Research Article 1315

Mohamed Bin Shams

Application of Statistical Design to an
Faisal Mumtaz
Ashwin Murali Industrial-Scale Dead-End Ultrafiltration
Waseem Akbar
Process
Nader Al-Bastaki

Department of Chemical
Engineering, University of
Bahrain, Isa Town, Kingdom
of Bahrain.
An industrial-scale dead-end ultrafiltration system was optimized using statisti-
cally designed experiments. Given a certain level of pollutant, a two-level full fac-
torial design and a central composite design were used to optimize the filtrate pro-
duction of a single 8-inch industrial ultrafiltration membrane while manipulating
the levels of four factors: feed pressure, backwash pressure, forward filtration time,
and backwash time. Analysis of variance and residual analysis were used to vali-
date and check the adequacy of the developed regression models. The optimal lev-
els were later validated experimentally. The predicted filtrate production was in
reasonable agreement with the experimental data.

Keywords: Factorial Design, Optimization, Ultrafiltration

Received: September 6, 2014; revised: March 19, 2015; accepted: April 24, 2015
DOI: 10.1002/ceat.201400535

1 Introduction occurs through a reduction in the membrane flux under con-

Developments in membrane technology have resulted in
increased applications in many areas. Ultrafiltration (UF)
membranes are used extensively in several industries, e.g., for
pretreatment in desalination plants, dairies, and paper pulp
mills, for industrial wastewater treatment and food processing,
and in biotechnology companies [1–4]. It has been reported by
several researchers and professionals in the field of membrane
technology that proper feed pretreatment and a well-developed
cleaning procedure are vital to ensure smooth operability
against fouling [1]. Fouling in UF systems causes the build-up
of foulant on the surface (external fouling) or in the pore struc-
ture of the membrane (internal fouling). Fouling can be further
classified into irreversible and reversible fouling based on the
extent of particle attachment to the membrane. While the for-
mer is more complex and requires chemical treatment, the lat-
ter is usually handled by mechanical means, e.g. backwashing.
A recent comprehensive review of fouling mechanisms and
cleaning of UF membranes is given by Shi et al. [1]. It has also
been emphasized that, even with the best feed pretreatment
schemes, the potential of fouling remains a significant con-
straint to the application of the membrane-based technologies
such as UF systems. UF fouling develops through several
mechanisms including adsorption, pore blocking, and cake/gel
formation. Fouling development may involve one or more
mechanisms working simultaneously. In practice, fouling
– trial applications. Chen et al. [7] used a statistical factorial de-
Correspondence: Dr. Mohamed Bin Shams (mshams@uob.edu.bh),
Department of Chemical Engineering, University of Bahrain, P.O. Box
32038, Isa Town, Kingdom of Bahrain.
stant driving force or transmembrane pressure (TMP). Never-
theless, the extent of fouling development is strongly related to
the operational parameters, feed conditions, and membrane
properties such as membrane pore size, surface porosity, and
pore morphology. Different instability mechanisms have been
proposed to re-enhance the operability of UF systems [1].
Mechanical instabilities, e.g., by using periodic backwashing,
can enhance the performance of membrane-based processes
through mitigation of reversible fouling. The productivity of
the UF system is adversely affected by the development of foul-
ing and the optimization of its operating parameters requires a
deep knowledge of the membrane fouling mechanisms. Since a
detailed understanding of the interaction between the foulant
and the membrane is usually difficult to obtain, a more practi-
cal and efficient approach is needed to rapidly optimize the
operating levels, especially of large-scale membrane systems. In
this paper, the operational parameters of an industrial-scale
dead-end filtration system are optimized using statistically
designed experiments. In a previous study, Al-Hammadi and
Al-Bastaki [5] investigated the effect of varying concentrations,
filtration/backwash cycles, and pressures on the onset and the
extent of the flux decline. In their study, the one-factor-at-a-
time (OFAT) approach was adopted. In contrast to the OFAT
experiments, factorial design significantly reduces the number
of runs required to determine the effect of a factor, especially
when the number of factors to be explored is large. More
importantly, factorial design is the only way to detect the pres-
ence of interaction between factors [6]. Different variations of
factorial designs have been successfully applied to many indus-
sign to identify significant factors and their interactions for the
chemical and physical cleaning of UF and reverse osmosis sys-
tems in municipal wastewater reclamation. Chen [8] investi-

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1316
gated the main and interaction effects affecting the decoloriza-
tion rate of methyl orange using a 25-1 fractional factorial
design and a central composite design (CCD). Cojocaru and
Trznadel [9] used response surface modeling to develop a pre-
dictive model for the optimization of copper removal using
polymer-assisted UF under different filtration modes. Shahaba-
di and Reyhani [10] investigated the main and the interaction
effects of temperature, transmembrane pressure, and cross-flow
velocity on permeate flux, fouling resistance, and total organic
carbon rejection using the PAN350 UF membrane. The analy-
sis of the 23 design revealed that temperature/transmembrane
pressure, temperature/cross-flow velocity, and transmembrane
pressure/cross-flow velocity interactions have significant effects
on the permeate flux, fouling resistance, and total organic car-
bons, respectively [10]. Through a replicated 25 factorial design,
Abdul-Wahab and Abdo [11] optimized the operating variables
of an industrial multistage flash desalination plant. Onsekizo-
glu et al. [12] used a two-level factorial design to study the
effects of the osmotic agent concentration, flow rate, and tem-
perature difference between feed and osmotic agent on the
evaporation flux and soluble solid content of apple juice
through osmotic distillation and membrane distillation pro-
cesses. Xu et al. [13] obtained mathematical expressions for the
optimum mean flow rate and filtration time for dead-end filtra-
tion using the conventional filtration theory based on Darcy’s
law. Although the obtained expressions are functions of the
physical parameters of the filtration system, usually these pa-
rameters are difficult to obtain for large-scale systems. In order
to reduce the experimental efforts, Gruschwitz et al. [14] pro-
posed a systematic framework for scaling up a dead-end filtra-
tion laboratory setup. The hourly filtrate rate and the pressure
drops were predicted over constant flow rate and constant
pressure operation modes for predetermined boundary condi-
tions, e.g., maximum/minimum pressure drops and flow rates.
The Darcy’s law-based equations showed good agreement
between predictions and experimental results. However, the ef-
fects of backwash pressure and backwash time have not been
explicitly addressed. The focus of this paper is to model and
optimize the operating conditions of an industrial-scale dead-
end UF system for a given level of foulant concentration with
the minimal number of experimental runs. The statistically de-
signed experiment is an attractive option when the relationship
between the response and the independent variables is un-
known and the interactions among the factors are thought to
be significant. For this reason, and in order to detect possible
interactions among the considered input factors, a full factorial
design and a central composite design (CCD) were applied se-
quentially.
2 Experimental
2.1 UF Setup and Solution Preparation
A schematic diagram of the dead-end UF setup under study is
shown in Fig. 1 a, and the real-scale setup is shown in Fig. 1 b.
The UF membrane is an 8-inch X-FLOW XIGA 40 hydrophilic
membrane composed of a blend of polyvinylpyrrolidone and
polyethersulfone. The membrane has an asymmetric micropo-
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Research Article
rous structure with a nominal pore size of 20 nm. The element
length is 1.5275 m. The element outer diameter is 200 mm and
the permeate collector inner diameter is 42.6 mm. The hydraul-
ic membrane diameter is 0.8 mm and the total membrane area
is 40 m2. Two centrifugal variable-speed pumps (Grundfos
Lenntech) are used to alter between the forward (filtration) and
backwash operations. The pump is equipped with a speed drive
for controlled up and down ramping.
Several pneumatic valves (Georg Fischer) are used to facili-
tate the different operation modes of the process. The quality
of the feed and the product streams are monitored online using
turbidity and pH meters. The pressures of the feed, product,
and backwash streams are monitored through pressure trans-
mitters (Endress + Hauser) while the corresponding flow rates
are monitored through magnetic flow transmitters (Endress +
Hauser). Bourdon gauges and rotameters are provided for on-
site monitoring. Measurements from all transmitters and the
operating conditions of the pumps and valves are acquired by
the Allen-Bradley programmable logic controller (PLC; Micro-
Logix 1200). The latter is connected to a supervisory control
and data acquisition (SCADA) system (RSLogix 500), which
provides full automation of the pilot plant. The sampling fre-
quency of the SCADA system was 1 s. A simulated wastewater
was synthesized using suspended AEROSIL 200. The latter is a
trade name of Degussa AG (Evonik Industries AG); the prod-
uct consists of hydrophilic fumed silica (99.8 % purity silicon
dioxide) with an average particle size of 12 nm and a specific
surface area of 200 m2g–1. The amount of silicon dioxide
(AEROSIL 200) was mixed with tap water and agitated for
about 20–30 min. Once the suspended solution was consis-
tently agitated, the system was started through the SCADA sys-
tem by entering the forward and backwash intervals, starting
the pumps and opening the required valves. The speeds of the
pumps were manually adjusted to achieve the required pres-
sures. The feed was pumped through the membrane and
directed through a series of pneumatic valves, and the filtrate
was collected in the product tank. Once the allotted forward
time had elapsed, backwashing started. During the backwash-
ing, part of the filtrate in the product tank was used to clear the
filter cake formed during the forward phase. The retentate was
fed back to the feed tank.
As mentioned above, backwashing is required to maintain
the efficiency and continuously reduce the flux decline. The lat-
ter is energy efficient compared with increasing the feed pres-
sure to prevent flux decline as a result of fouling. There are
many operating parameters (input factors) that can influence
the performance of the UF system under study, e.g., the for-
ward pressure, the backwash pressure, the forward time, the
backwash time, and the concentration of foulant in the feed
stream. In the current study, the performance of the UF system
was evaluated using the volume of the filtrate produced over a
predetermined time horizon.
2.2 Factorial Design and CCD
Factorial experimentation is an efficient procedure allowing
multiple factors to be tested at the same time without building
a detailed model based on mass, energy, or momentum balan-
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 Research Article 1317

a)

b)

Figure 1. (a) Schematic diagram of the UF setup. (b) The UF setup with its real dimensions.

ces. Factorial designs provide a systematic framework that backwash pressure, forward time, backward time) and their in-
allows the effects of several input factors (e.g. forward pressure, teractions on a response variable (e.g. filtrate) to be tested and

Chem. Eng. Technol. 2015, 38, No. 8, 1315–1326 ª 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim www.cet-journal.com
1318
statistically analyzed. In addition, factorial designs are the best
approach when interaction between factors is thought to be sig-
nificant.
Factor interaction occurs when the effect on a response due
to a change in the level of one factor from low to high depends
on the level of the other factor. Two-level factorial design (2k) is
a special case of the general factorial design. The two levels of
the input factors denoted by ‘‘high’’ and ‘‘low’’ are coded as +1
and –1, respectively. The i-th coded variable (xi) is related to its
natural variable (n) by the following equation:
n  ðnhigh þ nlow Þ=2
xi ¼
ðnhigh  nlow Þ=2
where nlow and nhigh are the original two levels of the natural
variables. A general practice is to choose the high and low lev-
els of a factor far enough so that a change in the response can
be detected, but not too far apart such that the expected operat-
ing ranges are exceeded. The use of only two levels of each fac-
tor implies that the response is linear over the range of investi-
gation; however, the assumption of linearity can be tested by
augmenting the factorial design with center points, which are
coded as 0. Center points are a replication of a certain trial in
the 2k factorial design and usually represent a known, but not
necessarily the best operating condition. Besides testing against
curvature (quadratic terms), center points provide an estimate
of the pure experimental error. If significant curvature is
detected, at least three levels of each factor are required to
model the curvature in the response function. Polynomial
equations combined with regression analysis are generally used
to summarize the results of factorial experiments. The
adequacy of the identified model is usually assessed through
the analysis of variance (ANOVA) and residual analysis [6].
When only first-order and interaction terms are considered,
the underlying model is given as follows:
X
k k X
X k
y ¼ b0 þ bi xi þ bij xi xj þ
i¼1 i¼1 j¼1
X
k X
k X
k (2)
i„j bijp xi xj xp þ::: þ e
i¼1 j¼1 p¼1
i„j„p
where k is the total number of factors, b0 is the overall mean
response, bi is the main effect coefficient for factor i = 1,2,Kk,
bij is the two-way interaction coefficient between the i-th and
j-th factors, bipj is the three-way interaction coefficient between
the i-th, j-th, and p-th factors, and e is an independently and
normally distributed component. When Eq. (2) is not adequate
in fitting the experimental data, a reasonable model that con-
siders quadratic effects can be used:
X
k X
k XX
y ¼ b0 þ bi xi þ bii xi2 þ bij xi xj þ e
i¼1 i¼1 i<j
In Eq. (3), only two-way interaction and quadratic terms are
considered. As can be seen, the fitted polynomial equations are
basically Taylor series approximations of the unknown true
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function of the response variable. The standard assumptions of
multivariable linear regression (MLR) hold: Mainly, the
uncertainty is concentrated in the response y (i.e., the filtrate
in the present work), the uncertainty in the filtrate is the
same for each combination of levels of the input factors, and
the independent variables (input factors) are perfectly known.
A three-level factorial design is required for the fitting of
Eq. (3). However, a three-level factorial design that considers
all possible level combinations requires a large number of
experiments, which in turn increases the experimentation
costs. CCD is an attractive alternative to model curvature
(quadratic terms), especially when the number of factors
(1)
under study is large. The additional points in CCD are called
axial or star points [6].
3 Results and Discussion
The objective of the current study is to systematically choose
the best attainable combination of the operating parameters of
a pilot-scale dead-end UF setup in order to maximize the fil-
trate production, given a certain level of foulant concentration.
For a pilot-scale filtration system, the volumetric operation
mode is generally preferred, at which a constant differential
pressure is maintained and the filter is regenerated whenever
the flow rate falls below a certain level [14]. Therefore, in this
study, the effects of forward pressure, backwash pressure, for-
ward time, backwash time, and their possible interaction effects
on the response variable (filtrate) were assessed.
First, the possible ranges of the four factors were identified.
The operating ranges of the feed and backwash pumps are
determined through their experimentally developed character-
istic curves and the maximum allowable pressure given by the
membrane manufacture. The ranges of the forward and back-
ward times are chosen based on a few trials such that different
degrees of flux declines are observed. In order to accelerate the
development of fouling, the UF setup was loaded with a feed
concentration of 4000 ppm of silicon dioxide. Tab. 1 shows the
natural and the corresponding coded values of the four input
factors.
Table 1. Uncoded and coded values for the factorial design
and the CCD.
Uncoded A (forward B (back- C (forward D (back-
(coded) pressure) ward pres- time) wash time)
[psi] sure) [psi] [s] [s]
High (+1) 38 26 240 90
Low (–1) 23 12 120 30
Center points (0) 31 19 180 60
Axial (+2) 46 33 300 120
(3) Axial (–2) 16 5 60 0
The experiments in this work were conducted sequentially.
That is, at the early stage of experimentation, it was hypothesized
that a full 24 factorial design would be sufficient to characterize
and model the filtrate production by using Eq. (2). Therefore, in
Chem. Eng. Technol. 2015, 38, No. 8, 1315–1326
 Research Article 1319

stage 1, the 16 runs required by the full factorial design (24) were data points) using MATLAB. Gruschwitz et al. [14] used a
conducted. The 7 center points were also conducted at this stage. similar approach to quantify the amount of filtrate. That is, for
A lack of fit was observed from the analysis of these 16 runs. a defined time period x, with n filtration and backwashing
Therefore, in stage 2, axial point experiments (three-level design) cycles, the amount of filtrate was given as:
were carried out in order to fit Eq. (3). Tab. 2 shows the design Xn
table (coded) for the factorial design and the CCD with 24 factori- Vfil;x ¼ Vi;fil  Vi;ret þ aVi;ret (4)
al experiments, 7 center points, and 8 axial points. i¼1

The filtrate was calculated numerically by integrating the for- where Vi,fil is the amount produced during the i-th forward
ward flow rate curves over an operation period of 12 min (720 cycle, Vi,ret is the portion of Vi,fil used for backwashing, and a is

Table 2. Factorial design and CCD with estimated filtrate (response).

Exp. no. Forward pressure [psi] Backwash pressure [psi] Forward time [s] Backwash time [s] Flow [L]

1 0 2 0 0 220.7

2 –1 1 –1 –1 223.6

3 1 –1 1 –1 116

4 2 0 0 0 207.7

5 0 0 0 –2 93.1

6 –1 –1 1 1 133.5

7 0 0 –2 0 185.3

8 1 1 –1 –1 258.2

9 –1 1 1 1 119.78

10 –1 –1 –1 1 133.8

11 1 –1 1 1 101.01

12 1 –1 –1 1 130.4

13 1 1 1 –1 97.5

14 1 –1 –1 –1 103.5

15 0 0 0 0 111.2

16 –1 –1 –1 –1 73.6

17 1 1 1 1 114.4

18 0 0 0 0 109.8

19 –1 1 –1 1 131.5

20 0 0 0 0 109.6

21 0 0 0 0 111.2

22 –1 1 1 –1 162.5

23 –1 –1 1 –1 61.4

24 1 1 –1 1 137.9

25 0 0 2 0 50.6

26 0 0 0 0 113.2

27 –2 0 0 0 57.61

28 0 0 0 0 110.1

29 0 0 0 0 108.6

30 0 0 0 2 75.48

31 0 –2 0 0 62.58

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1320
the fraction of Vi,ret that can be regained by secondary treat-
ment. In the current study, a is equal to 1; that is, we assume
that the backwashing is provided externally and the calculated
filtrate is the effective filtrate production. On the other hand,
the zeroth-order uncertainty [15] associated with the SCADA
readings is estimated as ±0.5 for all the acquired measure-
ments. Figs. 2 and 3 show the results from selected runs given
in Tab. 2, i.e., experiments 2 and 5.
The selected figures show two different realizations of the fil-
trate at different combinations of the input factor levels given
in Tab. 2. For example, Fig. 2 shows forward and backwash flow
rates during experiment 2. During this run, the input factor lev-
els were: forward pressure 23 psig, backwash pressure 26 psig,
forward time 120 s, and backwash time 30 s. During this ex-
periment, the total filtrate production was estimated as 223.6 L.
A constant flow can be observed before a flux decline is
started after approximately 4 min of forward operation. The
filtrate flow rate during the initial constant flow rate period is
20 L min–1. Fig. 3 shows the flow rates for different combina-
tions of factor levels (experiment 5). In the latter, the filtrate
production was only 93.1 L. Compared to experiment 2, a re-
duction of 140 % can be observed. The filtrate flow rate during
the initial constant flow rate period is 24 L min–1. The spike in
the flow rate that appears in the initial part of the filtrate flow
rate diagram is the result of a similar corresponding spike in
the pressure output (not shown here for brevity). This was a
result of the pump behavior. In actual cases, such quick onsets
of fouling and flow rate declines are avoided. Such behavior
may occur after a prolonged period of operation, which could
be several months. It may also accidentally occur if the feed
Figure 2. Flow rates during experiment 2: forward pressure = –1, backwash pressure = 1, forward time = –1, and backwash time = –1.
Filtrate production during 12 min = 223.6 L.
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concentration suddenly increases due to unexpected reasons.
For the purpose of simulation, as mentioned earlier, a very high
concentration of the foulant was used (4000 ppm) in the cur-
rent work, as a means of speeding up the onset of flux decline.
Comparing the results of experiments 5 (Fig. 3) and 2 (Fig. 2),
it is obvious that using a higher filtration pressure (31 psi) in
experiment 5 resulted in a faster onset of the flux decline com-
pared to the lower pressure (23 psi) used in experiment 2. The
onset of the flux decline in experiment 5 (Fig. 3) was at about
120 s, while the flux decline in experiment 2 started at about
150 s. The steepness of the flux decline also seems to increase
with the increased filtration pressure. Different patterns were
observed with different input level combinations. The formulas
for the calculated statistics are given in Tab. 3. Tab. 4 gives the
ANOVA table of the 24 full factorial designs.
In drawing statistical conclusions, ANOVA relies on the re-
sidual error, which consists of two components: the error due
to lack of fit and the pure experimental error (calculated from
center points). For 5 % significance level, it can be noticed form
Tab. 3 that the main effects B (backwash pressure) and C (for-
ward time) are significant with p values of 0.001 and 0.004, re-
spectively. This result implies that there is a 0.1 % chance that
the effect of changing the levels of factor B (backwash pressure)
on the filtrate production is because of random noise. The only
significant interaction was found between the backwash pres-
sure and the backwash time (B*D). Although the main effect of
the backwash time is not significant, it can be noticed that the
combined effect of the backwash pressure and the back wash
time is significant. These results agree with the previous theo-
retical findings for dead-end filtration of suspensions of fine
Chem. Eng. Technol. 2015, 38, No. 8, 1315–1326
 Research Article 1321

Figure 3. Operating pressures during experiment 5: forward pressure = 0, backwash pressure = 0, forward time = 0, and backwash time = –2.

Table 3. Formulas for the statistics used in the ANOVA tables.

Statistics Formula

x-effect sum of squares (SS) where x+ and x– denote the high 2k2 ðyxþ  yx Þ2
and low levels of x, respectively. x may be A, AB, ABC, etc.

Curvature SS, where nF, nC, yF and yC are the factorial observations, nF nC ðyF  yC Þ2 =ðnF þ nC Þ
center point observations, average of the factorial points,
and average of the center points, respectively

Total sum of squares (for Tabs. 4 and 5, the upper limit þnC
nFP

of the summation is nF + nC + nS, where nS denotes the star ðyi  yÞ2

i¼1
observations)

Pure error SS P
nC
ðyi  yC Þ2
i¼1

Lack of fit SS total sum of squares – SSR – SSPure Error

Degree of freedom (DF) number of level –1 for factor effects and curvature;
number of observations –1 for the rest

Mean of squares (MS) SS/DF

MSE (SSLack-of-fit + SSPure Error)/(DFLack-of-fit + DFPure Error)

F MSx/MSE

p 1  cdf ðF; DFx ; DFPureErrorþLackof fit Þ

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1322 Research Article

Table 4. ANOVA table for the factorial design in Tab. 2 (16 full factorial experiments + 7 center points).

Source DF SS MS F p

A 1 23.0 22.95 0.08 0.789

B 1 9599.3 9599.31 32.28 0.001

C 1 5124.3 5124.32 17.23 0.004

D 1 553.5 553.48 1.86 0.215

AB 1 380.2 380.21 1.28 0.295

AC 1 836.7 836.71 2.81 0.137

AD 1 495.1 495.11 1.66 0.238

BC 1 3242.2 3242.24 10.90 0.013

BD 1 9129.6 9129.61 30.70 0.001

CD 1 1532.0 1531.99 5.15 0.058

ABC 1 712.8 712.83 2.40 0.166

ABD 1 1439.6 1439.64 4.84 0.064

ACD 1 71.7 71.67 0.24 0.639

BCD 1 2930.5 2930.53 9.85 0.016

ABCD 1 1251.5 1251.46 4.21 0.079

Curvature 1 2068.6 2068.62 936.92 0.000

Pure error 6 13.2 2.21

Total 22 39403.9

particles [14]. Moreover, the ANOVA suggests a significant
lack of fit due to the small p value associated with the curvature
term. The underlying model that summarizes the results in
Tab. 4 can be given by Eq. (2), more specifically:
y ¼ 124:90 þ 1:2A þ 24:49B  17:90C  5:88D
 4:87AB þ 7:23AC  5:56AD  14:24BC
(5)
 23:89BD þ 9:79CD  6:67ABC þ 9:49ABD
þ 2:12ACD þ 13:53BCD þ 8:84ABCD
Residual analysis of Eq. (5) indicated that the normality and
independency assumptions are violated with residuals being
correlated with the predicted response (filtrate production).
The results from the first-order model Eq. (5) suggest that the
inclusion of second order terms may improve the fitting of the
filtrate data. As mentioned above, three-level design is required
for fitting a second-order model. For a four-factor experiment,
such as the one under study, three-level factorial design re-
quires 34 experiments to estimate 15 parameters. CCD can be
used to significantly reduce the number of required trials while
providing equivalent results [6]. CCD requires 31 experiments
(16 factorial experiments + 7 center points + 8 axial points).
Consequently, the trials corresponding to the star points in
Tab. 2 were carried out.
Tab. 5 shows the ANOVA table for the CCD design. The in-
clusion of the second-order model failed to adequately describe
the functional relationship over the chosen factors’ operating
levels (the p value of lack of fit is almost zero). To improve the
fit of the data, a common statistical practice is to pool the non-
significant terms with the pure error term. The ANOVA table
(Tab. 6) is recalculated by pooling insignificant terms while
considering only the B (backwash pressure), C (forward time),
and the BD (backwash pressure/backwash time interaction)
terms. Tab. 5 shows that the residual sum of squares (SSPure Error
+ SSLack-of-fit) is 16,779, while after pooling non-significant
terms with the pure error, it can be seen from Tab. 6 that the
updated residual sum of squares is 32 828. The difference is the
total sum of squares associated with the non-significant terms.
Therefore, the mean square error (MSE) used for the F test has
increased from 645.35 to 1262.6.
Tab. 6 indicates non-significant lack of fit, i.e., the linear
function that includes backwash pressure, forward time and
backwash pressure/backwash time interaction is found to be
adequate to capture the variability in the filtrate production.
Accordingly, the refined model to predict the filtrate produc-
tion is given as:
y ¼ 123:41 þ 29:51B  23:15C  23:88 B D (6)
An immediate observation from Eq. (6) is the absence of the
forward pressure. The latter can be explained using Figs. 2 and
3: in particular, the increase in the steepness as well as the rapid
onset of the flux decline as the filtration pressure increases.
This may be mainly due to the new condition of the mem-
brane. It is worth mentioning here that Eq. (6) describes the

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Table 5. ANOVA table for the factorial design in Tab. 2 (16 full factorial experiments + 7 center points + 8 axial points).

Source DF SS MS F p

A 1 4252.3 4252.3 4.05 0.061

B 1 20899.0 20899.0 19.93 0.000

C 1 12867.0 12867.0 12.27 0.003

D 1 696.3 696.3 0.66 0.427

AA 1 1336.8 1336.8 1.27 0.276

BB 1 2830.8 2830.8 2.69 0.121

CC 1 545.5 545.5 0.52 0.481

DD 1 596.7 596.7 0.57 0.461

AB 1 380.2 380.2 0.36 0.556

AC 1 836.7 836.7 0.80 0.385

AD 1 495.1 495.1 0.47 0.502

BC 1 3242.2 3242.2 3.09 0.098

BD 1 9129.6 9129.6 8.71 0.009

CD 1 1532.0 1532.0 1.46 0.244

Lack of fit 10 16765.9 1676.6 759.36 0.000

Pure error 6 13.3 2.2

Total 30 76419.8

Table 6. ANOVA table after pooling the non-significant effects. term in Eq. (6) is negative. So, when the backwash pressure and
the backwash time are in the same direction, i.e., both increase
Source DF Adj SS Adj MS F p or both decrease, this would reduce the filtrate production.
B 1 20899.2 20899.2 16.55 0.000 Fig. 4 depicts the residuals plots from Eq. (6). An improved re-
sidual behavior can be observed while satisfying the residual as-
C 1 12867.0 12867.0 10.19 0.004 sumptions, i.e., normality and independence. It is worth men-
D 1 696.3 696.3 0.55 0.464 tioning here that the factorial-based design framework allows
the interaction between the backwash pressure and the back-
BD 1 9129.7 9129.7 7.23 0.012 wash time to be detected, something that would be impossible
Lack of fit 10 15569.4 1556.9 1.44 0.247 to realize with the commonly used OFAT tests.
Another objective of this study is to optimize the operating
Pure error 16 17258.2 1078.6 levels of the UF system in order to maximize the amount of fil-
Total 30 76419.8 trate produced over a certain operating time. Fig. 5 shows the
contour plot produced by Eq. (6), where it can be seen that a
high level of backwash pressure and a low level of forward time
static correlation between the backwash pressure, forward time, give the maximum response when the backwash time is held at
backwash pressure/backwash time and the filtrate production. its lower settings.
Because of the high concentration of the pollutant, the back- Fig. 6 shows the main effect plots of the four factors consid-
wash pressure does have a significant effect due to its role in ered in this study. The two edges of the line are the means of
dislodging the deposited particulates on or in the membrane the responses (filtrate) at each level of a particular factor. For
structure, hence reducing the resistance to fluid flow [14]. On example, for factor B (backwash pressure), at low level (–1), the
the other hand, while it seems that increasing the filtration for- mean of the responses of the runs is 106.65. Similarly, at high
ward time increases the filtrate production, a negative correla- level (+1), the mean of the responses of the runs is 155.62. That
tion was found more feasible with the highly concentrated feed is, on average, the filtrate increases when the back pressure
used. changes from low to high level. On the other hand, it can be
Finally, the combined effect of the backwash pressure/back- seen that the filtrate remains nearly the same when the forward
wash time was found to be more important in predicting the pressure (factor A) changes from low to high level.
filtrate production, rather than the backwash pressure or the It is worth mentioning here that the main effect plots cannot
backwash time alone. Please note that the coefficient of the BD be used alone to draw conclusions if interactions among factors

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1324
Figure 4. Residuals plots from the prediction of Eq. (6).
Figure 5. Contour plot of filtrate versus backwash pressure and
forward time.
are found to be significant [6]. Therefore, the interaction plot
of BD (backwash pressure/backwash time) given in Fig. 7 was
used simultaneously to determine the optimal levels of the fac-
tors. That is, a high backwash pressure should be combined
with a low backwash time if high filtrate production is sought.
It is obvious from the slopes of the lines for factors A (for-
ward pressure) and D (backwash time) in Fig. 6 that the choice
of their levels does not considerably affect the filtrate produc-
tion; however, a relatively high forward pressure and a lower
backwash time are preferable in order to maximize the filtrate
production. Accordingly, the following settings were chosen:
high level of forward pressure, high level of backwash pressure,
low level of forward time, and low level of backwash time, i.e.,
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Research Article
Figure 6. Main effect plots of the four factors under study.
A = +2, B = +2, C = –2, and D = –2. However, since D = –2 (no
backwash) results in complete blockage of the membrane, the
lowest possible backwash time should be used. Using low back-
wash and forward times suggests a higher backwash frequency.
This finding is in agreement with the results reported by Kim
and DiGiano [16]. For this reason, different backwash times
were tested experimentally, i.e., 12, 15, 20, and 25 s. The corre-
sponding filtrate production rates were estimated as 248.1,
276.4, 248.4, and 238.4 L, respectively. The latter was produced
with the following settings: forward pressure = 46 psig, back-
wash pressure = 82 psig, forward time = 60 s, and backwash
time = 15 s. The highest backwash pressure permitted by the
system was used in these experiments. These operating condi-
tions give the optimum response (filtrate production), which is
equal to 275.08 L, within the allowable parameter operating
range. By comparing the optimum filtrate production with ex-
Chem. Eng. Technol. 2015, 38, No. 8, 1315–1326
 Research Article
Figure 7. Interaction plot for B (backwash pressure) and D
(backwash time).
periments 2 and 5, 23 % and 195 % increments were observed,
respectively.
Fig. 8 depicts the flow rate versus time at the optimal operat-
ing settings. While the optimal settings give maximum filtrate
production within the predetermined time window, i.e.,
12 min, it also allows for longer operation of the UF system.
Therefore, for the system under study, the forward-to-back-
wash time and forward-to-backwash pressure ratios are found
to be 4.0 and 1.8, respectively. The predicted filtrate using
Eq. (6) is calculated as 276.48 L. The latter is calculated at B = 2,
C = –2, and D = –1. The error between the predicted and the ex-
perimental filtrate is found to be within 1 %. Although the tur-
bidity of the filtrate was measured, it was not considered as a
constraint, since a new membrane was used in this study,
which gives turbidity levels close to zero for all runs. It is also
worth mentioning here that the optimal settings obtained from
the statistical designs are system dependent and cannot be gen-
eralized to other systems, although similar correlations among
Chem. Eng. Technol. 2015, 38, No. 8, 1315–1326 ª 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
1325
factors may be obtained. However, statistically based designs
still provide a rapid and reliable procedure for large-scale sys-
tems and help in understanding the effects of the factors and in
optimizing their settings.
4 Conclusion
In the present work, statistically based experimental designs
were used to rapidly predict and optimize the filtrate produc-
tion over a certain time window, given a constant level of fou-
lant (4000 ppm silicon dioxide). The main objective was to de-
termine the optimal levels of the operational factors that may
influence the filtrate production of a pilot-scale UF system.
Four factors were considered in this study: forward pressure,
backward pressure, forward time, and backwash time. A full
factorial design was used to identify significant effects, namely
the backwash pressure, the forward time, and the backwash
pressure/backwash time interaction. For the UF system under
study and for the given level of pollutant concentration, in-
creasing the backwash pressure (B) and reducing both the for-
ward (C) and backwash times (D) within the available operat-
ing ranges maximizes the filtrate production. For a newly
installed membrane, the forward pressure (A) showed no sig-
nificant effect.
Acknowledgment
The authors would like to acknowledge the Deanship of Scien-
tific Research at the University of Bahrain for financial sup-
port.
The authors have declared no conflict of interest.
Figure 8. Flow rate versus
time under the optimal op-
erating conditions. Filtrate
production during 12 min =
275.08 L.
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1326 Research Article

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