CPE 311 UNIT OPERATIONS LABORATORY I

Lab 3:

September 15

Flocculation and Filtration

Flocculation and filtration represent important unit operations for the separations of solids suspended in liquids.

Location:

EGB 67C Unit Operations Laboratory

References:

TAPPI Standard Method T-261 .

Samples:

A sample suspension will be provided for you. It contains organic fibers and a fine
particulate mineral. The approximate solid content is more than 0.5%. It must be diluted
to complete the lab.

Objectives:

After this laboratory exercise students will be able to:

Plan, set up, execute and analyze the data from a 2 3 factorial experiment.
Set up and use a dynamic drainage (Britt) jar to determine fine particle retention.
Set up and use a dynamic drainage (Britt) jar to perform fines fractionation of a
suspension.

Synopsis:

In this lab exercise, your group will use a factorial experimental design to investigate the
relationship between fine particle flocculation (retention) and three important variables:
mixing intensity, polymer concentration and mixing time. The advantages of experimental
design for reducing testing effort while maximizing insight into simple trends, interactions
between parameters and experimental error will be explored. Test will be conducted using
standard methods based on the dynamic drainage (Britt) jar.

Background:
Flocculation of fine particles is an important unit operation used for the efficient separation of suspended
solids from solutions. It is especially useful for isolating particles whose size falls into the colloidal range
with diameters, D<5 m. If sedimentation is to be used for separation, density difference between the
particle and the liquid, = (p -L), and particle diameter, D, contribute positively to the separation rate,
Vg, by Stokes law, cf. eq 1. This has important implications for the efficiency of a process.
Vg = D2 (p - 1) G / 18

eq1.

Density and liquid viscosity, , are often fixed by the material being processed. The gravitational force,
G, can be enhanced through centrifugation. One example is the Bird Screen Bowl Centrifuge (Andritz)
shown in the figure below.
Once again considering equation 1., notice that sedimentation rate of particles is determined by the square
of particle diameter. It is not difficult to determine that the separation of colloidal particles in an industrial
scale clarifier or settling tank could take weeks or months to travel to the sedimentation cake on the
bottom.

Lab 3:

Flocculation and Filtration

Figure 1

CPB 311 Fall 2015

Bird Screen Bowl Centrifuge (courtesy of Andritz)

There are additional physical forces, including Brownian (thermal) motion, that retard this rate even
further. To design for sedimentation process steps, slow rates translate to increased detention time and
storage capacity required to attain a given level of separation.
In order to enhance separation, flocculants are introduced to aggregate particles. The increased apparent
diameter effectively accelerates sedimentation by a power of 2, even though the density differential
between the aggregates and the surrounding liquid is somewhat less than for individual particles.
Flocculation may be induced using a number of chemical strategies that take advantage of the surface
charge of the particles in solution. Two common methods are: 1) charge neutralization, where electrostatic
repulsive forces are shielded so that the ever-present van der Waals attractive forces cause particles to
coagulate, and 2) the addition of charged polymers at electrostatically bind particles to form semi-rigid
flocs. The latter method offers the advantages of better control and effectiveness. This laboratory exercise
will provide you the opportunity to characterize how process variables (mixing time and turbulence) and
polymer concentration affect the performance of a commercial flocculant (also known as a retention aid
in papermaking).
The specific flocculant that you will use in this lab takes utilizes the anionic (negative) charge on the
surface of suspended particles by reacting with cationic (positive) charges that are distributed along a long
chain, high molecular weight polymer. When the chain attaches to two or more particles, these particles
are bridged together to form a cohesive floc that has some resistance to turbulent flow. If an excessive
amount of the polymer is added, then the polymer coats all of the particle surfaces and no bridging
between particles occurs. Therefore, depending on the surface chemistry of the particles, the specific
surface area exposed to the liquid, the solids concentration, and the solution chemistry, there is an optimal
concentration of flocculant additive that will maximize the flocculation of discrete particles. It is essential
that the chemical be uniformly blended into the system so that all particles are collected. However,
excessive mixing can also cause the flocs to break down. Thus, a balance between mixing time and
intensity needs to be found in order to optimize performance of a flocculant additive.

Dynamic Drainage Method

In the mid-1970s, Kenneth Britt introduced the Dynamic Drainage procedure and apparatus to allow the
rapid testing of fine particle suspension, especially the dilute stock used to make paper. The apparatus is
illustrated in Figure 2. The procedure, first adopted as a TAPPI standard method (T-261) in 1979, allows
for the characterization of flocculating agents as a dilute suspension of fine particles is mixed in turbulent
flow. The retention of fine particles, whether attached to larger fibers included in the suspension, or
Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

aggregated to one another other, is measured by doing a mass balance after the suspension is filtered
through a screen with precise hole openings. Since the screen is continually swept clean by the flow of
liquid over the surface, the standard method can also be used to determine the mass that is coarse or finer
than the screen, a process referred to as fractionation. The apparatus, known as a Dynamic Drainage Jar,
(DDJ or Britt Jar), is custom made and specifically designed for testing drainage and retention. It is most
commonly used in industry to test the performance of flocculating agents known as retention aids, as
briefly describe above. In this lab session, you will use the DDJ to test the synergistic interactions
between flocculant concentration, mixing speed (turbulent intensity), and mixing time. Performance will
be based on balance between those fines that are captured during filtration and those that remain
dispersed and pass through the filtration screen.
In dealing with multi-variable systems, experimental design is used to apply logical patterns in order to
draw valid conclusions from test array that varies each parameter. One goal is to maximize insight into
the relationships between factors and the occurrence of any trends or interdependencies that might exist,
while minimizing the required number of tests in the experiment. You should recognize the value of
experimental design as it allows you to vary several factors at a time and obtain valid results using a

Figure 2

Dynamic Drainage Jar, also known as the Britt Jar

(courtesy of Paper Research Materials Inc.)

minimal amount of time and effort to perform the experiments. In this laboratory exercise, you will use
the Factorial Design method to characterize the three variables important to drainage and retention.

Factorial Design
Factorial design is one of the more common forms of experimental design that is used to study processes
with two or more variables (factors). Two important questions to ask when setting up a factorial design
experiment are:
1) How many variables significantly influence the process? and
2) How many step differences or levels will each variable need testing?
If the answer to the second question is more than two levels than one use a general full factorial design,
which can be a bit complex. If only two levels, say low and high, are tested for each variable, then a two
level factorial design (2k design) is used. You will use this efficient design to examine the three variables
in the drainage and retention experiment in what is referred to as a two-level, three-factor factorial design
or simply 23 design.

Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

The 23 design may be easily visualized using a cubic geometry where experimental factors are located at
the vertices, see Figure 3. The three orthogonal axes, X, Y and Z, represent the three factors being tested,

Figure 3

A
Figure 4

Cubic geometry of a 23 factorial design.

Relationship between low and high levels for three factors, A, B and C.

e.g. A, B and C. Selected planes represent the level, low or high, for each variable. Figure 4a shows the
planes that represent low values (pale blue) and high values (gold) for factor A. Likewise, the low and
high planes are shown for factors B and C in in Figure 4b and 4c respectively. Proper selection of the low
and high values allows one to make predictions about the interactions between the three factors within the
boundaries of the cubic space, Fig 5, as the response for the eight corner points are determined.
Considering the plot in Fig 5, one could compare the response of low and high conditions for factor A as
the other two factors are held constant. For example, the line segment in the lower front face of the cube,
( L , L, L ) ( H , L , L ) ,

(adjacent to the arrow) compares the response for varying A as factors B and C are
held constant at low values. All other line segments that are parallel, ( L, L, H ) ( H , L, H ) ;
( L, H , L ) ( H , H , L )

; ( L, H , H ) ( H , H , H ) ; make similar comparisons of Factor A with factors B and C

held constant. Similar groups of comparisons can be made for factors B (holding A and C constant) and C

Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

Figure 5 Position of design parameters for three factors of a 2 3 factorial design.

(holding A and B constant). These single factor experiments provide simple effects of the independent
variables. This is also known as a one-factor-at-a-time treatment of the data which produces 12 plots, but
provides no 9 simplification of data analysis. An indication of the main effect of factor A can be
determined by averaging all responses within the low plane, cf. Fig 4a, and comparing with the average
value for responses in the high plane. The main effect for factors B and C can be determined in a similar
manner using respective planes shown in Figs 4b and 4c.

Analysis of Interaction
A comparison of simple effects allows the analysis of the interaction between two factors, for example A
and B while holding C constant, by using the cubic geometry. The first step is to average the high and low
values for C, shown as the ends of the vertical line segments shown in Fig 4c. This forms a square with
corners of ( L, L, C ) , ( H , L, C ) , ( L, H , C ) , ( H , H , C ) . By plotting the response, Y, for low and high A as B is
held low, and comparing this with the trend formed when B is high, one can determine the interaction
between A and B. There can be mild, strong or no interaction between variables. Figure 6 shows the
relationship between the trends for the three possible interactions that can occur. It should be obvious that
the interaction is simply characterized by the change in slope, and one can use this to quantify the
intensity of interaction, I, using the results from the equation:
I

(Y( L , H ,C ) Y( H , L ,C ) ) (Y( L , L ,C ) Y( H , H ,C ) )
2

One can see in Fig 6 that by forming a cross between the highest and lowest values of the two lines, and
comparing the midpoints of the line segments, i.e. the average values, then the distance between the two
indicates the intensity of interaction. By holding A or B constant and comparing the remaining factors, the
interaction of other factors may be calculated similarly. Note that if no interaction exists between two
variables, than it is best to compare the main effects, i.e. the average of two sets of four values, as
discussed in the preceding paragraph.

Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

Experimental Error
In experimentation, the replication of tests can be used to determine systematic and random error. The 2 3
design used in this experiment has eight corner points. An unbiased approach to determine the error
would be to repeat each corner multiple times, which would greatly increase the testing effort. If only a
selected number of points were chosen, then the results are biased by any underlying trends and
interactions between factors that might exist. An unbiased solution to this is to conduct repetitive test on
the center point of the cube. The center-point is defined as the average of the low and high values for each
factor, ( M , M , M ) , as shown in Fig 3. By repeating the center point multiple times (usually more than 5
times for this experiment) a close approximation of the expected scatter of the response values for each
point can be determined. Furthermore, if the center-point reps are distributed at intervals throughout the
experiment, an increasing or decreasing trend is an indication of an underlying systematic error.

Figure 6. Three possible results for the interaction between two factors, A and B. 6a:no
interaction; 6b mild interaction; 6c: strong interaction

Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

Figure 7. Plot of the repetition of center-point response measured at equal intervals during the experiment,
demonstrating 7a: random error only and; 7b: both random and systematic error.
Figure 7a shows the pattern of center point values plotted as a function of run order (time) which has
experimental scatter, or indeterminate error, but no systematic trend. Figure 7b illustrates both random
error and a systematic increasing trend which has an adverse effect on the results. If a systematic error
exists, one could easily apply a correction by using the equation of the line to calculate the fractional
increase or decrease from the first point and use this multiplier to adjust each measured point during the
experiment. Residual analysis of the data with respect to the systematic trend provides the random error
for the experiment. Finally, in order prevent data from the effects of a systematic trend, experimental
designs may also include randomization.

Figure 8. A cubic plot of a 23 factorial design including the position of the center point calculated from the
average of high and low values along diagonals (small green sphere) and the center-point determined
Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

experimentally from the middle values. The fact that the experimental falls below the calculated
center-point indicates that the surface has upward curvature as the factors increase.

Curvature
When testing lower and upper bounding values (low and high) for factors, no information about the
linearity of a trend can be inferred without intermediate points. If middle points were included on the
design cube, an additional 12 tests would need to be performed, one at each midway point of each line
segment. By measuring the center-point, the nature of each trend can be revealed. Departure from
linearity, or curvature, can be detected by calculating the difference between the calculated middle point
based on the average of low and high boundary values with the measured response value, ( M , M , M ) . If
this value is positive, then the measured point falls below the diagonal line and the relationship show an
upward curvature, for example cf. Fig 8. This additional information can be quite useful for characterizing
natural systems and for more improving predictive accuracy.
For additional reading on Factorial Design and the design of experiments please refer to the appendix.

Preparation for Laboratory:

In this laboratory exercise you will compare the three factors
DDJ Mixer RPM

low: 500 rpm

high: 1200 rpm

Polymer Concentration

low: 0.25 lb/t

high: 5 lb/t

(Low: 0.125 g/kg sample, high: 2.5 g/kg sample, Assuming 1t = 2000 lb)
Stirring Time after Polymer Addition

low: 5 sec

high: 1.5 min

You need to design an experimental plan that includes at least 5 middle points and randomizes the
sequence of tests according to the procedure outlined in the appendix. You should be able to present this
experimental plan before attempting to perform the lab on the day you are scheduled to.
You MUST read over the TAPPI standard method T-261, and be able to describe how to set up the DDJ
for fractionation testing. You should also be able to describe the method you will use to test fines
retention and the testing of the flocculating agent.
You will need to indicate how much of the 0.01% polymer solution will be added to the DDJ assuming
you have the proper volumes and solid contents of dilute suspension in the DDJ. READ T-261 very
carefully.

Safety:
Always think SAFETY FIRST and take care of your fellow group members. Review the MSDS sheets for
the polymer that may be found in the laboratory. You are required to use eye protection when performing
this laboratory. At the dilute concentrations of the polymer solution, and the inert nature of the
suspension, latex gloves are optional. Wipe up all spills. Waste water from these experiments may be
disposed of down the sink drain.
Be sure to clean up the apparatus, all glassware and the lab bench when you have completed the

experiment.

Experimental:

Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

Materials
A dilute suspension of fibers and fine particles will be available. You need to determine the solid content
of the suspension to the nearest 0.001% three replicates). The stock should be diluted to 0.5 wt%
according to TAPPI method T-261. A dilute solution of polymeric retention aid will be provided at a
known concentration.

Procedure
Please read the fractionation procedure of T-261 to know details of how to determine the fines content
(D<75 m) and read the Retention Procedure in T261 to understand how to characterize the three
variables, rpm, polymer concentration and mixing time. You will conduct the experiments following the
procedure adapted from the T-261 based on our laboratory need:

A. Determining total fibers and fines content: (duplicate the experiment)

1. Take a known amount of sample in an aluminum pan. Make sure you know the initial
weight of the pan. Mark the pan with a sample number. Numbering should be done in
way that you do not get confused with other groups sample.
2. Dry the pan & sample overnight in an oven at 105oC.
3. (next day) Weight the pan & sample until you get a constant weight. You have to
weigh several times to make sure you have a constant weight, indicating no remaining
moisture in the sample.
B. Determining the of fibers: (run in triplicate)
1. Take about 500 ml sample in beaker. Weigh the beaker & sample. Make sure you
know the weight of the dry beaker.
2. Prepare the Brit Jar with filter. Make sure to use the gasket.
3. Clamp the outlet tube of the jar.
4. Transfer the sample into the jar.
5. Stir the sample at 500 rpm for approximately 30 seconds.
6. Open the outlet tube after placing a beaker underneath; keep the stirrer running at the
same speed as step 5. Collect the filtrate in the beaker. You should see that the filtrate
is cloudy. The clouds are formed due the fines (small size fibers and filler materials.
Filler materials are CaCO3).
7. Clamp the outlet tube again.
8. Add about 500 ml DI water into the jar, to wash the fines in the fiber.
9. Follow step 5 &6. You should see that the filtrate is less cloudy.
10. Repeat step 7-8-5-6 until you get clear filtrate, to make sure no fines remain in with
the fiber.
4. Transfer the fibers from the Jar into an aluminum pan (Mark the pan with a sample
number. Numbering should be done in way that you do not get confused with samples
from other groups. They will use same oven.) Make sure no remaining fibers in the
jar and the filter. You may use small amount of DI water to wash out remaining fibers
in the filter and wall of the jar, if necessary. Dry the pan & sample overnight in an
oven at 105oC.
Revised: 9/7/15 by Alim Dewan

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

11. (next day) Weight the pan & sample until you get a constant weight. You have to
weigh several times to make sure you have a constant weight, indicating no remaining
moisture in the sample.
C. Determining the retention of the fines at different rpm, concentration of the
retention aid, and mixing time: (You have to run 8+5 = 13 set of experiments, ask one
of our TAs to confirm your plan and the value of the factors)
1. Take about 500 ml sample in beaker. Weigh the beaker & sample. You already know
the weight of the dry beaker.
2. Prepare the Brit Jar with filter. Make sure to use the gasket.
3. Clamp the outlet tube of the jar.
4. Transfer the sample into the jar.
5. Stir the sample at a specific rpm (as you have planned for one of your 13
experiments).
6. Add specific amount of polymer while stirring. Start the timer.
7. After adding polymer, stir for a specific period (mixing time).
8. Open the outlet tube after placing a beaker underneath; keep the stirrer running at the
same speed as step 7. Collect the filtrate in the beaker.
9. Transfer the fibers from the Jar into an aluminum pan. Make sure no remaining fibers
in the jar and the filter. You may use small amount of DI water to wash out remaining
fibers in the filter and wall of the jar, if necessary.
10. Dry the pan & sample overnight in an oven at 105oC.
11. (next day) Weight the pan & sample until you get a constant weight. You have to
weigh several times to make sure you have a constant weight, indicating no remaining
moisture in the sample.

Reporting:
Each group should write a laboratory report for this lab exercise. It should contain all of the standard
elements of a technical report. You should not replicate the experimental procedure from the TAPPI
standard. Rather, give a brief description of what was done and cite the TAPPI standard for more
details. Your report should describe all aspects of your experiment that were unique, especially your
experimental plan and those aspects that deviated from the standards.
In the results section, report any anomalies, important observations, and of course the data that you
collected. Conduct a thorough analysis of interactions, curvature and experimental error based on a 2 3
factorial design. Use plots and table where appropriate to explain results and defend your conclusion.
A considerable amount of the lab grade is based on your ability to demonstrate the logical
interpretation of the data to show the relationship between the three parameters under examination.
Specifically, the report should include:

Analysis of systematic errors in the data (Run order plots, center point plots). Apply
correction if necessary.

A complete graphical analysis including cube plot, interaction plots and other plots as needed.

Revised: 9/7/15 by Alim Dewan

10

Lab 3:

Flocculation and Filtration

CPB 311 Fall 2015

Computation of factor effects and interactions

Explanation of how factors were determined to be statistically significant or not

Development of a mathematical model from these effects (an equation relating the three
parameters)

Computation of the predicted retention under a set of conditions different from those used in
your experiment. (Within the constraints of your experimental cube)

Discussion should contain:

o

A discussion of the internal consistency of the data, i.e. does it make any sense? What
points did not fall within expectations? How did you deal with these?

A mechanistic explanation of the main factor effects and also the interaction effects.

Does your predicted value make sense?

Revised: 9/7/15 by Alim Dewan

11