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Biometrics & Biostatistics International Journal

Research Article Volume 5 Issue 5

Response surface methodology and its applications in agricultural and food sciences

Andre I Khuri

Department of Statistics, University of Florida, USA

Correspondence: Andre I Khuri, Department of Statistics, University of Florida, USA

Received: September 15, 2016 | Published: April 11, 2017

Citation: Khuri AI. Response surface methodology and its applications in agricultural and food sciences. Biom Biostat Int J. 2017;5(5):155-163. DOI: 10.15406/bbij.2017.05.00141

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Abstract

The purpose of this article is to provide an overview of response surface methodology (RSM) which includes the modeling of a response function, the corresponding choice of design, and the determination of optimum conditions. In addition, the use of RSM in agricultural and food sciences is highlighted by citing several examples taken from a variety of applied journals.

Introduction

Response surface methodology (RSM) consists of a group of mathematical and statistical techniques concerned with

  1. The selection and construction of an appropriate design that can provide adequate and reliable information concerning a certain Response variable, denoted by yy .
  2. The determination of a suitable model that best fits the data that can be generated from using the design chosen in (1). Such a model gives an approximate functional relationship between the response variable yy and a set of Control variables believed (by the experimenter) to have an effect on the response yy . These variables are denoted by x1,x2,...,xkx1,x2,...,xk .
  3. The finding of optimal settings on the control variables that produce maximum (or minimum) response values within a certain region of interest.

From the historical point of view, the article by Box and Wilson1 is considered to be the first for having laid the foundations for RSM. Some of the early papers that also contributed to the development of RSM include those by Box and Hunter2 and Box and Draper.3 Several review papers on RSM were subsequently published starting with the article by Hill and Hunter4 that emphasized practical applications of RSM in the chemical and processing fields. This was followed by more recent reviews by Myers et al.57 A review of RSM from a biometric viewpoint was given by8 who emphasized biological applications rather than applications in the physical and engineering sciences. In addition, several books were written on the subject of RSM by Myers, Khuri and Cornell, Box and Draper and Myers et al.912

In the early development of RSM, from 1951 up through the 1970s, the main focus of attention was on controlled experiments that can, for the most part, be performed in a laboratory. This was particularly suited in an industrial setting with possible applications in the physical and engineering sciences. The review paper by Hill and Hunter4 made reference to several applications in the chemical industry. It should be pointed out here that the seminal work of Box and Wilson1 occurred at a major chemical company, and Box himself was initially trained as a chemist in England.

One of the basic characteristics of a response surface investigation is its sequential nature whereby experiments are performed in stages. Information acquired from one set of experiments is used to plan the strategy for a follow-up set of experiments. This sequential pattern of experimentation was suggested by Box and Youle.13 Such an approach works well in an industrial setting since the response values in a given stage can be obtained in a relatively short time. However, this approach may not be feasible in an agricultural setting where experiments typically require long periods between stages. Furthermore, it is quite common in an agricultural experiment that the results of a single experiment may be the only ones available rather than having a series of experiments obtained sequentially. Another main difference between an industrial experiment and an agricultural one has to do with factors' levels. In an industrial experiment, the levels of quantitative factors can be accurately controlled and measured. This, however, may be difficult to do in an agricultural experiment. Edmondson14 Outlined several other major distinctions between industrial and agricultural experiments.

Mead and Pike8 were the first to bring attention to the role of RSM in agriculture and biometric research in general. They also provided a survey of bio- logical and agricultural journals that used response surface methods. However, they emphasized the use of nonlinear models to describe the behavior of biological data. Such models are usually referred to as Mechanistic. The traditional modeling scheme used in the early work on RSM was based on the so-called Empirical modeling where low-degree polynomials are used to fit the response data. These polynomials are chosen and tested on the basis of the observed data, but are not selected on the basis of information that pertain to certain chemical of physical laws, as is the case with mechanistic models.

While certain approaches used in RSM may not be quite suitable in an agricultural setting, there is a lot to be gained from using certain response surface techniques in an agricultural experiment. The purpose of this chapter is to provide an expose of some basic methods and models used in RSM. Several applications of RSM in agricultural and food sciences will also be mentioned using examples taken from the corresponding literature.

Response surface models

Let yy be a response variable of interest, and let x1,x2,...,xkx1,x2,...,xk denote control variables believed to have an effect on yy . As was mentioned earlier, one of the objectives of RSM is to establish a functional relationship between yy  and its associated control variables. Such a relationship is, in general, unknown, but can be approximated by a low-degree polynomial model of the form y=f'(x)β+ , where x=(x1,x2,...,xk)' f(x)  is a vector function of p elements that consists of powers and cross products of powers of x1,x2,...,xk  up to a certain degree denoted d(1), β  is a vector of p unknown constant coefficients referred to as parameters, and _ is a random experimental error assumed to have a zero mean. If model (2.1) provides an adequate representation of the response, then the quantity f'(x)β represents the so-called Mean response, or the Expected Value of y , and is denoted by μ(x) .

Two models are commonly used in RSM; they are the first-degree model (d = 1),

y=β0+ki=1βixi+ ;              (2.2)

and the second-degree model (d = 2),

y=β0+ki=1βixi+i<jβijxixj+ki=1βiix2i+ ;         (2.3)

Models (2.2) and (2.3) are special cases of model (2.1). The first model is usually used in the initial phase of the experiment representing part of an exploratory process to assess the important factors. The second model is subsequently developed after a series of experiments have been performed resulting in the identification of the important factors to be considered in the experiment. At this stage, the experimenter will be ready to use the model in doing data analysis to determine significance of the model's parameters, estimate the mean response, and to arrive at optimum operating conditions on the control variables that result in a maximum or a minimum response over a certain region of interest which we denote by R .

In order to estimate the unknown parameters in model (2.1), a series on n(>p)  experiments are performed in each of which the response y is measured for specified settings of the control variables. The totality of these settings constitutes the so called response surface design, or just design, which can be represented by a matrix, denoted by D , of order n×k called the design matrix,

D=[x11x12...x1kx21x22...x2k..................xn1xn2...xnk] ;(2.4)

Where xui denotes the uth  design setting of xi(i=1,2,...,k;u=1,2,...,n) . Each row of D  represents a point, referred to as a design point, in a k-dimensional u  clidean space. The response value obtained at the uth  setting of x , namely   xu=(xu1,xu2,...,xuk)' (u=1,2,...,n) , is denoted by yu . From (2.1) we thus have

yu=f'(xu)β+u, ; u=1,2,....,n (2.5)

Where u denotes the error term at the uth experimental run. Model (2.5) can be expressed in matrix form as

y=Xβ+ ;(2.6)

Where y=(y1,y2,...,yn)' 0, X  is a matrix of order n×p whose uth  row is f'(xu) , and =(1,2,....,n)' . Note that the first column of X  is the column of ones, 1n .

A common method for estimating the parameter vector in (2.6) is the one based on the method of ordinary least squares. This method requires that has a zero mean and a variance-covariance matrix given by σ2In  [see, for example, Khuri and Cornell (Section 2.3)].10 In this case, the least-squares estimator of β , denoted by ˆβ , is given by

ˆβ=(X'X)1X'y ; (2.7)

The variance-covariance matrix of ˆβ is then of the form

Var(ˆβ)=(X'X)1X'(σ2In)X(X'X)1

=σ2(X'X)1 :        (2.8)

An estimate ˆμ(xu) , of the mean response at xu , is obtained by replacing β  by ˆβ , that is,

 

  ˆμ(xu)=f'(xu)ˆβ, u=1,2,...,n. :       (2.9)

The quantity f'(xu)ˆβ also gives the value of the predicted response, ˆy(xu) , at the uth  design point (u=1,2,...,n) . In general, at any point, x , in the region R , the predicted response ˆy(x)  is

ˆy(x)=f'(x)ˆβ, xR : (2.10)

Using formula (2.8), the variance of ˆy(x) is then given by [Khuri and Cornell (1996, Section 6.1) or Khuri (2009, Section 12.4)]

Var[ˆy(x)]=σ2f'(x)(X'X)1f(x) : (2.11)

The expression on the right-hand side of (2.11) is called the Prediction variance. This is an important quantity since the quality of prediction depends on the size of this variance. Also, the determination of optimum operating conditions on the control Variables requires that the prediction variance be small over the region of interest, R , in order to arrive at reliable information about the true optimum of the response over R . This is of course dependent on the assumption that the postulated model in (2.1) does not suffer from Lack of fit (LOF). For a study of LOF of a fitted response surface model, see, for example, Khuri and Cornell (Section 2.6).10

Response surface designs

The choice of the design matrix, D , is quite important in any response surface investigation since the prediction variance depends on D  as can be seen from formula (2.11). Some common design properties are

  1. Orthogonality
  2. A design D  is said to be orthogonal if the matrix X'X  is diagonal, where X is the model matrix in (2.6). In this case, the elements of ˆβ  will be uncorrelated since the off-diagonal elements of Var(ˆβ) in (2.8) will be zero. If the error vector in (2.6) is assumed to be normally distributed as N(0,σ2In) , then these elements will be also stochastically independent. This makes it easier to test the significance of the unknown parameters in the model.

  3. Rotatability
  4. A design D is said to be rotatable if the prediction variance in (2.11) is constant at all points that are equidistant from the design center, which, by a proper coding of the control variables, can be chosen to be the point at the origin of the k -dimensional coordinates system. It follows that Var[ˆy(x)] is constant at all points that fall on the surface of a hyper sphere centered at the origin, if the design is rotatable. This causes the prediction variance to remain unchanged under any rotation of the coordinate axes. In addition, if optimization of ˆy(x) is desired on concentric hyper spheres, as in the application of ridge analysis, which will be discussed later, then it would be desirable for the design to be rotatable. This makes it easier to compare the values of ˆy(x) on a given hyper sphere as all such values will have the same variance.

    The necessary and sufficient condition for a design to be rotatable was given by Box and Hunter.2 See also Appendix 2B in15,16 introduced a measure that quantities the amount of rotatability in a response surface design. This measure can be helpful in comparing designs on the basis of rotatability, assessing the extent of departure from rotatability, and in improving readability by a proper augmentation of a non rotatable design.

  5. Optimal designs
  6. Optimal designs are those that are constructed on the basis of a certain optimality criterion that pertains to the 'closeness' of the predicted response, ˆy(x) , to the mean response, μ(x) over a certain region of interest, R . The design criteria that address the minimization of the variance associated with the estimation of model (2.1)'s unknown parameters are called Variance-related criteria. The most prominent of such criteria is the D-Optimality criterion which maximizes the determinant of the matrix X'X . This amounts to the minimization of the size of the confidence region on the vector β in model (2.6). Another variance-related criterion that is closely related to D-optimality is the G-Optimality criterion which requires the minimization of the maximum over R  of the prediction variance in (2.11).

    Such variance-related criteria are often referred to as Alphabetic optimality. They are meaningful when the fitted model in (2.1) represents the true relation- ship connecting y  to its control variables. There are, however, many situations Where this is not the case due to fitting the "wrong model". This results in the So-called Model bias. For example, a first-degree model may be fitted to a data set when in reality a second-degree model would be a better representative of the response data. Box and Draper3 placed a great emphasis on the role of bias in the choice of a response surface design and advocated choosing designs that minimized model bias. They considered the minimization of bias to be a very important design criterion, and in certain cases, even more important than the variance-related criteria.

Designs for first-degree models

Designs for fitting first-degree models as in (2.2) are called first-order designs. The most common of such designs are the 2k factorial ( k  is the number of control variables), and the Plackett-Burman design.

The 2k Factor 2k ial Design: In a  factorial design, each control variable is measured at two levels, which can be coded to take the values, -1, 1, that correspond to the so-called low and high levels, respectively, of each variable. This design consists of all possible combinations of such levels of the k factors. Thus, each row of the design matrix D in (2.4) consists of all 1's, all -1's, or a combination thereof. It therefore represents a particular treatment combination. In this case, the number, n , of experimental runs is equal to 2k  provided that no single design point is replicated more than once. For example, in an agricultural experiment, two levels of fertilizer A are combined with two levels of fertilizer B in order to study their effects on the yield of a certain vegetable crop over a certain period of time. This results in a 22 factorial experiment with four treatment combinations.

If k is large (k5) , the 2k  design requires a large number of design points. In this case, fractions of 2k  can be considered. For example, we can consider a one-half- fraction design which consists of one-half the number of points of a 2k  design, or a one-fourth-fraction design which consists of one- fourth the number of points of a 2k  design. In general, a 2mth  fraction of a 2k  design consists of 2km  points from a full 2k  design. Here, m is a positive integer such that 2kmk+1 so that all the k+1  parameters in model (2.2) can be estimated. The construction of fractions of a 2k  design is carried out in a particular manner, a description of which can be found in several experimental design textbooks, such as Box & Raktoe, et al.1719 See also Chapter 3 in Khuri and Cornell.15

The plackett-burman design: The Plackett-Burman design allows two levels for each of the k  control variables, just like a 2k design, but requires a much smaller number of experimental runs, especially if k  is large. It is therefore more economical than the 2k  design. Its number, n , of design points is equal to k+1 , which is the same as the number of parameters in model (2.2). In this respect, the design is said to be saturated because its number of design points is equal to the number of parameters to be estimated in the model. Furthermore, this design is available only when n is a multiple of 4. Therefore, it can be used when the number, k , of control variables is equal to 3, 7, 11, 15, ....

To construct a Plackett-Burman design in k  variables, a row is first selected whose elements are equal to -1 or 1 such that the number of 1's is k+12 and the number of -1's is k12 . The next k1 rows are generated from the first row by shifting it cyclically one place to the right k1 times. Then, a row of negative ones is added at the bottom of the design. For example, for k=7 , the design matrix, D , has 8 points whose coordinates are x1,x2,...,x7, , and is of the form

D=[11111111111111111111111111111111111111111111111111111111] :

Design arrangements for k=3,7,11,...,99 factors can be found in Plackett –Burman (1946).

Designs for second-degree models

These are designs for fitting second-degree models as in (2.3), which has p=1+2k+12k(k1) parameters (they are also referred to as second-order designs). The number of distinct design points of such design must therefore be at least equal to p. The design settings are sometimes coded so that 1nnu=1xui=0 and
1nnu=1x2ui=1, , i=1,2,...,k, , where n  is the number of experimental runs and xui  is the uth  setting of the ith control variable (u=1,2,...,n,i=1,2,...,k) .

The most frequently-used second-order designs are the 3k  factorial, central com- posite, and the Box-Behnken designs.

The   3k Factorial Design: The  factorial design consists of all the combinations of the levels of the k control variables which have three levels each. If the levels are equally spaced, then they can be coded so that they correspond to -1, 0, 1. For example, for k=2 , the design matrix, in coded form, consists of 9 points as shown below:

D=[111011010001111011] :

The number of design points for a 3k  design is 3k , which can be very large for a large k . The use of full factorial designs is therefore not feasible if the number of experimental units is limited. Fractions of a 3k  design can be considered to reduce the cost of running such an experiment. A general procedure for constructing fractions of 3k is described, for example, in.19 See also McLean and Anderson.20

The central composite design: The central composite design (CCD) is perhaps the most popular of all second-order designs. It was first introduced in1 as an alternative to the design. This design consists of the following three parts:

  1.  A complete (or a fraction of) 2k  factorial design whose factors' levels are coded as -1, 1. This is called the factorial portion of the design.
  2.  An axial portion consisting of 2k  points arranged so that two points are chosen on the axis of each control variable at a distance of α  from the design center (chosen as the point at the origin of the coordinates system). We refer to α as the axial parameter.
  3.  A certain number, n0 , of replications at the design center (n01) . This is called the center-point portion.

 Thus, the total number of design points in a CCD is n=2k+2k+n0 . For example, a CCD for k=2,α=2, n0=2 has the form

D=[11111111202002020000] :

We note that the CCD is obtained by augmenting a first-order design, namely, the and then n0  center-point replications. This design is usually developed in a manner consistent with the sequential nature of a response surface investigation in starting with a first- 2k  factorial with additional experimental runs, namely, the 2k  axial points order design, to fit a first-degree model, followed by the addition of design points to _t the larger second-degree model. The first-order design serves in a preliminary phase to get initial information about the response system and to assess the importance of the factors in a given experiment. The additional experimental runs are chosen for the purpose of estimating all the p parameters in model (2.3). The fitted model is then used in the determination of optimum operating conditions on the control variables over the region of experimentation.

When k  is large (k5) , the factorial portion can be replaced by a fraction of a 2k  design. For example, for k=5 , a one-half fraction of 25  can be used giving a total of 16 points in the factorial portion instead of 32 (for more details about fractionating in the factorial portion, see Khuri and Cornell, 1996, Section 4.5.3).

A CCD can become rotatable by assigning the value F1/4 to the axial parameter, α , where F denotes the number of points in its factorial portion, that is, α=F1/4 . In addition, the number of center-point replications, n0 , can be chosen so that a rotatable CCD will have the additional property of orthogonality (see Section 3). Note that orthogonality of a second-order design is attainable only after expressing model (2.3) in terms of orthogonal polynomials as explained in.2 See also.15 In particular, Table 4.3 in Khuri and Cornell's book can be used to determine the value of n0 in order for a rotatable CCD to have the additional orthogonality property.

The box-behnken design: This design was developed by Box GEP et al.21 It provides three levels for each factor and consists of a particular subset of the factorial combinations from the factorial design. The actual construction of such a design is described in the three RSM books,11 Khuri and Cornell (1996, Section 4.5.2), and.12 Some Box-Behnken designs are rotatable, but this design is not always rotatable. Box GEP21 list a number of design arrangements for k=3,4,5,6,7,9,10,11,12,and16  control variables.

The san cristobal design: Rojas22 introduced a variant of the CCD, called the San Cristobal Design (SCD), for sugar farming experiments. It is utilized in situations where the levels of k control variables are restricted to be nonnegative, as is the case with fertilizers experiments. The SCD consists of 2k factorial points combined with center and axial points, all contained within the positive orthant. It also includes a control where no fertilizers are applied. More recently, the performance of this design was evaluated by Haines LM23 who reviewed some of its properties.

Determination of optimum conditions

Optimization plays a key role in any response surface investigation. One of the main objectives of modeling the response is to use the fitted model in determining optimum conditions on the model's control variables that result in a maximum (or minimum) response over a certain region of interest, R . This, of course, assumes that the model has been screened to determine its suitability for providing an adequate representation of the mean response over the region R .

Quite often, a second-degree model is employed after a series of experiments have been sequentially carried out leading up to a region that is believed to contain the location of the optimum response. We shall therefore only mention optimization techniques that are applicable to such a model.

Optimization of a second-degree model

Let us consider the second-degree model in (2.3), which can be written as

y=β0+x'β*+x'Bx+ ;(4.1)

where x=(x1,x2,....,xk)',   β*=(β1,β2,....,βk)',  and B  is a symmetric matrix of order k×k whose ith  diagonal element is βii(i=1,2,...,k), , and its (i,j)th diagonal element is 12βij(i,j=1,2,...,k;ij) . If n  observations are obtained on  using a design matrix D as in (2.4), then (4.1) can be written in vector form as in (2.6), where the parameter vector β  consists of β0 and the elements of β*  and B . Assuming that E() = 0 and Var() = σ2In , the least-squares estimate of β  is ˆβ  as given in (2.7). The predicted response at a point x  in the region R  is then of the form    

ˆy(x)=ˆβ0+x'ˆβ*+x'ˆBx, (4.2)

where ˆβ0 and the elements of ˆβ*  and ˆB are the least-squares estimates of β0  and the corresponding elements of β* and B , respectively.

An unconstrained optimum is obtained by optimizing ˆy(x) unconditionally with respect to x . This is achieved by taking the partial derivatives of ˆy(x) with respect to x1,x2,...,xk , equating each one to zero and then solving the resulting k  equations. The solution to these equations provides the coordinates of the so-called stationarypoint which we denote by x0 . This point may not necessarily be a point of optimum. For a maximum at x0 , the matrix ˆB  must be negative definite, or equivalently, if its eigenvalues are all negative. For a minimum ˆB , must be positive definite, or Equivalently, if its eigenvalues are all positive (if some of the eigenvalues are positive and some are negative, then x0 is a saddle point). Of course, an optimum is only meaningful if x0 falls within the region R . If the location of the optimum falls outside this region, then it will be necessary to use the method of ridge analysis to determine Optimum conditions over R . This is explained in the next section.  

The method of ridge analysis: When the location of the stationary point falls outside the region of interest, R , the next step is to determine optimum operating conditions within the boundary of R . For this purpose we use the method of ridge analysis, which was originally introduced by Hoerl AE24 and later formalized by Draper NR.25 This method optimizes ˆy(x)  in (4.2) subject to x  being on the surface of a hyper sphere of radius r  and centered at the origin, namely,

ki=1x2i=r2  (4.3)

This constrained optimization is conducted using several values of  corresponding to hyper spheres contained within the region R . The rationale for doing this is to get information about the optimum at various distances from the origin within R . Since this optimization is subject to the equality constraint given by (4.3), the method of Lagrange multipliers can be used to search for the optimum. Let us there- fore consider the function

H=ˆβ0+x'ˆβ*+x'ˆBxλ(x'xr2), (4.4)

where λ is a Lagrange multiplier. Differentiating H  with respect to x and equating the derivative to zero, we get

ˆβ*+2(ˆBxλx)=0. (4.5)

Solving for x , we obtain

x=12(ˆBxλIn)1ˆβ*. (4.6)

A maximum (minimum) is achieved at this point if the matrix x[Hx']  of second- order partial derivatives of x  with respect to  is negative definite (positive definite). From (4.5), this matrix is given by

x[Hx']=2(ˆBλIn).

To achieve a maximum, Hoerl AE24 suggested that λ be chosen larger than the largest eigenvalue of ˆB . Such a choice causes ˆBλIn  to be negative definite. Choosing λ  smaller than the smallest eigenvalue of ˆB causes ˆBλIn  to be positive definite which results in a minimum. Thus, by choosing several values of in this fashion, we can, for each λ find the location of the optimum (maximum or minimum) by using formula (4.6) and hence obtain the value of x'x=r2 . The solution from (4.6) is feasible provided that corresponds to a hyper sphere that falls entirely within the region . The optimal value of ˆy(x) is computed by substituting x from (4.6) into the right-hand side of (4.2). This process generates plots of ˆy  and xi  against   (i=1,2,...,k).  These plots are useful in determining, at any given distance r  from the origin, the value of the optimum as well as its location. More details concerning this method can be found in Khuri AI,15 and.11

Khuri AI26 provided a modification of the method of ridge analysis by placing an added constraint on the size of the prediction variance associated with the predicted response in (4.2) within the region r . The rationale for the additional constraint stems from the fact that since optimization is based on using ^y(x), which is a random variable, it would be necessary for the prediction variance not to be highly variable within R . This modification can provide better optimization results, especially when the design used to _t model (4.2) is not rotatable.

The results of ridge analysis can be easily obtained using PROC RSREG in SAS Institute, Inc.27 and adding the "Ridge Max", or "Ridge Min" statements, depending on whether it is desired to have a maximum response or a minimum response, respectively, over the region R . It should be noted that regardless of how the control variables are coded, SAS codes the variables so that the boundary of R  has a radius equal to 1 (assuming that R  is spherical). The next numerical example gives details of the SAS code needed to _t the model, get its parameter estimates, determine the nature of the stationary point, and finally display the results of ridge analysis.

  1. Numerical example
  2. A central composite rotatable design with 6 center-point replications was set upto investigate the effects of three fertilizer ingredients on the yield of snap beans. The fertilizer ingredients and actual amounts applied were nitrogen (N), from 0.94 to 6.29 lb/plot; phosphoric acid (P2O5) , from 0.59 to 2.97 lb/plot; and potash (K2O) , from 0.60 to 4.22 lb/plot. The response of interest, y , is the average yield in pounds per plot of snap beans. The coded variables, x1,x2,x3, , are given by

   x1=N3.621.59,x2=P2O51.780.71,x3=K2O2.421.07

The design settings (in coded form) and corresponding response values are given in Table 1:15 We note that the design is rotatable since the axial parameter value is α=F1/4=1.682, , where F=8 is the number of points in the factorial portion of this CCD. The region R  is therefore spherical with a radius = 1.682.

In this example, the predicted response is

ˆy(x)=10.4620.574x1+0.183x2+0.456x30.678x1x2+1.183x1x3+0.233x2x30.676x21+0.563x220.273x23.

The matrix ˆB  [see formula (4.2)] is given by

ˆB=[0.6760.3390.5920.3390.5630.1170.5920.1170.273] :

x1

x2

x3

N

P2O5

K2O

Yield

-1

-1

-1

2.03

1.07

1.35

11.28

1

-1

-1

5.21

1.07

1.35

8.44

-1

1

-1

2.03

2.49

1.35

13.19

1

1

-1

5.21

2.49

1.35

7.71

-1

-1

1

2.03

1.07

3.49

8.94

1

-1

1

5.21

1.07

3.49

10.9

-1

1

1

2.03

2.49

3.49

11.85

1

1

1

5.21

2.49

3.49

11.03

-1.682

0

0

0.94

1.78

2.42

8.26

1.682

0

0

6.29

1.78

2.42

7.87

0

-1.682

0

3.62

0.59

2.42

12.08

0

1.682

0

3.62

2.97

2.42

11.06

0

0

-1.682

3.62

1.78

0.6

7.98

0

0

1.682

3.62

1.78

4.22

10.43

0

0

0

3.62

1.78

2.42

10.14

0

0

0

3.62

1.78

2.42

10.22

0

0

0

3.62

1.78

2.42

10.53

0

0

0

3.62

1.78

2.42

9.5

0

0

0

3.62

1.78

2.42

11.53

0

0

0

3.62

1.78

2.42

11.02

Table 1 Design Settings and Yield Values

The stationary point x0  corresponding to ˆy(x) is located at (- .394, - .364, - 0.175) is a saddle point since the eigenvalues of ˆB  are 1.841, 0.367, - 3.304 which have mixed signs. Thus ˆB  is neither positive definite nor negative definite, that is, it is indefinite. To find the maximum of ˆy(x) over R , it is necessary here to use the method of ridge analysis.

The needed SAS code to obtain the results of ridge analysis (using PROC RSREG) is given below

DATA;
INPUT x1,x2,x3. Y;
CARDS;
(enter here the data from Table 1)
PROC SORT;
BY X1X3 ;
RUN:
PROC RSREG;
MODEL Y=X1X3 /LACKFIT;
RIDGE MAX;
RUN;

The MODEL statement in PROC RSREG fits a second-degree model in the control variables, x1,x2,x3. . Note that the statements, "PROC SORT" and "BY X1X3 ," are needed to perform a lack-of-_t test [see Section 2.6 in Khuri and Cornell (1996)] on the second-degree model. The data are sorted by the variables x1,x2,x3. so that the eplicated observations at the design center are grouped together. The actual lack- of fit test is performed by adding the option "LACKFIT" to the MODEL statement in PROC RSREG. Using the data in Table 1, the resulting lack-of-fit F test statistic has the value with 5 and 5 degrees of freedom. The corresponding p-value is 0.1333 which is not significant at the 0.10 level.

The results of ridge analysis are shown in Table 2. We note that that the maximum response value, 12.886, is attained on the boundary of R  (identified by the coded radius 1 which corresponds to the radius r=1.682 ) at the point x1=0.544, x2=1.589, x3=0.089,  Expressed in units of pounds per plot, the corresponding levels of the original factors are N=2.755, P2O5=2.908, , and K2O=2.515.

Coded radius

Estimated response

x1

x2

x3

0

10.462

0

0

0

0.1

10.575

-0.106

0.102

0.081

0.2

10.693

-0.17

0.269

0.11

0.3

10.841

-0.221

0.438

0.118

0.4

11.024

-0.269

0.605

0.12

0.5

11.243

-0.316

0.771

0.117

0.6

11.499

-0.362

0.935

0.113

0.7

11.79

-0.408

1.099

0.108

0.8

12.119

-0.453

1.263

0.102

0.9

12.484

-0.499

1.426

0.096

1

12.886

-0.544

1.589

0.089

Table 2 Details of Ridge Analysis

Applications in agricultural and food sciences

Mead R, et al.8 were among the first authors to explore the use of RSM in biological research. They examined a large number of papers in biological journals to determine the extent of using RSM ideas. They reported that "not much awareness of current RSM methods was shown." They proposed a "joint development by the biologist and the statistician of particular biologically reasonable models for particular practical research problems." This is a good advice since the practical research worker will be more interested in methods that pertain to his (her) particular field of application rather than pursuing general results.

Fortunately, RSM has since become more applicable to a wide spectrum of applied research areas, including those with biological and agricultural applications. The development of new statistical software and the introduction of fast computers have made it a lot easier for practitioners to attempt more advanced RSM technique than was possible before. The food industry, in particular, has been a prime user of RSM since the early 1970s.5 devoted two sections to review various applications of RSM in the food and biological sciences. I myself was involved in one such application in determining the optimum combination of the levels of washing temperature, washing ratio of water volume to sample weight, and washing time on the quality of minced mullet flesh.28

In the remainder of this section, several papers will be cited to highlight some applications of RSM. These papers represent only a small sample since the actual number of papers with RSM applications is very large.

Edmondson RN14 provided an interesting application of RSM to greenhouse experiments and presented some valuable insights into the use of RSM in an agricultural setting versus an industrial one, as was mentioned earlier. Schmidt, et al.29 investigated the effects of cysteine and calcium chloride on the textural and water-holding characteristics of dialyzed whey protein concentrates gel systems. These characteristics were measured by hardness (y1) , cohesiveness (y2) , springiness (y3) , and compressible water (y4) . A central composite design with five center-point replications was used and a second-degree model was fitted to each of the four responses. This experiment involved four response variables and is therefore labeled as a multi response experiment. This is an important and a relatively recent area in RSM. It has attracted a lot of attention, especially in the context of simultaneous optimization of the various responses considered in the of operating conditions on the control variables that result in optimum, or near optimum, values for all the responses. Khuri, et al.15 applied a multi response optimization technique introduced by30 to the simultaneous maximization of the four responses, namely y1, y2, y3, y4, in29 experiment. A detailed review of multi response experiments can be found in Khuri.31,10 See also Chapter 7 in Khuri, A. I, et al.15 Another example concerning a multi response experiment was described in Evans RA, et al.32 who considered data of seed-germination percentages after four weeks incubation of four plant species in response to 55 alternating and constant-temperature regimes in dark laboratory germinators. A second-degree model was fitted to the data from each of the four species. This could have been treated as a multi response experiment involving the responses from the four species. Evans et al., however, chose to fit the models individually to their respective data, which is not advisable since the responses can be correlated and such individual fits ignore any interrelationships that may exist among the responses. Instead, multi response techniques should be used to fit the models in the multi response system [see, for example, Section 7.2 in].15

Keisling TC et al.33 utilized response surface techniques to predict weed age and future weed size from weed height. The objectives of their study were to: (a) utilize response models to generate data for describing weed interference in soybeans, (b) present strategies for estimating multispecies interference, and (c) project yield loss from existing data. Such a study was designed to produce information to assist soybean producers in recognizing economically detrimental threshold levels of weed infestations which require the initiation of control measures. Broudiscou et al34 investigated the effects of several mineral compounds on feed degradation and microbial growth in a continuous culture system using RSM. The models considered were of the second degree fitted to data generated by a nonstandard design that consisted of 16 points giving seven levels to each of the four factors in the experiment. The design had good characteristics (by comparison to a CCD with 25 experimental runs, as shown in their Table II on page 257), was close to being orthogonal, and almost rotatable. The authors used Khuri AI16 measure of rotatability to assess the percent rotatability of their design, which turned out to be 99.6 as compared to 89.2 for the CCD. Furthermore, the design was also more G-efficient.

 RSM has received attention for modeling the performance of agronomic experiments. For example,35 used inverse polynomials to model the yield of maize against three control variables, namely levels of nitrogen, phosphorous, and potassium. A 33 factorial design was used and the experiment was conducted in a randomized complete block layout with two replications per treatment combination. The inverse polynomial model36 provided a better fit than the traditional second-degree model. The latter model may produce negative estimates of the yield response, which, of course, must be positive. This shows that taking into account any physical knowledge known about the response can be very beneficial when choosing an appropriate model.

Food science has also benefited from the application of RSM to its various areas of research. Diniz FM et al.37 used RSM to study the effects of pH, temperature, and enzyme-substrate ratio (E/S) on the degree of hydrolysis of dogfish muscle protein. The effect of the hydrolysis variables was described using a Box-Behnken design (see Section 3.2.3). This design was also utilized by Cao W et al.38 to investigate the effects of x1  = ultrasonic temperature (30 70 oC), x2  = power (120 300 W), and x3  = time (10 50 min) on ultrasonic assisted extraction for oligosaccharides from longan fruit pericarp (OLFP). Their fitted second-degree model was then used to obtain optimum conditions on that maximize the OLFP response. Optimization was also the goal of a study conducted by Jiang G et al.39 to study the effects of temperature, pH, and enzyme concentration/substrate concentration (E/S) ratio on the response, degree of hydrolysis (DH) for a marine shrimp called acetes chinensis that was harvested in China. The design used was a CCD for three control variables with n0=6  center-point replications and an axial parameter α=1.682 . This causes the design to be rotatable. Also, since n0=6 , the design has the additional uniform precision property.15 By definition, a rotatable design has the uniform precision property if the prediction variance at the design center is equal to the prediction variance at a distance of one (in the coded space) from the center. Such a property for a rotatable design maintains approximate uniform distribution of precision (in estimating the response) in the vicinity of the design center.15 The results of Cao et al.'s study indicated that hydrolysis of shrimp (acetes chinensis) resulted in a maximum DH value of about 26.33 % under the optimal conditions on temperature, pH, and E/S ratio.

Another optimization experiment was carried out by Zhang, et al.40 in a study concerning pyriodoxine (PN), which is one of the three members of the vitamin B6 group. It has broad applications in the food industry, cosmetics, and medical supplies. RSM was successfully applied to determine optimum operating conditions for maximum conversion of PN. The control variables were reaction temperature, re- action time, enzyme loading, molar substrate ratio, and water activity. The response was the conversion of PN. The design used was a CCD whose factorial portion consisted of a one-half fraction of a 25 factorial, its axial portion contained 10 points with an axial parameter α=2, and n0=6  center-point replications. This design is rotatable since α=F14 where F=16 is the number of factorial points. It also has the uniform precision property since n0=6  (Table 4.3 in).15 A listing of several applications of RSM in the optimization of chemical and biochemical processes was given by.41 In addition to their review of the recent literature on RSM applications to the aforementioned areas, they also provided a critique concerning the misuses of RSM in some of the reviewed articles.4244

Acknowledgments

None.

Conflicts of interest

None.

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