standard formulation. We show that standard, orthogonally blocked, response surface designs, defined on a q ? 1 dimensional unit sphere, may be transformed into similarly orthogonally blocked q-ingredient mixture designs defined within an ellipsoid centered at the standard formulation. The method is illustrated using several examples of mixture experiments with three, four, and five ingredients, arranged in two, three, or four orthogonal blocks, obtained by projecting standard central composite designs and Box–Behnken designs into the ellipsoidal mixture region. Rotations of the resulting designs within the ellipsoidal regions are also considered.     

Split-plot designs with mirror image pairs as sub-plots

In this article we investigate two-level split-plot designs where the sub-plots consist of only two mirror image trials. Assuming third and higher order interactions negligible, we show that these designs divide the estimated effects into two orthogonal sub-spaces, separating sub-plot main effects and sub-plot by whole-plot interactions from the rest. Further we show how to construct split-plot designs of projectivity P≥3. We also introduce a new class of split-plot designs with mirror image pairs constructed from non-geometric Plackett-Burman designs. The design properties of such designs are very appealing with effects of major interest free from full aliasing assuming that 3rd and higher order interactions are negligible.     

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.     

On choosing between fixed and random block effects in some no-interaction models

The purpose of this article is to strengthen the understanding of the relationship between a fixed-blocks and random-blocks analysis in models that do not include interactions between treatments and blocks. Treating the block effects as random has been recommended in the literature for balanced incomplete block designs (BIBD) because it results in smaller variances of treatment contrasts. This reduction in variance is large if the block-to-block variation relative to the total variation is small. However, this analysis is also more complicated because it results in a subjective interpretation of results if the block variance component is non-positive. The probability of a non-positive variance component is large precisely in those situations where a random-blocks analysis is useful – that is, when the block-to-block variation, relative to the total variation, is small. In contrast, the analysis in which the block effects are fixed is computationally simpler and less subjective. The loss in power for some BIBD with a fixed effects analysis is trivial. In such cases, we recommend treating the block effects as fixed. For response surface experiments designed in blocks, however, an opposite recommendation is made. When block effects are fixed, the variance of the estimated response surface is not uniquely estimated, and in practice this variance is obtained by ignoring the block effect. It is argued that a more reasonable approach is to treat the block effects to be random than to ignore it.     

D-minimax Second-order Designs Over Hypercubes for Extrapolation and Restricted Interpolation Regions

The D-minimax criterion for estimating slopes of a response surface involving k factors is considered for situations where the experimental region χ and the region of interest ? are co-centered cubes but not necessarily identical. Taking χ = [ ? 1, 1]^k and ? = [ ? R, R]^k, optimal designs under the criterion for the full second-order model are derived for various values of R and their relative performances investigated. The asymptotically optimal design as R → ∞ is also derived and investigated. In addition, the optimal designs within the class of product designs are obtained. In the asymptotic case it is found that the optimal product design is given by a solution of a cubic equation that reduces to a quadratic equation for k = 3?and?6. Relative performances of various designs obtained are examined. In particular, the optimal asymptotic product design and the traditional D-optimal design are compared and it is found that the former performs very well.     

Optimal designs for non-competitive enzyme inhibition kinetic models

In this paper, we present a new method for determining optimal designs for enzyme inhibition kinetic models, which are used to model the influence of the concentration of a substrate and an inhibition on the velocity of a reaction. The approach uses a nonlinear transformation of the vector of predictors such that the model in the new coordinates is given by an incomplete response surface model. Although there exist no explicit solutions of the optimal design problem for incomplete response surface models so far, the corresponding design problem in the new coordinates is substantially more transparent, such that explicit or numerical solutions can be determined more easily. The designs for the original problem can finally be found by an inverse transformation of the optimal designs determined for the response surface model. We illustrate the method determining explicit solutions for the D-optimal design and for the optimal design problem for estimating the individual coefficients in a non-competitive enzyme inhibition kinetic model.     

A Comparison of Three-Level Orthogonal Arrays in the Presence of Different Correlation Structures in Observations

When the experimenter suspects that there might be a quadratic relation between the response variable and the explanatory parameters, a design with at least three points must be employed to establish and explore this relation (second-order design). Orthogonal arrays (OAs) with three levels are often used as second-order response surface designs. Generally, we assume that the data are independent observations; however, there are many situations where this assumption may not be sustainable. In this paper, we want to compare three-level OAs with 18, 27, and 36 runs under the presence of three specific forms of correlation in observations. The aim is to derive the best designs that can be efficiently used for response surface modeling.     

On The Optimal Choice of Cube and Star Replications in Restricted Second-Order Designs

This article examines the central composite design in which some of the experimental runs are replicated. Three different classes of N-point designs are compared using the criterion of Schur's ordering under orthogonality, rotatablity, and slope- rotatablity conditions. The response surface designs with the star portion replicated seem to have more potential than others under orthogonality condition, while the designs with the cube portion replicated is preferable to the designs with their star portion or only the center point replicated under rotatable and slope-rotatable conditions.     

Conditions of Slope-Rotatability for Third-Order Polynomial Regression Models

In experimental design for response surface analysis, it is sometimes of interest to estimate the difference of responses at two points. If differences at points close together are involved, the design that reliably estimates the slope of the response surface is important. In particular, Hader and Park (1978 Hader , R. J. , Park , S. H. ( 1978 ). Slope-rotatable central composite designs . Technometrics 20 : 413 – 417 .[Taylor & Francis Online], [Web of Science ®] , [Google Scholar]) suggested the concept of slope-rotatability and studied slope rotatable central composite designs. Until now, many response surface designs including central composite designs have been suggested for fitting second order response surface models. However, we often need to fit third-order polynomial regression models. In this article, we suggest extended central composite designs (ECCDs) to fit third-order models and find the necessary and sufficient conditions for slope-rotatability over all directions in the third-order polynomial models.