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5/15/07

Mixture Design Tutorial

(Part 1 – The Basics)
Introduction
In this tutorial you will get an introduction to mixture design. It will be assumed that at
this stage you’ve mastered many of Design-Expert® software’s basic features by
completing the preceding tutorials. At the very least you ought to first do the General
One-Factor tutorials, basic and advanced, prior to starting this one.

We will presume that you can handle the statistical aspects of mixture design. To gain a
working knowledge of this powerful tool, we recommend you attend our Mixture Design
for Optimal Formulations workshop. Call Stat-Ease or visit our website,
www.statease.com, for a schedule. If you want statistical detail on this topic, see, John
Cornell’s Experiments with Mixtures, 3rd edition published by John Wiley and Sons,
New York in 2002.

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 Case Study – Formulating a Detergent

A detergent must be re-formulated to fine-tune two product attributes, which will be
measured as responses from a designed experiment:
• Y1 - viscosity
• Y2 - turbidity.

Three primary components will be varied as shown:

• 3% ≤ A (water) ≤ 8%
• 2% ≤ B (alcohol) ≤ 4%
• 2% ≤ C (urea) ≤ 4%

These components represent nine weight-percent of the total formulation, that is:

A + B + C = 9%

The other materials (held constant) make up the difference: 91 weight-percent of the
detergent. For purposes of this experiment they can be ignored.

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.

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 X1
2

90

70

50

10

10
30
30
2
30

50

50

70
70

10

90
90

2 2
X2 X3

Augmented simplex lattice (second degree)

This case study leads you through all the steps of design and analysis for mixtures. The
next tutorial, Part 2, will detail how you can simultaneously optimize the two responses.

Design the Experiment

Start the program by finding and double clicking the Design-Expert software icon. 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 – New Design icon identified

Click on the Mixture folder tab. The design you want, a simplex lattice, comes up by
default.

Choosing a mixture design

Some detail is offered on-screen, but more can found by pressing the screen tips button
(or select Help, Screen Tips).

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On-screen details, plus more brought up via Tips button

Close Tips down by pressing the X button at its upper right corner. Then explore Help,
Contents.

Looking for more Help

Then double-click Mixture Designs and Mixture Design Choices and then select
Simplex-Lattice Design.

Detail on simplex-lattice design via Help contents

Close Help down by pressing X. Then change the number of Mixture Components to
3. Then enter the component and their limits as shown below in the Name, Low and
High fields, pressing the Tab key after each entry. Enter 9 in the Total field and % in
the Units field.

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 Entering components, limits and total

Press Continue. Immediately a warning appears.

Adjustment made to constraints

Press OK. Notice that, although you entered the high limit for water as 8%,
Design-Expert adjusts it to 5% which leaves room for 2% each of the other two
ingredients within the 9% total. Otherwise, at 8% water and the low levels of alcohol
and urea the total would become 12%, which the program realizes does not compute.
Very smart and very helpful!

Press Continue and this time the software lets you move on. Now you must choose the
order of the model that you expect to be appropriate for the system being studied. In this
case, you can assume that a quadratic polynomial, which includes second order terms for
curvature, will adequately model the responses. Therefore leave the order at
Quadratic. Accept the default check-off to Augment design, but change the Number
of runs to replicate to 3.

Simplex-lattice design form (after pressing Tab key)

By accepting “Augment design” you allow Design-Expert to add the overall centroid
and axial check blends to the design points. The “Number of runs to replicate” field,
defaulted to 4, causes the specified number of highest leverage experiments to be
duplicated. In this case, there are three points with highest leverage – the vertices of the
triangular simplex.

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Press Continue to the next step in the design process: Entering Responses. For the
number select 2. Then enter the response Names and Units as shown below.

Response entry

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.

Examine the Design and Modify It If You Like

The default columns in the design layout can be modified to be more informative in this
mixture case. Right click on the Select button at the upper-left corner and pick Design
ID. It then becomes a new field for uniquely identifying your mixture ‘recipes.’ Then
right-click Select again to turn off display of the Block column – superfluous for this
experiment. Also Select off the Std Order. Finally, Select on display of Point
Type. This will be very helpful for insights on the design geometry. Your selections
should now look like those depicted below (default shown for comparative purposes).

Changing what will be displayed on the design layout (versus the default)

Next, right click the top of the column now labeled Id, and select Sort by Design ID.
Now you get a feel for where the points are located and which ones are replicated. (Run
order is randomized and thus differs from what’s shown below.)

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 Initial design sorted by ID with point type shown (run order randomized)

The experimenters ran an additional centroid point, so in the box to the left of Id 0
(Type: “Center”) right-click and select Duplicate.

Duplicating the centroid

Whenever you insert, delete or duplicate rows, always right-click the Run column-
header and chose Randomize.

Re-randomizing the run order

A box will pop up asking if you’d like all blocks to be randomized. In this case there is
only one block, so simply press OK. Notice that run numbers now change.

Again, right-click the Run column-header, but this time choose Sort by Run Order.
Normally you’d now do a File, Print to produce a ‘recipe’ sheet for doing the
experiment. Go ahead if you have a printer available.

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Save Your Work

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 As. 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 dx7. (We suggest tut-mix). Then click
on Save.

Analyze the Results

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’s Data directory. Select File, Open Design. Click on the
file called Mix.dx7. Then press OK. You now should see response data. (Note that the
design layout returns to the default selection, which we did not bother to change.)

There’s no need for typing in this case, but normally you’d have put in a lot more work
at this stage, so always do a File, Save for preservation of entered response data.

Response data

Go to the Analysis branch of Design-Expert and click on the node for Viscosity. You
now will work across the buttons at the top of the window.

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 First step in analysis: Transformation options

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. In this case the ratio of maximum
to minimum response is only a bit over 4, which isn’t too excessive (see detail at bottom
of the screen), so leave the selection at its default, None, because no transformation will
be needed. Also, leave the coding for analysis as pseudo which re-scales the actual
component levels to 0 – 1. For complete details on coding mixtures see the textbook by
Cornell mentioned at the outset of the tutorial. In the meantime, bring up Help,
Contents and then double-click Mixture Designs and Mixture Statistical
Information and then select Component Scaling in Mixture Designs.

Statistical detail on coding available via Help

Close Help down by pressing X. Then click on the Fit Summary button. At this point
Design-Expert fits linear, quadratic, special cubic and full cubic polynomials to the
response.

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Fit summary reports

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 the response. The output then shows the significance of each set
of additional terms:
• “Linear vs Mean”: 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 vs Linear”: the significance of adding the quadratic terms to the
linear terms already in the model.
• “Sp Cubic vs Quadratic”: the contribution of the special cubic terms beyond
the quadratic and linear terms.
• “Cubic vs Sp Cubic”: the contribution of the full cubic terms beyond the
special cubic, quadratic, and linear terms. (In this case, these terms are
aliased.)

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 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.

Moving on to next table via the Bookmarks, click the Lack of Fit, which 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.

Lack of fit table

Now, take a look at the last table: “Model Summary Statistics.” Here you see several
comparative measures for model selection.

Summary statistics

Ignoring the aliased cubic model, the quadratic model comes out best: low standard
deviation (“Std Dev”), high “R-Squared” statistics and low “PRESS.”

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.

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Model Selection and Analysis of Variance (ANOVA)

Click the Model button to see the model suggested by Design-Expert software. Press
the screen tips button to see some very helpful information about what you can do at
this stage.

Choosing the model (Tips up on screen)

You may select alternate models to the default, in this case quadratic, 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.

As noted under the heading “Model Reduction” in Tips, Design-Expert 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.

Close Tips by clicking X. The press the ANOVA button for the details on the quadratic
model. There are two views available for the ANOVA report: plain or annotated. For
tutorial purposes it’s best you keep it in View, Annotated ANOVA to help with the
interpretation. The program will default to whichever view was last chosen.

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 ANOVA report with annotations toggled on

The statistics look very good. The model has a high F value, low probability values
(Prob > F). 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. Use the handy
Bookmarks for jumping to the next report with R-Squared statistics.

R-squared and other statistics after the ANOVA

These statistics, many of these you’ve seen already in the “Model Summary Statistics”
table, all look good. Note the more than adequate precision value of 27.9.

Next, take a look at the coefficients and associated confidence intervals for the quadratic
model.

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Coefficients for the quadratic model

Continue on to see several alternative models that vary by how the components are
coded. This may be of most interest to students of mixture design rather than actual
formulators, so it’s time to move on: Press the next button – Diagnostics.

Diagnose the Statistical Properties of the Model

The most important diagnostic, the normal probability plot of the residuals, comes up by
default.

Normal Probability Plot of the Residuals

The data points should be approximately linear. A non-linear pattern (look for an S-
shaped curve) indicates non-normality in the error term, which may be corrected by a
transformation. There are no signs of any problems in our data.

At the left of the screen you see the Diagnostics Tool palette. First of all, notice that
residuals will be studentized unless you uncheck the first box on the floating tool palette

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 (not advised). This counteracts varying leverages due to location of design points. For
example, the center points carry little weight in the fit and thus exhibit low leverage.
Each button on the palette represents a different diagnostics graph. Check out the other
graphs if you like. Explanations for most of these graphs were covered in prior
Tutorials. In this case, none of the graphs indicate any cause for alarm.

Now click the option for Influence. Here’s where you find the find plots for externally
studentized residuals (better known as “outlier t”) and other plots that may be helpful for
finding problem points in the design. Also, from here you can bring up case-by-case
details on many of the statistics shown graphically for diagnostic purposes: Press
Report. (In previous versions of Design-Expert, this report appeared under ANOVA.)

Diagnostics report

Notice that one value is flagged for exceeding suggested limits: DFFITs for standard
order 11. As we discussed in the General One-Factor Tutorial (Part 2 – Advanced
Features), this statistic stands for difference in fits. It measures the change in each
predicted value that occurs when that response is deleted. Given that only this one
diagnostic is flagged, it probably is not a cause for alarm. However, observe that it’s
one of the highest observed viscosity responses (130.00 Actual Value), so the
experimenter might want to double-check the accuracy of this response.

Examine Model Graphs

The diagnosis of residuals reveals no statistical problems, so you will now generate the
response surface plots. Click on the Model Graphs button. The 2D contour plot of
comes up by default in graduated color shading.

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Response surface contour plot

Note that Design-Expert will display any actual point included in the design space
shown. In this case you see a plot of viscosity as a function of the three mixture
components. This slice includes two centroids as indicated by the dot at the middle of
the contour plot.

The Factors Tool comes along with the default plot. Move this floating tool as needed
by clicking on the top blue border and dragging it. The tool controls which factor(s) are
plotted on the graph. The Gauges view is the default. Each component listed will either
have an axis label, indicating that it is currently shown on the graph, or a red slider bar,
which allows you to choose specific settings for those not currently plotted. This case
study involves only three components, all of which can fit on one mixture plot – a
ternary diagram. Therefore, you will not see a slider bar. If you did, it would default to
the midpoint levels of the components not currently assigned to axes. You could then
change a level by dragging the red slider bars. If you’d like to see a demonstration of
this feature, do the Multifactor RSM Tutorial (Part 1 – The Basics).

Place your mouse cursor over the contour graph. Notice in the lower left corner of the
screen that Design-Expert displays the predicted response and coordinates.

Coordinates display at lower, left corner of screen

To enable a handier tool for reading coordinates off contour plots, go to View, Show
Crosshairs Window.

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 Showing crosshairs window

Now move your mouse over the contour plot and notice that Design-Expert generates
the predicted response for specific values of the factors that correspond to that point. If
you place the crosshair over an actual point, for example – the check-blend above the
centroid, you also get that observed value (in this case: 35.1).

Prediction at upper check blend where an actual run was performed (Small vs Full)

Press the Full button to get confidence and prediction intervals in addition to the
coordinates and predicted response. Then close out the crosshairs window by clicking
X.

Zooming In and Out

Let’s say you were particularly interested in highest values for viscosity. With your left
mouse button pressed, drag over the lower right corner of the contour graph.

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Corner identified for zoom

Now you see just the area you chose magnified.

Zoomed-in area on contour plot

To revert back to the full triangle, right-click over the plot and select Zoom out.

Zoom out

Trace Plot
Wouldn’t it be handy to see all your factors on one response plot? You can do this with
the trace plot, which provides silhouette views of the response surface. The real benefit

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 from this plot is for selecting axes and constants in contour and 3D plots. Use the View,
Trace menu item to select it. For the screen shot below, go the floating Trace Graph
tool and change the Direction to Cox.

Trace plot – component A highlighted

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. For example,
click on the curve for A. (It will change color). Notice that viscosity is not very
sensitive to this component.

In this case where the experimental region forms a simplex, it matters little which
direction you take: Piepel, Cox or Orthogonal. In the Cox direction as the amount of
this component increases, the amounts of all other components decrease, but their ratio
to one another remains constant. Chemists may like this because it preserves the
reaction stoichiometry. However, when plotted in this direction, traces for highly-
constrained mixture components, such as a catalyst for a chemical reaction, become
truncated. Thus, experts in mixture design argue that although it no longer holds actual
ratios constant, Piepel’s direction provides a more helpful plot by providing the broadest
coverage of the experimental space. For this reason Piepel is the preferred plot in
Design-Expert.

Trace plots are highly dependent not only on direction (Cox vs Piepel for example), but
also on where you place the starting point (by default the centroid). Consider that the
traces are one-dimensional only, and thus cannot provide a very useful view of a
response surface. The 3D response plots provide better pictures of the surface and
ultimately provide the basis for numerical optimization -- the ultimate tool for
determining the most desirable mixture composition. In the end it may make no
difference as a practical matter which plot you use.

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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.

Contour Plot: Revisited

Return to the contour plots via the View, Contour selection. The colors are neat, but
what if you must print the graphs in black and white? That can be easily fixed by right-
clicking over the graph and selecting Graph Preferences. Then click the Graphs 2
tab and change the Contour graph shading to Std Error shading.

Graph preferences: Changing contour graph shading

Press OK to see the effect on your plot.

Contour plot with standard error shading

Design-Expert draws five contour levels by default. They range from the minimum
response to the maximum response. Click on a contour to highlight it. You can move
the contours by dragging them to new values. (Place the mouse cursor on the contour
and hold down the left button while moving the mouse.) Give this a try – it’s fun!

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 We recommend another approach to laying out contours. Right click in the drawing or
label area of the graph and choose Graph Preferences. Then choose Contours.
Now select the Incremental option and fill in the Start at 35, Step at 10 and Levels
at 20. Also, under Format choose 0 to display whole numbers (no decimals). Your
screen should now match that shown below.

Contours dialog box: Incremental option

Press OK to get a good-looking contour plot – suitable for printing. This one was
produced via Edit, Copy from Design-Expert and Edit, Paste into Microsoft Word. (The
triangle may not come in looking equilateral, but if this is bothersome, it can be easily
remedied by dragging the right border and widening the picture.)

Plot with incremental contours

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You can add new contours via a right mouse click. Find a vacant region on the plot, for
example – between the 35 and 45 contours, and check it out: Right-click and select Add
contour. Then drag the contour around (it will become highlighted) until it becomes
40.

Adding contours

To get a more precise contour level and locate it accurately, you can right-click it and
enter the desired value. On the new contour select Set contour value and enter 40.

Setting a contour value

That fills a gap nicely!

Move your mouse to a spot near the top of the graph, where the response hits the
minimum. Click the right mouse button and Add flag. To get more digits displayed,
right click for Graph Preferences and under Contours change Format to 0.00.
Then press OK.

Adding a flag (format re-set via Graph Preferences)

It displays the value of the response at that point. Now do a right click of the mouse on
the flag and select Toggle size.

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 Flag enlarged via Toggle Size option

The expanded flag displays a 95 percent confidence interval (CI) on the mean prediction.
It also provides the prediction interval (PI). Use this to ‘manage expectations’ about
individual confirmation runs near this point. The PI conveys how natural variability in
the process/sampling/testing plus imprecision in the estimate of the mean (SE mean)
causes actual outcomes to differ from the prediction. The larger flag also lists the point
coordinates. If you have a printer, you can print the contour plot by using the File, Print
menu item.

Generating a 3D View of the Response Surface

Now to really get a feel for how the response varies as a function of the two factors
chosen for display, select View, 3D Surface. You then will see three-dimensional
display of the response surface. If the coordinates encompass actual design points, these
will be displayed.

3D response surface plot

The Rotation tool allows you to view the 3D surface plot from any angle.

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Control for rotating 3D plot

Move your cursor over the tool. The pointer changes to a hand. Now use the hand to
rotate the vertical or horizontal wheel. Watch the 3D surface change. It’s fun! What’s
really neat is how it becomes transparent so you can see hidden points falling below the
surface.

Transparent view as surface is rotated, which allows points to be seen better

Also, be aware that Design-Expert offers many options for 3D graphs via its preferences,
which come up via a right-click over the plot. For example, if you don’t like the
graduated colors, go to the Graphs 2 tab and change the 3D graph to the hidden wire
view (a transparent look).

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.

Response Prediction
This feature in Design-Expert software falls under the Optimization branch, which will
be explored more fully in the next tutorial in this series. It allows you to generate
predicted response(s) for any set of factors. To see how this works, click on the Point
Prediction node (lower left on your screen).

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 Point Prediction

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. 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.
Be careful though, the ingredients must add up to the fixed total you specified – in this
case 9 wt %. Design-Expert will make adjustments as you go – perhaps in ways that you
do not anticipate. Don’t worry: If you get too far off, simply press the Default button to
get back to the centroid.

Analyze the Data for the Second Response

The last step is a BIG one. Analyze the data for the second response, turbidity (Y2). 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.)

Before you quit, do a File, Save to preserve your analysis. Design-Expert will save
your models. To leave Design-Expert, use the File, Exit menu selection. The program
will warn you to save again if you’ve modified any files.

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 Formulations, a
three-day workshop presented by Stat-Ease. Call or visit our web site
(www.statease.com) for a schedule.

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