sustainability
Article
Application of a 2k–p Fractional Experimental Design in
Coagulation-Flocculation Processes in the Treatment of
Wastewater from a Slaughterhouse
Javier Carpintero 1, * , Jennifer Villa-Dominguez 1 , María José Tavera-Quiroz 2 ,
Humberto Carlos Tavera-Quiroz 3 , Bartosz Kaźmierczak 4 , Jonathan Fábregas-Villegas 5
and Fausto A. Canales 1
Citation: Carpintero, J.;
Villa-Dominguez, J.; Tavera-Quiroz,
M.J.; Tavera-Quiroz, H.C.;
Kaźmierczak, B.; Fábregas-Villegas, J.;
Canales, F.A. Application of a 2k–p
Fractional Experimental Design in
Coagulation-Flocculation Processes
in the Treatment of Wastewater from
a Slaughterhouse. Sustainability 2022,
14, 10402. https://doi.org/10.3390/
su141610402
Academic Editor: Mohammadreza
Kamali
Received: 1 July 2022
Accepted: 16 August 2022
Published: 21 August 2022
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Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Sustainability 2022, 14, 10402. https://doi.org/10.3390/su141610402
1 Department of Civil and Environmental, Universidad de la Costa, Calle 58 #55-66,
Barranquilla 080002, Colombia
2 Department of Agroindustrial Engineering, Faculty of Engineering, DESINPA, Universidad de Sucre,
Cra. 28 #5-267, Puerta Roja, Sincelejo 700001, Colombia
3 Departamento de Ingeniería Ambiental, Universidad de Córdoba, Cra. 6 #No. 77-305,
Montería 230002, Colombia
4 Department of Water Supply and Sewerage Systems, Faculty of Environmental Engineering,
Wroclaw University of Science and Technology, 50-370 Wroclaw, Poland
5 Grupo Interdisciplinario de Investigación en Mineralurgia, Energía y Medio Ambiente (GIIMA),
Faculty of Engineering, Universidad Autónoma del Caribe, Barranquilla 080020, Colombia
* Correspondence: javier.carpintero20@gmail.com; Tel.: +57-5-3362252
Abstract: Determining the optimal dose of coagulant required to perform flocculation is critical in
most water treatment plants’ planning and operation. This study implemented a 2k–p fractional
factorial design of experiments to identify the factors influencing the color decrease of wastewater
from a slaughterhouse. The variables assessed were the velocity gradient, residence time, primary
coagulant dosage, chlorine dosage, and coagulation adjuvant dosage. The results indicate that the
primary coagulant dose and the velocity gradient significantly affect the samples’ color and that the
other factors can be run at a low technical-economic level to start up the water treatment plant. The
fractional factorial design allowed reducing the number of experimental points without affecting the
minimum information required to identify which factors are significant in reducing the color of a
wastewater sample.
Keywords: coagulation; coagulation adjuvant; residence time; design of experiments; chlorination; color
1. Introduction
The pollutants in wastewater negatively affect the ecological balance in the environ-
ment [1,2]. Livestock processing facilities generate wastewater with usually high concentra-
tions of organic matter [3], and they are pollution sources in terms of the volume of water
used in the process and the concentration of pollutants [4]. In this sense, the recycling
of wastewater from slaughterhouses has been investigated to improve the productivity
of processing plants of livestock [5,6], considering that the products of this wastewater
treatment can be used for washing pens from recycled water, recovery of nutrients, or
generation of energy from biomass, among others [7]. Wastewater treatment from this
sector usually employs chemical [8] and electrochemical [9,10] processes, unlike other key
industries (dairy [11], bakery [12]) where biological processes are frequently employed.
For wastewater treatment plants based on chemical processes, coagulation and floccu-
lation are used to destabilize the dispersed particles in the water and regroup them in small
masses of higher density called flocs to remove color, turbidity [13,14], and algae [15]. The
ASTM D2035-13 standard suggests an experimental procedure for systematically evaluating
treatments for removing colloidal, suspended, dissolved, or non-precipitable material in
https://www.mdpi.com/journal/sustainability
Sustainability 2022, 14, 10402 2 of 14

water, using coagulation, flocculation, and precipitation by gravity settling [16]. Although
this procedure is focused on varying each experimental factor in turn while leaving the
other factors fixed, this type of approach can be improved [17] if all of them are modi-
fied simultaneously to appreciate and decide which of all these factors are significant in
wastewater treatment [18,19] taking into account experimental variability. The design of
experiments (DOE) has proven to be a technique that allows verifying which factors and
their interactions can substantially influence one or multiple response variables, consid-
ering the cause-and-effect relationship between the observed system and the impact on
its results [20]. The fractional factorial design reduces the number of experimental runs
without affecting the minimum information required to identify those significant factors
in reducing the color of a wastewater sample. This research paper uses this statistical tool
to identify significant causes in the response variable with minimal information based on
a few experimental runs [18]. For the design of wastewater treatment plants that involve
coagulation-flocculation processes, this approach provides an alternative for the manage-
ment of several variables or factors that are modeled heuristically through regulations
or standards and also in the decisions that must be taken concerning those factors that
have a lesser incidence on the objective of reducing the color and managed at a moderate
or low technical-economic level [16]. Regarding applying fractional factorial design to
solve water quality research problems, Jiang et al. [21] have used this technique to degrade
volatile fatty acids in anaerobic digestion processes, using trace elements as experimental
factors. Traces of six of these elements were employed to measure their individual and
combined effect on the fatty acids studied. Thus, an experimental design 26−2 was modeled
to reduce the number of treatments or combinations between these factors to measure the
main effects and interactions on the response variable. Stewardson et al. [22] demonstrated
the usefulness of fractional experimental design for the parameter adjustment of genetic
algorithms. This document highlights the importance of this type of design of experiments
to save time when the research problems are extensive due to the number of factors to be
considered, without losing quality in the response obtained from the effective and efficient
use of this statistical technique of experimentation.
The main objective of this study is to analyze a 2k–p fractional factorial experimental
design in a jar test to study five experimental factors and to choose which of these factors
should be considered in the initial stages of sizing water treatment equipment, more
specifically, flocculators. This statistical tool might serve in designing the processes to
reduce the coloration of a wastewater sample from a slaughterhouse. This paper contributes
to the literature on the optimal sizing of wastewater treatment plants, the improvement
of their operating processes, and their efficient resource consumption. With color as the
response variable, this research hypothesizes that the 2k–p fractional experimental design is
a practical statistical tool for making decisions about factors or operating conditions that
may favor the removal of pollution and contaminants from wastewater.

2. Materials and Methods

Figure 1 presents the assembly of the two-station portable flocculation equipment
used in the experiment. This equipment’s characteristics follow those of the jar test [23,24],
allowing the operator to program the agitation speed and the contact time of the water
and the chemicals in the mixing volumes so that up to two experimental treatments can
be conducted simultaneously. Generally, the jar test results for the removal of colloidal-
sized particles can be scaled to full-size wastewater treatment plants [25,26]. Based on
DOE, this research evaluates how five factors (velocity gradient, residence time, pre-
chlorination, concentration of primary coagulant, and concentration of coagulation aid)
influence the reduction of the physical parameter of the color of a wastewater sample from
a slaughterhouse.
Sustainability 2022,14,
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15

Figure1.1.Experimental
Figure Experimentaldesign
designbenches.
benches.

2.1.
2.1.Case
CaseStudy
Study
This
Thisstudy
studyused
usedwastewater
wastewatercollected
collectedfrom
froman anoxidation
oxidationpondpondof ofaasmall
smallrefrigerating
refrigerating
and
andprocessing
processingfacility
facilityin
inMonteria,
Monteria,Colombia.
Colombia.The Thefacility
facility aims
aims to
to recover
recoverandand reuse
reuse30%
30%
to 40% of the discharged wastewater and employ it for irrigation activities
to 40% of the discharged wastewater and employ it for irrigation activities and cleaning and cleaning
livestock
livestockpens.
pens.This
Thisapplication
applicationprovides
provides ananeco-friendly
eco-friendly alternative to to
alternative improve
improve efficiency in
efficiency
managing water resources while reducing costs in billing for drinking water
in managing water resources while reducing costs in billing for drinking water and dis- and discharge
through wastewater
charge through recovery.recovery.
wastewater
The
Theslaughterhouse
slaughterhouseincludes
includesaawastewater
wastewatertreatment
treatmentsystem
systembased
basedon onthree
threelagoons
lagoons
(anaerobic, facultative, and maturation lagoon). The system’s volume
(anaerobic, facultative, and maturation lagoon). The system’s volume is approximately is approximately
21,000 3
21,000m m3and
andhashasaa hydraulic
hydraulicretention
retentiontime
timeof of70
70days.
days. Even
Eventhough
thoughthe thenatural
naturalprocesses
processes
of self-purification through the symbiotic relationships between
of self-purification through the symbiotic relationships between algae and algae and organisms
organisms re-
remove
move partpartofofthe
theorganic
organicload,
load,asasseen
seen in
in Table
Table 1,
1, the
the sewerage
sewerage company
company where wherethetheplant
plant
isislocated
locatedconsidered
consideredthat the
that effluent
the required
effluent required additional
additionaltreatment, mainly
treatment, because
mainly of the
because of
reddish color of this same.
the reddish color of this same.
Table 1. Average water quality parameters measured at the wastewater treatment plant.
Table 1. Average water quality parameters measured at the wastewater treatment plant.
Before
Before thethe Treatment
Treatment Afterthe
After theTreatment
Treatment
Output from Maturation Sampling Point at the
Parameter
Parameter RawRaw Wastewater,
Wastewater, ppmppmOutput from Maturation Parameter Sampling Point
Parameter at the Oxidation
Lagoon,
Lagoon, ppmppm Oxidation
Reactor, ppmReactor, ppm
DBO55
DBO 2690
2690 646646 DBO5 DBO5 72 72
DQO 4201 813 DQO
DQO 4201 813 DQO 178 178
SST 2070 233
SSTand oils
Grease 2070617 23321
Grease and oils
DETERGENTS 6173.4 212.61
DETERGENTS 3.4 2.61

Therefore, the wastewater treatment plant was expanded according to the diagram in
Therefore, the wastewater treatment plant was expanded according to the diagram
Figure 2, where water loaded with organic material is pumped into a high-rate, rectangular
in Figure 2, where water loaded with organic material is pumped into a high-rate, rectan-
cross-sectional sedimentation tank, where with the help of the factors studied in the exper-
gular cross-sectional sedimentation tank, where with the help of the factors studied in the
iment design, the suspended solid material is precipitated and then given final disposal
experiment design, the suspended solid material is precipitated and then given final dis-
in the form of sludge to landfills. The clarified water is conveyed through multimedia
posal in the form of sludge to landfills. The clarified water is conveyed through multime-
filters and an activated carbon bed to remove the remaining solids. Once the water passes
dia filters and an activated carbon bed to remove the remaining solids. Once the water
through these stages, it is placed in a chemical oxidation reactor tank where it is in contact
passes through these stages, it is placed in a chemical oxidation reactor tank where it is in
with sodium hypochlorite to remove the dissolved organic load and microorganisms (col-
contact with sodium hypochlorite to remove the dissolved organic load and microorgan-
iforms and pathogens). Finally, the reclaimed water goes into an automated storage tank
isms (coliforms and pathogens). Finally, the reclaimed water goes into an automated
Sustainability 2022,
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14, 10402
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storage
of tank of approximately
approximately 100 m3it, from
100 m3 , from where where itaccording
is employed is employed according
to the to theneeds.
consumption con-
sumption needs. The main objective of the coagulation in this site’s wastewater
The main objective of the coagulation in this site’s wastewater treatment plant is to reducetreatment
plant
the is to reduce
reddish color ofthe reddish
effluent color
from the of effluentprocessing
livestock from the activities.
livestock processing activities.
Therefore, according
Therefore,
to wastewater according
disposaltoand
wastewater disposal and
reuse regulations, reuse regulations,
the experimental designtheevaluates
experimental de-
the color
sign evaluates
variable the color
to identify whichvariable to identify
experimentation which
route experimentation
provides route provides
adequate wastewater ade-
in terms of
quate
this wastewater
factor [27,28]. in terms of this factor [27,28].

Figure 2.
Figure 2. Schematic
Schematic of
of the
the wastewater
wastewater treatment
treatment system.
system.

The color was measured in units of platinum cobalt color scale (Pt-Co), and the value
wastewater sample was 6920 Pt-Co. The measurement method was the SM
of the initial wastewater
[29], and
2120 B [29], andthe
theequipment
equipmentselected
selectedtotoperform
perform this
this test
test waswas a HACH
a HACH DRDR
890890 color-
colorime-
imeter.
ter. Table
Table 1 shows
1 shows otherother wastewater
wastewater characteristics
characteristics before
before andand
afterafter the treatment
the treatment in
in the
the system
system schematized
schematized in Figure
in Figure 2. 2.

2.2. Sewage Treatment

2.2. Sewage Treatment System
System
Figure
Figure 22 shows
shows aa schematic
schematic representation
representation of of the
the wastewater
wastewater treatment
treatment system
system used
used
in
in the slaughterhouse under study. This process consists of taking residual water at the
the slaughterhouse under study. This process consists of taking residual water at the
outlet 3
outlet of
of the
the oxidation
oxidation lagoon
lagoon atat aa rate
rate of
of500
500m m3/day
/day toto subject
subject itit to
to aa physicochemical
physicochemical
polishing that improves
polishing that improvesits itsquality,
quality,allowing
allowingitsitsrecycling
recycling forfor washing
washing pens
pens andand other
other in-
industrial activities of the facility. The residual water is conveyed to a high-rate
dustrial activities of the facility. The residual water is conveyed to a high-rate settler with settler
with a capacity
a capacity of 40.3ofm40.3 m3 , the
3, where where the suspended
suspended solids precipitate
solids precipitate by coagulation
by coagulation and
and floccula-
flocculation,
tion, reducing the water’s organic load and its reddish color. Subsequently, the waterthe
reducing the water’s organic load and its reddish color. Subsequently, is
water
pumped is pumped
through athrough
multimediaa multimedia
filter and filter
a bedand a bed of carbon
of activated activated carbonremaining
to retain to retain
remaining solids, and from there, the water passes through a chemical oxidation reactor
solids, and from there, the water passes through a chemical oxidation reactor whereby the
whereby the action of an oxidizing agent the dissolved organic load is removed as well
action of an oxidizing agent the dissolved organic load is removed as well as microorgan-
as microorganisms (coliforms and pathogens). Finally, this water reaches a storage tank
isms (coliforms and pathogens). Finally, this water reaches a storage tank from where it is
from where it is consumed according to the needs of the process. The area occupied by this
consumed according to the needs of the process. The area occupied by this wastewater
wastewater treatment plant in the slaughterhouse is 98 m2 .
treatment plant in the slaughterhouse is 98 m2.
2.3. Experimental Factors Studied
2.3. Experimental Factors Studied
This study analyzed five factors that can contribute to the decrease in the color of
This study
wastewater fromanalyzed five factorsThe
a slaughterhouse. thatfactors
can contribute
selected toto perform
the decrease in the colorde-
the experiment of
wastewater from a slaughterhouse. The factors selected to perform the experiment
sign were the concentration of primary coagulant, coagulation adjuvant, pre-chlorination, design
were thegradient,
velocity concentration of primary
and residence coagulant,
time. coagulation
The chosen adjuvant,
factors were pre-chlorination,
studied ve-
because they are
locity gradient,
controllable, andand
theresidence
literature time. The chosen
has shown factors
that they mightwere studied
directly because
influence thethey are con-
oxidization
trollable,
and andload
organic the remotion
literature processes
has shownthatthataddress
they might directly
the issue influence
of the reddishthe oxidization
appearance of
and organic load remotion processes that address the issue of the reddish
the wastewater from the slaughterhouse. It is worth mentioning that this research did appearance of
the wastewater from the slaughterhouse. It is worth mentioning that this research did not
Sustainability 2022, 14, 10402 5 of 14

not consider temperature and pH for practical reasons. In the case of temperature, this
factor was not assessed because the tropical climate and the operational resources of the
treatment plant would make it difficult to control this variable in actual conditions, and
the ambient air temperature remains relatively constant during the year. Regarding the
pH, the value measured in the wastewater effluent from the slaughterhouse entering the
treatment plant is 6, and in the case of the primary coagulant ferric chloride, it operates in
an optimal pH range between 4 and 12 [30]. Considering that reuse purpose and that the
wastewater has a pH within the adequate range for the coagulant, it was decided to leave
it fixed in this study. Before explaining the experimental design, we describe how these
selected five factors might help reduce the wastewater’s color.

2.3.1. Residence Time

The residence time is related to the duration of the coagulation process in a mixing
volume [31]. Excessive mixing time promotes breaking the connections between the
primary coagulant and the colloidal particles present in the wastewater [32], thus affecting
factors of interest in the design of industrial equipment for large-scale flocculation, such as
agitators, sedimentation tank volumes, among other components related to the flocculation
efficiency of the wastewater treatment plant. Therefore, the destabilization of the particles
as a function of the residence time is a critical factor in understanding the coagulation
mechanism in either fast or slow mixing in a water treatment plant [33]. In this investigation,
the lower and upper-level times of 1 and 3 min, respectively, were established based on the
process’s fast and slow mixing times reported in the literature [31,34].

2.3.2. Velocity Gradient

This factor sets the mixing intensity while dispersing the coagulant in a mixing cham-
ber. This factor is of interest in designing industrial wastewater treatment equipment,
such as flocculators, because it considers the power delivered to the fluid per volume unit.
Concerning the dynamic viscosity that it possesses [35,36], the expression is:
s
2×π×s×T
G= , (1)
V×µ

where:
G: Velocity gradient s−1 ,


•
• s: Rotor speed measured in revolutions per second (rev/s),
• T: Input torque on the rotor (N·m),
• V: Fluid volume (m3 ),
• µ: Dynamic viscosity of the fluid (Pa·s).
This study evaluates two levels of experimentation regarding the agitation speed: The
low level is set at 30 rpm and the high level at 100 rpm. The latter intends to avoid floc
breakdown by liquefaction associated with high agitation speeds [37,38].

2.3.3. Primary Coagulant Concentration

Primary coagulants serve in water clarification processes [39,40]. The inorganic com-
pound ferric chloride (FeCl3 ) was selected as the primary coagulant for this study due to
its availability and high efficiency in removing organic compounds. The tendency of iron
salts to form polymeric species when dissolved in water allows the formation of positively
charged, high surface area amorphous structures [39,41]. Colloidal particles of organic mat-
ter suspended in water tend to be highly stable due to the negative charges distributed on
their surface. Coagulation with iron salts is appropriate to destabilize the colloids of organic
matter. Their injection into effluents produces neutralization of charges, making the small
colloids agglomerate into larger particles until they form flocs consisting of iron cations
and bound organic anions [42]. This study set the lower level of this factor at 100 ppm and
Sustainability 2022, 14, x FOR PEER REVIEW 6 of 15

the small colloids agglomerate into larger particles until they form flocs consisting of iron
Sustainability 2022, 14, 10402 cations and bound organic anions [42]. This study set the lower level of this factor at6 of
100
14
ppm and the upper level at 600 ppm, aiming to propose a technical-economic alternative
that avoids excessive dosing of chemical products, consequently reducing wastewater
treatment
the upper costs.
level at 600 ppm, aiming to propose a technical-economic alternative that avoids
excessive dosing of chemical products, consequently reducing wastewater treatment costs.
2.3.4. Pre-Chlorination
2.3.4.This
Pre-Chlorination
factor refers to verifying if the dosage of an oxidizing agent, such as sodium
This factor
hypochlorite refers in
(NaOCl), to the
verifying
volumeifofthe thedosage
mixture ofcan
an reduce
oxidizingtheagent, such asfrom
color coming sodium
the
organic load of the wastewater. Previous studies have found that pre-chlorination isthe
hypochlorite (NaOCl), in the volume of the mixture can reduce the color coming from a
organic strategy
reliable load of the wastewater.
for removing Previous
organic studies
material, suchhave foundfollowed
as algae, that pre-chlorination
by a coagulation- is a
reliable strategy
flocculation for removing
process organic
[43,44]. Natural material,
organic such
matter as algae,
reacts withfollowed
chlorine by a coagulation-
to produce halo-
flocculation
genated process in
byproducts [43,44].
waterNatural
treatment organic matter
[45]. In reacts this
this sense, withfactor
chlorine to produce
is studied withhalo-
two
genated
levels byproducts in water
of experimentation: Thetreatment
lower level [45].
with In0this
ppm sense, thisupper
and the factorlevel
is studied
with awith
valuetwoof
levels of experimentation: The lower level with 0 ppm and the upper level
5 ppm. The lower level at 0 ppm refers to the absence of pre-chlorination in the coagula- with a value of
5 ppm. The lower level at 0 ppm refers to the absence of pre-chlorination
tion process analyzed in this jar test to know if this stage improves the color of the in the coagulation
process analyzed
wastewater samplein studied.
this jar test
Thisto way,
knowitifwill
thisbestage improves
possible the color
to validate of the
if this wastewater
factor signifi-
samplereduces
cantly studied. This
the way, color
water’s it willtobebepossible
analyzed. to validate if this factor significantly reduces
the water’s color to be analyzed.
2.3.5. Coagulation Adjuvant
2.3.5. Coagulation Adjuvant
Using flocculants facilitates the formation of flocs to attract suspended particles me-
Using flocculants facilitates the formation of flocs to attract suspended particles me-
chanically. These chemical substances improve the precipitation of organic substances dis-
chanically. These chemical substances improve the precipitation of organic substances
solved in the water to be treated [46,47]. This research worked with the synthetic poly-
dissolved in the water to be treated [46,47]. This research worked with the synthetic poly-
electrolyte PolyDADMAC [48,49], and Figure 3 shows its molecular structure. This high
electrolyte PolyDADMAC [48,49], and Figure 3 shows its molecular structure. This high
cationic charge density polymer provides a more favorable flocculation environment. This
cationic charge density polymer provides a more favorable flocculation environment. This
chemical component has been extensively used in studies about coagulation and floccu-
chemical component has been extensively used in studies about coagulation and floccula-
lation in wastewater treatment [49,50]. The two levels employed in this experiment to as-
tion in wastewater treatment [49,50]. The two levels employed in this experiment to assess
sess the effect of PolyDADMAC on the reduction of color in the wastewater are 1 ppm
the effect of PolyDADMAC on the reduction of color in the wastewater are 1 ppm (lower
(lower level)
level) and and 5(upper
5 ppm ppm (upper
level). level).

Figure 3.
Figure Molecular structure
3. Molecular structure of
of PolyDADMAC.
PolyDADMAC.

2.4. Experimental Design Planning

2.4. Experimental Design Planning
This study uses a jar test to evaluate the main effects of five factors on the coagulation
This study uses a jar test to evaluate the main effects of five factors on the coagulation
and flocculation behavior of wastewater from a slaughterhouse. It is possible to significantly
and flocculation behavior of wastewater from a slaughterhouse. It is possible to signifi-
reduce the number of experimental points while losing a minimum of valuable information
cantly reduce the number of experimental points while losing a minimum of valuable in-
by implementing a 2k–p fractional factorial experimental design [21,51]. Therefore, a 25–1
formation
factorial design is proposed toawork
by implementing 2k–p fractional factorial
with half of experimental
the treatments design [21,51].
of the complete There-
experimental
fore, a 2 Infactorial
design.
5–1 design
this 2k–p study,is kproposed to work
= 5 because therewith half
is an of the treatments
interest in studyingoffive
the factors
completeto
experimental design. In this 2k–p study, k = 5 because there is an interest in studying five
reduce the color of wastewater. Moreover, p = 1 because the number of experimental runs
factors to reduce
will be halved. the2color
Table of wastewater.
describes Moreover,
the experimental p with
factors = 1 their
because the number
respective levels of
of
experimentation for this study. This type of design of experiments allows knowing the
impact of various factors on a response variable while using a minimum number of runs
and blocks of experimentation to quickly and efficiently obtain the cause-effect relationship
between the variables evaluated. Assuming that the main effects are more important than
Sustainability 2022, 14, 10402 7 of 14

the interactions of two factors, it is convenient to use fractional factorial designs with high
resolution [18]. The resolution of the experimental design of this study is of type V since
the main effects are estimated concerning the alias of triple and higher-order interactions.
The experimental runs included four repetitions at the center of each factor to increase
the degrees of freedom of the experimental design error up to 19, and the design did not
include replications (one block only–BL). The statistical package used was Statgraphics
Centurion XVI. With these considerations, the wastewater volume employed for the study
was 20 L.

Table 2. Experimental factor and its levels of experimentation.

Factor Units Low Level (−1) Intermediate Level (0) High Level (+1)
A: Residence time minutes 1 2 3
B: Velocity gradient rpm 30 65 100
C: Coagulant concentration ppm 100 350 600
D: Pre-chlorination ppm 0 2.5 5
E: Coagulation adjuvant ppm 1 3 5

3. Results
Table 3 presents the worksheet developed for a 25−1 factorial design without replica-
tions and four repetitions at the center, displayed in lines related to runs 17 to 20. The last
column of the table shows the response of the color variable for each assessed combination.

Table 3. Experimental design worksheet and color variable response.

Run BL A B C D E Color (Pt-Co)

1 1 −1 −1 −1 −1 +1 8460
2 1 +1 −1 −1 −1 −1 7740
3 1 −1 +1 −1 −1 −1 5640
4 1 +1 +1 −1 −1 +1 4325
5 1 −1 −1 +1 −1 −1 1400
6 1 +1 −1 +1 −1 +1 3840
7 1 −1 +1 +1 −1 +1 1340
8 1 +1 +1 +1 −1 −1 640
9 1 −1 −1 −1 +1 −1 7260
10 1 +1 −1 −1 +1 +1 6875
11 1 −1 +1 −1 +1 +1 4320
12 1 +1 +1 −1 +1 −1 6140
13 1 −1 −1 +1 +1 +1 3460
14 1 +1 −1 +1 +1 −1 2120
15 1 −1 +1 +1 +1 −1 950
16 1 +1 +1 +1 +1 +1 487
17 1 0 0 0 0 0 6560
18 1 0 0 0 0 0 1420
19 1 0 0 0 0 0 5700
20 1 0 0 0 0 0 4200

Table 4 presents the analysis of variance (ANOVA) of the main effects examined in a jar
test through a factorial design of experiments with a confidence level of 95%. These results
suggest that the concentration of the primary coagulant and the velocity gradient are the
factors that significantly affect the decrease in the color of the residual water, according to
the results obtained in their respective p-value tests. The residence time, pre-chlorination,
and coagulation adjuvant factors do not significantly affect the color of the wastewater
sample analyzed in the jar test.

Sustainability 2022, 14, 10402
results suggest that the concentration of the primary coagulant and the velocity gradient
are the factors that significantly affect the decrease in the color of the residual water, ac-
cording to the results obtained in their respective p-value tests. The residence time, pre-
chlorination, and coagulation adjuvant factors do not significantly affect the color of the
wastewater sample analyzed in the jar test. 8 of 14

Table 4. ANOVA of the experimental design.

Table
Sum 4. ANOVA
of ofDegrees
the experimental
of design.
Source Mean Square F-Ratio p-Value
Squares Freedom
Source Sum of Squares Degrees of Freedom Mean Square F-Ratio p-Value
A: Residence time 27,473.1 1 27,473.1 0.02 0.9014
B:A:Velocity
Residence time
gradient 27,473.1
1.87337 × 107 7 1 1 1.87337 × 27,473.1
107 10.85 0.02 0.9014
0.0053
B: Velocity gradient 1.87337 × 10 1 1.87337 × 107 10.85 0.0053
C: Coagulant concentration 8.33706 × 107 7 1 8.33706 × 107 48.28 0.0000
C: Coagulant concentration 8.33706 × 10 1 8.33706 × 107 48.28 0.0000
D:
D: Pre-chlorination
Pre-chlorination 19,6471.0
196,471.0 1 1 19,6471.0
196,471.0 0.11 0.11 0.7409
0.7409
E:
E: Coagulation adjuvant
Coagulation adjuvant 92,568.1
92,568.1 1 1 92,568.192,568.1 0.05 0.05 0.8203
0.8203
Total Error
Total Error 2.41754 ××1010
2.41754 7 7 14 14 × 106 × 106
1.726811.72681

Figure
Figure44displays
displaysthe
thecontour
contourplot
plotofofthe
theresponse
responsesurface
surfacefor
forthe
thejar
jartest
testin
interms
termsofof
the
the color variations of the wastewater. The color range is between 2700 and 6000 Pt-Co
color variations of the wastewater. The color range is between 2700 and 6000 Pt-Co
units
unitsbased
basedon
onthe
theexperimental
experimental limits
limits of
of the
the primary
primary coagulant
coagulant and
and the
the velocity
velocity gradient.
gradient.
Contornos de la Superficie de Respuesta Estimada
Time=1.0, Prechlorination=0.0, Coag. Adjuvant=1.0

600 color
2700,0
3000,0
500
3300,0
Coag. Concentration

3600,0
400 3900,0
4200,0
4500,0
300
4800,0
5100,0
200 5400,0
5700,0
6000,0
100

0
30 50 70 90 110

Vel. Gradient

Figure
Figure4.4.Contour
Contourdiagram
diagramfor
forthe
theresponse
responseof
ofthe
thecolor
colorvariable.
variable.

Figure55shows
Figure showsthethemain
maineffects
effectsof
ofthe
thefactors
factorson
onthe
thecolor
colorvariable
variablein inthe
thewastewater
wastewater
samplefrom
sample fromthetheslaughterhouse.
slaughterhouse.According
Accordingto tothe
thewastewater
wastewatercolor
colortrends,
trends,as asthe
thelevels
levels
ofeach
of eachfactor
factorchange
changefrom
fromthe
thelowest
lowestto tothe
thehighest
highestlevel,
level,while
whilethe
theother
otherfactors
factorsremain
remain
constant, the
constant, the primary
primary coagulant
coagulantconcentration
concentrationisisthethevariable
variablewith
with the
the most
most significant
significant
impact
Sustainability 2022, 14, x FOR PEER REVIEW on the color decrease. Similarly, increasing the velocity gradient
impact on the color decrease. Similarly, increasing the velocity gradient decreasesdecreases the9 color
of
the15
of the water sample. The results related to the variation of the residence
color of the water sample. The results related to the variation of the residence time and time and the
coagulation adjuvant show no significant incidence in the color of the wastewater.
the coagulation adjuvant show no significant incidence in the color of the wastewater.
6800

5800
color (Pt Co)

4800

3800

2800

1800

Time Vel. Gradient Coag. Concentration Prechlorination Coag. Adjuvant

Figure 5. Main
Figure 5. Main effects
effects graph
graph for
for color
color in
in the
the wastewater
wastewater system.
system.

Figure 6 refers to the normal probability graph of the effects of the factors analyzed
in the jar test. In this plot, the standardized effects are ordered from smallest to largest
and plotted against quartiles of a normal distribution. In this case, the residence time, co-
agulation adjuvant, and pre-chlorination factors are aligned to the process noise since they
 2800

1800

Time Vel. Gradient Coag. Concentration Prechlorination Coag. Adjuvant

Sustainability 2022, 14, 10402 9 of 14
Figure 5. Main effects graph for color in the wastewater system.

Figure
Figure 6 refers to the normal probability graph of the effects of the factors analyzed
in
in the jar test. In
In this
this plot,
plot, the
the standardized
standardized effects
effects are
are ordered
ordered from smallest
smallest to largest
and
and plotted
plotted against
againstquartiles
quartilesofofa anormal
normal distribution.
distribution.In this case,
In this the the
case, residence time,time,
residence co-
agulation
coagulation adjuvant, and
adjuvant, pre-chlorination
and pre-chlorinationfactors
factorsare
arealigned
alignedtotothe
theprocess
processnoise
noisesince
sincethey
they
go in
in the
the same
same direction
direction as the straight line of this graph. On On the
the other
other hand,
hand, the
the coagulant
coagulant
velocity and concentration gradient
gradient factors
factors correspond
correspond to to signals
signals that
that significantly
significantly affect
affect
the color of the wastewater sample studied in the jar test.

Figure
Figure 6.
6. Normal
Normal probability
probability plot
plot for
for this
this study.
study.

Figure 7 presents the graph of residuals versus predicted values of the jar test experi- exper-
ment design.
iment design.This
Thischart
chartdisplays
displaysresiduals
residualsagainst
againstpredicted
predicted values
valueswith
witha horizontal
a horizontal line at
line
zero.
at It is
zero. It observed
is observedthat thethe
that residuals
residualsvary randomly
vary randomly around
aroundthethe
line. TheThe
line. lacklack
of aofpattern
a pat-
Sustainability 2022, 14, x FOR PEER REVIEW
or trend
tern in this
or trend ingraph suggests
this graph that there
suggests is no influence
that there of time
is no influence ofor anyorother
time external
any other 10 factor
of 15
external
during the experimental runs.
factor during the experimental runs.

Figure
Figure7.7.Residuals
Residualsversus
versuspredicted
predictedplot.
plot.

InIncorrespondence
correspondencewith
withthethesymbols
symbolsproposed
proposedforforeach
eachfactor
factorreferenced
referencedininTable
Table4,4,
thefitting
the fittingmodel
modelaccording
accordingtotothe
theresults
resultsfrom
fromthe
the2020experimental
experimentalruns
runsconducted
conductedfor
forthis
this
workis:
work is:

color =
color = 9428.75 −41.44
9428.75 − 41.44××AA−
− 30.92
30.92××BB−−9.13
9.13××CC−
− 44.33
44.33××DD +
+ 38.03
38.03××EE (2)
(2)
In this case, the adjusted correlation coefficient is 75%, which suggests that this math-
In this case, the adjusted correlation coefficient is 75%, which suggests that this mathe-
ematical function relates the main effects to the color of the wastewater at a moderate
matical function relates the main effects to the color of the wastewater at a moderate level.
level.

4. Discussion
Various advanced statistical tools are currently used to intensify and improve indus-
trial wastewater treatment processes [52]. On jar tests for the sizing of wastewater treat-
Sustainability 2022, 14, 10402 10 of 14

4. Discussion
Various advanced statistical tools are currently used to intensify and improve in-
dustrial wastewater treatment processes [52]. On jar tests for the sizing of wastewater
treatment plants, in the use of a statistical tool to detect those variables that commonly
demand resources for their operation, such as the consumption of chemicals (coagulants
and flocculants) and energy (electric motors to drive agitators) that, not being significant
in the response, can operate at a low level of consumption without affecting the purpose
of the equipment that recycles wastewater. With these results, optimization strategies
can subsequently be established on those physical-chemical parameters of interest in the
wastewater, considering the experimental modification of those factors that are statisti-
cally representative.
The concentration of primary coagulants is a factor of interest in designing large-scale
flocculation systems [53]. According to Figure 5, as the coagulant concentration in the jar
test increases, its color tends to decrease. This behavior occurs because higher coagulant
concentrations within the volume of the mixture affect the stability of the colloidal organic
matter due to the surface phenomena present in the wastewater during coagulation [54].
According to Oriekhova and Stoll, the optimal concentration of primary coagulant de-
pends on the suspended particle’s surface charge, size, and water composition. Their
findings indicate that using high concentrations of the primary coagulant generates poly-
mers of considerable size to precipitate by gravity and, therefore, clarify water samples with
polystyrene latex particles [55]. The results indicate that implementing the 2k–p factorial ex-
perimental design for the jar test allowed identifying the factors that significantly influence
color removal from wastewater. The use of DOE techniques facilitates the identification of
significant variables, allowing for their optimization, while the other elements involved
in the operation process are dimensioned at cost-effective technical-economic levels. This
observation is in line with the findings by De Paula et al., who applied DOE techniques to
estimate concentration ranges of coagulants, such as aluminum sulfate, ferric chloride, and
Moringa oleifera extract (MO), for wastewater treatment in the concrete industry [56]. In this
study, the efficiency in the removal of turbidity from wastewater was compared and the
results reported in a standardized Pareto diagram show that increasing the concentration of
the primary coagulant, whether it is a natural derivative or a traditional chemical coagulant,
improves the final quality of the water subjected to the coagulation process. These results
coincide with what is reported in Figure 6, which shows that a higher concentration of
primary coagulant corresponds with a higher effect on the color removal in the wastewater
sample from the slaughterhouse.
The velocity gradient has been analyzed as a criterion for improving the efficiency of
flocculation systems [57,58]. According to Figure 6, this study suggests that as the level of
the velocity gradient factor increases, the color of the analyzed wastewater decreases. The
hydrodynamic effect of mechanical agitation favors the contact of the primary coagulant
with the residual water, a necessary condition for the visible formation of flocs [59,60].
Rossini et al. developed statistical optimization strategies based on the influence of rapid
mixing for coagulation-flocculation processes in wastewater treatment plants. This research
concluded that rapid mixing strongly influences the reduction of wastewater turbidity
when coagulation and flocculation are operated with high values of rapid mixing [61].
These results differ from the findings detected in the present study, which may be justified
by the type of wastewater treated.
A recent investigation on the phosphate removal efficiency from anaerobic sludge
found that coagulant dosage, agitation speed, and residence time significantly impact the
elimination of the pollutant [62]. These findings indicate that DOE techniques, such as
those used in the present study, might be applied similarly and simultaneously to assess the
removal efficiency of different pollutants in wastewater. Unlike the results of this research,
in other types of residual water, such as those reported in the textile industry by Keerthi y
Vani, the residence time was found to be a significant factor for the application of statistical
Sustainability 2022, 14, 10402 11 of 14

techniques, such as the response surface methodology, to reduce the color of wastewater
from the textile industry [63].
Table 3 shows an increase in the magnitude of the color in those experimental treat-
ments where the concentration gradient and coagulant concentration factors were evaluated
at their low levels. This trend is mainly observed in runs 1, 2, 9, and 10 of Table 3. These
results confirm the main effects shown in Figure 5, where steeper slopes denote the sig-
nificant factors. The contour plot in Figure 4 shows a tendency for the color of the water
sample to increase if these factors decrease in the coagulation process.
Colombian legislation regulates the discharge of water contaminated by livestock
activities [27]. This study used statistical techniques to identify the factors that improve
wastewater coagulation from slaughterhouses. Therefore, these experimental techniques
can reduce efforts in designing, selecting components, and adjusting technologies that treat
wastewater of this nature.
PolyDADMAC polyelectrolyte as a coagulation adjuvant improves the color removal
of wastewater from the palm oil extraction industry if the clarification is combined with the
primary coagulant ferric chloride [50]. Although the present investigation was carried out
with the hypothesis that the combination of ferric chloride and PolyDADMAC reduce the
color of wastewater from slaughterhouses, the results of Table 3 and Figures 5 and 6 show
that adding this polyelectrolyte to the clarification process does not significantly affect
color removal and conversely, suggesting the dosage of this coagulation adjuvant in the
coagulation process makes water treatment more expensive. Coagulation is one of the most
critical processes in wastewater treatment to reduce the organic load that contributes to color
and COD, among other parameters. The experimental runs indicate that the color decreases
because of the formation of ferric hydroxide precipitates in the aqueous solution and by
the adsorption of ferric precipitates on the surface of the organic load that precipitates.
This tendency can be related to the supersaturation in the solution concerning the ferric
hydroxide under the chemical conditions considered in the experimental design. The results
from this statistical application suggest that wastewater from slaughterhouses can be treated
without a coagulation adjuvant or a pre-chlorination stage and even with a minimum
dosage of these factors, given its little effect on reducing the sample’s reddish color.

5. Conclusions
A 25−1 fractional factorial experimental design with four repetitions at the center was
conducted to evaluate the effects of five factors in the coagulation-flocculation process, for
the design of a treatment plant for wastewater from a slaughterhouse, through a jar test.
The fractional factorial design allowed reducing the number of experimental points without
affecting the minimum information required to identify which factors are significant in
reducing the color of a wastewater sample, which makes this DOE technique an appealing
option in budget and time-constrained assessments, especially regarding well-known water
treatment processes. It was observed that the dose of primary coagulant and the velocity
gradient are the two factors that have a statistically significant effect on the color of the
residual water. In this sense, operating these factors at higher levels could reduce the color
of the wastewater while the rest of the factors, such as residence time, pre-chlorination, and
coagulation adjuvant, can be sized at low technical-economic levels. From this study, it
is suggested to use statistical experimentation techniques to optimize this process so that,
from the economic point of view, the dose of primary coagulant can provide feasibility for
the assembly and operation of this water treatment plant. The results of this research apply
to color removal, but it is possible that the parameters evaluated and determined to be
irrelevant for color could be significant for other response variables related to contaminants
or type of industry.
Sustainability 2022, 14, 10402 12 of 14

Author Contributions: Conceptualization, J.C. and F.A.C.; methodology, J.C., J.F.-V., F.A.C. and
J.V.-D.; software, J.C.; validation, F.A.C., B.K., H.C.T.-Q. and M.J.T.-Q.; formal analysis, J.C. and F.A.C.;
resources, J.V.-D., M.J.T.-Q. and H.C.T.-Q.; data curation, J.V.-D.; writing—original draft preparation,
J.C., B.K. and F.A.C.; writing—review and editing, J.C. and F.A.C.; supervision, F.A.C. and J.F.-V. All
authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Data Availability Statement: The main data associated with this research paper is available at:
https://bit.ly/3Ahmy8k (accessed on 10 June 2022).
Acknowledgments: The Authors would like to thank Ernesto Jaramillo and Andrés Carpintero for
their collaboration in executing experimental procedures on jar testing equipment.
Conflicts of Interest: The authors declare no conflict of interest.

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