Quality Technology & Quantitative Management Vol. 12, No. 1, pp. 13-28, 2015 QTQM © ICAQM 2015 Experiments for Multi-Stage Processes John Tyssedal1,* and Murat Kulahci2,3 1 Department of Mathematical Sciences, The Norwegian University of Science and Technology, Trondheim, Norway Department of Applied Mathematics and Computer Science, Technical University of Denmark, Lyngby, Denmark 3 Department of Business Administration, Technology and Social Sciences, Luleå University of Technology, Luleå, Sweden 2 (Received October 2013, accepted February 2014) ______________________________________________________________________ Abstract: Multi-stage processes are very common in both process and manufacturing industries. In this article we present a methodology for designing experiments for multi-stage processes. Typically in these situations the design is expected to involve many factors from different stages. To minimize the required number of experimental runs, we suggest using mirror image pairs of experiments at each stage following the first. As the design criterion, we consider their projectivity and mainly focus on projectivity P 3 designs. We provide the methodology for generating these designs for processes with any number of stages and also show how to identify and estimate the effects. Both regular and non-regular designs are considered as base designs in generating the overall design. Keywords: Alias structure, nonregular designs, projective properties, regular designs, restriction on randomization, two-level designs. ______________________________________________________________________ 1. Introduction I n most industrial processes, the raw materials go through a series of stages before the final product is obtained. It is also often the case that the quality characteristics of the final product are affected by several factors at each stage. These relationships can be effectively determined via carefully designed experiments. The common practice in this case is to design separate sets of experiments for each stage. The main reason for this is that a more holistic approach in which the entire process is considered at once will most likely involve many factors which will further imply an excessive increase in the total number of experiments required. However the major drawback of running separate experiments independently for each stage is the fact that this strategy will fail to capture the often important interaction effects between factors from different stages. We will in this article provide a methodology for designing experiments for the entire process that will enable the practitioners to properly explore these relationships with the minimum number of runs. In the execution of the experiments for multi-stage processes, another important issue to consider is the randomization of the runs. In fact, a complete randomization will often lead to overwhelmingly large costs. Thus certain restrictions should be enforced on randomization. As depicted in Figure 1, a solution is to run the experiments in a splitting fashion. That is, the output from the first experiment in a stage is split into smaller pieces and used in the subsequent stage. This is in execution quite similar to the designs used in split-plot experimentation [7]. In fact a typical split-plot experiment can be considered as an experiment for a two-stage process. Similarly a split-split-plot design can be considered as a design for a three-stage process. * Corresponding author. E-mail: [email protected] 14 Tyssedal and Kulahci Figure 1. Experiments for a Multi-stage Process. The earlier studies in split-plot experimentation can be found in agriculture [29] and in manufacturing [1, 20]. Some recent work can be found in [2, 3, 4, 5, 6, 13]. These studies were mainly concerned with two-level fractional factorial split plot designs. On the other hand in [15] and [16] the general methodology for the use of Plackett and Burman (PB) designs [23] in split-plot experiments is provided. Further work [28] provide the methodology for designing split-plot designs of high projectivity based on regular and nonregular designs using only two mirror image pairs at the sub-plot level for each level combination of the whole-plot factors. This allows for keeping the total number of experiments as small as possible while achieving desirable projectivity of 3 or higher. Split-plot designs and their extensions for processes with more than two-stages are characterized by having a nested unit structure. An example of a two-level screening design with such a structure, a four stage split-split-split-plot design for identifying factors causing rancidity of stored meat loaf, is given in [11]. D-optimal designs of split-split-plot experiments are considered in [14]. The purpose of this paper is to extend the ideas presented in [28] to two-level experiments for multi-stage processes using mirror image pairs at each stage except the first. We obtain similar appealing properties. As for split-plot designs with mirror image pairs as sub-plots (SPMIP designs) the identification of and inference about active effects can be broken down to as many steps as there are stages and can in most cases be performed by ordinary least square which saves computational time and effort. In addition their projective properties can be quite attractive compared to their run sizes making them very appealing for screening purposes. To our knowledge this way of constructing experiments for multi-stage processes and the discussion on the possible obtainable simplifications in the analysis have never been addressed in the literature before. Similarly we believe that multi-stage experiments constructed from nonregular designs have never been proposed previously. Designs with a crossed unit structure have also been studied and used for multistage processes. Examples are strip-strip-block and split–lot designs. For construction and analysis of these we refer to [6, 10, 21, 24-25]. This paper is organized as follows: In Section 2 we first explain the general structure of multi-stage split plot designs with mirror image pairs. Thereafter in Section 3 a short introduction to the concept of projectivity and its general usefulness is given before we in Section 4 and Section 5 show how multi-stage split-plot designs of projectivity P 3 can be constructed from both regular and nonregular designs. In Section 6 we then proceed to show that for these designs the generalized least squares estimates equals the ordinary least squares estimates, develop the structure of aliasing between main effects and two-factor interactions and show how the identification of active factors and the estimation of the corresponding effects can be done in k steps using ordinary least squares (OLS) in each step. Concluding remarks are given in Section 7. Experiments for Multi-Stage Processes 15 2. Multi-stage Split-plot Designs with Mirror Image Pairs, MSPMIP DESIGNS The major concern in a holistic approach to designing experiments for multi-stage processes is the number of experiments that are needed to accommodate the increasing number of factors as the number of stages increases. In fact the smallest set of experiments will be achieved if only two experiments are run at each stage for each experiment from the previous stage. A possibility is to run these two experiments as mirror image pairs. We will call the new class of designs obtained by this construction multi-stage split-plot designs with mirror image pairs, abbreviated as MSPMIP designs. Figure 2 shows an illustration of a three-stage MSPMIP design. Now let 1 1 B . 1 1 Then using the standard convention letting -1 denote the low level of a factor and 1 the high level, a MSPMIP design for two stages can be obtained from B B B B . (1) It should be noted that this design can accommodate 1 factor at the first stage and 2 factors at the second stage. Stage 1 Stage 2 Stage 3 Figure 2. A three-stage MSPMIP design with 1, 2 and 4 factors in stages one, two and three respectively. Only the signs are used for the levels. For a three-stage process we can have B B B B B B B B . B B B B B B B B (2) In this design, we can allocate 1, 2 and 4 factors in stages one, two and three respectively. If we now let D be any design matrix for a two-level design expanded with a column of +1’s and use it as the ”basis” design, matrix representations for two-, three- and four-stage processes constructed from D by successive doubling, can be found in Figure 3. It can then be shown that for a given D that can accommodate up to p factors, the design in Figure 3 can accommodate up to p factors at the first stage, p 1 factors at second stage, 2( p 1) factors at stage 3 and 4( p 1) factors at stage 4. In general designs constructed in this manner can accommodate up to 2 k 2 p 1 factors at stage k where k2. 16 Tyssedal and Kulahci To further generalize the above procedure to any MSPMIP design and allow for different factorial designs to be used at each stage, we can write any k -stage design as a two-stage design in the following way. (a) two-stage (b) three-stage (c) four-stage Figure 3. The matrix representations for the designs for multi-stage processes. D* D*k *k 1 Dk 1 Dk . Dk (3) Here D*k 1 consists of the design columns for a k 1 stage process and Dk Dk consists of the design columns at stage k . It should be noted that Dk can be any factorial design. The same decomposition can also be performed for the previous stages except the first. Provided that the smallest possible design is employed at the first stage, MSPMIP designs offer designs with the least amount of total number of experiments possible. The drawback of this is the fact that if many factors are to be considered in each stage, the alias structure may become quite cumbersome. For the rest of this paper we will only consider MSPMIP designs constructed from orthogonal two-level designs. The aliasing between main effects and two-factor interactions can then be simplified using designs of projectivity P 3 or higher. In the next section we will define projectivity and explain the usefulness of exploring projective properties of MSPMIP designs. 3. Projective Properties and MSPMIP Designs According to the definition of projectivity for two-level designs given in [8], a N k design with N runs and k factors each at two levels is said to be of projectivity P and is called a ( N , k, P ) screen if every subset of P factors out of possible k contains a complete 2 P factorial design, possibly with some points replicated. The projective properties of a design are considered most important for screening experiments where only a few out of many factors considered are assumed to be active. For two-level fractional factorial designs, i.e. 1 2 p , p 0,2,, k 1 fractions of 2 k factorials also called regular designs, there is a close relationship between the concepts of resolution and projectivity. In fact for two-level fractional factorial designs with p 1 , P R 1 where R is the resolution. Another class of two-level designs is the nonregular designs i.e. those orthogonal two-level designs that do not belong to the 2 k p family. These designs apparently exist for every N a multiple of four, N 12 , and thereby provide a lot more design alternatives than the 2 k p fractional factorials. For many of these nonregular designs the projectivity P is greater or equal to 3 while their resolution is also 3. Therefore design properties of nonregular designs are not well described in terms of resolution while the concept of Experiments for Multi-Stage Processes 17 projectivity is useful for both regular and nonregular designs. Besides its more general applicability, projectivity P ensures that all main effects and all interactions of any P factors can be estimated with no bias if the other factors are inert and projectivity P 3 implies that it is possible to de-alias main effects from two-factor interactions. 4. Construction of MSPMIP Designs from Regular Designs Consider the four stage design in Figure 3 and let i 1 1 and 1 1 1 . It may then be given the following representation. i i i i i i i i 1 2 12 1 i 1 1 1 1 1 1 1 1 i i i i i i i 1 1 1 1 1 1 1 3 13 i 1 i i 1 i 1 i i 1 i 1 1 i 1 i 1 i 1 i 1 i 1 i 1 i 1 1 i i 23 123 1 1 4 14 24 124 34 134 234 1234 i i i i 1 i 1 i 1 i 1 i 1 i 1 i 1 1 i 1 i 1 i 1 1 i 1 i 1 i 1 . i i i i 1 i 1 i 1 i 1 1 i 1 i 1 i 1 1 i 1 i 1 i 1 1 i 1 i 1 i 1 1 (4) In (4), the column headings represent the main effects and interactions in a 2 4 design. Following the arguments from the previous section, we can see that this design can accommodate up to one, two, four and eight factors in stages 1, 2, 3 and 4 respectively. We also notice that the representation in (4) can be used to construct a design in three stages with three factors at stage 1 (allocated in columns labeled 1, 2 and 12), four factors at stage 2 (in columns 3, 13, 23 and 123) and eight factors at stage 3 (in columns 4, 14, 24, 124, 34, 134, 234 and 1234) as well as a two-stage design with seven factors at stage 1 (1,2,12, 3, 13, 23, 123). In general the possible splitting of a saturated regular two level designs into k stages can easily be accomplished by in each splitting considering it as a two-stage design as illustrated in (3). Since the decomposition given in (3) also applies for the previous stages we can write D* Dk-i i 0,1,, k - 2, (5) D*k-i *k-i -1 , D k-i -1 Dk-i where D*k-i -1 consists of the design columns for all stages up to k - i 1 and Dk i Dk i consists of the design columns at stage k i . The maximum possible numbers of factors on stage k is then N 2 where N is the total number of runs. Similarly the maximum number of factor columns at stage k 1 can be found by treating D*k 1 as a two-stage design in N 2 runs and so on. The alias structure for these designs is identical to the alias structure of the corresponding fractional factorial. In the following we will concentrate on designs of projectivity P 3 . The procedure given above also applies to these designs. In [28] it is shown that the maximum number of factors in each stage for a two stage P 3 design is N 4 . To generalize the notation introduced in [28], we will define the designs for a k-stage process using the notation N , n1 , n2 ,, nk , P where N is the total number of experiments, ni is the number of factors in stage i and P is the projectivity. It is then for instance possible to construct a (16, 4, 4, 3) screen for a two-stage process. If we want to construct a design for a three-stage process of projectivity P 3 , we can use the (8, 2, 2, 3) screen as D*2 in (3) and construct 18 Tyssedal and Kulahci a (16, 2, 2, 4, 3) screen. Similarly, a P 3 design for a four-stage process is then possible with four factors at stage 4 and two factors at stage 3. We will then be left with two factors for stages 1 and 2 yielding a (16, 1, 1, 2, 4, 3) screen for a four-stage process. In general for a three-stage process with total number of experiments N, a N , N 23 , N 23 , N 22 ,3 screen can be obtained using this construction technique. In this design up to N 23 factors can be allocated in each of the first two stages and up to N 2 2 in the last stage to ensure a projectivity P 3 design. To further generalize this to k-stage processes, we can have N , N 2 k , N 2 k , N 2 k 1 ,, N 22 , 3 screens following the same design construction methodology. In Tables 1 and 2, we summarize design possibilities and factor allocations for 16, 32 and 64 runs experiments for three-stage and four-stage processes. These tables correspond to the maximum allowable number of factors at each stage in order to have a design of projectivity P 3 . Table 1. Designs of Projectivity P 3 for a three-stage process with the maximum number of columns. Factor allocation is done according to the column labels of the corresponding full factorial design augmented with interaction columns. Total Number of Runs 8 16 32 64 Design (8,1, 1, 2, 3) (16, 2, 2, 4, 3) (32, 4, 4, 8, 3) (64, 8, 8, 16, 3) Factor Allocation Stage 1 Stage 2 Stage 3 1 1,2 1,2,3,123 1,2,3,123,4, 124,134,234 2 3,123 4,124,134,234 5,125,135,145, 235,245,345,12345 3,123 4,124,134,234 5,125,135,145,235, 245, 345,12345 6,126,136,146,156,236,246,256,346,356 ,456,12346,12356,12456,13456,23456 Table 2. Designs of Projectivity P 3 for a four-stage process with the maximum number of columns. Factor allocation is done according to the column labels of the corresponding full factorial design augmented with interaction columns. Total Number of Runs 16 Design Factor Allocation Stage 1 Stage 2 Stage 3 (16,1,1,2,4,3) 1 2 3,123 32 (32,2,2,4,8,3) 1,2 3,123 4,124,134,234 64 (64,4,4,8,16,3) 1,2,3, 123 4,124, 134,234 5,125,135,145,235, 245,345,12345 Stage 4 4,124,134,234 5,125,135,145,235, 245,345,12345 6,126,136,146,156,236,246, 256,346,356,456,12346, 12356,12456,13456,23456 MSPMIP designs with projectivity P 3 can also be obtained following this construction methodology starting with a two-stage P 3 design. A list of such designs is given in [28]. For instance there exists a (16, 3, 2, 4) design and thereby one can construct (16, 2, 1, 2, 4) or (16, 1, 2, 2, 4) three-stages designs or a (16, 1, 1, 1, 2, 4) four-stage design. If at any stage less number of factors is to be considered, the designs provided in Tables 1 and 2 can still be used by only allocating the necessary amount of factors in any of the columns suggested in these tables. However other choices of designs may lead to designs with less aliasing or a more favourable alias pattern for the given experimental situation. In Appendix A, tables of projectivity P =3 designs are provided for N 16 and 32 (Table A1) and also for projectivity P 4 designs for N 16 , 32 and 64 (Table A2). These are constructed from tables for two-stage designs provided in [28] following the procedure presented above. However as the number of stages increases, the total number of experiments needed gets large. Furthermore there will be more restrictions on the number of factors that can be allocated in each stage to ensure the desired projectivity. Therefore MSPMIP designs based Experiments for Multi-Stage Processes 19 on nonregular designs offer more appealing alternatives. 5. Construction of MSPMIP Designs from Nonregular Designs The best known nonregular designs are the Plackett and Burman (PB) designs with the number of runs N 2 k . Classification of PB designs with respect to projectivity P 2 , P 3 and P 4 can be found in [8] and [26]. Most nonregular PB designs are in fact N , N 1,3 screens from which 2 N , N 1, N 1,3 screens can be constructed for two-stage processes using the technique of doubling described below. The exceptions are for the number of runs N 40, 56, 88 or 96 where only N 2 of the main effects columns can be used. From these designs, 2 N , N 2, N 2,3 screens can be constructed for two-stage processes. The 24, 11, 11, 3 screen obtained by doubling the 12-run PB design (PB12) is given below PB12 PB12 (6) PB12 PB12 . This design is of projectivity 3 and can accommodate up to 11 factors in the first stage allocated to the columns 1 to 11, and up to 11 factors in the second stage that can be allocated to the last 11 columns. As in the case of regular designs, MSPMIP designs can be generated for processes with more than two stages. For a three-stage process for example, the following 48,11,11,22,3 screen can be obtained as PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 PB12 . PB12 PB12 (7) In general a MSPMIP design for a k -stage process can be obtained from a N ,(( N 2 k 1 ) 1),(( N 2 k 1 ) 1),(( N 2 k 1 ) 1)21 ,,(( N 2 k 1 ) 1)2 k 2 ,3 screen con-structed by successively doubling a nonregular two-level design of projectivity P 3 . As it can be seen from this general representation, nonregular designs offer better alternatives compared to regular designs in terms of the number of factors allowed in each stage while still ensuring a projectivity P 3 design. As mentioned in [28] for two-stage cases, the construction methodology given in (6) may lead to designs where some two-factor interactions are fully aliased with other two-factor interactions which may complicate the identification of active effects. This can be avoided using distinct columns of the same nonregular design at different stages as for example the following design for a three-stage process. Stage 1 i i i i S1 S1 S1 S1 Stage 2 Stage 3 i S3 i S2 S2 i S3 i , S2 i S3 i S2 i S3 i (8) where S1 S2 S3 PB12 . It should be noted that the columns i i i i and i i i i are added for the stages two and three respectively. This implies that the 20 Tyssedal and Kulahci total number of factors that can be allocated in this design is 13. We represent this design as a (48, n1 , n2 , n3 ,3) n1 n2 n3 13 screen. In general, it can be shown that we have ( N , n1 , n2 , n3 ,3) n1 n2 n3 n 32 screens where a n run nonregular P 3 design is used as the base design and N 4 n . In the same way we can generalize this representation to k -stage processes by constructing (2 k 1 n, n1 , n2 ,, nk ,3) n1 n2 nk n k 2 screens. 6. Inference for MSPMIP Designs Let the columns for the main effects and interactions be given in X and let Σ be the covariance matrix for the responses. The generalized least squares (GLS) estimator and the OLS estimator for the coefficients are given by β * ( XΣ 1 X) 1 XΣ 1Y and βˆ ( XX) -1 XY respectively. For SPMIP designs for two-stage processes as given in [28] it follows from the results given in [19] that these two estimators are equal, see also [27]. It is also explained in [27] how inference about and identification of active effects can be done in two separate steps when SPMIP designs are used. These results also generalize to the MSPMIP designs. Result: Let X contain the columns for the main effects and interactions to be estimated for a three stage MSPMIP design. Furthermore assume that the error terms on different stages are uncorrelated and that the error terms in stage i , i 1,2,, k are identically and independently distributed with expectation 0 and variance i2 . Then the generalized least squares estimates of the coefficients are identical to the ordinary least squares estimates. Proof. The covariance matrix for the response in a three-stage process can be written as the N N matrix C 0 0 0 0 C 0 0 . V 0 0 0 0 0 0 C where 12 22 32 12 22 12 12 2 2 2 2 2 2 2 1 2 3 1 1 1 2 C . 2 2 2 2 2 2 2 1 1 1 2 3 1 2 12 12 12 22 12 22 32 C-1 0 0 0 -1 0 0 0 C -1 . We also have V O 0 0 0 C-1 Let 2 12 22 and 1 1 1 . Then C can be written as: Σ 2 32 2 12 11 where Σ C 22 , 2 2 2 32 Σ 2 1 11 has the form of the C matrix for the corresponding two-stage process. From [18] p. 459, it can be shown that Experiments for Multi-Stage Processes 21 Σ21 k1 11 k2 11 C , Σ21 k1 11 k2 11 1 where k1 and k 2 are two constants. In [19] it is shown that for the least squares estimates to be equal to the generalized least squares estimates, Xy 0 should imply XV 1y 0 , where X is the design matrix. Following the notation in [17] any column in X may be written as x1 x 2 x 3 where is the Kronecker product. It should be noted that the elements in x2 x3 are either equal to 1 or the elements in at least one of x 2 and x 3 sum to zero. Case 1. The elements in x2 x3 are all equal to 1. Thereby x2 x3 = 114 and x1 x2 x3 V 1y x1 1C1 y . The elements in C-1 will column wise sum to the same constant, say a (see also [17]). Therefore x 1C y a x 1 y a x x x y 0 1 1 1 1 2 if 3 x1 x2 x3 y 0 . Case 2. The elements in at least one of x 2 and x 3 sum to zero. Then also the elements in x2 x3 sum to zero. If the elements in x 3 sum to zero, the two first elements in x2 x3 as well as the two last ones also sum to zero. Let the two first elements in x2 x3 be x . For the two stage process we know [17] that if x is a 2 1 vector with elements that sum to zero, x 21 y 0 if Xy 0 and obviously k1 x11 k2 x11 0 and the result follows. If the elements in x3 are equal to 1 then x2 x3 = x3 x3 or x3 x3 . In both cases x2 x3 C1 a1 x2 x3 where a1 is a constant and x1 x2 x3 V 1y x1 x2 x3 C1 y a1 x1 x2 x3 y 0 if x1 x2 x3 y 0. The general proof for a k -stage process can then be fulfilled by induction in exactly the same way assuming the result is true for the k 1 -stage process and from that derive that it also must be true for a k -stage process. In MSPMIP designs, one concern is about the potentially excessive confounding among the effects. To assess the degree of aliasing in these designs we will use the alias matrix originally introduced in [9]. Suppose we fit the regression model E( Y ) X1β1 but the true expectation is given by E( Y) X1β1 X2 β2 . The expected value of the OLS estimator βˆ 1 ( X1 X1 ) 1 X1 Y is then E βˆ 1 βˆ 1 ( X1 X1 ) 1 X1 X2 βˆ 2 . The matrix A ( X1 X1 ) 1 X1 X 2 is the alias matrix showing to what extent an assumed model potentially will be biased by additional effects in X2 . The equivalence of the GLS and OLS estimators makes the expression for the OLS alias matrix also valid for the effects from MSPMIP designs. In order to derive an expression for A in a k -stage process, we again write the design matrix as in (3). The matrix of two-factor interactions can then be written as: D*k 1 D*k 1 X2 D* D* k 1 k 1 D D * k 1 D D D Dk * k 1 k Dk , k Dk k (9) where D*k 1 D*k 1 represents the matrix with the two-factor interaction columns between the factors in D*k 1 , D*k 1 Dk represents the matrix with the two-factor interaction columns between the factors in D*k 1 and Dk , and Dk Dk represents the matrix with the two-factor interaction columns between the factors in Dk . 22 Tyssedal and Kulahci We will now assume that interactions of order higher than two can be neglected and restrict ourselves to the case where the matrix of main effects columns, X 1 , is orthogonal. Then X1 X1 NI and following the procedure in [28], we have after some rearranging 2 D k-1 Dk 1 Dk 1 A= N 0 . Dk Dk 1 D k Dk 1 D k Dk 0 0 To elaborate further we use (5) and write D*k 2 Dk -1 * Dk 1 * , Dk 2 Dk -1 which gives for A 0 2 D k 2 Dk 2 Dk 2 0 2 Dk 2 D k 1 Dk 1 D Dk -2 k -1 Dk Dk Dk Dk - D k -1 Dk -2 2 A = N 2 D D D 0 k -2 k -1 k 1 0 0 0 0 (10) (11) 0 0 . 0 Dk -2 Dk Dk D k -2 Dk -1 Dk Dk - D k -1 0 (12) To investigate the alias structure given in (12), let i , j represent a two factor interaction between a factor from stage i and a factor from stage j . It can then be seen that a main effect from stage k is possibly aliased with two-factor interactions of the type i , k where i k 1, k 2,,1 . In fact it can be shown that except for the first stage, a main effect from stage i is possibly aliased with two-factor interactions of the type i , j where j i 1, i 2,,1 and with two-factor interactions of the type l , l where l i 1, i 2,, k . The main effects from the first stage are possibly aliased with two-factor interactions of type i , i where i 1,, k 1, k . For example the alias matrix for a three-stage process is given by 2 D1 D D 1 1 2 A 0 N 0 2 D1 D2 D2 0 0 D1 D D3 D3 1 0 D2 D D3 D3 2 D2 D1D2 2 0 0 0 0 D D3 1 D3 D1 . (13) 0 D D3 2 D3 D2 0 Experiments for Multi-Stage Processes 23 Equation (13) reveals that there is a possible aliasing between main effects from stage one and two factor interactions of the type (1,1), (2,2) and (3,3), between main effects from stage two and two factor interactions of the type (1,2) and (3,3) and between main effects from stage three and two factor interactions of the type (1,3) and (2,3). However in most of the cases discussed here, the MSPMIP design is constructed from a base design D and the factor columns on a given stage can be split up further. For instance in Figure 3, the design factors on stage 2 are D D D D and the design factors on stage 3 are D D D D D D D D . A closer inspection of the multi-stage processes in Figure 3 also reveals that the sign pattern for the base design D in a k-stage design is the same as for an ordinary 2 k -1 design. As a result, a specific interaction between two factors on the same stage can only be aliased with main effects on exactly one of the stages and two-factor interactions aliased with main effects on different stages are orthogonal. A further simplification is achieved if the columns on each stage are constructed from different main effects columns of the same design as in (8). Then the main effects on a specific stage after the first can only be aliased with two-factor interactions between factors on that stage and the first stage. For the cases given above, define X * D1* , D*2 ,, D*k where Di* contains the columns for the main effects at stage i and their possibly aliased two-factor interactions to be estimated as explained after equation (12). From the discussion above it follows that Di*D*j 0, i, j =1,2,,k, i j . The covariance matrix for the GLS estimator of the coefficients, β̂ , can be derived the same way as for SPMIP designs in [27]. With Y the vector of observations, the GLS estimator is equal to the OLS estimator ˆ ( X * X * ) 1 X * Y and, hence Cov(ˆ ) ( X *X * ) 1 ( X * VX * )( X *X * ) 1 , where V = Cov Y . Now following the same procedure as in [27], V can be written as: k 1 V k2-i M k -i , i 0 where M k I N N and in general M k -i B k -i 0 0 0 0 B k -i 0 0 0 0 0 0 , 0 0 B k -i where B k -i 2i 2i matrices of 1’s. From this we can derive the following expression for Cov βˆ . Cov βˆ 2 k * * D1 D1 0 0 1 0 * * D 2 D 2 0 0 0 1 0 0 0 * * Dk Dk 2 2 k -1 1 * * D1 D1 1 0 0 0 0 0 0 * * D k 1 D k 1 0 0 1 k 1 2 2 1 0 0 * * D1 D1 1 0 0 0 0 0 0 0 0 0 0 0 . 24 Tyssedal and Kulahci Assuming interactions of order higher than two are negligible, this shows that inference about the effects for a k -stage process can be done in k separate steps, where we in each step consider the main effects for the factors at the respective stage and their possibly aliased two-factor interactions. In [27] it is also shown how the identification of active factors for a two-stage process can be done in two separate steps. Writing a k -stage design as a two-stage design as in (3) and thereafter successively using (5), it follows that the same identification procedure generalizes to the k -stage process. Starting with stage k and working backwards we can for each stage perform a search procedure based on OLS to identify the respective active effects among the main effects for that stage and their possibly aliased two-factor interactions. In some applications it is not realistic to assume that the error terms at a given stage have identical variances. V is still a block diagonal matrix but the blocks need not to be identical and the OLS and GLS estimates may differ. It is expected that the occurrence of unequal variances is more likely to happen for the first stages of the experimentation. If the error terms within a certain stage have equal variances and this is also true for all the following stages, the OLS estimates will still equal the GLS estimates for all main effects and their possibly aliased two-factor interactions on that stage and the succeeding ones. The generalization of the two stage procedure given [27] also applies to these stages. To treat the more general situation we refer to [22]. 7. Concluding Remarks Generating designs for multi-stage processes where in each stage the experiments are run as mirror image trials ensures that the total number of experiments can be minimized. Saturated fractional factorials have a structure that fits well into the MSPMIP scheme. However, in order to have designs of projectivity P 3 , there will be strict restrictions on the number of factors allowed at each stage. Nonregular designs such as Plackett Burman designs with the number of runs N 2 k for instance are therefore very appealing alternatives as base designs, offering a wide variety of choices and being able to accommodate considerably more number of factors compared to their regular counterparts. Especially designs created by using different columns in a nonregular designs, the (2 k 1 n, n1 , n2 ,, nk ,3) n1 n2 nk n k 2 designs, has great flexibility and desirable alias structure, avoiding full aliasing between two-factor interactions. As for two-level split-plot mirror image pairs designs, the GLS estimates and OLS estimates of the effects in MSPMIP designs are identical using the standard assumptions, and in most cases the identification of active factors and estimation of the corresponding effects can be done in k steps using OLS in each step. References 1. 2. 3. 4. 5. 6. Addelman, S. (1964). Some two-level fractional factorial plans with split-plot confounding. Technometrics, 6, 253-258. Bingham, D. and Sitter, R. S. (1999). Minimum aberration two-level fractional factorial split-plot designs. Technometrics, 41, 62-70. Bingham, D. and Sitter, R. R. (2001). Design issues in fractional factorial split-plot experiments. Journal of Quality Technology, 33, 2-15. 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Technometrics, 47, 495-501. Kulahci, M. and Bisgaard, S. (2006). A generalization of the alias matrix. Journal of Applied Statistic, 33(4), 387-395. Mardia, K. V., Kent, J. T. and Bibby, J. M. (1982). Multivariate Analysis, Academic Press Inc, London. McElroy, F. W. (1967). A necessary and sufficient condition that the ordinary least squares estimators be best linear unbiased. Journal of the American Statistical Association, 62, 1302-1304. Michaels, S. E. (1964). The usefulness of experimental designs. Journal of the Royal Statistical Society, Series C, 13, 221-235. Mee, R. W. and Bates, R. L. (1998). Split-lot designs: experiments for multistage batch processes. Technometrics, 40(2), 127-140. Myers, R. H. and Montgomery, D. C. (2002). Response Surface Methodology. Wiley & Sons, New York. Plackett, R. L. and Burman, J. P. (1946). The design of optimum multifactorial experiments. Biometrika, 33, 305-325. Paniagua-Quiñones, C. and Box, G. E. P. (2008). Use of strip-strip-block design for multi-stage processes to reduce cost of experimentation. Quality Engineering, 20(1), 46-52. Paniagua-Quiñones, C. and Box, G. E. P. (2009). A post-fractionated strip-strip-block design for multi-stage processes. Quality Engineering, 21(2), 156-167. Samset, O. and Tyssedal, J. (1999). Two-level designs with good projection properties. Technical Report 12, Department of Mathematical Sciences, The Norwegian University of Science and Technology, Norway. Tyssedal, J. and Kulahci, M. (2005). Analysis of split-plot designs with economical run sizes. Journal of Quality and Reliability Engineering International, 21(5), 539-551. Tyssedal, J., Kulahci, M. and Bisgaard, S. (2011). Split-plot designs with mirror image pairs as sub-plots. Journal of Statistical Planning and Inference. 141, 3686-3696. Yates, F. (1935). Complex experiments. Supplement to the Journal of the Royal Statistical Society, 2, 181-247. 26 Tyssedal and Kulahci Appendix A Table A1. A list of P 3 MSPMIP design for N =16 and 32. The notation N , x , y,, nk ,3 s m means that x , y, can take any number in the set 1,2,, s as long as their sum is m . Factor allocation can be done assigning 1,, x in Stage 1, x 1,, x y in Stage 2 and so on. Total Number of Runs 16 32 Factor allocation Design (16,2,2,4,3) (16,1,1,2,4,4) (32,1,1,8,3) Stage 1 Stage 2 1,2 1 1 3,123 2 2 (32,1,4,5,3) 1 (32,2,3,5,3) 1,2 (32,3,2,5,3) 1,2,3 4,24,34, 1234 4, 34, 1234 4,1234 (32,2,3,6,3) 1,2 (32,3,2,7,3) 1,2,3 (32,4,1,8,3) (32,2,4,8,3) 1,2,3, 123 1,2 (32,3,4,8,3) 1,2,3 (32,4,2,4,3) 1,2,3, 123 1,2,3, 123 1,2,3, 123 1 1 (32,x,y,4,3)s=3 (32,x,y,8,3)s=3 (32,x,y,5,3)s=4 (32,x,y,8,3)s=4 (32,4,2,8,3) (32,4,4,8,3) (32,1,1,1,4,3) (32,1,1,1,8,3) 4,34, 1234 4,1234 4 4,134, 124,234 4,134, 124,234 4,124 4, 124 Stage 3 4,124,134,234 3,123 4,124,134,234 5,35,45,1345,2345, 1245,1235,125 5,45,1235,12345 5,45,125,1345, 2345,135,1245,235 5, 1235,1245, 1345,2345 5,12345,125,345, 135,245,145,235 5,1235,1245, 1345,2345 5,1235,1245, 1345,2345 5,1235,1245, 1345,2345 5,125,135,145, 235,245 5,125,135,145, 235,245,345 5,12345,125,345, 135,245,145,235 5,12345,125,345, 135,245,145,235 5,12345,125,345, 135,245,145,235 5,1345,2345,125 4,124, 134,234 2 2 5,12345,125,345, 135,245,145,235 5,12345,125,345, 135,245,145,235 3 3 (32,x,y,z,5,3)s=4 (32,x,y,z,8,3)s=4 (32,1,1,3,5,3) (32,1,2,2,5,3) (32,2,1,2,5,3) (32,2,2,1,5,3) (32,1,1,4,8,3) 1 1 1,2 1,2 1 2 3,23 3 3,123 2 4,34,1234 4,1234 4,1234 4 4,134,124, 234 (32,1,2,4,8,3) 1 3,123 4,124,134,234 (32,2,2,4,8,3) 1,2 3,123 4,124,134,234 2 3,123 (32,1,1,2,4,8,3) 1 Stage 4 5,45,1235,12345 5,45,125,1345,2345, 135,1245,235 5,1235,1245,1345,2345 5,12345,125,345, 135,245,145,235 5,1235,1245,1345,2345 5,1235,1245,1345,2345 5,1235,1245,1345,2345 5,125,1245,1345,2345 5,12345,125,135, 245,145,235,345 5,12345,125,135, 245,145,235,345 5,12345,125,345, 135,245,145,235 4,124,134,234 5,12345,125,135, 245,145,235,345 Experiments for Multi-Stage Processes 27 Table A2. A list of P 4 MSPMIP designs for N =16, 32 and 64. The notation N , x , y,, nk ,3s m means that x , y, can take any number in the set 1,2,, s as long as their sum is m . Factor allocation can be done assigning 1,, x in Stage 1, x 1,, x y in Stage 2 and so on. Total Number of Runs 16 32 64 Design Factor allocation Stage 1 Stage 2 4,1234 (16, x, y, 2, 4)s=3 (16, 1, 1, 1, 2,4) 1 2 (32, x, y, 3, 4)s=3 (32, 3, 2, 1, 4) (32, 1, 4, 1, 4) 1,2,3 1 4,1234 4,24,34, 1234 (32, x, y, 2, 5)s=4 (32, 1, 1, 4, 5) 1 2 1 2 1 1 1 2 2 2 (64, x, y, 3, 4)s=5 (64, 1, 1, 5, 5) 1 2 (64, x, y, 3, 5)s=4 (64, 2, 4, 1, 5) 1,2 1,2,3,4 5,45,35, 12345 5,12345 1 2 (32, 1, 1, 1, 3, 4) (32, x, y, 2, 1, 4)s=3 (32, x, y, z, 2, 5)s=4 (32, 1, 1, 1, 2, 1, 4) (32, 1, 1, 1, 1, 2, 5) (64, 1, 1, 6, 4) (64, x, y, 5, 4)s=3 (64, x, y, 4, 4)s=4 (64, 4, 2, 1, 5) (64, x, y, 4, 6)s=3 (64, x, y, 2, 6)s=5 (64, 1, 1, 1, 5, 4) Stage 3 3 Stage 4 Stage 5 4,1234 4,1234 5, 45, 12345 5 5 5,12345 5,35,45, 12345 3 4,1234 3 3 6,36,46,56, 1346,23456 6,46,56,1456 23456 6,56,1236, 23456 6,1236,3456 6,56,46,36, 123456 6,56,123456 6 6 6,56,46, 123456 6,123456 3 (64, x ,y, z, 4, 4)s=4 (64, x, y, z, 3, 4)s=5 (64, x, y, z, 2, 4)s=6 (64, x, y, z, 3, 5)s=4 (64, x, y, 2, 1, 5)s=4 (64, 1, 1, 1, 1, 4, 4) 5,45, 12345 5 5,12345 4,1234 4 5 5,12345 6,56,46,1456, 23456 6,56,1236, 23456 6,1236,3456 6, 1236 6,56,12346 6 6,56,1236, 23456 (64, x, y, z, v, 3, 4)s=5 (64, x, y, z, 2, 1, 5)s=4 (64, x, y, z, v, 2, 6)s=5 (64, 1, 1, 1, 1, 1, 3, 4) 1 2 3 4 6,1236, 3456 6,1236 6,1236 6,56, 12346 6 6,12345 5 (64, 1, 1, 1, 1, 2, 2, 4) (64, 1, 1, 1, 2, 1, 2, 4) (64, 1, 1, 1, 1, 2, 1, 5) (64, 1, 1, 1, 1, 1, 2, 6) 1 1 1 1 2 2 2 2 3 3 3 3 4 4,1234 4 4 5,12345 5 5,12345 5 (64, x, y, z, 2, 2, 4)s=4 (64, x, y, 2, 1, 2, 4)s=3 (64, 1,1, 1, 1, 3, 5) 1 2 Stage 6 4,1234 3 5, 12345 5 4 5,12345 6,1236, 3456 6,1236 6,1236 6 6,123456 28 Tyssedal and Kulahci Authors’ Biographies: John Tyssedal is an Associate Professor at the Department of Mathematical Sciences at the Norwegian University of Science and Technology. He serves as an Associate Editor for QTQM. His research interests are in design of experiments and time series analysis. Murat Kulahci is an Associate Professor in the Department of Applied Mathematics and Computer Science at the Technical University of Denmark and in the Department of Business Administration, Technology and Social Sciences at Luleå University of Technology in Sweden. His research focuses on design of physical and computer experiments, statistical process control, time series analysis and forecasting, and financial engineering. He has presented his work in international conferences, and published over 50 articles in archival journals. He is the co-author of two books on time series analysis and forecasting.
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