25 Design of Experiments
Design of experiments, referred to as DOE, is
a systematic approach to understanding how process
and product parameters affect response variables
such as processability, physical properties, or product
performance. It is a tool similar to any other tool,
device, or procedure that makes the job easier. Unlike
quality, mechanical, or process tools, DOE is
a mathematical tool used to define the importance of
specific processing and/or product variables, and how
to control them to optimize the system performance
while maximizing properties. DOE uses statistical
methodology to analyze data and predict product
property performance under all possible conditions
within the limits selected for the experimental
design. In addition to understanding how a particular
variable affects product performance, interactions
between different process and product variables are
identified. Design of experiments is a technique or
procedure to generate the required information with
the minimum amount of experimentation, using the
following:

Experimental limits

Specific experimental conditions

Mathematical analysis to predict the response at
any point within the experimental limits.
DOE is used to determine which factors or vari-
ables and interactions are significant in contributing to
the effect being measured, and those variables and
interactions that are insignificant and do not
contribute to either a particular product property or
processing condition. Using DOE saves both time and
money by providing a usable understanding of the
properties and process. The best time to use a DOE is
during new product or process development, existing
product or process optimization, and while solving
technical problems when more than one variable is
present. Where is DOE used? It is used for solving any
technical problem when you want to fully understand
the response to different process or product variables
that can be changed or controlled during the experi-
mentation. Problems in industry typically get recycled
Extrusion. http://dx.doi.org/10.1016/B978-1-4377-3481-2.00025-9
Copyright Ó 2014 Elsevier Inc. All rights reserved.
from time to time, because an idea that was originally
a good idea could not be accomplished because the
technology was not available or the project was
aborted because of lack of time and resources. Since
the original work, new technology has been developed
or resources are available that now make a solution
possible. The advantage of using a DOE approach is
that systematic data are generated, summarized, and
evaluated to definitively determine whether a project
should be carried forward or if it is fundamentally
impossible to resolve and needs to be dropped.
Regardless of whether the DOE results are positive
(experiment showed desired response) or negative
(experiment showed undesired response), it is
important to complete the project and document the
results so that the project will not be recycled at a later
time. The DOE results provide an understanding of the
processing and/or product parameters and their
interactions over the experimental space studied.
Design of experiments is not the procedure to use to
solve production problems on the floor during the
second shift when the product being produced must be
shipped first thing the following morning to keep your
customer’s production running. To solve problems
under these circumstances, change one variable at
a time, slow the production line down, do whatever is
necessary to produce the product to meet the
customer’s requirements. After production is complete,
go back and evaluate the situation to determine if
a designed experiment can be used to define the process
limits and capabilities so that the next time the same
product is run it can be produced more cost effectively
at higher yields with fewer problems.
25.1 DOE Process
The process involved in conducting a successful
design of experiments can be broken down into five
steps:

Define the problem.

Plan the experiment.

Run the experiment.
291
292

Analyze the data by using statistical methods.

Report the results.
25.1.1 Defining the Problem
As with the discussion in Chapter 24, this may
seem obvious, but in practice, it is sometimes
difficult to do. Input from different people may
conflict, and deciding on the specific variables to
control may be controversial. Some input may stress
the need for a DOE, whereas other suggestions may
imply that a DOE is a waste of time. Verify that the
problem is properly defined and clearly understood
before starting any work. As an example, assume an
extrusion profile at a customer is reported to have
unacceptable dimensional stability and you have
been requested to solve the problem. Although
a DOE to understand the effect of processing
conditions on part dimensions may be advisable, the
first step is to define what is meant by “unacceptable
dimensional stability”. Questions to ask are as
follows:

Do dimensional changes occur in the x, y, or z
direction over time?

Is one dimension outside the specification limit,
and is this temperature related?

Do the parts warp inconsistently from piece to
piece?

Do the dimensions change in a controlled
manner over time?

Have the dimensions changed because of
a change in raw materials?

Are the dimensional issues due to shrinkage
caused by the raw materials?

Are the dimensions different from run to run
because of process changes?
Before deciding on the proper course of action and
whether a DOE is necessary, make sure the problem
is properly defined.
It is critical to fully understand the problem
before you try to solve it. If the problem is only
viewed as a problem in some people’s eyes, and
after evaluating the issues you realize that solving
the problem will not generate more business,
improve customer satisfaction with the product, or
make the product better, you are probably wasting
the company’s resources by addressing or spending
time on the problem. An example is a compounded
product produced in an oval shape rather than the
E XTRUSION
typical cylindrical shaped pellet. Customer Service
states that it cannot sell an oval shaped pellet
because all customers normally receive cylindrical
shaped pellets. Since the oval shaped pellets are
free flowing and process the same in both injection
molding and extrusion equipment, working on the
problem to make the pellets cylindrical is a waste
of valuable company resources that can be better
spent on other developmental programs. Fortu-
nately, the decision is made not to spend time or
effort trying to solve the oval pellet problem, and
the product is accepted in the field without
comments.
25.1.2 Plan the Experiment
After the problem is properly defined, the second
step in the DOE process is to select the independent
variables, with their limits for evaluation, and the
dependent variables (responses to measure for each
experiment). Independent variables or factors are
parameters of either processing or product that are set
at specific values (levels) and controlled in the
experimental design. For extrusion, some potential
independent factors are barrel and die temperatures,
screw speed, raw material formulations, drying time,
drying temperature, puller speed, and downstream
conditions such as roll temperatures, roll gaps, draw
ratio, water temperature, oven temperature, vacuum
level, and so forth. Dependent variables or factors are
the responses being measured for each experiment to
determine whether the independent variables have an
effect on properties or processing conditions being
evaluated.
Dependent factors might include physical prop-
erties (impact, tensile, and flexural properties in the
machine and transverse directions, heat resistance,
and so forth), surface or appearance properties
(surface roughness, gloss, distinctness of image,
color, and transparency), formulation cost in
a product composition experiment, and dimensions
(shrinkage, warpage, thickness, length, and so
forth). Many processing variables in extrusion are
dependent variables related to the selected inde-
pendent process variable; these include melt
temperature, melt pressure (die and barrel pressure),
and extruder torque. Melt temperature may be either
an independent or dependent response, depending
on how it is used and/or controlled in the experi-
mental design. In some processes, the melt
temperature can be controlled and is treated as an
25: D ESIGN OF E XPERIMENTS
independent variable; in other processes, the barrel
temperatures are controlled, and the melt tempera-
ture is measured as a dependent response to the
selected barrel temperatures and screw speed. Melt
pressure is normally a dependent variable or
response unless there is a valve to control and set the
melt pressure, at which time it becomes an inde-
pendent variable. In deciding whether a factor or
variable is independent or dependent, ask the ques-
tion, “Is there a knob to turn to set that variable to
a predetermined value?” If the answer is that no
controller exists to set a particular variable in the
process to a fixed value, it is a dependent variable
and is measured as a response to factors that are
preset and controlled.
Independent variables are normally quantitative in
nature, meaning that they are set at a specific
numerical value. However, in some experimental
designs, the independent variables are qualitative,
meaning that a particular switch is on or off, a high or
low setting is used, or a control variable is yes or no.
It is better to use quantitative factors if possible. With
quantitative variables, the high and low levels for
each factor are defined. As an example, the high/low
screw speed levels for a twin screw extruder experi-
ment may be set at 250 and 150 rpm. This sets the
experimental space for that factor. After the experi-
mentation stage is complete, mathematical models
predict the response within the 150- to 250-rpm
range. As this is a linear model, it does not predict
well outside the experimental limits, such as 100 or
300 rpm, if the response is nonlinear. Therefore, the
experimental limits need to be carefully selected in
the planning stage and set as wide as is experimen-
tally practical. After the experimentation is complete,
you do not want to come back and wish the limits
were wider. The points selected to test over the range
of the experimental limits are called levels. Going
back to the screw’s revolutions per minute, if
experimental points are run at 150, 175, 200, 225,
and 250 rpm, there are five levels. In determining the
experimental limits, do a few preliminary experi-
ments to verify that the experiment can physically be
run when all the independent factors are at either
their high or low values. If a particular experiment
cannot be run, for example, at low screw speed and
low barrel temperature because the torque exceeds
the high limit on the extruder, this set of conditions is
impractical and another set of low independent
variables needs to be selected where the process can
be run practically.
293
Dependent variables or responses are easy to
measure and evaluate when using quantitative tests
such as tensile, flexural, and impact, which provide
very specific values for each experiment. In some
situations, responses are more qualitative than
quantitative. Normal qualitative responses such as
pass/fail, good/bad, or yes/no do not provide a good
response to model. A procedure has to be developed
to quantitatively differentiate between the different
samples for that particular response. Instead of
measuring the sample as pass or fail, develop
a grading system that allows differentiation on
a basis of 1e10, even if 1e3 are considered failures,
4e7 are mediocre, and 8e10 are good. The best
results are obtained under processing conditions that
produce a 10. The number of dependent variables or
factors that can be evaluated is almost limitless for
all experiments as the independent variables are
changed. If a particular property response is almost
the same at all sets of experimental conditions, no
significant effect exists for this property over the
range of processing or product conditions tested. If
each response value used in the analysis for
a particular set of processing conditions is the
average of 10 measurements, the standard deviation
obtained from the measurements at each set of
experimental conditions can be evaluated to deter-
mine which set of conditions generates the most
reproducible results.
The number of data points evaluated for each
experimental response depends on the number of
tests required for statistical significance, based on the
precision and accuracy of the test. Precision is how
close the measurements are to each other. If the
measurement precision is high, the number of
samples needed to obtain an accurate mean is smaller
than if the precision is low. Accuracy is how close the
average value for a particular test is to the true value.
If the accuracy is high, the value for the response in
the test is very close to the true value; if accuracy is
low, the response is significantly different from the
true value. It is possible to have high precision and
low accuracy.
How large does the difference in response vari-
ables have to be to indicate a significant effect is
present in the data? This is determined by comparing
the magnitude of the differences between the
dependent responses at the various experimental
points in the matrix. Duplicate or replicate experi-
ments are run either at the center point or some other
selected point within the experimental matrix. The
294
difference in dependent responses between the
replicated points determines the precision or varia-
tion within the data due to unassigned experimental
error. The smaller the differences between the
response values at the replicated points, the more
significant larger differences are between responses
at different experimental points within the design
matrix. This concept will be discussed in more detail
later.
The experiments comprising the DOE are run in
random order to minimize systematic error that can
lead to the wrong conclusions. As an example,
assume that a processing experiment is being run
with two different raw materials. On the first day, all
the experiments are processed using resin A. On the
second day, the same experiments are run using resin
B. If something happened to the dryer, heater bands
are burnt out on the extruder, the extruder or feed
throat cooling is not operating properly, or the takeoff
equipment temperatures are higher the second day
and the malfunction or discrepancy is not noticed, the
results might indicate that there is a difference
between resin A and resin B. If the experiments had
been run in random order with some of resins A and
B processed on both days, the conclusions from the
DOE might be quite different.
This previous example raises a control question.
Before doing any experimentation, verify that all
components in the extrusion system are operating
properly. The temperature controllers, heaters, ther-
mocouples, and cooling in the various extruder zones
must be operating properly. Temperature controllers,
heaters, and cooling associated with the downstream
equipment must be operating correctly. After all
experimentation is complete, you do not want to have
to apologize for the data because something
mechanical malfunctioned. DOEs require significant
time and effort to do properly, but the results are very
rewarding, assuming that everything is operating
properly during the experimental phase.
Independent variables or factors are either fixed or
manipulated during the experimentation. Fixed
variables are not changed in the experimental design;
these can be the extruder, downstream equipment,
raw materials, environmental temperature, feeders
used for additives, screw design, screen pack, die
design, cooling temperature, draw ratio, and so forth.
The other approach is to manipulate the independent
variables by changing them over a specified range
that defines the experiment and the experimental
space.
E XTRUSION
25.1.3 Data Collection
The third step in the process is data collection.
Once the experiments are defined, it is time to go into
the laboratory or the production facility to execute
the experiments and collect the data. Keep in mind
that it is easier to run the experiments in a nonrandom
order. However, this may introduce inherent errors
that can lead to the wrong conclusion. Randomize the
experimental order as much as possible and do not
run all the replicates or duplicate experiments one
after the other. Collect all available processing data
during the experimental phase on both the fixed and
manipulated independent variables. Measure the
response variables for each experimental test condi-
tion or treatment combination.
25.1.4 Data Analysis
The fourth step in the DOE process is to analyze
the data. There are good computer programs avail-
able to do this. Computer programs predict which
independent factors and interactions are significant
(have an important effect) for a particular response,
generate models to predict the dependent response at
any experimental point or composition within the
experimental matrix, plot the model equations to
provide a visual comparison of the data, predict the
experimental process condition or composition
where the response is maximum, and predict or
define an experimental operating range or composi-
tion where the properties meet the specifications or
desired values. If the experimental design is for
optimizing five different properties, one may define
an experimental operating range where four of the
criteria meet the goal but not all five. Possibly only
two out of the five response variables can be opti-
mized at a given set of processing conditions. The
five properties can be weighted to define a processing
region that maximizes the properties in the order of
importance. In other words, an operating range is
defined where properties 1 and 4 are maximum, 2 and
5 are slightly below their maximum value, and
property 3 is average. The operating conditions to
obtain this were selected on the basis that properties 1
and 4 are the most important, followed by 2 and 5,
and then 3.
Conclusions are based on statistical analysis and
confidence levels. Statistics cannot prove that a factor
has an effect, but they do verify reliability and test
validity. The confidence limit determines a particular
factor has an effect based on a specific level of
25: D ESIGN OF E XPERIMENTS
confidence. Most computer programs use a 95%
confidence limit as a means of saying a particular
factor has a significant effect. The confidence level
can be manually varied if desired. However, 95% is
a good confidence limit when determining which
factors or interactions have an effect.
Some computer programs to set up DOE designs
and analyze the data are Design Expert by Stat-Ease,
Inc. [1], Statgraphics Plus [2], S-Matrix [3], JMP [4],
and MiniTab [5].
25.1.5 Report Conclusions
The fifth and final step in a good DOE is to report
the conclusions. Results generated but never reported
or summarized did not happen. Without a summary
report, the work will probably be repeated in the
future because people will not remember that the
work was done or the results were generated. With
turnover in personnel, not only is the work forgotten
but the people who did the work also may have
moved on to different jobs. If the work is important
enough to do, it is important enough to write a report
and take credit for a job that is well done.
25.2 Experimental Design
There are three experimental designs: mixture
experiments, factorial design, and response surface.
Each design is used in specific situations to gather
information from a particular set of independent
variables. Mixture designs are used to optimize
formulations where the independent variables are
ingredients of a mixture or recipe. Formulation
optimization is based on measuring property perfor-
mance (dependent variables or responses) over
different compositions. Typical plastic or polymer
formulation optimization includes the following:

Selecting the correct additive level to provide
the optimum performance profile for heat, UV
stability, or oxidative stability

Evaluating the best filler concentration in one or
more polymers

Identifying the optimum polymer ratio in blends
and alloys

Determining optimum reinforcement and/or
filler levels

Optimizing an existing formulation for physical
properties and cost effectiveness
295
Factorial design is used to screen process and/or
product variables to determine which factors are
significant in controlling the process. Normally,
factorial designs are two-level designs, meaning a high
and low value for each factor is used to determine
whether an effect is present. Fractional factorial
designs reduce the experimentation required and also
decrease the information that can be obtained about
potential interactions between independent variables
in the experimental space. As the independent vari-
ables increase, the experiments required to understand
which factors and interactions are significant increase.
Response surface designs are used after several
independent variables have been identified and one
wants a better description of their curvature and
interactions in the experimental space. Response
surface experiments, unlike factorial design, show
curvature. A response surface is a geometric repre-
sentation obtained when a response variable is plotted
as a function of one or more quantitative independent
factors. The results are graphed in two or three
dimensions, showing the response as a function of the
independent factors of interest. Response surfaces
typically replace three-level factorial designs (three-
level factorials contain a low, high, and center value for
each independent variable), because fewer experi-
ments are required to obtain the same information.
Mixture experiments are a special response surface
experiment.
Some terms used in design of experiments are
defined below:

The statistical model is a model based on the
dependent responses or variables. The model is
based on observations and measurement error.

Observation is the data obtained from the
dependent responses for each set of independent
variables evaluated.

Data are characterized by mathematical terms;
five terms are as follows:
e mean or average
e range
e standard deviation
e median
e coefficient of variance
The mean is the average value and is defined by
Eqn (25.1):
Pn
Xi
i1
X ¼ (25.1)
n
296 E XTRUSION

where
Experimental space (factor space) is the region

defined by the high and low levels for the inde-
xi ¼ Response value pendent factors in an experiment.
n ¼ The number of x values
Interactions occur when the response is different
depending on the settings of two factors. Graphs
The range is the difference between the maximum of response y versus independent variable A at
and minimum response values. the high and low levels of B will appear with
The sample standard deviation (s), given by two nonparallel lines, indicating that the effect
Eqn (25.2), measures the variability within a given of one factor depends on the level of the other.
data set:
Duplicate tests or replications are when an
vffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
uP entire experimental trial or treatment combina-
un  2
u Xi  X tion with the same independent factor levels is
t
s ¼ i1 (25.2) repeated one or more times to determine the
n1 inherent error in the various tests.

Degrees of freedom is the number of indepen-
The median is the middle value in a group of dent comparisons available to estimate a param-
samples. The coefficient of variance is a percentage, eter. It is usually the number of model
given by Eqn (25.3): parameters minus 1 or the number of free
s choices to estimate a parameter.
COV or CV ¼  100 (25.3)
Error comes from either assignable causes or
X random causes. Assignable causes are variations
due to changes in the independent factors that

Experimental design (layout) lists the experi-
are known and can be identified during the
mental trials or treatment combinations. The
experimentation phase. Random errors are
design shows the randomization, replication,
uncontrolled variations that are inherent in the
and independent factor levels within the design.
measurement techniques and the test methods.

Effect is the difference in the average response
These are unexplained errors that prevent
between two different levels of a given factor
responses from a similar set of experiments
or between two experimental runs. A positive
from producing identical results each time the
effect, shown in Figure 25.1, increases as the
experiment is run.

Analysis of variance (ANOVA) is a mathematical
procedure to compare the response data with the
ffect error data to determine whether an independent
ive e
Posit variable or interactions are significant. When
Property

No effect analyzing a DOE, ANOVA uses the sum of

Nega
squares to compare effects with the error vari-
tive e ance to determine statistical significance.
ffect

The F test is used to test for significance of
factors and interactions at a given probability
–A Factor +A
level. The F test is based on a sampling distribu-
Figure 25.1 Effect definition. tion that predicts whether the results are signifi-
cant at a given probability level, based on
a sample variance. At a predefined confidence
independent factor changes from its low to level (75%, 90%, 95%, 99%, and so forth), the
high value. A negative effect decreases as the F test predicts the probability that the F statistic
independent factor increases from its minimum is greater than the F value in an F value table. If
to maximum value. the F value is greater than the value in the table

Factor effect is the average response for an inde- at a given probability level, the independent
pendent factor at its high value compared to the factor and/or interaction from which the F test
average response for the same factor at its low is calculated is deemed to have a significant
value. effect on the response.
25: D ESIGN OF E XPERIMENTS

Model is an empirical mathematical expression
that describes the response variable in terms of
the independent variables and their interactions
within the experimental matrix. Typically,
models are linear, quadratic, or cubic. The
number of experimental trials in the design
must exceed the number of terms in the model
for the model to predict the response at any other
point within the experimental matrix. A linear
response surface model is a combination of
independent factors given by Eqn (25.4):
Yi ¼ C þ Ca A þ Cb B þ Cc C þ . (25.4)
where
Yi ¼ Dependent response variable
C ¼ Constant
Ca ¼ Factor for independent variable A
Cb ¼ Factor for independent variable B
Cc ¼ Factor for independent variable C
If more than three independent factors are evalu-
ated, the final model can have as many terms plus the
constant as there are independent variables being
studied.
A quadratic model used to define the response
surface is given by Eqn (25.5):
Yi ¼ C þ Linear Terms þ Cab AB þ Cac AC
þ Cac BC þ . þ Ca2 A2 þ Cb2 B2 þ Cc2 C 2
þ.
(25.5)
where the linear terms are those in the linear model;
AC, AB, BC, . represent the potential two-factor
interactions; and A2, B2, C2, . represent the potential
square terms.
A cubic model for a response surface series of
experiments is given by Eqn (25.6):
Yi ¼ C þ Linear and Quadratic Terms þ Cabc ABC
þ . þ Ca2b A2 B þ Ca2c A2 C þ Cb2c B2 C þ .
þ Ca3 A3 þ Cb3 B3 þ Cc3 C 3 þ .
(25.6)
In response surface experiments, the quadratic
model will fit approximately 95% of all problems.
297
Table 25.1 Degree and Description for Mixture
Models
Degree Description
Linear ABC.
Quadratic AB, AC, BC .
Special cubic ABC .
Cubic AB(AB) þ AC(AC)
.
In mixture experiments, the degree of the model
indicates the presence of certain terms. Table 25.1
shows the degree and model description for linear,
quadratic, special cubic, and cubic models.
Mixture experiments are unique, as the sum of all
components equals 100%. This imparts special
restrictions on the experimental points and formula-
tions. Taking the high and low values for the exper-
imental design points does not work, because the
combination of these values must add to 100%. In
most mixture experiments, a degree 2-quadratic or
degree 3-special cubic model fits most of the data. In
data analysis, always use the highest order model
(model with the most terms) that is statistically
significant. Never use a model with more terms than
the number of experiments in the design matrix or
evaluated during the experimental phase of the DOE.
Typical mixture designs are Simplex-Lattice,
Simplex-Centroid, and Simplex Augmentation.
Terms appearing in the computer analysis are as
follows:

Residuals refer to experimental error.

ANOVA is the analysis of variance.

Mean square is the sum of the squares for the
model divided by the degrees of freedom.

Root MSE or root mean square is the square root
of the mean square, which is the standard
deviation.

R2 is the correlation coefficient. The closer the
R2 is to 1, the better the model predicts the
response behavior.

Pure error is the error expected in a response
value if the experiment is completely rerun as
a replicate.
To determine if a difference in measured responses
is a true measure of a difference in the process, the
data are analyzed using an ANOVA. Analysis of
variance is a mathematical method that uses statis-
tical tools to take into account the data and the errors.
298 E XTRUSION

It gives you an understanding of what is a relevant
difference versus a difference in data caused by errors
through the use of an F test. The F test allows you to
determine the significance of an independent variable
on some dependent response at a specific confidence
interval, such as 75%, 90%, 95%, or 99% confidence
limits. If the F value calculated in the ANOVA is
greater than the value in the F tables, the independent
factor or interaction is deemed to be significant at that
probability or confidence limit [6].
The math for calculating an ANOVA is beyond the
scope of this book. An effective way to calculate an
ANOVA is to use one of the computerized statistical
analysis programs.
As an example, assume that four materials are
being compared for flow through a specific die under
a fixed set of processing conditions. The four resins
are designated as A, B, C, and D. Flow is critical to
obtain the proper molecular orientation in the profile
and surface aesthetics in the final part. The
management is going to purchase one of these four
materials, based on the die flow evaluation. The costs
of the four resins vary slightly, with A being $1.63/lb,
B being $1.78/lb, C being $1.68/lb, and D costing
$1.72/lb. Four flow rates are measured for each resin,
using the same processing conditions, and are given
in Table 25.2 in units of lb/h. Based on the results,
what material do you recommend to management for
purchase and why?
Table 25.2 Experimental Data on Resin Flow
Resin Run 1 Run 2 Run 3 Run 4
A 23.3 19.7 25.9 24.4
B 25.9 25.8 34.3 30.5
C 18.3 28.4 26.4 25.8
D 23.3 32.8 26.7 26.9
The following output was generated with Mini-
TabÔ v. 13.3. From this output, one sees that the F
value is 1.86, which gives a p value of 0.191. This
means that there is an 80.9% chance that there is
a significant difference in the data. The F value for
95% confidence can be looked up in an F distribution
table for resin with three degrees of freedom, error at
12 degrees of freedom, and 95% confidence limit.
The F value is 3.49 (Fm1, m2a ¼ F3, 12, 0.05 ¼ 3.49). If
the F value from the MiniTabÔ output is >3.49, then
there would be a 95% chance that there is a difference
in the data. Along with the calculations, MiniTabÔ
provides a graphical output showing the four resins,
their averages, standard deviations, and a bar graph
with the averages and 95% confidence interval. From
the numbers and observing the bar chart, one can see
that the confidence intervals overlap, which means
there is no difference in flow. In this case, one would
buy the cheapest resin.
However, let us assume that you see the large
variability in the flow data for each resin and decide
to look into the matter. On careful examination, you
find some transcribing errors and some calculation
errors. The revised data are presented in Table 25.3
with the corrected data highlighted in bold.
The following revised output (see the next page)
was generated with MiniTabÔ v. 13.3. From this
output, one sees that the F value is now 22.53 with a p
value of 0.000. This means that there is almost a 100%
chance that there is a significant difference in the data.
Looking at the averages and the bar chart, now we see
that resin B has a statistically significant higher flow
than the other three resins. Even though resin B is
9.2% more expensive than the lowest cost resin, it has
a 41.6% higher flow. Thus, one has a case for rec-
ommending resin B because of its higher productivity.
One-way ANOVA: Flow versus Resin

Analysis of Variance for Flow

Source DF SS MS F p
Resin 3 81.9 27.3 1.86 0.191
Error 12 176.5 14.7
Total 15 258.5
Individual 95% CIs For Mean
Based on Pooled StDev
Level N Mean StDev –––––+–––––––––+–––––––––+–––––––––+–
A 4 23.325 2.641 (–––––––––*–––––––––)
B 4 29.125 4.088 (–––––––––*–––––––––)
C 4 24.725 4.425 (–––––––––*–––––––––)
D 4 27.425 3.946 (–––––––––*–––––––––)
–––––+–––––––––+–––––––––+–––––––––+–
Pooled StDev = 3.835 20.0 24.0 28.0 32.0
25: D ESIGN OF E XPERIMENTS 299

One-way ANOVA: Flow 2 versus Resin

Analysis of Variance for Flow 2

Source DF SS MS F p
Resin 3 198.74 66.25 22.53 0.000
Error 12 35.29 2.94
Total 15 234.03
Individual 95% CIs For Mean
Based on Pooled StDev
Level N Mean StDev –––––+–––––––––+–––––––––+–––––––––+–
A 4 24.025 1.473 (–––––*–––––)
B 4 33.350 2.261 (–––––*–––––)
C 4 27.225 1.323 (–––––*–––––)
D 4 25.675 1.654 (–––––*–––––)
–––––+–––––––––+–––––––––+–––––––––+–
Pooled StDev = 1.715 24.0 28.0 32.0 36.0

Table 25.3 Revised Resin Flow Data

thick, extruded on a single screw extruder using
Resin Run 1 Run 2 Run 3 Run 4 a three-roll stack and a flexible lip die. An under-
A 23.3 22.5 25.9 24.4 standing of how processing conditions affect product
B 35.9 32.8 34.3 30.5 properties is desired. The processing conditions
(independent variables) being evaluated are through-
C 28.3 28.4 26.4 25.8
put rate, screw speed, barrel temperature, die lip
D 23.3 25.8 26.7 26.9 opening, and roll temperatures. Physical properties
Corrected data in bold.
and process parameters (response variables) being
measured are color, gloss, impact, tensile properties in
both the machine and transverse directions, melt
The above example shows an ANOVA analysis
temperature, torque, and die pressure. What is the
and how to interpret the results. When doing DOE
best procedure to optimize the process? A factorial
experiments, the ANOVA is performed by the
design provides a systematic approach to determine
computer program. The same computer programs set
which experimental factors and interactions are
up the experimental design and do the math neces-
significant in controlling the different responses being
sary to generate the equations and models. To
evaluated.
summarize the procedure, to do DOE experiments in
The first step is to define the experimental range
extrusion, define the problem, establish the experi-
for each dependent variable. Let us choose the
mental limits, run the experiments, input the depen-
following processing limits:
dent responses into the program to analyze the data,
and interpret the results.

Throughput rate: 200e300 lb/h

Screw speed: 250e400 rpm
25.3 Experiments
Barrel temperatures: High and low temperature
profile
The last section in this chapter sets up some
Die lip opening: 0.125e0.250 in. (3.2e6.4 mm)
experimental design examples for different DOE
Roll temperatures: 125e175  F (52e79  C)
experiments.
Using a full factorial design to identify all the
25.3.1 Factorial Design significant effects and interactions, there are 2k
Factorial experiments are used to screen many experiments, where k is the number of independent
independent variables to determine what independent variables. For five independent variables, there are
factors are significant in controlling the performance 25 or 32 experiments. Fractional factorial designs
of various response variables being evaluated. As an require less experimentation but do not define all the
example, consider a plastic sheet 0.125 in. (3.2 mm) interactions that can be present. A 1/2 factorial with
300 E XTRUSION

five independent variables requires 16 experiments,
while a 1/4 factorial requires eight experiments. In
laying out full factorial experiments, the high and
low values for each independent factor are combined
with the high and low values of all other
independent variables. To set up the experiments
using a full factorial design, generate a table with
a column for each factor. In the first column, insert
the high independent factor value in the first n/2
(where n ¼ 2k) rows and the value for the low

Table 25.4 Full Factorial Experiments for Five Factor Examples

Throughput, Screw Speed, Barrel Die Lip, Roll Temperature,

Experiment
lb/h rpm Temperature,  F in. 
F
1 300 400 Hi 0.250 175
2 300 400 Hi 0.250 125
3 300 400 Hi 0.125 175
4 300 400 Hi 0.125 125
5 300 400 Lo 0.250 175
6 300 400 Lo 0.250 125
7 300 400 Lo 0.125 175
8 300 400 Lo 0.125 125
9 300 250 Hi 0.250 175
10 300 250 Hi 0.250 125
11 300 250 Hi 0.125 175
12 300 250 Hi 0.125 125
13 300 250 Lo 0.250 175
14 300 250 Lo 0.250 125
15 300 250 Lo 0.125 175
16 300 250 Lo 0.125 125
17 200 400 Hi 0.250 175
18 200 400 Hi 0.250 125
19 200 400 Hi 0.125 175
20 200 400 Hi 0.125 125
21 200 400 Lo 0.250 175
22 200 400 Lo 0.250 125
23 200 400 Lo 0.125 175
24 200 400 Lo 0.125 125
25 200 250 Hi 0.250 175
26 200 250 Hi 0.250 125
27 200 250 Hi 0.125 175
28 200 250 Hi 0.125 125
29 200 250 Lo 0.250 175
30 200 250 Lo 0.250 125
31 200 250 Lo 0.125 175
32 200 250 Lo 0.125 125
25: D ESIGN OF E XPERIMENTS
independent factor in the second set of n/2 rows. For
the second independent factor, set the first n/4 rows
at the high value, the second n/4 rows at the low
value, the third n/4 rows at the high value, and the
final n/4 rows at the low value. The same procedure
is followed with the third column, except that the
first n/8 rows contain the high value and the next n/8
rows contain the low value, and so forth, until the
column is full. The fourth factor is treated the same
way, except that the number of rows alternated is
n/16. The fifth factor rows alternate every other row,
with one being the high value and the other low, or
n/32 rows with the high value followed by n/32 rows
with the low value.
This procedure produces all possible combinations
of maximum and minimum values.
Table 25.4 contains the 32 experiments for the
full factorial design to screen the five independent
processing factors. Response variables are collected
for all 32 experiments or treatment combinations.
The response model contains the main effects plus
all the interactions. Factorials or screening experi-
ments are used to screen many variables to deter-
mine which factors and interactions are significant.
Fractional factorials are used to determine which
main effects are important and the effect of some
interactions, while minimizing the number of
experiments. Fractional factorials are normally one
of the first steps in an evaluation procedure. The
important variables can be identified and then
evaluated in more detail. After screening experi-
ments are completed, the next step is to take the
significant factors (hopefully a smaller set of
independent variables) and perform a response
surface DOE to define the optimum processing
conditions, or complete a factorial design with
a center point and replicate experiments. Qualitative
variablesdsuch as the barrel temperature in the
example, are high or low, on or off, and yes or
nodcan be used in factorial design but not in
response surface designs.
25.3.2 Response Surface
A response surface is a geometrical representation
of a response variable plotted as a function of the
independent variables. This experiment provides
more information about a dependent or response
variable than a two-level factorial or frac-
tionalefactorial design. A three-level factorial design
has a center point included for each independent
301
variable along with the high and low points, requiring
three experiments for each independent variable.
This is called a three-level factorial design because of
the third factor level. Inclusion of the third factor
greatly increases the number of experiments. In the
previous factorial design with five variables, there are
2k or 25 ¼ 32 experiments. The same independent
factors using a three-level factorial design has 3k or
35 ¼ 243 experiments. Qualitative variables with
only two levels (high/low, on/off, yes/no) cannot be
used in a three-level factorial design.
A three-level, two-factor design with 32 or 9
experiments is shown in Table 25.5, with the high and
low values for factors A and B being represented as 1
and 1, and the middle value as 0.
As three-level factorial designs generate large
treatment combinations or experimental points,
alternate response surface designs were developed to
reduce the number of experiments required while
providing similar information. Response surface
analysis generates models that are used to plot
contours in one or two dimensions, depending on the
factors used to describe the response variable
throughout the experimental space. The experiments
in response surface designs are special cases of
factorial design that include center points in the
experimental space plus edge center points or face
center points. The multilevel experimental points
allow fitting the responses to quadratic or cubic
equations, which provides a better model of the
response variable in the experimental space. Designs
that are more practical than the three-level factorial
designs are Central Composite and Box Behnken
designs.
Table 25.5 Three-Level, Two-Factor Factorial
Design
Experiment Factor A Factor B
1 1 1
2 1 0
3 1 1
4 0 1
5 0 0
6 0 1
7 1 1
8 1 0
9 1 1
302
The Central Composite design is based on a two-
level factorial design with the addition of 2k (k is
the number of independent variables) points (star
points) between the axes plus repeat points at the
centroid. As with all good experimental designs,
the experiments are randomized. Consider an
example similar to that used for the factorial
design, with the exception that the variables are as
follows:

Screw speed (250e400 rpm)

Throughput (200e300 lb/h)

Die lip opening (0.125e0.250 in. [3.2e6.4 mm])
What are the experiments and what is the
appearance of the experimental space? Figure 25.2
Star points
In plane Out of plane
Experimental points in the experimental space
Figure 25.2 Central Composite design with star
points.
shows the experimental space for a three-factor
Central Composite design. Depending on the
design, the star points or the center points in each
face may extend out past the face, as shown in
Figure 25.2. In most plastic or extrusion designs,
the star points have to be located in the plane with
the other coordinate points (shown in the left-hand
drawing of Figure 25.2), because star points
outside the plane may not be practical processing
conditions. In the current example, high values
associated with the star points on the throughput
may exceed the torque or screw speed limitations
of the equipment; the very high screw speed
would be about 450 rpm. In any design, all
experimental points must be physically possible to
process.
The other common response surface design is
a Box Behnken design, where the experimental
points are located at the center points of the edges
(Figure 25.3). The centroid or center point of the
E XTRUSION
Centroid
Figure 25.3 Box Behnken design.
experimental space is replicated. A full three-level
factorial design with three independent variables
requires 3k experiments or 33 ¼ 27 experiments
(Figure 25.4). In addition to the high and low
Figure 25.4 Three-level factorial.
experimental values, the three-level factorial design
includes center points on each edge, the center point
of each face, and the center point plus replications to
determine experimental error. A three-level factorial
design to obtain similar information as a Central
Composite or Box Behnken design contains 32
experiments.
Using the example to determine the effect of
screw speed, throughput, and die lip opening on
physical properties, the randomized experimental
layout for the three designs is given in Tables
25.6e25.9, with Tables 25.6 and 25.7 showing
Central Composite design with the star points in
and out of the plane, corresponding to the left- and
right-hand schematics in Figure 25.2. Table 25.8
provides a Box Behnken design, and Table 25.9
shows the three-level factorial design. In Table
25.7, the star points that are not within the plane
represent experiments 3, 4, 6, 9, 13, and 16;
experiment 4, making a 0.125-in.-thick sheet
product with a 0.08-in. die opening, is probably
impossible to achieve. Experiment 9, requiring
250 lb/h throughput rate with a 199-rpm screw
speed, may be impossible to run without torqueing
25: D ESIGN OF E XPERIMENTS 303

Table 25.6 Central Composite Design with Star Points in the Plane

Experiment Screw Speed, rpm Throughput, lb/h Die Opening, in.

1 325 250 0.25
2 250 300 0.12
3 400 300 0.25
4 250 250 0.19
5 400 200 0.25
6 325 250 0.19
7 325 250 0.19
8 325 200 0.19
9 250 300 0.25
10 325 250 0.19
11 250 200 0.25
12 325 300 0.19
13 325 250 0.19
14 400 250 0.19
15 325 250 0.19
16 325 250 0.19
17 400 200 0.12
18 400 300 0.12
19 250 200 0.12
20 325 250 0.12

out the extruder. Experiment 6, with a 451-rpm
screw speed, may exceed the extruder screw speed
capabilities. The die opening in experiment 13 may
be too large to draw down the sheet to 0.125-in.
thickness without excessive molecular orientation
or necking in the sheet. Central Composite exper-
iments laid out in Table 25.6 are more practical to
use for the experimental design. The center points
repeated in Table 25.6 are experiments 6, 7, 10, 13,
and 16. Table 25.8 shows the experimental points
using a Box Behnken design which has 17
experiments versus 20 required for the Central
Composite designs. As with the other designs, the
experimental order is randomized, and the center
point is repeated, experiments 2, 5, 10, 13, and 17.
Table 25.9 shows the experimental points with
a three-level factorial design with the center point
replicated six times in experiments 4, 8, 13, 19, 21,
and 31. The advantage of using either the Central
Composite or Box Behnken designs to generate
response surfaces is that fewer experiments are
required.
Using either the Central Composite or Box
Behnken design to fit a cubic model requires more
experimentation so that there is at least one
experiment for each term in the model. Since
quadratic models fit 95% of all experimental
designs, starting with a quadratic model makes
sense. Additional experiments can be added later if
a higher order model is required to predict the
responses.
25.3.3 Mixture Experiments
Mixture experiments are used when experiment-
ing with composition ingredients. Typical uses
include the following:

Formulation optimization and optimizing prop-
erty profiles with different additive levels
304 E XTRUSION

Table 25.7 Central Composite Design with Star Points Outside the Plane

Experiment Screw Speed, rpm Throughput, lb/h Die Opening, in.

1 325 250 0.19
2 325 250 0.19
3 325 334 0.19
4 325 250 0.08
5 325 250 0.19
6 451 250 0.19
7 400 200 0.25
8 325 250 0.19
9 199 250 0.19
10 250 300 0.25
11 325 250 0.19
12 250 200 0.12
13 325 250 0.29
14 400 200 0.12
15 250 300 0.12
16 325 166 0.19
17 325 250 0.19
18 400 300 0.12
19 250 200 0.25
20 400 300 0.25

Combinations of different resins in alloys or
blends

Determination of impact modifier concentrations

Flame retardant formulation optimization

Effect of filler and/or reinforcement concentrations

Effect of regrind levels
Experimental responses include the following:
you want to understand the proper proportions of
each ingredient to optimize tensile strength, flexural
modulus, and impact strength. The experimental
limits are defined as follows:

D is present from 38% to 72%.

E ¼ 5%e85%.

Talc ¼ 10%e55%.

Physical properties What experiments are required to establish the

Cost property profiles at any composition within the

Flame retardance design matrix, and what is the appearance of the

Chemical resistance experimental space?

UV stability Figure 25.5 shows the experimental space for

Thermal stability a mixture experiment with three variables. Trian-

Dimensional stability gular coordinates are used to satisfy the mixture
constraint, which requires all components to add to
As an example of a mixture experiment, assume 100% for each experimental condition. Any point
that resin D, resin E, and talc are being mixed, and within the experimental matrix in Figure 25.5
25: D ESIGN OF E XPERIMENTS 305

Table 25.8 Box Behnken Design

Experiment Screw Speed, rpm Throughput, lb/h Die Opening, in.

1 400 300 0.19
2 325 250 0.19
3 400 250 0.12
4 400 200 0.19
5 325 250 0.19
6 250 250 0.25
7 400 250 0.25
8 325 200 0.12
9 250 200 0.19
10 325 250 0.19
11 325 200 0.25
12 325 300 0.12
13 325 250 0.19
14 325 250 0.19
15 250 250 0.12
16 325 300 0.25
17 325 250 0.19

totals to 100%. The horizontal axis starting at the
bottom of the triangle is 0% talc, with each
horizontal line representing a 10% change until the
apex is reached at 100% talc. The other axes are
interpreted in the same manner. Consequently, any
point in the experimental space is a combina-
tion of the three components. Using the three-
component coordinate space in the mixture example,
the experimental space is defined by the limits shown
in Figure 25.6. Combinations of independent
factors to define the response variables within
the experimental space are the vertices, the mid-
points of long edges, the centroid, and a check-
point. With the duplicate experiments included
to define the experimental error, the coordinates
of the experimental compositions are given in
Table 25.10. Thirteen experiments provide sufficient
data to generate models and response curves
to predict the dependent response at any compo-
sition within the experimental limits. Experiments
1 and 2, 4 and 8, 5 and 13, and 8 and 12 are
repeated experiments used to determine experimental
error.
Once the dependent responses are determined and
models are generated, a processing or compositional
window can be defined where the dependent
responses are better. In most situations, it is
a compromise, because all response variables or, in
this case, physical properties are not normally
maximized at the same compositional or processing
point. Optimization of one dependent response may
be at a completely different location within the
experimental space compared to the maximum for
the next dependent response. A decision is required
to determine where the best property balance is
obtained within the experimental matrix. If
a composition is selected where all the responses are
not at their maximum value, does the compromise
meet the customer requirements?
In any factorial, response surface, or mixture
experiment, once the optimum combination of pro-
cessing conditions or compositional ingredients is
chosen based on a predicted response, additional
experimentation is needed to verify the predictions
and verify the response profile predicted is routinely
attainable in practice.
306 E XTRUSION

Table 25.9 Three-Level Factorial Design

Experiment Screw Speed, rpm Throughput, lb/h Die Opening, in.

1 250 200 0.12
2 250 250 0.25
3 400 250 0.19
4 325 250 0.19
5 400 200 0.12
6 400 300 0.12
7 400 250 0.25
8 325 250 0.19
9 325 250 0.25
10 400 200 0.19
11 325 200 0.12
12 250 300 0.25
13 325 250 0.19
14 250 300 0.12
15 325 200 0.25
16 250 250 0.19
17 250 200 0.19
18 325 300 0.25
19 325 250 0.19
20 325 300 0.19
21 325 250 0.19
22 250 300 0.19
23 400 300 0.19
24 250 250 0.12
25 400 200 0.25
26 325 200 0.19
27 250 200 0.25
28 325 250 0.12
29 325 300 0.12
30 400 250 0.12
31 325 250 0.19
32 400 300 0.25
25: D ESIGN OF E XPERIMENTS 307

Talc = 100% Table 25.10 Mixture Experiment Example

Experimental point is
40% Talc, 30% Resin E, Talc, Resin Resin
and 30% Resin D Experiment
% E, % D, %
1 32.5 29.5 38.0
2 32.5 29.5 38.0
%

Re
=0

s
3 10.0 35.0 55.0

in
E

D
in

=0
4 10.0 52.0 38.0
s
Re

%
5 10.0 18.0 72.0
6 30.6 17.4 52.0
Re
s

0%
in

7 39.0 5.0 56.0

D

10
=1

8 55.0 7.0 38.0

E=
Talc = 0%
00

sin
%

Re 9 10.0 52.0 38.0

10 20.3 34.7 45.0
Figure 25.5 Experimental coordinates for a three-
11 23.0 5.0 72.0
component mixture experiment.
12 55.0 7.0 38.0
13 10.0 18.0 72.0
5
E=

Talc
sin
Re

Re
sin
D=
38

Talc=55
References
X [1] Design Expert. Stat-Ease, Inc., 2021 E. Hennepin
Re
sin

Avenue, Minneapolis, MN.

85
Ex

X
D=

E=
pe

[2] Statgraphics Plus. Manugistics, Inc., 2115 East

72

X
sin
rim

X Jefferson Street, Rockville, MD.

sp

Re

X
en

X
ac

Talc=10 [3] CARD. S-Matrix Corporation, 317 Third Street,

tal
e

X X X Suite 5, Eureka, CA.

Re

[4] JMP. SAS Institute, Inc., SAS Campus Drive,

E
sin

sin
D

Cary, NC.
Re

[5] MiniTab. MiniTab, Inc., State College, PA.

Figure 25.6 Mixture experiment exampled [6] H.F. Giles, SPE Plastics Technician’s Toolbox,
composition points and definition experimental Society of Plastics Engineers, Brookfield, CT,
space. 2002 (Chapter 1) 50.
308 E XTRUSION

Review Questions
1. What is the definition of experimental space?
2. What are three experimental designs and where is each used?
3. Why use a DOE?
4. Where should DOE experiments be used and where are they inappropriate?
5. What are the five steps in doing a DOE? What is the objective of each step?
6. What is the difference between independent and dependent variables? Give some examples in
extrusion applications.
7. What is the difference between an independent variable and a factor?
8. Why is it critical to run experiments in random order?
9. Why is it necessary to run duplicate experiments or repetitions?
10. What is a statistical model and how is it used?
11. What are four mathematical terms describing variability, and how do they differ from one another?
12. What is the definition of an effect? What is the difference between positive, negative, and no effects?
13. Why is an F test important in DOE?
14. How is analysis of variance used in DOE?
15. In response surface experiments, what terms are included in quadratic, linear, and cubic models?
16. In mixture experiments, what is the difference between quadratic, special cubic, and cubic models?
17. What type of experimental design can use qualitative variables?
18. How many experiments are required in a full two-level factorial with six variables, in a 1/2 factorial,
and in a 1/4 factorial?
19. What is lost by doing fractional factorials?
20. What is a three-level factorial design and how many experiments are required with four independent
variables?
21. What is the difference between a Central Composite and a Box Behnken design?
22. What constraint is present in mixture experiments, and how does this affect the experimental space?
23. How are data analyzed in DOEs?