STATGRAPHICS – Rev.

9/19/2009

DOE Wizard –Designs with Both Process and Mixture Factors

Summary
This document describes the construction and analysis of designs that include both process
factors and mixture components. The DOE Wizard facilitates the construction and analysis of
such designs by:

1. Creating two separate designs, one for the process factors and a second for the mixture
components.
2. Combining the 2 designs by generating runs for the mixture components at each
combination of the process factors.
3. Reducing the number of runs if desired using the D-efficiency criterion.
4. Analyzing the results using a combined model containing terms for both the process and
mixture variables.

Example
Myers, Montgomery and Anderson-Cook (2009) describe an example of such an experiment to
study an adhesive. The adhesive consists of 3 mixture components: a resin (X1) and two
crosslinkers (X2 and X3). The constraints on the components are:

X1 + X2 + X3 = 1
0.7 ≤ X1 ≤ 0.9
0.05 ≤ X2 ≤ 0.1
0.05 ≤ X3 ≤ 0.2

There are also two process variables: temperature (Z1) and relative humidity (Z2). Reasonable
ranges for these factors are:

40°F ≤ Z1 ≤ 100°F
15% ≤ Z2 ≤ 85%

There is one response variable:

Y: pulloff force (%)

that must exceed 40 pounds.

This document describes the construction and analysis of such an experiment.

Sample StatFolio: doewiz combined.sgp

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Design Creation
To begin the design creation process, start with an empty StatFolio. Select DOE – Experimental
Design Wizard to load the DOE Wizard’s main window. Then push each button in sequence to
create the design.

Step #1 – Define Responses

The first step of the design creation process displays a dialog box used to specify the response
variables. For the current example, there is a single response variable:

 Name: The name for the variable is pulloff force.

 Units: Pulloff force is measured as a percentage.

 Analyze: The parameter of interest is the mean pulloff force.

 Goal: The goal of the experiment is to maximize the mean.

 Impact: The relative importance of each response (not relevant if only one response).

 Sensitivity: The importance of being close to the best desired value (in this case, the
Maximum). Setting Sensitivity to Medium implies that the desirability attributed to the
response rises linearly between the Minimum and Maximum values indicated.

 Minimum and Maximum: Range of desirable values for the response.

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Step #2 – Define Experimental Factors

The second step displays a dialog box used to specify the factors that will be varied. In the
current example, there are 5 factors:

 Name – Each factor must be assigned a unique name.

 Units – Units are optional.

 Type – The first 2 factors are continuous process variables, while the others are mixture
components.

 Role – The role of each factor is Controllable.

 Low - the lower limits for the factors.

 High - the upper limits for the factors.

 Total for controllable mixture components – the constraint on the sum of the mixture
components.

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Step #3 – Select Design
The third step begins by displaying the dialog box shown below:

Two Options button are enabled, one for the process factors and one for the mixture components.
Pressing the first of the two displays the dialog box shown below:

Select the basic design class to use for the process variables. If you select Screening and press
OK, a second dialog box will be displayed listing different screening designs for two factors:

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For the example, a simple 2 by 2 factorial design was selected. After pressing OK, a third dialog
box will be displayed on which centerpoints or replicates could be requested:

The only non-default selection for this example is that the Randomize box has been unchecked to
allow users to duplicate the order of runs in this document.

Pressing OK one last time causes the 4 runs in the factorial design to be placed in the Select
Design dialog box:

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To select the design for the mixture components, press the second Options button. This will
display a list of available mixture designs:

Since the constraints on the 3 components do not allow experimental throughout a complete
simplex region, the only prefined design listed is the Extreme vertices design, which consists of 4
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runs at the vertices of the constrained experimental region. Selecting that design and pressing
OK displays the design options dialog box shown below:

Following Montgomery et al., we have:

1. Selected a quadratic model as the model of choice for the mixture components.

2. Selected Augment design to add 9 additional runs to the design (4 edge centers, the
centroid, and 4 axial checkblends).

We have also unchecked the Randomize option so that the runs will be created in standard order.

After OK is pressed, the mixture design will be added to the Select Design dialog box:

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Each of the 13 runs in the mixture experiment is performed at each of the 4 combinations of the
process factors, resulting in a total of 52 runs. If the design is acceptable, press OK one last time
to place the combined design in the STATGRAPHICS Databook and update the DOE Wizard’s
main window:

Step #4: Specify Model

Before evaluating the properties of the design, a tentative model must be specified. Pressing the
fourth button on the DOE Wizard’s toolbar displays a dialog box to make that choice:

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The default model includes a total of 24 terms. This includes 6 terms for the quadratic mixture
model by itself, plus all combinations of the 6 terms in the mixture model and the 3 terms in the
2-factor interaction process model. Note that the process components do not occur by themselves
in any of the model terms.

Step #5: Select Runs

Since the generated design contains 52 experimental runs while the model has only 24
coefficients, it may be desirable to reduce the number of runs in the design. To do so, press the
button labeled Step 5: Select runs and follow the procedure for creating a D-optimal design. You
may also selectively omit runs or add additional runs to the bottom of the design.

To reproduce the example in Montgomery et al., the experimental runs were reentered in the
order displayed in their Table 12.20, as shown below:

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Worksheet for C:\DocData16\combined.sgx - Design with both process and mixture factors
run temperature humidity resin crosslinker1 crosslinker2 pulloff force
degrees F % pounds
1 40 15 .9 .05 .05
2 100 15 .9 .05 .05
3 40 85 .9 .05 .05
4 100 85 .9 .05 .05
5 40 15 .7 .1 .2
6 100 15 .7 .1 .2
7 40 85 .7 .1 .2
8 100 85 .7 .1 .2
9 40 15 .75 .05 .2
10 100 15 .75 .05 .2
11 40 85 .75 .05 .2
12 100 85 .75 .05 .2
13 40 15 .85 .1 .05
14 100 15 .85 .1 .05
15 40 85 .85 .1 .05
16 100 85 .85 .1 .05
17 40 85 .8 .075 .125
18 100 15 .725 .075 .2
19 40 15 .725 .075 .2
20 40 15 .775 .1 .125
21 100 85 .8 .075 .125
22 40 85 .775 .1 .125
23 100 15 .775 .1 .125
24 100 85 .775 .1 .125
25 40 15 .825 .05 .125
26 100 15 .825 .05 .125
27 40 85 .85 .0625 .0875
28 100 85 .85 .0625 .0875
29 40 15 .825 .0875 .0875
30 40 85 .775 .1 .125
31 100 15 .725 .075 .2
32 40 85 .85 .1 .05
33 100 85 .775 .1 .125
34 100 85 .85 .1 .05

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You can also use the Design Plot to display the final design:

100
temperature
40
85
humidity
15
0.9
resin
0.7
0.1
crosslinker1
0.05
0.2
crosslinker2
0.05

Because of the tight constraint on crosslinker1, there is a fairly strong negative correlation
between the settings of resin and crosslinker2.

Design Properties

Step #6: Evaluate Design

Several of the selections presented when pressing button #6 are helpful in evaluating the selected
design:

ANOVA Table
The ANOVA table shows the breakdown of the degrees of freedom in the design:

ANOVA Table

Source D.F.
Model 24
Total Error 10
Lack-of-fit 5
Pure error 5
Total (corr.) 34

There are 24 coefficients in the model, which does not have a constant term. The 10 residual
degrees of freedom are split between lack-of-fit and pure error.

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Saving the Design File

Step #7: Save experiment

Once the experiment has been created and any additional runs entered, it must be saved on disk.
Press the button labeled Step 7 and select a name for the experiment file:

Design files are extended data files and have the extension .sgx. They include the data together
with other information that was entered on the input dialog boxes.

To reopen an experiment file, select Open Data File from the File menu. The data will be loaded
into the datasheet, and the Experimental Design Wizard window will be displayed.

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Analyzing the Results

After the design file has been created and saved, the experiments would be performed. At a later
date, once the results have been collected, the experimenter would return to STATGRAPHICS
and reopen the saved design file using the Open Data Source selection on the main File menu.
The results can then be typed into the response columns. The results for the example are
displayed below:

Worksheet for C:\DocData16\combined.sgx - Design with both process and mixture factors
run temperature humidity resin crosslinker1 crosslinker2 pulloff force
degrees F % pounds
1 40 15 .9 .05 .05 44
2 100 15 .9 .05 .05 70
3 40 85 .9 .05 .05 19
4 100 85 .9 .05 .05 33
5 40 15 .7 .1 .2 48
6 100 15 .7 .1 .2 72
7 40 85 .7 .1 .2 32
8 100 85 .7 .1 .2 59
9 40 15 .75 .05 .2 32
10 100 15 .75 .05 .2 58
11 40 85 .75 .05 .2 21
12 100 85 .75 .05 .2 38
13 40 15 .85 .1 .05 51
14 100 15 .85 .1 .05 76
15 40 85 .85 .1 .05 22
16 100 85 .85 .1 .05 49
17 40 85 .8 .075 .125 17
18 100 15 .725 .075 .2 69
19 40 15 .725 .075 .2 40
20 40 15 .775 .1 .125 37
21 100 85 .8 .075 .125 46
22 40 85 .775 .1 .125 21
23 100 15 .775 .1 .125 82
24 100 85 .775 .1 .125 43
25 40 15 .825 .05 .125 32
26 100 15 .825 .05 .125 60
27 40 85 .85 .0625 .0875 14
28 100 85 .85 .0625 .0875 38
29 40 15 .825 .0875 .0875 45
30 40 85 .775 .1 .125 18
31 100 15 .725 .075 .2 70
32 40 85 .85 .1 .05 10
33 100 85 .775 .1 .125 52
34 100 85 .85 .1 .05 42

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Step #8: Analyze data

Once the data have been entered, press the button labeled Step #8 on the Experiment Design
Wizard toolbar. This will display a dialog box listing each of the response variables:

 Response: column containing the response variable to be analyzed.

 Transformation: the desired transformation to be applied before the model is fit.

 Power and addend: the transformation parameters if a Power or Box-Cox transformation is

selected.

If more than one response has been measured, you should repeat this step once for each response.

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Analysis Summary
Designs with both quantitative and categorical factors are analyzed using the General Linear
Models procedure. The Analysis Summary of that procedure begins by displaying an analysis of
variance:

Analyze Experiment - pulloff force

File name: C:\DocData16\combined.sgx
Comment: Design with both process and mixture factors

Number of runs: 34

Analysis of Variance for pulloff force (pounds)

Source Sum of Squares Df Mean Square F-Ratio P-Value
Model 12133.7 23 527.551 24.4011 0.0000
Residual 216.2 10 21.62
Lack-of-fit 74.1997 5 14.8399 0.522533 0.7533
Pure error 142.0 5 28.4
Total (corr.) 12349.9 33
R-squared = 98.2494 percent
R-squared (adjusted for d.f.) = 94.2229 percent
Standard Error of Est. = 4.64973
Mean absolute error = 1.88645
Durbin-Watson statistic = 2.50433
Lag 1 residual autocorrelation = -0.283626

Analysis of Effects
Quantitative factors:
A=temperature (degrees F)
B=humidity (%)
Mixture components:
C=resin
D=crosslinker1
E=crosslinker2
Source Sum of Squares Df Mean Square F-Ratio P-Value
Linear mixture 640.408 2 320.204 14.8106 0.0010
AC 371.48 1 371.48 17.1823 0.0020
BC 1044.33 1 1044.33 48.3042 0.0000
ABC 20.8889 1 20.8889 0.966187 0.3488
AD 11.0427 1 11.0427 0.510763 0.4912
BD 0.00121379 1 0.00121379 0.0000561423 0.9942
ABD 4.37393 1 4.37393 0.20231 0.6625
AE 31.908 1 31.908 1.47586 0.2523
BE 8.91862 1 8.91862 0.412518 0.5351
ABE 8.56771 1 8.56771 0.396287 0.5431
CD 29.1837 1 29.1837 1.34985 0.2723
ACD 19.3464 1 19.3464 0.894839 0.3665
BCD 0.552854 1 0.552854 0.0255715 0.8761
ABCD 5.75647 1 5.75647 0.266257 0.6171
CE 78.1002 1 78.1002 3.61241 0.0865
ACE 32.1678 1 32.1678 1.48787 0.2505
BCE 3.03626 1 3.03626 0.140438 0.7157
ABCE 35.2655 1 35.2655 1.63115 0.2304
DE 37.5442 1 37.5442 1.73655 0.2170
ADE 22.3238 1 22.3238 1.03256 0.3335
BDE 0.487891 1 0.487891 0.0225667 0.8836
ABDE 2.89339 1 2.89339 0.133829 0.7221

Included in the output are:

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 Analysis of Variance: a decomposition of the sum of squares for the response variable into
components for the model and for the residuals. The F-test for the model tests the statistical
significance of the model as a whole. A small P-value (less than 0.05 if operating at the 5%
significance level) indicates that at least one factor in the model is significantly related to the
dependent variable. In the current example, the model is highly significant. The F-test for
lack-of-fit tests whether the fitted model is adequate for the data or whether a more
complicated model should be considered. A small P-value indicates that the model is NOT
adequate. In the current example, the lack-of-fit P-value is well above 0.05, indicating an
acceptable fit.

 Model statistics: summarize the fitted model. Included are:

o R-squared - represents the percentage of the variability in the response variable which
has been explained by the fitted regression model, ranging from 0% to 100%.
o Adjusted R-Squared – the R-squared statistic, adjusted for the number of coefficients
in the model. This value is often used to compare models with different numbers of
coefficients.
o Standard Error of Est. – the estimated standard deviation of the residuals (the
deviations around the model). This value is used to create prediction limits for new
observations.
o Mean Absolute Error – the average absolute value of the residuals.
o Durbin-Watson Statistic – a measure of serial correlation in the residuals. If the
residuals vary randomly, this value should be close to 2. A small P-value indicates a
non-random pattern in the residuals. For data recorded over time, a small P-value
could indicate that some trend over time has not been accounted for. In the current
example, the P-value is less than 0.05, so there is may be some serial correlation in
the residual.
o Lag 1 residual autocorrelation: a measure of the serial correlation between
consecutive residuals on a scale ranging from -1 to +1.

 Analysis of Effects: decomposition of the model sum of squares into components for each
term in the fitted statistical model. For a model with both mixture and process variables, the
table contains:

o A term labeled Linear mixture which shows the combined contribution of the first-
order terms for the mixture components. Since the first-order terms do not express
the separate contribution of each component, it does not make sense to separate those
terms.
o Higher-order terms involving combinations of mixture components, such as AB.
o Higher-order terms involving combinations of mixture components with process
variables, such as AD. Note that process variables do not occur by themselves in the
model.

Small P-values such as those for the Linear mixture terms correspond to significant
effects. However, since the other terms are correlated, it would be wrong to assume that
they all could be removed from the model.

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Simplifying the Model

In many cases, it may be desirable to remove insignificant effects from the model. Selecting
Analysis Options displays the dialog box shown below:

Double-click on an effect to move it from the Include field to the Exclude field or vice versa.
Then press OK to refit the model.

For the sample data, it is best to proceed in a stepwise fashion removing insignificant higher-
order terms and refitting the model. For example, after removing the 3 effects involving 4 factors
each, the Analysis of Effects is as follows:

Analyze Experiment - pulloff force

File name: C:\DocData16\combined.sgx
Comment: Design with both process and mixture factors

Number of runs: 34

Analysis of Variance for pulloff force (pounds)

Source Sum of Squares Df Mean Square F-Ratio P-Value
Model 12095.2 20 604.758 30.8633 0.0000
Residual 254.731 13 19.5947
Lack-of-fit 112.731 8 14.0914 0.496175 0.8195
Pure error 142.0 5 28.4
Total (corr.) 12349.9 33
R-squared = 97.9374 percent
R-squared (adjusted for d.f.) = 94.7641 percent
Standard Error of Est. = 4.42659
Mean absolute error = 2.01177
Durbin-Watson statistic = 2.28696
Lag 1 residual autocorrelation = -0.15607

Analysis of Effects
Quantitative factors:
A=temperature (degrees F)
B=humidity (%)

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Mixture components:
C=resin
D=crosslinker1
E=crosslinker2
Source Sum of Squares Df Mean Square F-Ratio P-Value
Linear mixture 640.408 2 320.204 16.3414 0.0003
AC 425.117 1 425.117 21.6955 0.0004
BC 1043.68 1 1043.68 53.2634 0.0000
ABC 30.9913 1 30.9913 1.58162 0.2307
AD 0.563659 1 0.563659 0.0287659 0.8679
BD 0.137474 1 0.137474 0.00701588 0.9345
ABD 6.56602 1 6.56602 0.335092 0.5726
AE 33.3383 1 33.3383 1.70139 0.2147
BE 10.1141 1 10.1141 0.516164 0.4852
ABE 27.1595 1 27.1595 1.38606 0.2602
CD 25.8026 1 25.8026 1.31682 0.2718
ACD 3.76434 1 3.76434 0.19211 0.6684
BCD 0.165637 1 0.165637 0.00845317 0.9281
CE 81.1942 1 81.1942 4.14368 0.0627
ACE 51.6435 1 51.6435 2.63559 0.1285
BCE 2.58522 1 2.58522 0.131935 0.7223
DE 33.6159 1 33.6159 1.71556 0.2129
ADE 5.09661 1 5.09661 0.260102 0.6186
BDE 0.122979 1 0.122979 0.00627615 0.9381

Clearly, the model can be simplified even further. Following Montgomery et al., we will remove
all of the terms shown below:

The resulting Analysis Summary is shown below:

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Analyze Experiment - pulloff force

File name: C:\DocData16\combined.sgx
Comment: Design with both process and mixture factors

Number of runs: 34

Analysis of Variance for pulloff force (pounds)

Source Sum of Squares Df Mean Square F-Ratio P-Value
Model 12009.1 11 1091.73 70.4719 0.0000
Residual 340.819 22 15.4918
Lack-of-fit 198.819 17 11.6952 0.411803 0.9221
Pure error 142.0 5 28.4
Total (corr.) 12349.9 33
R-squared = 97.2403 percent
R-squared (adjusted for d.f.) = 95.8605 percent
Standard Error of Est. = 3.93596
Mean absolute error = 2.62078
Durbin-Watson statistic = 2.38911
Lag 1 residual autocorrelation = -0.233281

Analysis of Effects
Quantitative factors:
A=temperature (degrees F)
B=humidity (%)
Mixture components:
C=resin
D=crosslinker1
E=crosslinker2
Source Sum of Squares Df Mean Square F-Ratio P-Value
Linear mixture 640.408 2 320.204 20.6693 0.0000
AC 460.697 1 460.697 29.7382 0.0000
BC 1768.65 1 1768.65 114.167 0.0000
AD 425.881 1 425.881 27.4908 0.0000
BD 210.526 1 210.526 13.5895 0.0013
AE 119.781 1 119.781 7.73189 0.0109
BE 91.2646 1 91.2646 5.89117 0.0239
ABE 48.3234 1 48.3234 3.1193 0.0912
CE 151.076 1 151.076 9.75202 0.0050
ACE 61.325 1 61.325 3.95856 0.0592

Most of the P-values are less than 0.05, indicating that the corresponding terms are statistically
significant at the 5% level.

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Pareto Chart
The analysis window summarizes the contribution of each effect to the overall variability in the
response using a Pareto chart:

Pareto Chart for pulloff force

BC
Sig. at 5%
Linear mixture Not sig.
AC
AD
BD
CE
AE
BE
ACE
ABE

0 3 6 9 12 15
Contribution to variation (%)

The length of each bar equals the contribution of an effect to the overall variation in the
response, where an effect’s contribution is calculated by dividing its sum of squares by the total
corrected sum of squares from the ANOVA table. The color of each bar indicates whether an
effect is statistically significant at the indicated significance level.

Of particular note is the large contribution of AE, corresponding to an interaction between resin
and humidity.

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Means Table
The analysis window also displays the estimated mean response at different locations within the
design space:

Means table for pulloff force with 95% confidence intervals

Estimated Standard Lower Upper

Factor Level Mean Error Limit Limit
Grand mean 49.5242 1.57608 46.2557 52.7928
temperature
40.0 31.8129 2.14992 27.3542 36.2715
100.0 67.2356 2.25984 62.549 71.9222
humidity
15.0 62.8859 2.31411 58.0867 67.6851
85.0 36.1626 1.86866 32.2872 40.038
resin
0.7 59.0529 2.37236 54.1329 63.9729
0.9 40.6588 1.71299 37.1063 44.2113
crosslinker1
0.05 35.7651 1.53938 32.5726 38.9576
0.25 71.9466 5.7702 59.9799 83.9132
crosslinker2
0.05 56.3027 2.51013 51.097 61.5084
0.25 46.1592 2.67835 40.6047 51.7138
temperature by humidity
40.1,15.0 44.3076 2.76918 38.5647 50.0506
40.1,85.0 19.3181 2.43006 14.2784 24.3577
40.1,15.0 81.4642 2.93549 75.3763 87.552
40.1,85.0 53.0071 2.44726 47.9318 58.0824
temperature by resin
40.1,0.8 29.6137 1.67834 26.133 33.0944
40.1,0.8 62.4541 1.80384 58.7131 66.195
temperature by crosslinker1
40.1,0.15 35.4062 3.43655 28.2793 42.5332
40.1,0.15 76.1274 3.56141 68.7415 83.5133
temperature by crosslinker2
40.1,0.15 31.4595 1.56036 28.2235 34.6955
40.1,0.15 63.3585 1.60324 60.0335 66.6834
humidity by resin
15.1,0.8 59.9283 1.79889 56.1976 63.659
15.1,0.8 32.1395 1.37923 29.2792 34.9999
humidity by crosslinker1
15.1,0.15 70.8327 3.69884 63.1617 78.5036
15.1,0.15 40.701 3.15197 34.1641 47.2378
humidity by crosslinker2
15.1,0.15 58.5337 1.63238 55.1484 61.9191
15.1,0.15 36.2843 1.42321 33.3327 39.2358
resin by crosslinker1
0.8,0.15 56.3027 2.51013 51.097 61.5084
resin by crosslinker2
0.8,0.15 35.7651 1.53938 32.5726 38.9576
crosslinker1 by crosslinker2
0.15,0.15 59.0529 2.37236 54.1329 63.9729

The line labeled Grand mean shows the estimated mean at the center of the design space, where:

1. Each quantitative factor is set halfway between its lower level Li and its upper level Ui:

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Li  U i
Xi  (1)
2

2. The q mixture variables are set at the centroid of the mixture space:

q
T   Li
X i  Li  i 1
(2)
q

where T is the sum of the mixture variables.

Estimated means are also shown for different combinations of pairs of factors. The table
indicates the fixed levels of the indicated factors, with other variables set at their central levels
(except for mixture variables, which are adjusted proportionately if necessary to preserve the
mixture total).

In addition to the means, the table also shows the estimated standard error for each mean and
interval estimates. The Pane Options dialog box selects the type of limits displayed:

The choices are:

1. Confidence limits: a separate confidence interval is displayed for each mean, calculated
using Student’s t distribution according to


Yˆ  t / 2,n  p s Yˆ (3)


where Ŷ is the predicted mean response, s Yˆ is the estimated standard error, n is the
number of observed runs, and p is the number of coefficients in the fitted model.

2. Bonferroni limits (by effect): limits are calculated for each variable and combination of
two variables, calculated using Student’s t distribution according to


Yˆ  t / 2 g ,n  p s Yˆ (4)

where g is the number of levels for the variable or combination of variables. Bonferroni
limits provide at least the stated confidence for all means in the set.
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3. Working-Hotelling limits: limits are calculated for all means simultaneously using
Snedecor’s F distribution according to

Yˆ  
pF1 , p ,n  p s Yˆ (5)

Working-Hotelling limits provide at least the stated confidence for all of the means.

Main Effects Plot

The means displayed in the Means Table can be displayed graphically using the Main Effects
Plot:

Main Effects Plot for pulloff force

81

71
pulloff force

61

51

41

31
temperature resin crosslinker2
humidity crosslinker1

Each factor is varied between its low level and its high level, holding other factors constant in the
same manner as in the Means Table. If the plot is too crowded, Pane Options may be used to
select a subset of the factors:

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Interaction Plot
The means displayed in the Means Table for combinations of factors can be displayed
graphically using the Interaction Plot:

Interaction Plot for pulloff force

75
humidity=15.0
65
pulloff force

55 humidity=15.0

45 humidity=85.0

35

25 humidity=85.0
0.7 0.9
resin

In the plot above, the mean pulloff force is displayed as a function of resin for 2 different levels
of humidity. It will be noticed that humdity has a larger effect when resin is at its high level.

As with the Main Effects Plot, the factors displayed may be selected using Pane Options:

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If Reverse Factors is checked, the second factor rather than the first will be plotted along the
horizontal axis.

Trace Plot
An interesting way of visualizing the effects of each factor in the fitted regression models is
through a Trace Plot. Starting at a selected reference point within the experiment region, each
factor is moved above and below that point, holding each of the other factors constant. The
estimated response is then displayed, as in the plot below:

Trace Plot for pulloff force

71
Factor
temperature
61 humidity
pulloff force

resin
crosslinker1
51 crosslinker2

41

31
-1 -0.6 -0.2 0.2 0.6 1
Factor range

As each continuous factor is changed, all of the other factors are held constant. As each mixture
component is changed, the other mixture components are adjusted proportionately to maintain
the required mixture total. In the trace plot, the horizontal axis is defined for continuous factors
as

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 STATGRAPHICS – Rev. 9/19/2009

2 X i  Ri 
x (6)
U i  Li

where Xi is the value of factor i, Ri is the reference point for factor i, Ui is the upper level for
factor i defined when the experiment was created, and Li is the low level. For mixture
components, the horizontal axis is defined as

X i  Ri
x  Ri  q
(7)
T   Li
i 1

The default reference point corresponds to the center of the design space for the continuous
factors and the simplex centroid for the mixture components.

By comparing the changes in yield over the range of each factor, the most important factors can
be determined. If a line is relatively flat for a particular factor, the response is insensitive to
changes in that factor in the vicinity of the reference point.

Pane Options can be used to change the reference point:

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 STATGRAPHICS – Rev. 9/19/2009
Standardized Regression Coefficients
The statistical output displayed above is based on fitting a multiple linear regression model. Such
models take the general form

Yi   1 X 1   2 X 2  ...   p 1 X p 1 (8)

where the ’s are coefficients that need to be estimated from the data and the X’s are calculated
from the levels of the experimental factors. The table of Standardized Regression Coefficients
displays the estimated ’s when the X’s are defined as follows:

1. For continuous factors, the standardized value of the i-th factor is given by

X i  Li  U i  / 2
X  (9)
U i  Li  / 2
With this scaling, X = -1 at the low level, 0 at the center level, and +1 at the high level.

2. For categorical factors at k levels, k - 1 X’s are created where

Xj = -1 if the factor is at level 1

Xj = +1 if the factor is at level j+1 (10)

Xj = 0 otherwise

With this scaling, the ’s constrast each additional level of the factor with the first level.

3. For mixture factors, the standardized value of the i-th factor is the pseudo component

X i  Li
X  q
(11)
T   Lj
j 1

With this scaling, X = 0 at the low level and 1 at the highest possible level.

The table for the current example is shown below:

Standardized Regression Coefficients

Effect Estimate Stnd. Error V.I.F.
C:resin 40.6588 1.71299 2.14272
AC 9.31527 1.7082 2.13076
BC -15.4926 1.44995 1.53519
D:crosslinker1 71.9466 5.7702 2.40948
AD 29.9238 5.7072 2.35715
BD -20.1785 5.47376 2.16827
E:crosslinker2 46.1592 2.67835 3.56518
AE 7.43232 2.67289 3.55066
BE -4.41395 1.81856 1.64361
ABE -2.60066 1.4725 1.07759
CE -30.5756 9.79103 3.21226

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ACE 19.3882 9.74472 3.18194

It provides the estimated coefficients, standard errors, and variance inflation factors. The
StatAdvisor shows the fitted model as:

pulloff force = 40.6588*resin + 9.31527*temperature*resin - 15.4926*humidity*resin + 71.9466*crosslinker1 +

29.9238*temperature*crosslinker1 - 20.1785*humidity*crosslinker1 + 46.1592*crosslinker2 +
7.43232*temperature*crosslinker2 - 4.41395*humidity*crosslinker2 - 2.60066*temperature*humidity*crosslinker2 -
30.5756*resin*crosslinker2 + 19.3882*temperature*resin*crosslinker2

The Predictions table described later used this model to predict values of yield at different
combinations of the experimental factors.

Unstandardized Regression Coefficients

The regression model can also be written with the continuous factors and mixture components
expressed in their original units. The estimated coefficients for this unstandardized model as
shown below for the sample data:

Unstandardized Regression Coefficients

Coefficient Estimate
C:resin 73.6019
AC -0.0904326
BC -0.488553
D:crosslinker1 -75.2424
AD 4.22385
BD -1.1699
E:crosslinker2 1247.66
AE -10.5546
BE 1.75779
ABE -0.00940951
CE -1900.47
ACE 16.298

The StatAdvisor shows the fitted model as:

pulloff force = 73.6019*resin - 0.0904326*temperature*resin - 0.488553*humidity*resin - 75.2424*crosslinker1 +

4.22385*temperature*crosslinker1 - 1.1699*humidity*crosslinker1 + 1247.66*crosslinker2 - 10.5546*temperature*crosslinker2
+ 1.75779*humidity*crosslinker2 - 0.00940951*temperature*humidity*crosslinker2 - 1900.47*resin*crosslinker2 +
16.298*temperature*resin*crosslinker2

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Surface and Contour Plots

The fitted statistical models can also be displayed using surface and contour plots. A typical
surface plot shows the predicted response as a function of either two continuous factors or three
mixture components, with all other factors held constant:

Estimated Response Surface

resin=0.8,crosslinker1=0.075,crosslinker2=0.125
pulloff force
35.0
38.0
41.0
44.0
80 47.0
pulloff force

60 50.0
40 53.0
20 100 56.0
0 80 59.0
40 60 62.0
50 65.0
60 40
70 20 humidity 68.0
80
90 0
temperature 100

The above plot shows that high elongation is achieved at high temperature and low humidity, at
least for the indicated values of the mixture components.

The Pane Options dialog box is used to select the type of plot to be displayed:

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 Type: type of response plot to create. The standard error may be plotted as a surface, a two-
dimensional contour plot, a three-dimensional contour plot, or a three-dimensional mesh plot.

 Contours – options for a contour plot.

o From: location at which the first contour line is drawn, or the start of the first region.

o To: location at which the last contour line is drawn, or the end of the last region.

o By: spacing between contour lines or regions.

o Lines: if selected, a sequence of contour lines is drawn at selected levels of the predicted
response, as on a topographical map.

o Painted Regions: if selected, a set of regions is drawn covering various ranges of the
predicted response.

o Continuous: draws contours using a continuous range of colors.

o Continuous with Grid: draws contours using a continuous range of colors and adds a
grid.

 Resolution: defines the resolution m of an m-by-m grid of predicted values which is used to
draw the surface and contour lines. Increasing the resolution may improve the smoothness
and definition of the plots, at the expense of computer time and memory.

 Surface – options for a surface plot.

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o Horizontal Divisions: the number of divisions along the first experimental axis. This
determines how many vertical lines will be drawn on the surface plot.

o Vertical Divisions: the number of divisions along the second experimental axis. This
determines how many horizontal lines will be drawn on the surface plot.

o Contours Below: requests that a contour plot, of type specified below, be drawn in the
bottom face of the 3-D plot.

o Wire Frame: requests that the surface be drawn using cross-hatched lines as shown in
the figure above. This is the most effective choice for black-and-white presentation.

o Solid: requests that the surface be drawn using a solid color.

o Contoured: requests that the surface be drawn showing contour levels of the response.

 Factors button: displays a dialog box to select the factors to be plotted on each axis and the
levels at which the other factors will be held:

The current example plots the predicted response versus temperature and humidity, with resin =
0.8, crosslinker1 = 0.75, and crosslinker2 = 0.125.

The same information shown as a contour plot with continuous contours is displayed below:

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Estimated Response Surface

resin=0.8,crosslinker1=0.075,crosslinker2=0.125

100 pulloff force

35.0
38.0
80
41.0
44.0
60
humidity

47.0
50.0
40 53.0
56.0
20 59.0
62.0
65.0
0
68.0
40 50 60 70 80 90 100
temperature

If 3 mixture components are selected rather than 2 continuous factors, the surface will be plotted
over a simplex:

Estimated Response Surface

pulloff force
temperature=70.0,humidity=50.0 35.0
resin=0.9 38.0
41.0
44.0
47.0
50.0
53.0
crosslinker2=0.05 crosslinker1=0.05
56.0
59.0
62.0
65.0
68.0

crosslinker1=0.25 resin=0.7 crosslinker2=0.25

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Predictions
The Predictions pane may be used to generate predictions from the fitted model:

Estimation Results for pulloff force

Observed Fitted Studentized Lower 95.0% CL Upper 95.0% CL
Row Value Value Residual Residual for Mean for Mean
1 44.0 46.8361 -2.83609 -1.05803 40.873 52.7991
2 70.0 65.4666 4.53336 1.76751 59.4997 71.4336
3 19.0 15.851 3.14901 1.13102 10.1181 21.5839
4 33.0 34.4815 -1.48154 -0.519587 28.7525 40.2106
5 48.0 45.9554 2.04455 0.732103 40.1423 51.7686
6 72.0 75.9668 -3.96682 -1.35432 70.6441 81.2896
7 32.0 33.1463 -1.14628 -0.468798 26.6789 39.6137
8 59.0 55.3557 3.64432 1.58541 48.8487 61.8626
9 32.0 32.7459 -0.745947 -0.242847 27.4748 38.0171
10 58.0 59.7236 -1.72363 -0.53619 54.8631 64.5841
11 21.0 22.2797 -1.27973 -0.475306 16.2342 28.3252
12 38.0 41.4554 -3.45545 -1.32854 35.4121 47.4988
13 51.0 50.6774 0.32263 0.0989721 45.8833 55.4714
14 76.0 79.6122 -3.61219 -1.17555 74.5807 84.6436
15 22.0 17.3493 4.65069 1.41094 13.1307 21.5679
16 49.0 46.2841 2.71587 0.798047 42.0841 50.4842
17 17.0 15.1304 1.86959 0.522064 11.4842 18.7766
18 69.0 67.8452 1.15477 0.328276 63.8997 71.7908
19 40.0 39.3507 0.649302 0.193487 34.8436 43.8578
20 37.0 41.2902 -4.29024 -1.32161 36.8442 45.7363
21 46.0 42.821 3.17903 0.901572 39.1319 46.51
22 21.0 18.2216 2.77837 0.797108 14.3175 22.1258
23 82.0 76.2163 5.78373 1.91231 71.4691 80.9634
24 43.0 49.2467 -6.24667 -1.92022 45.3028 53.1905
25 32.0 32.7649 -0.764852 -0.239474 27.8014 37.7283
26 60.0 61.0219 -1.0219 -0.323812 55.9685 66.0754
27 14.0 13.1486 0.851358 0.23703 9.47116 16.8261
28 38.0 38.1268 -0.12684 -0.0353229 34.427 41.8267
29 45.0 42.6814 2.31857 0.648667 39.0583 46.3045
30 18.0 18.2216 -0.221627 -0.0626494 14.3175 22.1258
31 70.0 67.8452 2.15477 0.616491 63.8997 71.7908
32 10.0 17.3493 -7.34931 -2.407 13.1307 21.5679
33 52.0 49.2467 2.75333 0.792185 45.3028 53.1905
34 42.0 46.2841 -4.28413 -1.28828 42.0841 50.4842

The table may include all rows in the datasheet, or only rows for which the value of the response
variable Y has not been entered. The latter feature allows the analyst to make predictions at
combinations of X that were not included in the experiment. For example, the above table shows
the result of adding an 18th row with temperature = 175, concentration = 35, and catalyst = A.
The predicted value of yield is 69.62. The 95% confidence interval for the mean value of yield at
that same combination of the factors ranges from 67.5 to 71.7.

One other noticeable entry in the above table is the Studentized residual for row #7. The
Studentized residual measures the difference between the observed response and the predicted
response, in units of its standard error, when the observation in question is not used to fit the
model. The Studentized residual for observation #7 equals 2.8. Values in excess of 3.0 are
unusual and would typically require further scrutiny.

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Pane Options

 Include: items to include in the table:

1. Observed Y - the observed response values Yi .

2. Fitted Y - the predicted values Yi calculated from the fitted model.

3. Residuals - the residuals ei .

4. Studentized Residuals - a type of standardized residual, where each residual is divided by

an estimate of its standard error. STATGRAPHICS computes Studentized deleted
residuals, in which each observation is removed one at a time and the model refit without
that data value. The deleted residual then equals the observed response minus the value
predicted from a model fit without that observation, i.e.,

d i  Yi  Y( i ) (12)

The Studentized residual is calculated from

di
ei*  (13)
s( d i )
where


s 2 (d i )  MSE (i ) 1  X i ( X (i ) X ( i ) ) 1 X i  (14)

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The deleted residuals should follow a t distribution with n - p - 1 degrees of freedom,
where p is the number of estimated coefficients in the fitted model.

1. Standard Errors for Forecasts - the standard error for new observations at a selected
combination of the experimental factors Xh, given by


MSE 1  X h ( X  X ) 1 X h  (15)

2. Confidence Limits for Individual Forecasts - confidence limits for new observations at a
selected combination of the experimental factors Xh, given by


Yh  t n  p MSE 1  X h ( X  X ) 1 X h  (16)

3. Confidence Limits for Forecast Means - confidence limits for the mean response at a
selected combination of the experimental factors Xh, given by


Yh  t n  p MSE X h ( X  X ) 1 X h  (17)

 Predict - whether forecasts are displayed for all of the runs in the experiment data file, or
only for runs that have a missing value in the response column.

 Confidence level - the confidence levels for the intervals.

Unusual Residuals
The Unusual Residuals table displays all rows with Studentized residuals less than -2 or greater
than +2:

Unusual Residuals for pulloff force

Predicted Studentized
Row Y Y Residual Residual
32 10.0 17.3493 -7.34931 -2.41

While row #32 appears on the list, it is less than 3 in absolute value so may not be that serious.

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Diagnostic Plots
Several plots are also provided under Diagnostic Plots to examine the residuals from the fitted
model. The Pane Options dialog box displays the various choices, which include the following:

Observed versus Predicted

This plot displays the observed response Yi versus the fitted values Yi , together with a diagonal
line:

Plot of pulloff force

100

80
observed

60

40

20

0
0 20 40 60 80 100
predicted

If the model fits well, the values should lie close to the line, as in the example above. Curvature
around the line may suggest the need to transform the values of Yi using a logarithm or similar
function.

Residual versus Predicted

This plot displays the residuals ei versus the fitted values Yi , with a horizontal line at zero:

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Residual Plot for pulloff force

4
residual

-4

-8
0 20 40 60 80 100
predicted

The residuals should vary randomly around the line. Changes in the magnitude of the residuals
from left to right may signal that the variance of the experimental error varies with the mean
level of the response. Such heteroscedasticity may frequently be eliminated by a variance-
stabilizing transformation such as a logarithm or a square root.

Residuals versus Run Order

This plot displays the residuals ei versus run number i, with a horizontal line at zero:

Residual Plot for pulloff force

4
residual

-4

-8
0 10 20 30 40
run number

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Any non-random pattern may indicate a time trend or other effect. In such cases, addition of a
factor to account for the change may improve the fit of the model. The above plot does suggest
an increase in variability during the second half of the experiment, which would be worthy of
further investigation.

Residuals versus Factor

This plot displays the residuals ei versus the observed values of a selected experimental factor:

Residual Plot for pulloff force

4
residual

-4

-8
0.69 0.73 0.77 0.81 0.85 0.89 0.93
resin

Any curvature around the line may suggest the need for a model with quadratic effects.

Normal Probability Plot of Residuals

This plot displays the residuals ei versus quantiles of a normal distribution, with an optional
fitted line as reference:

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Normal Probability Plot for Residuals

99.9
99
95
percentage

80
50
20
5
1
0.1
-8 -5 -2 1 4 7
residuals

If the experimental error follows a normal distribution, the points should lie along a straight line.

Pane Options

 Plot: the type of plot to be created.

 Plot versus: selects the experimental factor to be shown in the plot, for those plots where a
factor is needed.

 Direction: defines the orientation of the normal probability plot.

 Fitted Line: specifies whether a line should be fit to the data on the normal probability plot.

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Optimization
Each analysis window gives the ability to optimize an individual response variable. The
Optimization text pane will automatically calculate and display the optimal settings of the
experimental factors:

Optimize Response
Goal: maximize pulloff force

Optimum value = 79.6122

Factor Low High Optimum

temperature 40.0 100.0 100.0
humidity 15.0 85.0 15.0
resin 0.7 0.9 0.85
crosslinker1 0.05 0.1 0.1
crosslinker2 0.05 0.2 0.05

The table shows:

 Goal - the type of optimization desired, defined when the experiment was created.

 Optimum value - the predicted response at the optimum setting.

 Low - the low level of the region over which the optimization is performed.

 High - the high level of the region over which the optimization is performed.

 Optimum - the optimum setting of the experimental factors.

In the above example, pull force has been maximized with respect to the 5 experimental factors.

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Pane Options

 Factor – If the box for a factor is checked, it will be optimized over the indicated range if the
factor is continuous or over all levels if the factor is categorical. Otherwise, it will be
constrained to match the value specified in the Hold field.

 Low – lowest level considered for each factor.

 High – highest level considered for each factor.

 Hold – if not being optimized, the level at which each factor is set.

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Optimization

Step #9: Optimize responses

Once a statistical model has been developed for each response, the analyst may now determine
what combination of factors will yield the best results for all responses simultaneously.
Returning to the main DOE Wizard window and Pressing the button labeled Step #9 begins
searching the experimental region for the combination of the experimental factors that maximize
the desirability of the result. To avoid finding a local optimum, a search is performed beginning
at each design point.

When the optimization is complete, a message similar to that shown below will be displayed:

The dialog box indicates the “Desirability” of the final result, based on a metric designed to
balance competing requirements of multiple responses (see the document titled DOE Wizard for
full details). The value displayed in this case indicates that the predicted pull force at the
optimum factor settings is 90.03% of the distance between 40 and 80, which was the desired
range specified when the design was created.

If you press OK, additional information will be added to the main DOE Wizard window:

Step 9: Optimize the responses

Response Values at Optimum
Response Prediction Lower 95.0% Limit Upper 95.0% Limit Desirability
pulloff force 78.5762 73.0598 84.0926 0.964405

Factor Settings at Optimum

Factor Setting
temperature 100.0
humidity 15.0
resin 0.85
crosslinker1 0.1
crosslinker2 0.05

The table shows the estimated response at the optimal settings of the experimental factors. For
the sample data, it is estimated that the mean pull force will equal 78.58 when the factors are set
at resin = 0.85, crosslinker1 = 0.1, crosslinker2 = 0.05, temperature = 100, and humidity = 15.
The 95% confidence interval for the mean pull force ranges between 73.06 and 84.09.

If you push the Tables and Graphs button on the analysis toolbar, you can display the estimated
desirability throughout the experimental region. An interesting type of display is the contoured
surface plot shown below (use Pane Options and the Factors button to select the factors to plot
on each axis):
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Desirability Plot
resin=0.85,crosslinker1=0.1,crosslinker2=0.05

Desirability
0.0
0.1
0.2
0.3
0.4
1 100 0.5
0.8
Desirability

0.6 0.6
80
0.4 0.7
0.2 60 0.8
0
40 humidity 0.9
40
50 60 20 1.0
70
80 90 0
100
temperature

It is clear that the best place to operate is in the right front corner of the experimental region.

Likewise, plotting desirability with respect to the 3 mixture components yields the following
contour plot:

Desirability Plot
temperature=100.0,humidity=15.0 Desirability
resin=0.9 0.0
0.1
0.2
0.3
0.4
0.5
crosslinker2=0.05 crosslinker1=0.05 0.6
0.7
0.8
0.9
1.0

crosslinker1=0.25 resin=0.7 crosslinker2=0.25

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Step 10: Save results

The button labeled Step 10 allows you to save the results in a StatFolio:

Actually, the StatFolio can be saved at any point and reloaded at a later date.

IMPORTANT: When using the Experimental Design Wizard, two files are created:

1. An experiment file with the extension .sgx which stores information about the
experimental data.

2. A StatFolio with the extension .sgp that stores the results of the analysis.

If you move the experiment to another computer, be sure to transfer both files.

Step 11: Augment Design

Since the conclusions from the design are fairly clear, there is no need to augment the design.

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Extrapolation

Step 12: Extrapolate

The maximum predicted pull force within the design space is 79.61%. To use the statistical
model to predict settings of the factors outside the experimental region that might produce even
better results, press the button labeled Step 12. The following dialog box will be displayed:

 Start at: the position from which to start the search.

 Change: the factors you wish to consider changing. Only quantitative factors may be
checked.

 Display steps of: The program will begin at the starting location and follow the path of
steepest ascent in an attempt to increase the desirability of the predicted response. Specify the
increment of increased desirability at which the results should be displayed.

 2009 by StatPoint Technologies, Inc. DOE Wizard – Process and Mixture Factors - 45
 STATGRAPHICS – Rev. 9/19/2009
 Low and high: The limits within which the factors will be changed.

In this case, we have asked to program to search from the derived optimal conditions and display
improvement of 0.1% in desirability, changing only temperature and humidity.

The results of the search are shown in the following table, which will be added to the main DOE
Wizard window:

Step 12: Extrapolate model

Extrapolated Response Values
Step Desirability pulloff force
0 0.990305 79.6122
1 0.997611 79.9044
2 1.0 80.2157
3 1.0 80.2157

Factor Settings for Extrapolation

Step resin crosslinker1 crosslinker2 temperature humidity
0 0.85 0.1 0.05 100.0 15.0
1 0.85 0.1 0.05 100.26 14.65
2 0.85 0.1 0.05 100.56 14.3
3 0.85 0.1 0.05 100.56 14.3

The program suggests that the best course of action would be to increase temperature while
decreasing humidity. While the model predicts that the desirability metric will reach 100% at a
temperature of 100.26 degrees and a humidity of 14.3, confirmatory runs would be necessary to
determine whether the model gives reasonable predictions that far outside the experimental
region.

 2009 by StatPoint Technologies, Inc. DOE Wizard – Process and Mixture Factors - 46