Waste Management Bulletin 1 (2024) 172–181

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Waste Management Bulletin

journal homepage: www.elsevier.com/locate/wmb

Biodiesel production from waste cat fish oil using heterogeneous catalyst
from cat fish born: A viable waste management approach, and ANN
modeling of biodiesel yield
Chinedu M. Agu a, *, Kingsley A. Ani b, Prince O. Abiazieije a, Juliet A. Omeje a, Jane C. Ekuma a,
Uchenna E. Umelo a, Osondu H. Omukwu a, Emeka D. Nwankwo a, Mmesoma P. Chinedu c
a
Chemical Engineering Department, Michael Okpara University of Agriculture, Umudike, Nigeria
b
Chemical Engineering Department, Nnamdi Azikiwe University, Awka, Nigeria
c
Applid Biochemistry Department, Enugu State University of Science and Technology, Enugu, Nigeria

A R T I C L E I N F O A B S T R A C T

Keywords: Biodiesel from vegetable or animal feedstock can serve as a suitable source for renewable energy. This study
ANN utilized heterogeneous catalyst obtained from fish bone for biodiesel production from raw cat fish waste (CFW)
Fish bone catalyst oil. The CFW oil yield obtained using wet reduction extraction method was 96.85 %. The heterogeneous catalyst
Transesterification
was prepared by calcination at 600 ◦ C, for 4 h and characterized using SEM-EDX. Catalyst characterization
Catfish waste oil
showed suitable elements that can improve the catalytic activity. Physiochemical characterization results showed
Biodiesel
that viscosity of CFW oil (48.782 mm2/s), reduced to 9.391 mm2/s in the produced biodiesel. Similarly, after
transesterification free fatty acid (3.593 mg/KOH/Kg) and acid value (7.186 mg/KOH/Kg) of CFW oil reduced to
1.48 mg/KOH/Kg and 2.96 mg/KOH/Kg, respectively, in the biodiesel. Finding from the Fourier Transform
Infrared (FTIR) Spectrum of the raw CFW oil showed the presence of –OH and was assigned to the axial
deformation of water molecule. However, the –OH group disappeared in the FTIR spectrum of biodiesel due to
the transesterification process. This observation is consistent with the findings for moisture contents of raw CFW
oil (0.073 %) and biodiesel (0.00 %), which showed disappearance of water after transesterification. The bio­
diesel yield was further modeled using three algorithms (Scaled conjugate gradient, Bayesian regularization and
Levenberg maraquardt) of the artificial neural network (ANN). It was evident that the predictions from the
Scaled conjugate gradient algorithm were comparable to the experimental responses. Finally, transesterification
of raw CFW oil using heterogeneous catalyst from fish bone, was a cost-effective approach for biodiesel
production.

Introduction
Global demand for energy is continuously on the increase and bio­
diesel from renewable feedstock is seen as a suitable alternative to the
conventional diesel fuel with remarkable environmental challenge
(Anguebes-Franseschi et al., 2019; David et al., 2019). Vegetable and
animal fats have been used as feedstock to produce biodiesel through a
process known as transesterification (Dutta et al., 2014). The trans­
esterification process is basically the reaction between the extracted oil
from vegetable or animal fat, with an alcohol in the presence of suitable
homogenous or heterogeneous catalyst (Ling et al., 2019). However, the
challenge with most vegetable and animal fat feedstock for biodiesel
production is in their high free fatty acid and viscosity. The implication
of high viscosity and free fatty acid is the generation of carbon deposits
and undesirable atomization in the combustion engine (Muhammad
et al., 2015).
Amongst the identified animal fat oil bearing feedstock considered
for biodiesel production are wastes from fishes, which attracts strong
consideration because they constitute significant amount of byproducts
like bones, scales, viscera etc. (Ghaly et al., 2013). These waste products
from fishes contain significant amount of oil that needs further explo­
ration to determine its potentials as biodiesel feedstock (Kudre et al.,
2017) and also as a solution for their disposal (Karkal and Kudre, 2021).
This approach could ensure the availability of feedstock for local

* Corresponding author.
E-mail addresses: agu.chinedum@mouau.edu.ng, eduetal@yahoo.com (C.M. Agu).

https://doi.org/10.1016/j.wmb.2023.11.002

Available online 18 November 2023

2949-7507/© 2023 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
C.M. Agu et al.
biodiesel producing firms. However, oil yield from fish wastes differs
and depends on extraction methods, species and age (koiakowska et al.,
2011). Kudre et al. (2017) investigated biodiesel production from rohu
(Labeo rohita) fish waste oil and reported oil yields of 72.1 %, 95.2 % and
90.40 % obtained using solvent extraction, wet reduction and acid
ensilage methods, respectively.
Biodiesel transesterification conventionally employs homogeneous
catalyst due to their high catalytic activity (Karkal and Kudre, 2021,
2023). However, some challenges with homogeneous catalyst that ne­
cessitates the search for a suitable alternative include non-reusable, and
saponification reaction in the presence of moisture (Chen et al., 2015).
In this case, the heterogeneous catalysts are employed to tackle the
drawbacks of the homogeneous catalysts, because they are eco-friendly,
non-corrosive and can be synthesized from biomass and non-biomass
sources (Ling et al., 2019). Piloto-Rodríguez et al. (2013) reported
that the reduced reaction time, economically viable and enhanced bio­
diesel conversion rate are some of the advantages of heterogeneous
catalyst over their homogenous counterparts. Since there is no accept­
able waste management process for CFW and fish bone, this study
therefore explores ways of its conversion to biodiesel, as it could serve as
a cost effective feedstock. Since the fish bone heterogeneous catalyst
could be rich in some elements that can as well increase its catalytic
activity. In other to ensure optimum biodiesel production, modeling the
production process becomes very important. Since process modeling is
very important in Chemical Engineering, therefore, biodiesel production
from waste catfish oil was modeled using artificial neural network
(ANN).
Over the years, researchers have modeled biodiesel/methyl ester
yields from different base oil sources, using ANN and other modelling
tools like Adaptive Neuro-fuzzy Inference System (ANFIS), Artificial
Neural Network (ANN) and Response Surface Methodology (RSM). For
instance, ANN and RSM were used in modelling methyl ester yield from
Prunus amygdalus seed oil by Esonye et al. (2019) and reported that ANN
was better predictive model than RSM, with the former having higher R2
value of 0.96637, as against 0.9446 obtained for the later model. Most
recently, Agu et al. (2023) compared the modelling efficiencies of
ANFIS, ANN and RSM, for the methyl ester production yield from Aza­
dirachta Indica seed oil, in which they reported the supremacy of ANFIS,
followed by ANN. For the modelling of biodiesel yield from palm oil
using Moringa oleifera leaves as heterogeneous catalyst, Kolakoti et al.
(2022) reported that ANN was a better predictive model than RSM.
Similarly, in modelling biodiesel yield from microalgae, ANN was also
reported to be better predictive model than RSM, according to the re­
sults obtained by Gul et al. (2022). In like manner as regards the use of
waste oils, ANN and RSM were used to model/predict biodiesel yield
from waste cooking oil, and it was also found that ANN was better
predictive model (Soji-Adekunle et al., 2018). From the aforementioned
cited previous similar works, it could been seen that ANN in most cases
was a better modeling tool, compared to RSM. In other words, the reason
behind the choice of ANN as the modeling tool used in this current study.
The artificial neural network (ANN) has been widely used to model
and predict different behavior of complex system (Ayoola et al., 2019;
Hamid et al., 2016). The ANN tool gives insight and helps to understand
the effects of different process parameters in numerous industrial ap­
plications. However, Turan et al. (2011) reported that the function
approximation is the common application of the ANN and there is no
specific formula available that explains how the ANN design architec­
ture or algorithm will solve a particular problem. The levenberg mar­
aquardt algorithm of the neural network modeling permits the
evaluations of complex systems through its predictive capability with
unique flexibility (Rocabruno-Valdés et al., 2015). In this study the
modeling strength of three neural network algorithms in predicting
biodiesel yield were examined. These algorithm include scaled conju­
gate gradient, bayesian regularization and levenberg maraquardt.
Consequently, since to the best knowledge of the authors, there is no
existing literature information on the extensive use of ANN model for the
173
Waste Management Bulletin 1 (2024) 172–181
modeling of biodiesel yield from raw cat fish waste (CFW) oil, which also
made use of the calcined cat fish born as heterogeneous catalyst for the
transesterification reaction. Hence, the present study was necessitated to
close this existing research gap, especially as it explores the utilization of
the entire cat fish wastes, thereby ensuring proper management of the
industrial waste.
Therefore, this present study examines the biodiesel production from
raw catfish waste (CFW) oil through transesterification approach, using
calcined fish bone as heterogeneous catalyst. Also, the physiochemical
properties of the raw CFW oil and biodiesel were carried out to inves­
tigate the possible impacts of transesterification on the oil properties. In
addition, the calcined fish bone, which before now has not be utilized as
catalyst for biodiesel production was characterized using SEMEDX to
determine its elemental compositions that could hasten the raw oil
transesterification process to produce biodiesel. Furthermore, the
experimental biodiesel yield from the combinations of process param­
eters such as temperature, time, catalyst concentration, methanol/mole
ratio, and agitations speed were also compared to the ANN predictions.
Materials and methods
Oil extraction processes from catfish waste
Reasonable quantities of catfish wastes (CFW) were collected from a
cat fish commercial farm and immediately used to extract the oil before
characterization. The extraction process followed the wet reduction
method by Karlkal and Kudre (2021). In this procedure, 10 kg of the
CFW was mixed with 10L of water (1:1w/v) and heated in a water bath
(W530 model, Schwabach, Germany) with temperature regulator at
65 ◦ C for 40 min. The mixture was manually stirred every 10 min and
after 40 min, and was allowed to cool till its temperature dropped to
30 ◦ C. The oil afloat was collected and centrifuged (8000 rpm for
30mins) to remove impurities and unwanted particles. The oil was
transferred into a screw capped bottle and stored. Soxhlet extraction
procedure following official method of Analysis AOAC 981.11 (2000)
was further employed to extract the total amount of oil from the CFW.
The oil yield was estimated using Equation (1)
Amountofextractedoil(g)
Oilyield(%) = × 100 (1)
Totalamountofoilinsample(g)
Physiochemical characterization of the extracted oil
The test methods detailed herein were followed to examine the
physiochemical characteristics of both the extracted (raw) and produced
biodiesel from CFW oil. The kinematic viscosity (mm2/s) at 40 ◦ C and
acid value (mgKOH/Kg) were determined following the ASTM test
method of D445 (2011) and D664 (2019), respectively. The moisture
content (%) was determined using ASTM method D2709 (2022). The
flash point was examined following ASTM method D93 (2012). The
saponification value was determined using the method described by the
AOCS cd 3-25 (2017). The molecular weight of the raw CFW oil was
estimated using Equation (2), where SV and AV represent the saponifi­
cation and acid values, respectively.
( g ) 168300
molecularweight = (2)
mol SV − AV
For the produced biodiesel, the cetane number was estimated following
test method of ASTM D613 (2023). The density was estimated using
ASTM D1298 (2023), while the automatic aniline point tester was ac­
cording to ASTM test method D611 (2016). The (method A for trans­
parent sample) was used to determine the aniline point, while the
calorific value was estimated using the bomb calorimeter (model-IKA
c2000).
C.M. Agu et al. Waste Management Bulletin 1 (2024) 172–181

Transesterification process Fourier transforms infrared spectroscopy (FTIR)

5 N of potassium hydroxide (KOH) was used to neutralize the
extracted oil from CFW. The mixture was heated at 110 ◦ C for 15 min to
remove any leftover moisture. The transesterification process was car­
ried out in a corked Erlenmeyer flask (250 ml) containing reaction
mixture of 150 ml. The flask was placed in a water bath with tempera­
ture regulator. The water bath was fitted on a magnetic stirrer and the
stirring rate was kept constant at 200 rpm. At the end of 30 min reaction
time, the catalyst was separated from the mixture by centrifugation at
6000 rpm for 15 min. After centrifugation, the supernatant consisting
glycerol (lower phase) and biodiesel (upper phase) were separated using
a separating funnel. Traces of unreacted catalyst, methanol and glycerol
were removed by washing the biodiesel with 0.5 M citric acid for 30 min,
followed by additional 10 min heating to dry off any residual moisture.
The critic acid was removed by centrifugation at 4000 rpm for 7 min.
The biodiesel phase was collected and the yield was calculated using
Equation (3).
Biodieselyield(wt%) =
weightofbiodiesel(methylester)
× 100 (3)
weightofCFWoil
Catalyst preparation
The fish bone catalyst was dried in an oven at 120 ◦ C for 3 h to
remove water and other unwanted materials. The oven dried fish bone
was crushed into a powdered form using mortar and pestle. Thereafter,
the powdered fish bone was calcined at 600 ◦ C for 4 h in a muffle
furnace. The calcined fish bone was stored in a screw-capped tube
placed in a desiccator to prevent poisoning from air and humidity. The
catalyst was further characterized using SEM-EDX before its application
in the transesterification process.
Both the raw CFW oil and biodiesel produced from CFW oil were
evaluated using the infrared spectroscopy to examine the functional
group compositions of the samples. The spectroscopic analysis was made
using a Bruker FTIR spectrophotometer (TENSOR II Bruker, Germany).
The spectrum pattern was recorded in transmission (%) versus wave­
length (cm‾1) mode in the ranges of 3500 – 1000 cm‾1.
Artificial neural network (ANN) modeling
This study employs the neural network algorithm of the scaled
conjugate gradient (trainscg), bayesian regularization (trainbr), leven­
berg maraquardt (tainlm) were used to predict biodiesel yield from CFW
oil. The data set for the experiment as shown in Table 1 was generated
through a central composite design (CCD) procedure (Ani and Agu,
2022). The CCD shows experimental layout consisting of the various
combinations of the considered independent variable and the corre­
sponding biodiesel yield. Hamid et al. (2016) also reported that the
generated data set through CCD were used to determine the optimal
ANN design architecture. The neuron in the hidden layer has two pri­
mary functions which are the summation and multiplication of all
weighted input as well as the summation of the output for subsequent
transfer to the logic part (Turan et al., 2011). To minimize error, the
weighted input and output are added to the bias through a nonlinear
approximation (Rocabruno-Valdés et al., 2015). The randomly designed
data set were trained using the three selected algorithms and a linear
regression between the network output and target of the best performed
algorithm was presented.
The design architecture for the three algorithms is as shown in Fig. 1.
The architecture consists of 5 variables in the input layer and one var­
iable in the output layer. The input variables include catalyst concen­
tration, methanol/mole ratio, temperature, time and agitation speed,

Table 1
Experimental design Matrix for biodiesel production.
Run Catalyst Conc. Methanol/oil ratio Temperature Time Agitation speed Exp. Biodiesel
(wt%) (◦ C) (hours) (rpm) Yield (%)

1 1 6 40 2 400 76.70
2 2 6 40 2 200 72.00
3 1 10 30 2 200 63.30
4 2 10 30 2 400 63.30
5 1 6 30 2 200 79.50
6 2 6 50 2 400 81.10
7 1 10 50 2 400 82.50
8 2 10 50 2 200 70.20
9 1 6 40 4 200 70.20
10 2 6 40 4 400 74.50
11 1 10 40 4 400 73.50
12 2 10 40 4 200 76.90
13 1 6 30 4 400 85.60
14 2 6 30 4 200 81.70
15 1 10 30 4 200 88.30
16 2 10 30 4 400 86.40
17 0.5 8 50 3 300 90.80
18 2.5 8 50 3 300 81.30
19 1.5 4 50 3 300 77.10
20 1.5 12 50 3 300 93.40
21 1.5 8 40 3 300 78.10
22 1.5 8 60 3 300 89.50
23 1.5 8 70 1 300 72.00
24 1.5 8 70 5 300 82.90
25 1.5 8 70 3 100 78.20
26 1.5 8 70 3 500 84.60
27 1.5 8 70 3 300 91.70
28 1.5 8 50 3 300 91.70
29 1.5 8 50 3 300 91.70
30 1.5 8 50 3 300 91.70
31 1.5 8 50 3 300 91.70
32 1.5 8 50 3 300 91.70

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C.M. Agu et al. Waste Management Bulletin 1 (2024) 172–181

Fig. 1. ANN design architecture.

while the biodiesel yield is the output. The examined three algorithms properties. Similarly, the oil extraction method (wet reduction) was
were selected from the neural network app of MATLAB r2018a. 32 previously used by Karlkal and Kudre (2021) and they obtained a yield
experimental runs were designed out of which 22 data were used for of about 95.2 wt% from marine fish waste (MFW). The percentage
training (70 %) while 5 data each (15 %) were used for testing and moisture content (0.073 %) of the CFW oil was lower than (0.65 %)
validation. The testing and validation data provide independent evalu­ previously reported by de Medeiros et al., (2019) for fish waste residue
ation of the algorithm performance and have little or no effect during or used for biodiesel production, which was at extraction condition of 60 ◦ C
after training. Bench mark comparisons between the three investigated and 120 min. The moisture content was also lower than the 0.14 wt%
algorithms were done through the mean square error (MSE) and corre­ previously reported by Karlkal and Kudre (2021) for MFW. However, the
lation coefficient (R2). The MSE measures the average square difference moisture of the CFW oil (0.00) reported in this wok (Table 2) was lower
between input data set (Yexpi ) and the predicted target/output (Ypredi ) than the ASTM biodiesel standard (0.050) for water and sediment vol­
as shown in Equation (4), while the lower value of the MSE is desirable. ume using test method D2709.
The free fatty acid (3.593 mgKOH/Kg) and acid value (7.186
1 ∑N
mgKOH/Kg) for CFW oil as shown in Table 2 were higher than the ASTM
MSE = (Ypredi − Yexpi )2 (4)
N i=1 standard for B6 - B20 biodiesel. However, these values were comparable
with 6.07 mgKOH/g and 3.1 % for acid value and free fatty acid,
Results and discussion respectively, reported previously for MFW extracted oil (Karlkal and
Kudre, 2021). The implication of these values suggests further refining
Physiochemical characterization extracted CFW oil or esterification processes are necessary before transesterification. The
saponification value (295.557 mg/KOH/Kg) as shown in Table 2 were
The cat fish waste (CFW) oil yield of 96.85 % obtained after higher than the value of 196.35 mg/g obtained for river catfish oil
extraction is as shown in Table 2, alongside other physiochemical (Santya et al., 2019) and indicated a considerable concentration of tri­
glyceride suitable as a feedstock for biodiesel.
The viscosity (48.782 mm2s‾1 @ 40 ◦ C) of the CFW oil, which relates
Table 2
its atomization process in diesel engine was comparable to 43 cP @25 ◦ C
Physiochemical characterization of Extracted oil from CFW oil.
reported for MFW by Karlkal and Kudre (2021). However, these values
Parameters Values
were higher than the ASTM recommended standard of 1.9 to 4.1. These
Oil yield (%) 96.85 values showed that further processing of the raw CFW oil via the
Moisture (%) 0.073 transesterification reaction process, was necessary to examine its po­
Density (Kg/m3) 884.6
tential as a suitability feedstock for biodiesel production.
Molecular weight (g/mol) 589.375
Saponification (mgKOH/kg) 295.557
Free fatty acid (mgKOH/kg) 3.593
Smoke point ◦ C 108 Physiochemical characterizations of produced biodiesel from CFW oil
Kinematic viscosity @ 40 ◦ C (mm2s− 1) 48.782
Refractive index @ 29 ◦ C 1.4648 The physiochemical characterization of the produced biodiesel from
Boiling point ◦ C 138 raw CFW oil through transesterification is presented in Table 3. Some of
Acid value (mgKOH/kg) 7.186
the parameters in Table 3 were specific to biodiesel oil and was used to

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Table 3 density value of the CFW biodiesel (867.2 Kg/m3) is comparable with
Physiochemical characterization of the produced biodiesel from CFW oil. those previously reported by Yahyaee et al. (2013) for waste fish oil (867
Parameters Values – 869 Kg/m3) and Tanwar et al. (2013) for fish oil methyl ester (850 -
880 Kg/m3).
Free fatty acid (mgKOH/kg) 1.48
Acid value (mgKOH/kg) 2.96
Cetane number 55.77 FTIR
Boiling point (0C) 107.0
Smoke point (0C) 80.0 The FTIR spectra pattern of the raw (a) and biodiesel (b) produced
Gross calorific value (KJ/g) 10.820
Calorific value (MJ/kg) 44.566
from CFW oil are presented in Fig. 2. The FTIR spectroscopic analysis
API Gravity 30.771 was used to understand the possible changes in functional group and
Diesel index 58.77 tentative peak assignment of the raw and produced biodiesel from CFW
Aniline Point (0F) 191.0 oil (Table 4). As shown in Table 4, the raw oil adsorption band at 3477
Kinematic Viscosity @ 40 ◦ C (mm2s− 1) 9.391
cm‾1 relating to the axial deformation of OH (Kudre et al., 2017) dis­
Density (Kg/m3) 867.2
Flash point (◦ C) 172.0 appeared in the biodiesel. This suggests that the water molecule in the
Fire point (◦ C) 180.0 raw oil could have disappeared after the transesrifictation process. This
Moisture (%) 0.00 is also consistent with the results from the physiochemical character­
izations where the moisture contents were 0.073 % and 0.00 % before
and after transesterification, respectively (Tables 2 and 3). The absence
assess the quality of the transesterified oil, as well its comparison with
of water molecule in the biodiesel further guarantees that the reactions
previously reported studies and biodiesel standards. The combustion
of glycerides to produce soap and water, which contributes to engine
rate and ignition quality measured by the cetane number, higher cetane
corrosion is significantly reduced/controlled (Anguebes-Franseschi
value is essential for engine performance enabling smooth operation
et al., 2019). Similar result by Kudre et al. (2017) reported no adsorption
(Mahmudula et al., 2017). Thus, higher cetane number also suggests
band within the peak ranges of 3500–3000 cm‾1 and attributed it to the
reduced/shorter ignition delays, enabling the immediate start of engine
absence of water in Lebeo rohita fish oil and biodiesel.
(Knothe et al., 2003; Mofijur et al., 2015). However, the cetane number
The weak peak at 3008 cm‾1 in both raw and biodiesel from CFW oil
of the CFW biodiesel (55.77) is comparable to the biodiesel produced
(Table 4) was assigned to the = C–H stretching vibration of alkene
from other feedstock such as palm (59), Jatroha (51) and diesel fuel (48)
(Kudre et al., 2017). Also, in Cyprinu carpio and Lebeo rohita fish oil,
(Mahmudula et al., 2017; Mofijur et al., 2015; 2014).
Fadhil et al. (2015) and Kudre et al. (2017), respectively revealed that
After the transesterification process, the produced biodiesel from
the = C–H stretching vibration of alkene is observed in the upper
raw CFW oil showed remarkable decrease in free fatty acid and acid
adsorption band of slightly above 3000 cm‾1. The strong peaks at
value (Table 3) compared to the raw CFW oil (Table 2). This shows the
2922.2 and 2855.1 cm‾1 in both raw and biodiesel CFW oil (Table 4),
crucial role of transesterification in biodiesel production. However, the
were indicative of the vibrational characteristics of methyl (CH3) found
acid value of the biodiesel did not meet the recommended ASTM stan­
in ester chain of biodiesel (Fadhil et al., 2015; de Medeiros et al., 2019;
dard of 0.50 suggesting that the produced oil from CFW oil requires
Anand et al., 2015). The weak peaks at 2150.7 and 2023.9 cm‾1 in the
further processing.
raw CFW oil disappeared in the biodiesel possibly as a result of the
The kinematic viscosity is essential to monitor atomization processes
transesterification process.
in diesel engine due to insufficient lubrication. Low viscosity contributes
The adsorption peak at 1744.4 cm‾1 in the raw CFW oil appeared at
to leakage, while high viscosity fuel results to incomplete combustion
1736.9 cm‾1 in the biodiesel and was assigned to the C = O stretching of
(Bhuiya et al., 2016; Balat et al., 2011). In this view, acceptable viscosity
carbonyl ester. Previously, Fadhil et al. (2015) assigned similar peak
range and standard is often outlined by regulatory agencies and stan­
(1751 cm‾1) in Cyprinu carpio fish oil to the C = O stretching vibration of
dardization authorities. The kinematic viscosity @ 40 ◦ C of the trans­
carbonyl ester. In addition, de Medeiros et al., (2019) also assigned
esterified biodiesel from CFW oil is 9.391 mm2s‾1 (Table 2). This value is
similar peak (1740 cm‾1) in fish waste oil residue to C = O stretching of
slightly higher than the ASTM recommended values of 1.6 – 6mm2s‾1.
carbonyl group. The peaks at 1461.1 – 1376.4 cm‾1 in the raw oil and
However a significant reduction was observed from the viscosity of the
1461.1 – 1375.1 cm‾1 in biodiesel (Table 4) correspond to the vibra­
raw CFW oil (48.782 mm2s‾1) in Table 2 and the transesterified product,
tional characteristics of –CH group of methyl ester. This observation
biodiesel (9.391 mm2s‾1) in Table 3.
clearly indicated the conversion of CFW oil triglycerides to fatty acid
Flash point indicates the flammability of fuel and handling safety
methyl ester.
(Mahmudula et al., 2017). The higher flash point (172 ◦ C) of the CFW
The peaks at 1237.5 – 1159.2 cm‾1 in the raw oil and those at
biodiesel shown in Table 3 was high than US and EU standard limits of
1241.2, 1159.2 and 1118.2 cm‾1 in the biodiesel (Table 4) were
93 ◦ C and 120 ◦ C for biodiesel, respectively, suggesting the safe handling
assigned to the stretching vibrations of the –C-O- ester group (Fadhil
of the CFW biodiesel. Previous studies reported that biodiesel is asso­
et al., 2015; Mothé et al., 2011). As a result of the transesterification
ciated with higher flash point compared to conventional diesel indi­
process, new peaks appeared in the CFW biodiesel oil at 1036.2 and
cating their safe handing (Bhuiya et al., 2016; Balat et al., 2011; Jayed
857.3 cm‾1. These peaks were absent in the raw oil and were attributed
et al., 2011; Lim and Teong, 2010). The calorific value measures the
to the O-CH3 stretching (Kudre et al., 2017). The overlapping methylene
amount thermal energy released per quantity of fuel burned. The heat­
–CH₂ was assigned to the peak located at 723.1 cm‾1 observed in both
ing value of the transesterified biodiesel from CFW oil as shown in
the raw and biodiesel of CFW oil.
Table 3 was below the method EN14213 recommended heating value of
35 MJ/Kg for biodiesel (Atabani et al., 2012).
SEM-EDX of the fish bone catalyst
It is evident that density affects internal combustion engine by
altering the mass of the injected fuel (Chauhan et al., 2010; 2012). Diesel
The structural surface morphology of the calcined fish bone used as
engine is also a function density as higher density fuel could cause
heterogeneous catalyst, as well as its elemental compositions is shown in
particulate matter and NOx emission (Mahmudula et al., 2017). It can be
Fig. 3. During the SEM-EDX analysis, sample excitement through an
seen that the densities of the raw CFW oil (Table 2) and transesterified
energy source such as electron allows the dissipation of the adsorbed
biodiesel (Table 3) were relatively low and comparable to other bio­
energy and generates the sample compositions. Peak position in the
diesel from edible feedstock such as crude coconut oil (908.9 Kg/m3)
spectrum is associated with the element, while the signal intensity gives
and corn oil (0.9089 Kg/m3) (Mahmudul et al., 2017). In addition, the
the elemental concentration. The surface morphology of the calcined

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C.M. Agu et al. Waste Management Bulletin 1 (2024) 172–181

Fig. 2. FTIR spectroscopic analysis of the raw (a) and biodiesel (b) produced from CFW oil.

composition table (Fig. 3), it was evident that carbon, calcium, phos­
Table 4
phorous and sodium with weight concentrations of 69.96, 16.32, 8.24,
Peak and spectroscopic assignments of the CFW raw and biodiesel oil.
and 1.81, respectively were the primary elements in the fish bone
Wave number (cm‾1) catalyst. Carbon was the major element by weight and atomic mass,
Raw CFW oil CFW biodiesel Peak assignments indicating that the fish bone could be synthesized further to a carbon
3477 – OH axial deformation
based catalyst to offer enhance catalytic activity. The presence of cal­
3008 3008 =C–H stretching vibration (alkene group) cium and phosphorous indicates the potentials of the calcined fish bone
2922.2 2922.2 methyl (CH3) or methylene group in ester for biodiesel production. Jayakumar et al. (2021) revealed that the
2855.1 2855.1 methyl (CH3) or methylene group in ester application of calcined catalyst for the conversion of feed stock (animal
2150.7
fat/vegetable oil) into biodiesel is not only effective, but safe with
– –
2023.9 – –
1744.4 1736.9 C = O Carbonyl group enhanced yield of about 98 %.
1461.1 1461.1 C–H stretching of methyl ester
1376.4 1375.1 C–H stretching of methyl ester
1237.5 1241.2 -C-O- ester group stretching ANN modeling
1159.2 1162.9 -C-O- ester group stretching
1118.2 -C-O- ester group stretching
Three algorithm of the ANN design architecture were used to predict
–
– 1036.2 O-CH3 stretching
– 857.3 O-CH3 stretching biodiesel yield from CFW oil. The predictions and performance evalua­
723.1 723.1 methylene –CH2 stretching tions of these three algorithms were compared with the experimental
biodiesel responses to identify the optimum training algorithm as shown
in Table 5. Comparing the ANN predicted biodiesel responses from the
fish bone was obtained before the transesterification process. From the
scaled conjugate gradient (trainscg), bayesian regularization (trainbr),
SEM image, the irregular shape of the calcined catalyst was evident
levenberg maraquardt (tainlm) (Table 5), algorithm; it was observed
indicating that its particle size was not uniform. From the EDX elemental
that the best fit is associated with the scaled conjugate gradient

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C.M. Agu et al. Waste Management Bulletin 1 (2024) 172–181

Fig. 3. SEMEDX of the fish bone catalyst.

Table 5
Design matrix for biodiesel production with ANN predicted responses.
Cat conc. Methanol/oil ratio Temperature Time Agitation speed Exp. Biodiesel yield ANN predicted

trainscg trainbr tainlm

1 6 40 2 400 76.7 76.8291 56.9173 66.8271

2 6 40 2 200 72.0 70.5920 40.5927 60.8807
1 10 30 2 200 63.3 72.9172 62.7249 52.9108
2 10 30 2 400 63.3 63.4242 33.4228 53.7840
1 6 30 2 200 79.5 78.5427 48.2762 58.5476
2 6 50 2 400 81.1 81.1638 41.3861 41.1663
1 10 50 2 400 82.5 82.5136 22.3675 32.5676
2 10 50 2 200 70.2 70.2500 30.0037 60.2530
1 6 40 4 200 70.2 76.4555 46.5526 66.4527
2 6 40 4 400 74.5 78.4323 48.2393 68.4304
1 10 40 4 400 73.5 90.6369 30.6911 70.6980
2 10 40 4 200 76.9 76.9598 26.9865 56.9861
1 6 30 4 400 85.6 85.6300 15.0048 55.6045
2 6 30 4 200 81.7 81.7909 51.6098 51.7666
1 10 30 4 200 88.3 88.3276 38.7673 68.3611
2 10 30 4 400 86.4 86.4576 46.5765 48.8409
0.5 8 50 3 300 90.8 90.8083 30.8326 40.8377
2.5 8 50 3 300 81.3 81.2916 21.1667 21.2666
1.5 4 50 3 300 77.1 77.1992 27.9299 37.1290
1.5 12 50 3 300 93.4 88.8649 28.4912 48.8910
1.5 8 40 3 300 78.1 78.2154 38.5442 58.2448
1.5 8 60 3 300 89.5 89.4962 19.6259 59.4256
1.5 8 70 1 300 72.0 71.9867 51.6792 51.9794
1.5 8 70 5 300 82.9 92.5753 32.5314 42.5318
1.5 8 70 3 100 78.2 75.7151 45.5171 55.7173
1.5 8 70 3 500 84.6 84.5846 24.4601 54.5607
1.5 8 70 3 300 91.7 91.6664 11.6413 51.6477
1.5 8 50 3 300 91.7 91.7009 11.1094 61.7097
1.5 8 50 3 300 91.7 90.7009 10.6094 40.7609
1.5 8 50 3 300 91.7 90.7009 20.0094 60.7074
1.5 8 50 3 300 91.7 91.7009 21.0094 71.7095
1.5 8 50 3 300 91.7 91.7009 19.0094 41.7098

Trainscg: Scaled conjugate gradient, trainbr: Bayesian regularization, trainlm: Levenberg maraquardt.

(trainscg). Fig. 4 shows the ANN regression from the best fit algorithm
[scaled conjugate gradient (trainscg)]. The ANN algorithm with trainscg
produced comparable predictions to the experimental, indicating the
derivative functions of the weight and transfer function. In this case,
attaining the maximum number of epoch stops the training. Further­
more, the scaled conjugate gradient (trainscg) is specifically based on
conjugate direction and without the ability to perform line search
(Babani et al., 2016). However, Babani et al. (2016) reported that the
scaled conjugate gradient is computationally expensive and was
developed as an alternative to line search due to its reduced processing
time. The average means square error (MSE) versus epoch plot for the
trainscg algorithm as shown in Fig. 5, indicates that the best validation
performance was obtained at epoch 7 with the value of 29.7604.
The correlation between outputs and targets is measured by the R2
value and was examined and compared between the three algorithms,
while the average squared difference (MSE) between outputs and targets
were computed as shown in Table 6. Yetilmezsoy and Demirel (2008)
reported that the optimum ANN design architecture and its parameter

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C.M. Agu et al. Waste Management Bulletin 1 (2024) 172–181

Fig. 4. Regression of the ANN output for scaled conjugate gradient (trainscg).

Fig. 5. Training, validation and test of the mean square error of the scaled conjugate gradient (trainscg).

179
C.M. Agu et al.
Table 6
Performance evaluation of the selected ANN algorithm.
Data set MSE R2
Scaled conjugate gradient (trainscg)
Training 22 0.16334 0.8287
Validation 5 12.3543 0.9429
Testing 5 1.08334 0.9906
Levenberg maraquardt (trainlm)
Training 22 9.56433 0.7811
Validation 5 17.3423 0.8167
Testing 5 11.3452 0.6172
Bayesian regularization (trainbr)
Training 22 15.0023 0.6723
Validation 5 81.3542 0.7112
Testing 5 10.4663 0.7821
differences were evaluated through the minimum value of the MSE. Ani
et al. (2021) also reported that the learning protocols of ANN, such as
the training, validation and testing with respect to R2 could be used to
evaluate performance.
In the optimization and performance evaluations of the three algo­
rithms, 10 neurons were used in the hidden layer as initial guess.
Increasing the number of neurons from 10 to 30, the three algorithms
gave minimum values for the MSE. Table 6 illustrates the performance
evaluation comparisons of the three algorithms. Considering the per­
formance evaluation factors, Table 6 shows that lowest and highest MSE
and R2 were obtained for the scaled conjugate gradient (trainscg). In
addition, the MSE and R2 for the training, validation and testing pa­
rameters for the scaled conjugate gradient were considerably better
compared to the Bayesian regularization and Levenberg maraquardt
algorithms (Table 6). For instance, the bulk of the data set used in
training (70 %) indicated that the trainscg with R2 of 0.8287 (82.87 %)
performed better, compared to the 0.7811 (78.11 %) and 0.6723 (67.23
%) for the trainlm and trainbr, respectively.
Similar modelling results using ANN and other modelling tools have
been reported in the literature by many researchers. For instance, ANN
and RSM were used in modelling methyl ester yield from Prunus amyg­
dalus seed oil by Esonye et al. (2019) and reported that ANN was better
predictive model than RSM, with the former having higher R2 value of
0.96637, as against 0.9446 obtained for the later model. Most recently,
Agu et al. (2023) compared the modelling efficiencies of Adaptive
Neuro-fuzzy Inference System (ANFIS), Artificial Neural Network (ANN)
and Response Surface Methodology (RSM), for the methyl ester pro­
duction yield from Azadirachta Indica seed oil. In their work, which they
reported the supremacy of ANFIS, followed by ANN, with R2 values of
0.9768, 0.9995 and 0.9999, for RSM, ANN and ANFIS, respectively. For
the modelling of biodiesel yield from palm oil using Moringa oleifera
leaves as heterogeneous catalyst, Kolakoti et al. (2022) reported that
ANN was a better predictive model than RSM. They found out that the
models predicted biodiesel yields of 92.97 % and 91.14 %, for ANN and
RSM, respectively. Similarly, in modelling biodiesel yield from micro­
algae, ANN was also reported to be better predictive model than RSM,
according to the results obtained by Gul et al. (2022). The result indi­
cated RSM and ANN models predicted values have R2 values of 0.92 and
0.94, respectively. In like manner as regards use of waste oil, ANN and
RSM were used to model/predict biodiesel yield from waste cooking oil,
and it was also found that ANN was better predictive model (Soji-Ade­
kunle et al., 2018). They reported that the ANN model had R2 value of
0.9843, compared to 0.9376 for the RSM model.
Conclusion
In this present study, calcined (600 ◦ C for 4 h) fish bone heteroge­
neous catalyst was used in the transesterification process of CFW oil to
produce biodiesel. The elemental compositions of the calcined fish bone
catalyst through the SEM-EDX showed the presence of calcium, carbon,
phosphorous and sodium. These elements are indicative of the catalytic
180
Waste Management Bulletin 1 (2024) 172–181
activity of the fish bone catalyst. The physiochemical properties of the
raw CFW oil highlight the need for transesterification. However, the
produced biodiesel showed enhanced physiochemical properties but
needs further treatment to meet the requirements of the conventional
biodiesel standards. The appearance of the ester group stretching vi­
brations as observed from the FTIR result was indicative of the raw CFW
oil conversion to biodiesel. Amongst the three algorithms of the ANN,
the scaled conjugate gradient (trainscg) produced comparable pre­
dictions with the experimental results, as well as the lowest MSE and
highest R2 values. Therefore, local biodiesel producing firms could
harnessed the potential of CFW oil and fish bone as heterogeneous
catalyst, as suitable low-cost feedstock, as well as help curb the menace
of catfish waste disposal problems.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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