Section 7 Mixture Design Tutorials

Transcription

1 Rev. 11/16/00 Section 7 Mixture Design Tutorials Mixture Design and Analysis This tutorial shows how you can use Design-Expert software for mixture experiments. A case study provides a real-life feel to the exercise. Due to the specific nature of the case study, a number of features that could be helpful to you on mixtures will not be exercised in this tutorial. Many of these features are used in the Factorial and Response Surface tutorials, so you will benefit by doing them also. We presume that you can handle the statistical aspects of mixture designs. If you need further background, look in the Help system of Design-Expert. To learn all the tricks, attend our Mixture Design For Optimal Formulation workshop. Call Stat-Ease for a schedule or visit our web site ( This tutorial provides only the essential program functions. For more details, check out the Help system, which you can access at any time by pressing F1. Its hypertext search capability makes it easy for you to track down the information you need. The formulators measured two responses in a detergent formulation: Y 1 - viscosity Y 2 - turbidity. while varying three components as shown: 3% A (water) 8% 2% B (alcohol) 4% 2% C (urea) 4% They required that these three active components always equal nine weight-percent of the total formulation, that is, A + B + C = 9%. The other components (held constant) then must equal 91 weight-percent of the detergent. The experimenters chose a standard mixture design called a simplex-lattice. They augmented this design with axial check blends and the overall centroid. The vertices and overall centroid were replicated, which increased the size of the experiment to a total of 14 blends. Design-Expert 6 User s Guide Mixture Design Tutorials 7-1

2 Design the Experiment This case study leads you through all the steps of design and analysis for mixtures. Follow up with the next tutorial to see how you can simultaneously optimize the two responses. Start the program by finding and double clicking on the Design-Expert icon. The menu bar will display at the top of the program window. Take the quickest route to initiating a new design by clicking on the blank-sheet icon on the left of the toolbar. The other route is via File, New Design (or associated Alt keys). Main Menu and Tool Bar Click on the Mixture tab. Design-Expert offers extensive choices for your design. Detailed information on these can be found in the Help system. Simplex Lattice Design In this case, the formulator wants to use the default mixture design: the simplex-lattice, but for 3 components, not 2. Click on the Mix Components pull down list and select 7-2 Mixture Design Tutorials Design-Expert 6 User s Guide

3 Rev. 11/16/00 3. Enter the component and constraint information as shown below in the Name, Low and High fields, pressing the Tab key after each entry. Then enter 9 in the Total field and % in the Units field. Upon completing your data entry, your screen should look like the following screen. Mixture Components - Entered Values Continue with the process by pressing the Continue button at the lower right of the screen. Immediately a warning appears. Warning of Adjustment Press OK. Notice that, although you entered the high limit for water as 8%, Design- Expert adjusts it to 5%. Mixture Components - Adjusted Values It must do this because of the constraints: 1. All components must add to 9%. 2. Alcohol must be at least 2%. 3. Urea must be at least 2%. That leaves 5% maximum of water (9 2 2 = 5) in any one experimental run. An alternative way to adjust constraints would be to keep the upper limit of water at 8% and then reduce the lower limits of the other two components to 0.5% each. Then the total Design-Expert 6 User s Guide Mixture Design Tutorials 7-3

4 would meet the 9% goal. Design-Expert adjusts the upper constraint, but you can override this by making your own adjustments. If you ask for unattainable lower limits of your mixture components, the program will adjust the lower limit. In any case, Design-Expert will help you build rational constraints. Click on Continue to further specify the design. Now you must choose the order of the model that you expect to be appropriate for the system being studied. By default, Design-Expert uses Scheffe polynomials as mixture models. In this case, you can assume that a quadratic polynomial, which includes second order terms for curvature, will adequately model the responses. Leave the default at Quadratic. Simplex-Lattice Design Form Via the following fields, Design-Expert provides options to strengthen the core simplex design: Augment design, checked ( ) by default, adds the overall centroid and axial check blends to the design points. Number of runs to replicate, defaulted to 4, causes the specified number of highest leverage experiments to be duplicated. Accept these defaults by pressing Continue to the next step in the design process. For Responses, select 2. Then enter the response Names and Units as shown below. Response Names and Units 7-4 Mixture Design Tutorials Design-Expert 6 User s Guide

5 Rev. 11/16/00 You can step Back through the design forms and change what you want anywhere along the way. When you press Continue on this page, Design-Expert will complete the design setup for you. Your standard ( Std ) order will most likely be different from the one we show below. The software re-randomizes the run order each time a design is created. Always save your design to disk to preserve a particular run order. Completed Mixture Design - Run Order (Your run order may differ) Save the Data to a File Now that you ve invested some time into your design, it would be prudent to save your work. Click on File menu item and select Save A s. Save As Selection The program displays a standard file dialog box. Use it to specify the name and destination of your data file. Enter a file name in the field with the default extension of dx6. (We suggest tut-mix). Then click on Save. Design-Expert 6 User s Guide Mixture Design Tutorials 7-5

6 The three columns on the left of the design layout identify the experimental runs in different ways by standard order, by run order and by block number. Do a right click with the mouse at the top of the column labeled Std. Then select Sort by Standard Order. Sorting by Standard Order Components in Coded Values It s convenient to put the design in a coded format so calculations remain unaffected by units of measure. You may be familiar with the coding used for factorial design, where -1 designates the lowest level and +1 the highest level of each factor. Mixtures get treated a bit differently, with a coding of 0 for lowest concentration and 1 for the highest concentration. These coded values are called Pseudocomponents. They are calculated from an intermediate stage called real values. Check these out by selecting Display Options, Mixture Components, Real. Components in Real Values Real components are defined as: ( ) Real = Actual / Total of Actuals R = A / A i i i For the first experiment in standard order: 7-6 Mixture Design Tutorials Design-Expert 6 User s Guide

7 Rev. 11/16/00 R 1 = 5/9 = R 2 = 2/9 = R 3 = 2/9 = Notice that the real values always sum to 1.0. To look at the design in pseudo values, select Display Options, Mixture Components, Pseudo. Components in Pseudo Values Pseudocomponents are defined as: Pseudo = (Real L i ) / (1 L) where L i = lower constraint in real value L =sum of lower constraints in real value P i = (R i L i ) / (1 L) For the first experiment: P 1 = ( )/( ) = 1 P 2 = ( )/( ) = 0 P 3 = ( )/( ) = 0 The value of one for P 1 indicates that blend number one in standard order will be at the richest possible level for water: 5%. Edit the Design Now you will edit the design. In design selection you chose a simplex-lattice design to fit a quadratic model. The design was augmented with the overall centroid and the axial check blends. You asked that four experiments be replicated. Design-Expert chose the four with the highest leverages: the three vertices and one edge. Assume that the formulator wants to duplicate the overall centroid rather than the one edge. You can do this in the design layout. First, right click on the top of the Std column (the header) and Display Design ID, then right click again and choose Sort by Design ID. The ID identifies unique combinations and thus reveals duplicates explicitly. Now right click on the Block Design-Expert 6 User s Guide Mixture Design Tutorials 7-7

8 column header and choose Display Point Type. This identifies the points and makes it easier to find the ones you need. Look for the edge point that has been duplicated. It will be a binary blend of two of the components, each with a pseudo value of 0.5, and the remaining component with a pseudo value of 0. Click on the button just to the left of the duplicated row to select it. Then eliminate it by right clicking on the row button and selecting Delete Row(s). Deleting a Duplicate Row (your duplicate may be a different edge point than shown) Click Yes when prompted. Now locate the overall centroid, which is the row with equal amounts of each factor: in pseudocomponent coding. Click on the button just to the left of the row. Then right click on the row button and select Duplicate. Duplicating an Experiment You can also add points by right clicking on the row button and selecting Insert Row. You can edit component and response names by right clicking on the response column heading and selecting Edit Info. Run or block numbers can also be changed. Finally, since the design runs are changed, you should assign a new random run order. Right click on the Run column heading and select Randomize. Then click on OK for the default of All blocks. Randomize Run Order Dialog Box 7-8 Mixture Design Tutorials Design-Expert 6 User s Guide

9 Rev. 11/16/00 Analyze the Results Having changed your experiment design, you should now save the changes. First put it back into the form you will need to actually run the experiment: Select Display Options, Mixture Components, Actual and View, Run Order. Then select File, Save to store the changes in your current file. Assume that the experiments are now complete. You now need to enter the responses into the Design-Expert software. For tutorial purposes, we see no benefit to making you type all the numbers. Therefore, to save time, read the response data in from a file that we ve put on your program disk. Select File, Open Design. Click on the file called Mix.dx6. Then press OK. You now should see response data (no need to type it in!). Before moving on to the analysis, do a right mouse click on the top of the Block column and select Display Point Type. Showing Point Type on Filled-in Run Sheet (from file that comes with program) Again do a right click on what is now labeled as the Type column. This time select Sort by Point Type. You now get a very useful layout of the design. Mixture Design Sorted by Point Type Design-Expert 6 User s Guide Mixture Design Tutorials 7-9

10 The next step in the process is to analyze the data. Begin the analysis phase by clicking on the node for Viscosity (to left of window). First Step in the Analysis: Transformation Dialog Box You now will work across the buttons at the top of the window. First, consider doing a transformation on the response. In some cases this will improve the statistical properties of the analysis. For example, when responses vary over several orders of magnitude, the log scale usually works best. For this data, leave the selection at its default, None, because no transformation will be needed. Click on the Fit Summary button next. At this point Design-Expert fits linear, quadratic, special cubic and full cubic polynomials to the response. Fit Summary Table: Sequential Model Sum of Squares 7-10 Mixture Design Tutorials Design-Expert 6 User s Guide

11 Rev. 11/16/00 You may need to widen your window to get the entire output showing. Just move the cursor to the left edge until it changes to a double-ended arrow. Then drag it open. In similar fashion, you can also adjust column widths in any table or report. This may be necessary to uncover the entire text. To move around the display, use the side and/or bottom scroll bars, if necessary. First, look for any warnings about aliasing. In this case, the full cubic model could not be estimated by the chosen design - an augmented simplex design. Remember that you chose only to fit a quadratic model, so this should be no surprise. Next, you see the Sequential Model Sum of Squares table. The analysis proceeds from a basis of the mean response. This is the default model if none of the factors cause a significant effect on response. The output then shows the significance of each set of additional terms: Linear : the significance of adding the linear terms after accounting for the mean. (Due to the constraint that the three components must sum to a fixed total, you will see only two degrees of freedom associated with the linear mixture model.) Quadratic : the significance of adding the quadratic terms to the linear terms already in the model. Special Cubic : the contribution of the special cubic terms beyond the quadratic and linear terms. Cubic : the contribution of the full cubic terms beyond the special cubic, quadratic, and linear terms. (In this case, these terms are aliased.) For each set of terms, the probability ( Prob > F ) should be examined to see if it falls below 0.05 (or whatever statistical significance level you choose). Adding terms up to quadratic will significantly improve this particular model, but when you get to the special cubic level, there s no further improvement. The program automatically underlines at least one Suggested model. Always confirm this suggestion by reviewing all the tables under Fit Summary. See the on-line Help system for more information about the procedure for choosing model(s). Scroll down to see if the quadratic model adequately fits the data. Fit Summary Table: Lack of Fit Tests Design-Expert 6 User s Guide Mixture Design Tutorials 7-11

12 The lack of fit table compares the residual error to the pure error from replication. If the residual error significantly exceeds the pure error, then something remains in the residuals that can be removed by a more appropriate model. The residual error from the linear model shows significant lack of fit (bad), while the quadratic, special cubic and full cubic do not show significant lack of fit (good). At this point the quadratic model looks very good. Now, scroll down to the last table: Model Summary Statistics. Fit Summary Tables: Summary Statistics of Models Fit The Model Summary Statistics lists other statistics useful in comparing models. The quadratic model comes out best: low standard deviation ( Std Dev ), high Predicted R- Squared and low PRESS. Remember that the full cubic model is aliased, so it should not be chosen. Before moving on, you may want to print the Fit Summary tables by doing a File, Print. These tables, or any selected subset, can be also cut and pasted into a word processor, spreadsheet or any other Window s application. You re now ready to take an in-depth look at the quadratic model. Model Selection and Statistical Analysis Click the Model button to move to the screen where you can select the desired model. Model Dialog Box 7-12 Mixture Design Tutorials Design-Expert 6 User s Guide

13 Rev. 11/16/00 The default automatically is a Suggested model from the Fit Summary screen. You may select alternate models from the pull down list if you want. (Be sure to do this in the rare cases when Design-Expert suggests more than one model.) On this screen you are allowed to manually reduce the model by clicking off terms that are not statistically significant. For example, in this case, you will see in a moment that the AB term is not statistically significant. Design-Expert also provides several automatic reduction algorithms as alternatives to the manual method: Backward, Forward and Stepwise. Click the down arrow on the list box if you d like to try one. We recommend that you not reduce mixture models unless you re sure from subject matter knowledge that this makes sense. Click the ANOVA button for the details on the quadratic model. There are two views available for the ANOVA report. Choose View, ANOVA to see just the statistics. Choose View, Annotated ANOVA to see the same statistics, but with text added to help with the interpretation. The program will default to whichever view was last chosen. In this case the ANOVA report provides all the details on the quadratic model. ANOVA Table (Shown without annotations) The statistics look very good. The model has a high F value, low probability values (Prob > F) and more than adequate precision. The probability values show the significance of each term. Because the mixture model does not contain an intercept term, the main effect coefficients (linear terms) incorporate the overall average response and are tested together. All the other statistics look good. Many of these you ve seen already in the Model Summary Statistics table. It s now safe to look at the Design-Expert 6 User s Guide Mixture Design Tutorials 7-13

14 coefficients and associated confidence intervals for the quadratic model. Scroll down to see these statistics. Post-ANOVA - Coefficients for the Quadratic Model The standard error given is the standard deviation associated with the coefficient estimates. This is used along with a t-value to generate a 95% confidence interval on each coefficient. The interval should bracket the true coefficient 95% of the time. Scroll down further to the next section of the output, which shows the predictive models in terms of pseudo (coded), real (coded) and actual components. Final Equation in Terms of Pseudo versus Real (Coded) Components Final Equation in Terms of Actual Components Design-Expert now uses the equations to make a list of actual versus predicted response values. These can be seen by scrolling down to the last part of this output screen - the Diagnostics table Mixture Design Tutorials Design-Expert 6 User s Guide

15 Rev. 11/16/00 Diagnostics Case Statistics (partially shown) Review Diagnostic Graphs The main thing to check in this table is the column labeled Outlier t. The program flags any values that fall outside of plus or minus 3.5. These unusual runs should be investigated for possible special causes. You might find something as simple as a transposition in data entry, or it could be something more dramatic, or you may find no special cause at all. Depending on your findings, you can decide to keep it in the data set, delete it, or right-click the button next to the suspect run and select Toggle Ignore Status. Other problems in the analysis will become more evident in plots of these statistics. You will do this in a moment. Before moving on, you may want to print these tables by doing a File, Print. Click on the Diagnostics button to open a palette of diagnostic tools. Normal Probability Plot of Studentized Residuals Design-Expert 6 User s Guide Mixture Design Tutorials 7-15

16 As you can see, Design-Expert provides a complete selection of graphs that will help you validate your statistical analysis. We suggest you look at these in Studentized form. Notice that this option is checked by default. It allows you to view the residual graphs in units of standard deviation, rather than the measured units of the response. The diagnostics selection presents the most important graph by default: the normal probability plot of studentized residuals. Departures from a straight line indicate nonnormality of the error term, which may be corrected by a transformation. Use your mouse to drag or rotate the line to fit the points. There are no indications of any problems in our data. You can identify data points on the graph by using the mouse to click on the points. Try it! You will now construct another key residual plot: the studentized residuals versus the predicted value. Click on the Predicted diagnostics selection to make the plot. Plot of Residuals Versus Predicted Values You want to see no pattern on this plot, just random scatter about the zero line as seen on the plot above. Patterns in the plot of residuals versus predicted values might be corrected by making a transformation of the response. If desired, you may now look at the other residual plots offered by Design-Expert. Check them out Mixture Design Tutorials Design-Expert 6 User s Guide

17 Rev. 11/16/00 Examine Response Plots Trace Plot Finally, after passing all the diagnostic tests, the response data can be plotted. Select the Model Graph button to produce the plots you want. Select View, Trace for a silhouette of the response surface. Response Trace Plot Contour Plots The trace plot shows the effects of changing each component along an imaginary line from the reference blend (defaulted to the overall centroid) to the vertex. As the amount of this component increases, the amounts of all other components decrease, but their ratio to one another remains constant. Click on the curve for A. (It will change color). Notice that viscosity is not very sensitive to this component. If you experiment on more than three mixture components, use the trace plot to find those components that most affect the response. Choose these influential components for the axes on the contour plots. Set as constants those components that create relatively small effects. Your 2D contour and 3D plots will then be sliced up in way that s most interesting visually. The View, Contour menu selection generates the following plot. Design-Expert 6 User s Guide Mixture Design Tutorials 7-17

18 Contour Plot You can adjust contour levels in several ways: 1. Click and drag to change the level of any contour displayed. Try it! 2. Right click on the contour to Delete contour. 3. Right click anywhere on the graph to Add contour. Do it! Here s the best option of all: right click anywhere on the graph. Then select the Graph preferences option. Tools for Modifying Contour Graph Pick the Contours option if it doesn t come up by default. You now can see the actual minimum ( Min ) and maximum ( Max ) predicted values. This helps you decide the range for your contours. Click on the button labeled Incremental. Fill in the Start, Step and Levels as shown below Mixture Design Tutorials Design-Expert 6 User s Guide

19 Rev. 11/16/00 Incremental Option for Contour Levels Click on OK. Now the contours are cleaned up. Move the mouse pointer to the lower center of the plot. Right click the mouse and Add flag. Mixture Contour Plot With Flag Planted Right click on the flag and Toggle size to produce detailed information about the point. Design-Expert 6 User s Guide Mixture Design Tutorials 7-19

20 Flag Toggled to Larger Size The flag shows the predicted response at that point on the plot, plus: Lower 95% confidence bound of prediction Upper 95% confidence bound of prediction Standard error of the mean Standard error of one prediction Exact composition at the flag location You can plant as many flags as you want. Go ahead, have some fun! Don t bother doing it now, but you can print the contour plot (or other model graphs) by selecting File, Print. 3D plot of the Response Surface To look at the surface in three dimensions, select View, 3D Surface. 3D Mixture Plot 7-20 Mixture Design Tutorials Design-Expert 6 User s Guide

21 Rev. 11/16/00 Now try rotating the plot for a different perspective. Just use the hand to drag the rim of each wheel. Watch the 3D surface change. It s fun! See if you can get a better viewing angle. Control for Rotating 3D Response Plot Standard Error Plot Press the Default button when you re done playing. The graph then re-sets to its original position. Notice that you can also specify the horizontal ( h ) and vertical ( v ) coordinates. It is now time to leave the contour plots and examine the standard error plot. The standard error plot shows how the variance associated with prediction changes over your design space. Select View, Standard E rror and 3D Surface to generate the graph. In order to get a realistic view of the graph, let s change the z-axis scale. Right click somewhere on the graph and select the Graph Preferences option. Change the Z axis scale (default choice) to these settings: Low of 2, High of 10, Ticks of 5 (the default). Then click on OK and the graph should look like the one shown below. Standard Error Plot with Z-Axis Modified Design-Expert 6 User s Guide Mixture Design Tutorials 7-21

22 Response Prediction Design-Expert allows you to generate predicted response(s) for any composition. To see how this works, click on the Point Prediction node under optimization. Point Prediction Results You now see the predicted responses from this particular blend - the centroid. Be sure to look at the 95% prediction interval ( PI low to PI high ). This tells you what to expect for an individual confirmation test. You might be surprised at how much variability could affect the outcome. Although there s no reason to do so now, you can print the results by using the File, Print command. The Factors Tool will open along with the point prediction window. Move the floating tool as needed by clicking on the top border and dragging it. You can drag the handy sliders on the component gauges to look at other blends. Note that in a mixture you can only vary two of the three components independently. Can you find a combination that produces viscosity of 43? (Hint: push Urea up a bit.) Don t try too hard, because in the next section of this tutorial you will make use of Design-Expert s optimization features to accomplish this objective. Click on the Sheet button to get a convenient entry form for specific component values. For example, to get the centroid back, enter the values shown below. Factors Tool Gauges versus Sheet View (with value being entered for Urea) Click back to the Gauges view before proceeding Mixture Design Tutorials Design-Expert 6 User s Guide

23 Rev. 11/16/00 Analyze the Data for the Second Response The last step is a BIG one. Analyze the data for the second response, turbidity (Y 2 ). Be sure you find the appropriate polynomial to fit the data, examine the residuals and plot the response surface. (Hint: The correct model is special cubic.) You can also view the propagation of error graph for this response. When you are done, use File, Save if you have made changes to your data. To leave Design-Expert software, select File, Exit and you re out of the program. This tutorial gets you off to a good start using Design-Expert software for mixtures. We suggest that you now go on to the Mixture Optimization Tutorial. You also may want to do the tutorials on use of response surface methods (RSM) for process variables. To learn more about mixture design, attend Mixture Design For Optimal Formulation, a three-day workshop presented by Stat-Ease. Call or visit our web site ( for a schedule. Design-Expert 6 User s Guide Mixture Design Tutorials 7-23

24 Mixture Optimization Tutorial This tutorial shows the use of Design-Expert software for optimization of mixture experiments. It s based on the data from the preceding tutorial. You should go back to this section if you ve not already completed it. For details on optimization, use the on-line program Help. Also, Stat-Ease provides indepth training in its Mixture Designs For Optimal Formulation workshop. Call for information on content and schedules, or better yet, visit our web site at Start the program by finding and double clicking on the Design-Expert software icon. The detergent design, response data and appropriate response models are stored in a file named Mix-a.dx6. To load this file, use the File, Open Design menu item. File, Open Dialog Box Once you have found the proper drive, directory and file name, click on Open to load the data. To see a description of the data analysis, click on the Status icon under the design node. Design Status Screen 7-24 Mixture Design Tutorials Design-Expert 6 User s Guide

25 Rev. 11/16/00 Numerical Optimization The file you loaded includes analyzed models as well as the raw data for each response. Recall that the formulators chose a three-component simplex design to study a detergent formulation. The components were water, alcohol and urea. The experimenters held all other ingredients constant. They measured two responses: viscosity and turbidity. You will optimize the mixture using their analyzed models. From the design status screen you can see that we modeled viscosity with a quadratic mixture model and turbidity with a special cubic model. Design-Expert software s numerical optimization will maximize (or minimize): A single response A single response, subject to upper and/or lower boundaries on other responses Combinations of two or more responses. We will lead you through a multiple response optimization (the latter option on the list above). For an in-depth discussion of how Design-Expert does numerical optimization see the on-line Help system. Press the Numerical optimization node to start the process. Setting Numerical Optimization Criteria Now you get to the crucial phase of numerical optimization: assignment of optimization parameters. For each component and response, you can establish a goal as well as set lower and upper limits. These three parameters will be used to assign desirability indices (d i ), which range from zero to one. Design-Expert can then search for the Design-Expert 6 User s Guide Mixture Design Tutorials 7-25

26 greatest overall desirability. A desirability value of one represents the ideal case. A zero indicates that one or more responses fall outside desirable limits. You can set objectives for the components, but in this case leave them at their default constraints. Move on to the responses. Click on Viscosity. Then click on the list arrow by Goal and choose is target. Enter a value of 43, with a Lower Limit of 39 and an Upper Limit of 48. These limits indicate that it is most desirable to achieve the targeted value of 43, but values in the range of are acceptable. Values outside that range are not acceptable. Your screen should now match the one shown below. Setting Target for First Response Now click on the other response, Turbidity. Select the Goal of is minimum, with a Lower Limit of 800 and an Upper Limit of 900. Aiming for Minimum on Second Response 7-26 Mixture Design Tutorials Design-Expert 6 User s Guide

27 Rev. 11/16/00 These settings create the following desirability functions: 1. Viscosity: if less than 39, then desirability (d i ) equals zero from 39 to 43, d i ramps up from zero to one from 43 to 48, d i ramps back down to zero if greater than 48, then d i equals zero. 2. Turbidity: if less than 800, then d i equals one from 800 to 900, d i ramps down from one to zero if over 900, then d i equals zero. The user can select additional parameters, called weights, for each response. Weights give added emphasis to upper or lower bounds or emphasize a target value. With a weight of 1, the d i will vary from zero to one in linear fashion. Weights greater than one (maximum weight is 10) give more emphasis to the goal. Weights less than one (minimum weight is 0.1) give less emphasis to the goal. Leave the Weights fields at their default values of 1. Importance is a relative scale for weighting each of the resulting d i in the overall desirability product. Set the most important response(s) to the highest level of five pluses (+++++). The lowest rated response(s) should be set at only one plus (+). Caution: setting all responses at the same importance scale defeats the purpose. It s the contrast in importance ratings that makes the difference. Leave the Importance for both responses at the default setting of three pluses (+++) for this exercise, a medium setting. See the on-line Help system for a more in-depth explanation of the construction of the desirability function, and formulas for the weights and importance. The Options button controls the number of cycles (searches) per optimization. If you have a very complex combination of response surfaces, increasing the number of cycles will give you more opportunities to find the optimal solution. The duplicate solution filter, adjusted via a slider, establishes the minimum difference (the Epsilon) for eliminating duplicate solutions. Push the slider to the right to filter out more solutions. Moving the slider to the left creates the opposite effect you get more solutions, some of which may be nearly identical. For this case study, leave these options at their default levels (shown below). Optimization Options Design-Expert 6 User s Guide Mixture Design Tutorials 7-27

28 Running the Optimization Start the optimization by clicking on the Solutions button. After grinding through ten cycles of optimization, the results appear. Each solution generated meets all your criteria, with varying degrees of desirability. For each solution you want to look at: Factors - the composition at this optimum. Responses - the value of each response at this optimum. Desirability - the value at this optimum (ideally 1.0). Design-Expert sorts the results for you. It shows the best solution first in report format. You get a summary of all the cycles. If the report doesn t fit in the window, move your cursor to the left border and drag it open. In addition to the solutions, the report includes a recap of your optimization specifications as well as the random starting points for the search. Your results will most likely NOT perfectly match those shown here. Also, the number of solutions generated may be different. Optimization Report (Your results may differ) You should see at least one outcome at the bottom of the list of solutions that s inferior to the others. It will have a desirability well below the ideal of one. There may also be some duplicates. These passed through the filter discussed earlier. If you want to adjust the filter, go to the Options button and change the Duplicate Solutions Filter. Remember that if you move the filter bar to the right you will decrease the number of 7-28 Mixture Design Tutorials Design-Expert 6 User s Guide

29 Rev. 11/16/00 solutions shown. Likewise, moving the bar to the left increases the number of solutions. Go ahead run and check Solutions with the filter set at one end or the other. The report on Solutions comes in two other formats Ramps and Histograms. Click on the Ramps option for a very handy display that shows solutions in the context of desirability functions. Optimization solutions, Ramps Option In this case you may find as many as three distinct optimums. Because the software begins its search at a random starting point, you may get somewhat different results than those shown in this manual. The program will try to eliminate duplicates, but due to the presence of plateaus (indicated by the multiple solutions with a desirability of one) you may see several solutions that differ slightly. The red dots indicate settings of input factors and the resulting predictions for each response. Now press the different solution buttons while watching the dots. Do they change much? Now choose the Histogram option. Although not particularly interesting in this case, the histogram shows graphically how well each factor and response achieved its goal. Design-Expert 6 User s Guide Mixture Design Tutorials 7-29

30 Optimization Solutions, Histogram Optimization Graphs Click on the Graphs button to generate contour plots for each of the solutions. Pick the last solution on your list: the worst one. Contour Plot of Desirability, Worst Region Pick a solution with a desirability of one to see how the optimum shifts. It should look a lot better. If your best result shows a flag planted in a different location, but still on the same hill, it s because there s a ridge-line where almost any spot will be good. When 7-30 Mixture Design Tutorials Design-Expert 6 User s Guide

31 Rev. 11/16/00 you view the 3D surface, this will become more apparent. The software will give varying results on surfaces like this, so you should explore different solutions before making a final recommendation. Once you settle on the best outcome (Solution 1), right click on the flag planted at the optimum point and Toggle Size to display a larger flag with the optimum coordinates displayed. Try it. Contour Plot of Desirability, Larger Flag at Better Region (results may differ slightly) Check the other solutions. They may change only slightly in some cases, especially where there s a relatively flat peak. To view the responses associated with the desirability, select the desired Response from the drop down list. For example, click on the response for Viscosity. Viscosity Contour Plot (with optimum flagged) Design-Expert 6 User s Guide Mixture Design Tutorials 7-31

32 Notice that the optimum is flagged. Now, go back to the Response selection of Desirability. Then select View, 3D surface. Then go back to View and click to turn the Show Legend off. Use the rotation tool to get the best vantage point to see the three local peaks. 3D Desirability Plot with Show Legend Off Right click on the graph and select Graph Preferences. Then click on the Graph option to change Graph resolution to High. Plotting at High Resolution 7-32 Mixture Design Tutorials Design-Expert 6 User s Guide

33 Rev. 11/16/00 The high resolution may look better, but be prepared for longer print times, so re-set Graph resolution to Normal. When you have more than three components to plot, Design-Expert software uses the composition at the optimum as the default for the remaining constant axes. For example, if you design for four components, the experimental space is a tetrahedron. Within this three-dimensional space you may find several optimums, which require multiple triangular slices, one for each optimum. Adding Propagation of Error (POE) to the Optimization If you have prior knowledge of the variation in your component amounts, this information can be fed into Design-Expert software. Then you can generate propagation of error (POE) plots that show how that error is transmitted to the response. Look for compositions that minimize the transmitted variation, thus creating a formula that s robust to slight variations in the measured amounts. Start by clicking on the Design node on the left side of the screen to get back to the design layout. Then select View, Column Info Sheet. Enter the following information into the Std. Dev. column: Water: 0.08, Alcohol: 0.06, Urea: 0.06, as shown on the screen below. Column Info Sheet with Standard Deviations Filled In In order to generate the propagation of error graph, the analysis must be completed a second time. Since you haven t changed any other data, the software will remember your previous analysis choices and you can simply click through the analysis buttons. This time the Propagation of Error (POE) graph, which was grayed out before, will be available from the Model Graph node. Click on the Viscosity analysis node on the left to start the analysis again. Simply click through the buttons across the top of the screen. When you get to the Model Graphs button, select View, Propagation of Error. Also choose the 3D Surface view. If it s still in the high-resolution mode that you specified earlier, right click on the graph and select Graph Preferences. Then click on the Graph option to change Graph resolution to Normal. Now your screen should match what s shown below. Design-Expert 6 User s Guide Mixture Design Tutorials 7-33

34 3D Surface View of the POE Graph Where the surface reaches a minimum is where the least amount of error is transmitted, or propagated, to the viscosity response. At this composition the formulation will be most robust to varying amounts of components. For additional details on the POE technique and how to develop robust processes and products, attend Stat-Ease s workshop Robust Design, DOE Tools for Reducing Variability. Now that you ve found optimum conditions for the two responses, let s go back and add criteria for the propagation of error. Click on the Numerical optimization node. Set the POE (Viscosity) Goal to is minimum with a Lower Limit of 5 and an Upper Limit of 8 Set Goal and Limits for POE (Viscosity) 7-34 Mixture Design Tutorials Design-Expert 6 User s Guide

35 Rev. 11/16/00 Select POE (Turbidity) and set its Goal to is minimum with a Lower Limit of 90 and an Upper Limit of 120. Criteria for POE (Turbidity) Now click on the Solutions button to generate new solutions with the additional criteria. The number 1 solution represents the formulation that best achieves the target value of 43 for viscosity and minimizes turbidity, while at the same time finds the spot with the minimum POE (most robust to slight variations in the component amounts). Solutions Generated with Added POE Criteria (Your results may differ) Be sure to review the alternative solutions, which may be nearly as good based on the criteria you entered. In this case, the number 2 solution, which you may or may not get due to the random nature of the optimization, increases the water level (presumably cheaper) and reduces turbidity, so it may actually be preferred by the formulators. Design-Expert 6 User s Guide Mixture Design Tutorials 7-35

36 Select the Graphs button to see the number 1 solution flagged on a contour plot of desirability. Optimal solution with added POE criteria Graphical Optimization By shading out regions that fall outside of specified contours, you can identify a desirable window for each response. If plotted on clear view foils (overheads), all response plots can be overlaid to identify the sweet spot for the mixture formulation an area where all specifications can be met. In this case, the response specifications are: 39 < Viscosity < 48 POE (Viscosity) < 8 Turbidity < 900 POE (Turbidity) < 120 To overlay the plots for all these responses, click on the Graphical optimization node at the lower left of your screen. For the Viscosity response enter a Lower limit of 39 and an Upper limit of Mixture Design Tutorials Design-Expert 6 User s Guide

37 Rev. 11/16/00 Setting Criteria for Graphical Optimization: Viscosity Click on the POE(Viscosity) response. Enter an Upper limit of 8. Leave the lower limit blank. (You do not need to enter a lower limit for the graphical optimization to work.) Click on the Turbidity response and enter an Upper limit of 900. Finally, click on the POE(Turbidity) response and enter an Upper limit of 120. (Neither of these turbidity-related responses need a lower limit.) Click on the Graph button to produce the display. Graphical Optimization Display Design-Expert 6 User s Guide Mixture Design Tutorials 7-37

38 The shaded areas on the graphical optimization plot do not meet the selection criteria. The lines mark the boundaries on the responses. Unless you have changed your color preferences, the yellow window shows where you can set the components to satisfy the requirements on both responses. If there s no window, or it s too small, grab the boundaries and widen them. Give this a try! There s virtually no limit to the number of responses you can optimize. Just be sure you analyze them first, because the program needs models for every response. Also, you must enter either a lower or an upper level to include a response in the optimization. Move your mouse pointer into the yellow area, right click and select Add flag to plant a flag showing details for any composition. Graphical Optimization Plot - Mixture Prediction at Flagged Point Final Comments The flag shows the predicted viscosity and turbidity, and associated POE s, at that point on the plot. Graphical optimization works great for three factors, but as the factors increase, it becomes more and more tedious. With Design-Expert software, you can explore multiple factors and multiple responses, and find solutions much more quickly, by using the numerical optimization feature. Then finish up with a graphical overlay plot at the optimum slice. If you want to learn more about mixture design, come to our Mixture Designs For Optimal Formulation workshop. To get the latest class schedules, give Stat-Ease a call Mixture Design Tutorials Design-Expert 6 User s Guide