67 Verification of Pore Size Effect

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Veriﬁcation of Pore Size Effect on Aqueous-Phase Adsorption Kinetics: A Case

Study of Methylene Blue
Article in Colloids and Surfaces A Physicochemical and Engineering Aspects · July 2021

DOI: 10.1016/j.colsurfa.2021.127119
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Verification of Pore Size Effect on Aqueous-Phase

Adsorption Kinetics: A Case Study of Methylene
Blue
Joshua O. Ighalo, Kingsley O. Iwuozor, Chinenye

Adaobi Igwegbe, Adewale George Adeniyi
PII: S0927-7757(21)00988-2
DOI: https://doi.org/10.1016/j.colsurfa.2021.127119
Reference: COLSUA127119
To appear in: Colloids and Surfaces A: Physicochemical and Engineering

Aspects
Received 9 May 2021
date:
Revised date: 26 June 2021
Accepted 30 June 2021
date:
Please cite this article as: Joshua O. Ighalo, Kingsley O. Iwuozor, Chinenye
Adaobi Igwegbe and Adewale George Adeniyi, Verification of Pore Size Effect
on Aqueous-Phase Adsorption Kinetics: A Case Study of Methylene Blue,
Colloids and Surfaces A: Physicochemical and Engineering Aspects, (2021)
doi:https://doi.org/10.1016/j.colsurfa.2021.127119
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Verification of Pore Size Effect on Aqueous-Phase Adsorption Kinetics: A Case Study of
Methylene Blue
Joshua O. Ighalo1, 2*, Kingsley O. Iwuozor3, 4, Chinenye Adaobi Igwegbe1**, Adewale

George Adeniyi2
1
Department of Chemical Engineering, Nnamdi Azikiwe University, P. M. B. 5025, Awka, Nigeria
2
Department of Chemical Engineering, University of Ilorin, P. M. B. 1515, Ilorin, Nigeria
3
Department of Chemistry, University of Lagos, P. M. B. 1029, Lagos, Nigeria.
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4
Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University, P. M. B. 5025, Awka,
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Nigeria.
*
Corresponding author, Email address: oshea.ighalo@yahoo.com ; jo.ighalo@unizik.edu.ng
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**
Corresponding author, Email address: ca.igwegbe@unizik.edu.ng
ORCID
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Joshua O. Ighalo, https://orcid.org/0000-0002-8709-100X
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Kingsley O. Iwuozor, https://orcid.org/0000-0002-1161-2147
Chinenye Adaobi Igwegbe, https://orcid.org/0000-0002-5766-7047
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Adewale George Adeniyi, https://orcid.org/0000-0001-6615-5361

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Abstract
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Due to the negative environmental effect of methylene blue (MB), researchers have been
investigating several aspects of its adsorption. The kinetics/rapidity is an important aspect of its
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uptake which is affected by the adsorbent pore properties. The aim of this study was to
investigate the effect of pore size on the adsorption kinetics of methylene blue (MB). The paper
employed a novel methodology where empirical findings across studies were summarised,
analysed juxtaposed to derive observations. It was observed from the study that the kinetic
constant increased as the pore size progressed from the macroporous to the mesoporous range.
However, MB uptake was significantly slower for micropores. Microporous pore size leads to a
drop in kinetic constant because the diffusion of MB through very small pores is restricted and
gradual due to the adsorbate size. The mesoporous range is the superior pore size for MB
adsorption kinetics. The Pseudo-second-order (PSO) model was best suited for all cases.
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However, 15% of the studies for mesoporous adsorbent had Pseudo-second-order (PFO) model
as best-fit and 6% for microporous adsorbents. PSO is superior to PFO because it captures both
the amount of active sites and the concentration of adsorbate as rate-limiting factors. It was
observed that 10% of the studies had PFO as best-fit when linear modelling was used but 15%
was best-fit with non-linear modelling. This was due to the mathematical simplicity of the
linearised form of the PSO and the errors generally associated with the linearisation of kinetic
models.
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Graphical abstract
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Keywords: Adsorption; Kinetics; Methylene Blue; Pore size; Pseudo-first-order; Pseudo-
second-order
1. Introduction
The knowledge of the pore structure of adsorbents such as pore size and shape, pore
surface chemistry and pore volume allows adsorbents to be tailored and designed for enhanced or
selective removal of specific contaminants [1]. This, therefore, has led to an increase in the
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demand for porous materials to be used as adsorbents [2]. Pore size refers to the distance
between two opposite walls of the pores in an adsorbent [3]. According to the International
Union of Pure and Applied Chemistry (IUPAC), pore sizes can be classified into three;
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macropores (pore sizes greater than 50 nm), mesopores (pore sizes between 2-50 nm), and
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micropores (pore sizes below 2 nm) [4, 5]. Although, the pore size distribution affects the uptake
of adsorbate by the adsorbent, there exist limited studies on its relationship with the adsorption
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kinetics [6].
Adsorption can either be physical or chemical with respect to its mechanism. When the
adsorbate species are to be bonded chemically, it is expected that the contact time and the
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equilibration time should be longer than when it is to bind physically [2]. Irrespective of whether
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the adsorption is physical or chemical, it has been reported in the literature that the uptake of the
adsorbate species slows down as the reaction time increases [6, 7]. This could be as a result of
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the reduction in the vacant active sites on the adsorbent and an increase in repulsive forces
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between the solute molecules on the solid and bulk phases [8].
Modelling in general (such as isotherm, thermodynamics, statistical response, statistical
physics) and kinetic modelling, in particular, are a very important aspect of any adsorption study
[9-12]. For kinetics, the rapid uptake of the adsorbate by the adsorbent, the residence time, and
its speed to attain equilibrium is an important yardstick for the determination of an efficient
adsorbent [2, 13, 14]. It can provide valuable information into the sorption mechanism albeit not
to a conclusive extent [15-17]. The kinetic models that are regularly observed as best-fits for
adsorption are the pseudo-first-order (PFO) and the pseudo-second-order (PSO). This is because
they are classical models with mathematically simple expressions that fit adsorption data well,
especially when the modelling is done with non-linear techniques [18-20]. The PFO model was
3
developed by Lagergren and Svenska [21]. It assumes that adsorption first order in nature as it is
only dependent on the number of adsorbate present at the specific time in the solution [22, 23].
The PSO model was initially developed by Blanchard et. al [24] but publicised in the field of
adsorption by Ho and McKay [25]. It assumes that the adsorption is dependent on the number of
metal ions present in the solution as well as the free sites on the adsorbent surface [26].
Methylene Blue (MB) also referred to as Tetramethylthionine chloride as shown in
Figure 1 is a cationic thiazine dye with IUPAC name 3,7-bis(dimethylamino)-phenothiazin-5-
ium chloride and chemical formula C16H18N3SCl. It is popularly used as a drug, for biological
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staining, as a chemical indicator and dye [27-29]. The characteristics of MB without the chloride
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ion is outlined in Table 1 as stated by Pelekani and Snoeyink [30]. MB is widely used in the
rubber, plastics, paper, textile, cosmetics, wool, and pharmaceutical industries [31]. It usually
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enters the environment from the effluents of these industries in which it is used [32]. High MB
concentration in the aqueous environment can lead to cytotoxic, neurotoxic and mutagenic
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effects [31]. Methods for MB removal from water includes ozonation [33, 34], photodegradation
[35], membrane processes [36-38], electro-coagulation [39, 40], and biological processes [41,
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42]. These degradation and membrane processes can be quite expensive and also generate
sludge. Due to its complex aromatic nature, MB is difficult to break down via biological process
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[43]. Among various strategies for removing MB from water, adsorption is considered one of the
most effective [44]. Just as for most other dyes, it is cheap and easy to implement [45-48].
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Figure 1. Chemical structure of Methylene Blue (MB)
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Table 1. Properties of MB [49]
Properties Value
Molecular weight (g/mol) 319.9
Molar volume (cm3/mol) 241.9
Solubility at 25oC (g/L) 43.6
Log Kow 0.75
pKa 3.14
Length (nm) 1.447
Width (nm) 0.950
Thickness (nm) 0.40
To gain better insights into the adsorption rate, this research utilised and applied two
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kinetic models, viz; Pseudo-first order and pseudo-second order kinetic models to interpret the
result as they are the commonly used models in methylene blue (MB) adsorption kinetics. The
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aim of this study was to investigate the effect of pore size on the adsorption kinetics of MB. The
paper employed a novel methodology where empirical findings were analysed and juxtaposed to
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derive observations. MB was considered for this analysis because it is the most regularly
occurring and regularly investigated dye for adsorption technology [50]. Considering the
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widespread issues from its proliferation, the results of this study will be relevant to a broader
audience and will help in a better understanding of the MB adsorption process.
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2. Methodology
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2.1 Data collection and description

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For this study, all published literature on MB adsorption from aqueous media within the
past five (5) years was considered. Over 500 research papers have been published on the subject
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in this period. However, only studies reporting the pore sizes of the adsorbent were analysed for
this study. The pore sizes were reported in nm and corresponding kinetics constants were also
reported. The adsorbents were classed into macroporous (> 50 nm), mesoporous (2 – 50 nm) and
microporous (< 2 nm) The finalised data used for this analysis is shown in Table 2. Also, the
technique of modelling whether linear (L) or non-linear (NL) is reported as this bears a
significance on modelling accuracy. The K values for either PSO or PFO was reported based on
which was best-fit. For cases where both were well fitted, both and were stated.
Only MB was considered in this analysis adsorbate type influence adsorption kinetics.
The molecular size and weight influence the mobility of the adsorbate in the aqueous phase. To
eliminate this as an extraneous factor, only MB was chosen. MB itself is the most studied dye in
5
literature [51] with a vast pool of recent papers. Also, equilibrium time was not considered for
this investigation because it is unsuitable for making a comparison across different
investigations. The time for achieving equilibrium is overly dependent on the choice of adsorbate
initial concentration and adsorbent dosage.
2.2 Research problem

To verify the effect of pore size on adsorption kinetics, the data were analysed in a
variety of ways. The key goal was to evaluate how pore size relates to the kinetic constants. The
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study will try to evaluate if there was there a relationship from empirical investigations between
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pore size and uptake kinetics. In regards to model best fits, the study also tries to identify if the
pore sizes influence the type of model that fits the kinetic data. The study also examines the
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influence of the modelling technique (whether linear or non-linear) on adsorption kinetics.
Adsorbent name Average

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Table 2. Data on MB uptake pore sizes and adsorption kinetic constants
PFO PSO Modelling Ref.
pore size (1/min) R2 R2 type
Pr
(nm) (g/mg.min)
Modified graphene oxide hydrogel 200.0 - - 0.052 1.0000 L [52]
Silica aerogel/ Ni/ C/ N 126.0 - - 0.01825 0.9996 L [53]
SiO2 100.0 - - - - - [54]
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Graphene alginate nanocomposite 55.70 - - - 0.998 L [55]

Kaolinite 54.20 - - 0.034 0.9997 L [56]
Montmorillonite 47.41 - - - - - [57]
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Fe3O4/ Montmorillonite 46.39 - - 0.011 0.9999 L [57]

AC from banana peel 36.88 - - 0.4630 1.000 L [58]
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Hydroxyapatite/ 5% sodium alginate 35.73 - - 0.026 0.9990 NL [59]

Hydroxyapatite 30.00 - - 0.006 0.9990 NL [59]
Magnetite NPs @ pH 12 30.00 - - - - - [60]
Hydroxyapatite/ 10% sodium alginate 28.68 - - 0.015 0.9990 NL [59]
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Porous PVA/Zn-Fe-Mn oxide nanocomposite 26.00 - - 1.8500 0.9485 L [61]

Pine biomass/magnetite 25.86 - - - - - [62]
Na2SiO3.5H2O/Cr2(SO4)3 24.30 0.0180 0.9975 - - L [63]
MCC 22.72 - - 34.32 1.0000 L [64]
Fe3O4 22.50 - - - - - [57]
Gum ghatti/TiO2 NPs 20.56 - - 0.497 0.9990 L [65]
Biosorbent from Metroxylon sagu/ H3PO4 20.23 - - 0.0000947 0.9998 L [66]
Biosorbent from Metroxylon sagu 18.81 - - 0.00000951 0.9999 L [66]
Biosorbent from coffee husk 17.83 - - 0.00215 0.9798 NL [67]
Montmorillonite/MnO2 nanosheets 17.30 - - 0.00355 0.9900 L [68]
Montmorillonite/MnO2 nanowires 17.29 - - - - - [68]
Tannin from persimmon/graphene oxide 16.92 - - 0.013 0.9960 NL [69]
Montmorillonite 16.51 - - - - - [68]
Oiltea shell/Trametes versicolor 16.50 0.0020 0.9939 L [70]
Oiltea shell/Pycnoporus sp. 16.32 0.0030 0.9957 L [70]
Magnetic graphene oxide/citric acid 16.00 - - 0.000039 0.9983 L [71]
Modified MnO 15.97 - - 0.000047 0.9710 L [72]
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Oiltea shell 15.95 - - 0.0050 0.9951 L [70]
Fe3O4-TiO2 NPs/ methyltrimethoxysilane 15.86 - - 0.4900 0.9990 L [73]
Gelatin/alginate composite 15.60 - - 0.0001071 0.9990 NL [74]
Polyamide-vermiculite nanocomposites 15.39 - - 0.0023 0.9900 NL [75]
Biochar from vermicompost 15.05 - - 0.033 0.9996 NL [76]
Na2SiO3.5H2O/ZnSO4.7H2O 15.00 0.0140 0.9967 - - L [63]
Poly (trimesoyl chloride-melamine)/Palygorskite 14.20 - - 0.0755 0.9995 L [77]
Polyaniline/TiO2 14.09 - - 0.0009 0.9959 NL [78]
Polyaniline/ZnO/Seaweed 13.68 - - - 0.9986 - [79]
Biochar from Barley malt bagasse 13.35 - - - - - [80]
Fe-Mn binary oxide nanoparticles 12.65 - - 0.2105 0.9900 NL [81]
Sodium dodecyl sulfonate modified ZnFe2O4 12.42 - - 0.00214 0.9980 L [82]
Woody Biochar 12.31 - - - - - [83]
Montmorillonite/LDH nanoflakes 11.10 0.1190 0.9920 0.003325 0.9970 NL [84]
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β-cyclodextrin/Pinus radiata cones 10.98 - - - 0.9642 NL [85]
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Corn starch/nano-SiO2 10.80 - - 0.0274 0.9990 NL [86]
Sheep manure biochar 10.03 - - 0.0010 0.9829 NL [87]
Magnetic γ-Fe2O3/ SiO2 nanocomposite 10.00 - - 12.42 0.9990 NL [88]
Graphene oxide/ citric acid/corn straw 10.00 - - 0.00056 0.9911 L [71]
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Microwave modified SiO2 NPs 9.840 - - 0.0826 0.9720 NL [89]
Bentonite/alginate 9.600 - - 0.000192 0.9900 NL [90]
Iraqi red kaolin clay 9.540 0.1800 0.9900 - - NL [91]
Graphene oxide/TiO2 9.500 -
e- - - - - [92]
Rabbit faeces biochar 8.640 - - 0.0150 0.9674 NL [87]
Chitosan/sepiolite 8.470 0.020 0.9960 0.00385 0.9960 NL [93]
SiO2 NPs from Rice husk 8.440 - - 0.0838 0.9848 NL [89]
Pr
Bovine bone biochar 8.321 - - 0.003 0.9990 NL [94]
Bovine bone biochar/ Mg 2:1 Al 8.006 0.1874 0.9990 0.009 0.9990 NL [94]
Kaolinite/H2SO4 7.800 - - 0.023 0.9999 L [56]
Clay 7.560 - - - - - [95]
Biosorbent from Metroxylon sagu 7.484 - - 0.00000199 0.9999 L [66]
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Commercial AC/AgCl 7.477 - - 0.0267 0.9999 - [96]

Pig manure biochar 7.330 - - 0.0060 0.9639 NL [87]
Graphene oxide/citric acid/corn straw 7.000 - - 0.00072 0.9951 L [71]
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Modified Biochar from Empty fruit bunch 6.840 - - 0.008 1.0000 NL [97]
Zeolite AC 6.800 - - 3164000 0.9900 NL [98]
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Magnesium silicate/AC 6.510 - - 22.76 0.9970 L [99]

AC from matured tea leaf/ Sulfonic acid 6.000 - - - - - [100]
Magnetite NPs @ pH 11 6.000 - - - - - [60]
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AC from tomato waste 5.916 - - - - - [101]

Modified montmorillonite 5.883 - - 0.0007 0.9990 L [102]
Cyanobacteria/Polypropylene 5.860 - - - - - [103]
AC/clay from pomace oil 5.830 0.056 0.9900 0.007230 0.9900 NL [104]
Bentonite/zeolite 5.800 - - 0.00123 0.9967 NL [105]
AC/Cu 5.741 - - 0.000336 0.9991 L [106]
Manganous (II) based MOF 5.618 - - - 0.9997 L [107]
AC 5.510 - - 0.000941 0.9990 L [108]
Fe3O4 NPs/Sodium alginate/AC 5.490 8.630 0.9925 0.00056 0.9997 NL [109]
Biochar from Eichornia crassipes 5.319 - - 0.002 0.9900 NL [110]
Nanogel polyvinyl alcohol 5.300 - - 0.00442 0.9998 L [111]
Na2SiO3.5H2O/Fe2(SO4)3 5.291 0.0270 0.9902 - - L [63]
Biochar from weeds 5.140 - - - - - [112]
Biochar from Eucalptus sheathiana bark 5.100 - - 0.017 0.9990 L [113]
Biosorbent from Pinus durangensis 5.100 - - - - - [114]
Magnetite NPs @ pH 10 5.000 - - - - - [60]
SiO2 4.900 - - 0.114 1.0000 L [115]
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Bovine bone biochar/ Mg 3:1 Al 4.737 - - 0.036 0.9980 NL [94]
Mesoporous silica 4.732 - - 0.0110 0.9950 NL [116]
TiO2/Carbon 4.650 - - 0.005 0.9980 L [117]
Titanate nanotube 4.640 - - - - - [118]
AC from shrimp shell 4.500 - - 0.00001087 0.9914 NL [119]
AC 4.430 - - - - - [120]
AC from Eucalyptus residue 4.400 - - 0.000995 0.9998 L [121]
Biochar from Empty fruit bunch 4.350 - - 0.013 1.0000 NL [97]
Carbon fiber aerogel from cotton 4.169 0.05129 0.9957 0.004935 0.9986 L [122]
Biochar from Carbon waste 4.130 - - 0.010 0.9900 NL [123]
γ-Alumina NPs 4.130 - - - - - [124]
α-cellulose from oil palm fronds pulp 4.060 - - - - - [125]
(Fe3O4/Polyacrylic acid)-MOF 4.030 - - 0.0000167 0.9980 L [126]
Mesoporous carbon 4.000 0.1670 0.9960 0.0030 0.9990 NL [127]
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Mesoporous carbon nanofibers 4.000 0.04666 0.9923 0.001602 0.9978 L [128]
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Polyvinyl alcohol/sodium alginate/graphene oxide 3.954 - - 0.0003 0.9998 L [129]
Terminalia catappa shell/Nitric acid 3.844 - - 25.819 1.0000 L [130]
Sewage sludge-derived biochar 3.828 - - 0.1455 1.0000 L [131]
Ball-milled biochar/Fe3O4 NPs 3.820 - - 0.0000755 0.9870 NL [132]
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TiO2/Polyvinyl alcohol nanocomposite 3.814 - - - 0.9974 L [133]
AC from cellulose/montmorillonite 3.810 - - 0.001 0.9999 L [134]
Bamboo AC (aqueous carbonised) 3.804 - - 0.0003880 0.9998 NL [135]
Bamboo AC (acid carbonised) 3.781 -
e- - 0.0001972 0.9999 NL [135]
Biochar from weeds/ 20% HNO3 3.740 - - - - - [112]
Graphene oxide/chitosan/Cu-MOF 3.711 - - 0.092 0.9976 NL [136]
AC from charcoal/TiO2 3.710 - - - - - [137]
Pr
AC from charcoal 3.708 - - - - - [137]
AC from loofah sponge @ 1000˚C 3.700 0.0121 0.9851 - - L [138]
Unmilled sugarcane bagasse biochar 3.700 - - - - - [139]
Birnessite 3.700 - - - - NL [140]
Biochar from weeds/ 40% HNO3 3.660 - - - - - [112]
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AC from Coconut leaf 3.650 - - 0.0470 1.0000 NL [141]

Lathyrus sativus husk + H2SO4 3.640 - - 2034 1.0000 L [142]
Biochar from weeds/ 65% HNO3 3.570 - - 0.0002 0.9909 NL [112]
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AC from olive ash 3.560 0.0976 0.9900 0.04738 0.9900 NL [143]

Charcoal 3.558 - - - - - [137]
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Lacosperma secundiflorum hydrochar 3.550 0.1730 0.9900 0.01880 0.9900 NL [144]

Bovine bone biochar/ Mg 4:1 Al 3.513 0.323 0.9980 0.026 0.9980 NL [94]
AC/ alginate beads 3.430 - - 0.0001638 0.9990 L [120]
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Macrogel polyvinyl alcohol 3.400 - - 0.00292 0.9991 L [111]

AC/ Iron/ Cerium 3.390 - - 0.000623 0.9990 L [108]
AC from Acacia mangium using CO2/KOH 3.390 - - - - - [145]
AC from pine wood sawdust 3.316 - - 8.00 0.9999 L [146]
β-cyclodextrin/chitosan/graphene oxide 3.293 - - 0.000153 0.9952 NL [147]
CuO/ Meso-silica nano composite 3.240 - - 0.0245 0.9960 NL [148]
AC from chitosan 3.204 0.113 0.9990 0.0376 0.9990 NL [149]
Red mud/sucrose carbon 3.200 - - 0.0300 0.9990 NL [150]
Na2SiO3.5H2O/NiSO4.7H2O 3.190 0.0190 0.9966 - - L [63]
Magnetic sawdust carbon/EDTA 3.180 - - 0.1670 0.9990 L [151]
Meso-silica nano composite 3.180 - - 0.0243 0.9890 NL [148]
Untreated Lathyrus sativus husk 3.139 - - 878.0 0.9999 L [142]
Lathyrus sativus husk + H3PO4 3.132 - - 3189 1.0000 L [142]
AC From Grass waste 3.120 - - 0.01454 0.9900 NL [152]
Zeolite/HCl 3.090 - - - 0.9999 NL [153]
Biochar from Camellia oleifera seed shell 3.086 - - 0.000812 1.0000 NL [154]
Ultrasound AC 3.070 - - - - - [108]
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Oil palm ash zeolite/Chitosan 3.048 4360 0.9900 48100 0.9900 NL [155]
Hectorite/alginate 2.920 - - - 0.9980 NL [156]
Fe/ AC from Acorn shell 2.904 - - 0.0000947 - NL [157]
Resin from diallylammonioethanoate and maleic 2.900 - - 1.8600 1.0000 L [158]
acid
AC from loofah sponge @ 800˚C 2.900 - - 0.0000030 0.9981 L [138]
Ball-milled biochar 2.820 - - 0.0002235 0.9800 NL [132]
Nano-clay Magadiite 2.800 - - - 0.9900 L [159]
AC from fox nutshell 2.750 - - 0.0310 1.0000 NL [160]
Modified porous carbon from petroleum pitch 2.740 - - 0.00051 0.9990 NL [161]
Agro-food organic waste 2.728 - - 0.1310 0.9990 L [162]
Tea waste 2.611 - - 0.2317 0.9908 NL [163]
Ball-milled AC /Fe3O4 NPs 2.600 - - 0.0005447 0.9440 NL [132]
AC from loofah sponge @ 600˚C 2.600 - - 0.0000491 0.9891 L [138]
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Commercial AC (Darco S-51) 2.550 - - - - - [164]
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AC from Acorn shell 2.538 - - - - - [157]
AC/Cellulose from sisal fibre 2.520 - - - - - [165]
AC from fish waste 2.500 0.380 0.9990 0.516 0.9990 NL [166]
AC from Arundo donax 2.490 - - 0.001808 1.0000 NL [167]
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Biochar from Gelidiella acerosa 2.450 - - 0.0600 0.9940 NL [168]
Modified carbon quantum dots/silica 2.450 - - 0.0000105 0.9997 L [169]
Modified silica aerogel 2.434 - - 0.0873 0.9974 L [170]
AC from Sugarcane bagasse 2.400 -
e- - 0.006 0.9880 NL [171]
Polyvinyl alcohol/sodium alginate 2.396 - - - - - [129]
AC from Sugar beet pulp 2.393 - - 0.0027 0.9990 L [172]
Maize silk powder 2.380 - - 0.0007 0.9787 L [173]
Pr
Modified MIL-101 MOF 2.350 - - 0.000411 0.9990 NL [174]
Zr(IV)-MOF 2.331 0.0171 0.9944 - - NL [175]
Chabazite 2.330 - - 4.8000 1.0000 L [176]
Ball-milled AC 2.300 - - 0.0008145 0.9970 NL [132]
AC from Elaeagnus stone 2.270 - - 0.000875 1.0000 NL [177]
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AC from Acacia mangium using CO2/ CaO 2.250 - - - - - [145]

AC from spent coffee ground 2.196 - - - - - [178]
AC from sorghum 2.190 - - 0.000188 0.9983 NL [179]
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AC from Acacia mangium using N2/ KOH 2.170 - - - - - [145]

AC from Acacia mangium using N2/ CaO 2.150 - - - - - [145]
ur
AC from Mangosteen peel 2.137 - - 0.001388 1.0000 L [180]

AC 2.100 - - 0.0002397 0.9970 NL [132]
Carbonized bamboo leaves powder 2.090 - - 0.015 1.0000 NL [181]
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BC from hickory chips 2.090 - - 0.00005117 0.9670 NL [132]

Hydrophilic hydroxyl-group silica aerogel 2.083 - - 0.2572 0.9951 L [170]
AC from Acacia mangium using CO2/ H3PO4 2.080 - - - - - [145]
Zeolite/NaOH 2.060 - - - 0.9999 NL [153]
AC from bean dreg 2.055 - - 0.001 1.0000 L [182]
AC coconut shell based hydrochar 2.013 0.1250 0.9993 0.02468 0.9995 NL [183]
Commercial AC (Darco KB-M) 2.012 - - - - - [164]
AC from KOH activation 2.000 1.1109 0.9997 0.0177 0.9994 NL [184]
AC from cotton 2.000 - - 0.00016 0.9970 NL [185]
AC from Pongamia pinnata fruit hulls 1.992 - - 0.0007 0.9993 NL [186]
MCC from oil palm fronds pulp 1.970 - - 1.6930 0.9990 L [125]
AC from Acacia mangium using N2/ H3PO4 1.960 - - - - - [145]
AC from Date press cake/ Ultrasound 1.904 - - 0.0013 0.9980 NL [187]
AC from Date press cake/ Stirring 1.904 - - 0.0003 0.9760 NL [187]
Biochar from Oil palm shell 1.900 - - - - - [188]
AC from coconut shell 1.870 - - 0.0214 0.9990 L [189]
AC from CO2 activation 1.870 - - 0.0100 0.9984 NL [190]
9
Aluminium based Magnetic MOF 1.850 - - 0.0007 0.9740 NL [191]
Carbonized Glycerol/ H2SO4 @ 120˚C 1.838 - - 0.0000417 0.9900 L [192]
Carbonized Glycerol/ H2SO4 @ 350˚C 1.827 - - 0.0000514 0.9900 L [192]
Eucalptus sheathiana bark 1.800 - - - - - [113]
AC from cashew shell 1.800 - - - - - [193]
AC fiber felts activated under water vapour (125 1.770 - - 0.00004419 0.9998 L [194]
m3/h for 7 mins)
AC from Acacia mangium using N2/ ZnCl2 1.750 - - - - - [145]
AC from Acacia mangium using CO2/ ZnCl2 1.740 - - - - - [145]
AC from Groundnut shell 1.714 - - - - - [195]
UiO-66 MOF 1.700 - - 0.0062 0.9900 NL [196]
AC fiber felts activated under water vapour (110 1.670 - - 0.000007309 0.9747 L [194]
m3/h for 5 mins)
Graphene-like carbon from sugar 1.650 - - 0.3900 1.0000 L [197]
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Biochar from coffee husk 1.540 - - 0.0455 1.0000 L [198]
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Fe3O4/ Fe based MIL-100 MOF 1.495 - - 0.0116 0.9995 NL [199]
Nano-TiO2 1.491 - - - - - [200]
AC from waste carpets 1:3 H3PO4 1.480 - - 0.0474 0.9973 NL [201]
MnO/AC 1.450 - - - - - [202]
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AC from wood sawdust 1.340 - - 0.011 0.9999 L [203]
Ball milled sugarcane bagasse biochar 1.300 -
e- - - - - [139]
MCC from oil palm fronds 1.290 - - 0.2808 0.9999 L [204]
Posidonia oceanica leaves 1.260 - - - - - [205]
AC from sugarcane bagasse/ 10% nano-TiO2 1.250 - - 0.0079 0.9984 L [200]
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Zeolite from Kaolin of Dehessa, Egypt 1.230 - - - - - [206]
AC from sugarcane bagasse/ 50% nano-TiO2 1.194 0.0022 0.9929 0.0071 0.9987 L [200]
Biochar from Barley malt bagasse/ CO2 1.160 - - 0.0053 0.9993 NL [80]
Zeolite from Kaolin of Saint Catherine, Egypt 1.160 - - - - - [206]
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Biochar 1.151 - - 0.000201 0.9435 NL [207]
Biochar/ 6 mg/L SDS 1.150 - - 0.000203 0.9221 NL [207]
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Commercial AC (PAC 200) 1.144 - - - - - [164]

Zeolite from Kaolin from Kalabsha, Egypt 1.110 - - - - - [206]
AC from sugarcane bagasse 1.083 - - 0.0023 0.9962 L [200]
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Posidonia oceanica leaves/ Acetic acid 0.740 - - 0.000068 1.0000 L [205]

Fe/bentonite 0.656 - - 0.0014 0.9906 NL [208]
Wet-torrefied Chlorella sp. microalgal biochar 0.655 0.0001683 0.9088 - - L [209]
3. Results and Discussion

3.1 Pore size effect on MB adsorption kinetics
The results of the analysis of the data in Table 2 are presented in Tables 3-4. It can be
observed from Table 2 that the kinetic constant increased as the pore size progressed from the
macroporous to the mesoporous range. However, MB uptake was significantly slower at the
microporous range. It must be noted that adsorbents usually do not have a homogenous pore size
but a range of sizes. Reported values of pore sizes are averages. Based on the nature of the
10
material, it could have more pores in a specific size range than in other ranges. The interplay of
these size range also affects the eventual uptake capacity. Kumar et. al [210] observed that a
large amount of the pores being in the mesoporous range significantly improves the uptake
capacity for adsorption. An important take-away from the study was that pores >10 nm enhances
adsorption kinetics. The mesoporous range is the superior pore size for MB adsorption kinetics
and smaller pore sizes lead to a drop in the kinetic constant. This might not necessarily
corroborate with lower adsorption capacity as that depends on other physico-chemical
interactions. The movement of MB adsorbate within microporous pores is restricted and more
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gradual. The dimensions of the MB molecule are shown in Figure 2. It can be inferred that a
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micropore (< 2 nm diameter) will only allow one MB laterally and two longitudinally. This
limitation of space is more significant at the molecular level of adsorption because the mass
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transfer driving force is adsorbate concentration. Furthermore, MB will not diffuse into pores
below 0.95 nm diameter. These observations confirm the reason for the drop in kinetic constant
e-
observed for micropore diameter (from Table 3). Furthermore, multilayers of MB uptake will
not be possible in these pores. More intense agitation on higher initial concentration at the
Pr
experimental stage is needed to provide a better mass transfer driving force. However, it can still
lead to a protracted contact time before equilibrium is achieved.
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11
f
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pr
e-
Pr
n al
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Figure 2. Dimensions of the MB molecule and its preference for mesopores

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Table 3. Variation of pore size with mean values

Regime Pore size Mean (g/mg.min)
Macroporous 200 – 50 nm 0.03475
Mesoporous 50 – 30 nm 0.12650
Microporous 0 – 2 nm 0.08456
3.2 Kinetics models and MB adsorption

From Table 4, the PSO model was best suited for all cases where macroporous adsorbent
was used. However, 15% of the studies had PFO as best-fit for mesoporous adsorbent and 6% for
12
microporous. The observed superiority of PSO might not just be due to the suitability of the
conceptual assumptions but the simplicity of the mathematical expression of the model itself
[211, 212]. PSO as the most significant model best-fit has been observed in other adsorption
review papers [18-20, 213-215]. Both PFO and PSO supposes that adsorption kinetics is
dependent on the amount of MB in the aqueous phase. This is important because adsorption is a
mass transfer process therefore the concentration gradient will always be a driving force for
adsorbate movement from one phase to the other. The major difference between the PFO and
PSO is that the latter proceeds to capture the availability of active sites on the adsorbent as
f
another factor that affects the kinetics. This makes the PSO more superior in describing the
oo
adsorption process. PFO is usually best-fit in cases where the active site is not a limiting factor.
This can be achieved in two scenarios: when a very low adsorbate concentration is used for the
pr
experiments or when an extremely high dosage is employed.
Regime PFO
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Table 4. Distribution of best-fit kinetic model with pore size
PSO
Macroporous 0% 100%
Pr
Mesoporous 15.23% 84.77%
Microporous 5.88% 94.12%
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3.3 Modelling technique for MB adsorption

From Figure 3a-b, it can be observed that 10% of the studies had PFO as best-fit when
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linear modelling was used but 15% was best-fit with non-linear modelling. The PSO is
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inherently non-linear because it is a second-order differential equation. This would suggest that
non-linear modelling could have given a greater proportion of PSO modelling. However, this is
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not the case. This leads us to some of the issues around the mathematical aspects of kinetic
modelling. There are two major concerns: the first is the mathematical simplicity of the
linearised form of the PSO and the second is the errors associated with the linearisation of kinetic
models. Tran et. al [216] argued that the linearised form PSO fits well with both adsorption data.
However, it would be erroneous to take this as the basis for inferring the mechanism of uptake as
chemisorption. The amount of active sites being a rate-limiting step does not infer
chemisorption. Hence, Tran et. al [216] deemed such a position by researchers to be faulty.
Linearisation of the kinetic models also leads to certain issues that affect the modelling accuracy.
Linearisation has inherent bias arising from the variations in the y-axis for the linear form of the
13
expression [213]. Though more rigorous, non-linear regression modelling gives better accuracy
for the intended purpose. Based on a recent critical review article by Lima et. al [217], using the
linear form of pseudo kinetic models in adsorption studies may lead to wrong conclusions. For
this purpose, the kinetic results in the literature which used the linear approach (Table 2) should
be considered with caution. For more details on this, it is suggested that the explanations in Lima
et. al [217] be studied.
Linear
f
oo
pr
e- PFO
PSO
Pr
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(a)
Non-Linear
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PFO
PSO
(b)
Figure 3a-b. Distribution of model best-fits with modelling type
14
3.4 Other pore properties on MB adsorption
Though this investigation has elaborated the pore size effect, the effects of other
properties such as pore volume and the specific surface area (albeit not specifically a pore
property) are discussed in this section. The pore volume and specific surface area are related
properties as they have a direct effect on the MB adsorption capacity. A larger magnitude of both
properties directly translates into larger MB adsorption capacity though not explicitly (this is
only a simplification as adsorption itself is a complex physico-chemical process). Now let us try
and relate this to adsorption kinetics. Since both pore volume and specific surface area are finite,
f
a smaller magnitude of these properties will lead to lesser overall adsorption time at a
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specific/unchanging rate constant. The ratio of the mesoporous to microporous pore volume also
affects rapidity. Considering two adsorbents where , the rapidity of uptake
pr
would be lower than another adsorbent of the same total pore volume where
, albeit for the same adsorbate. Besides these considerations, these properties might not
e-
have other effects on uptake rapidity. A more detailed explanation of other possible adsorption
Pr
MB mechanisms besides the pore properties is presented in Iwuozor et. al [50].
4. Conclusion
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Considering the widespread issues from the proliferation of MB in the environment, the
results of this study is important to environmental engineers to gain a better understanding of the
n
MB adsorption process. Several interesting conclusions were derived from this study. It was
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observed that the adsorption kinetic constant increased as the pore size progressed from the
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macroporous to the mesoporous range suggesting an increase in uptake rapidity. However, MB

uptake was significantly slower for micropores. The mesoporous size range was the superior
pore size for MB adsorption kinetics. Microporous pore size led to a drop in the kinetic constant
because the diffusion of MB adsorbate through very small pores is restricted and gradual. The
PSO model was best suited for all cases. PSO is superior because it captures both the amount of
active sites and the concentration of adsorbate as rate-limiting factors. This was due to the
mathematical simplicity of the linearised form of the PSO and the errors generally associated
with the linearisation of kinetic models. Since both pore volume and specific surface area are
finite, a smaller magnitude of these properties will lead to lesser overall adsorption time at an
unchanging rate constant.
15
Disclosure statements
Conflict of Interest: The authors declare that there are no conflicts of interest.
Funding: There was no external funding for the study.
Compliance with Ethical Standards: This article does not contain any studies involving human
or animal subjects.
Author contributions
f
Joshua O. Ighalo, Conceptualisation, Methodology, Investigation, Writing - original draft;
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Writing - review & editing; Supervision; Validation; Project administration
Kingsley O. Iwuozor, Conceptualisation; Data curation; Writing - original draft; Writing - review
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& editing; Validation
Chinenye Adaobi Igwegbe, Conceptualisation; Writing - review & editing; Validation
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Adewale George Adeniyi, Writing - review & editing; Validation
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CRediT authorship contribution statement
Joshua O. Ighalo, Conceptualisation, Methodology, Investigation, Writing - original draft;
Writing - review & editing; Supervision; Validation; Project administration. Kingsley O.
Iwuozor, Conceptualisation; Data curation; Writing - original draft; Writing - review & editing;
Validation. Chinenye Adaobi Igwegbe, Conceptualisation; Writing - review & editing;
Validation. Adewale George Adeniyi, Writing - review & editing; Validation.
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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.
☐The authors declare the following financial interests/personal relationships which may be considered
as potential competing interests:
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Highlights
 The effect of pore size on MB adsorption was investigated.
 The kinetic constant increased from the macroporous to the mesoporous pore sizes.
 The mesoporous range was the superior pore size for MB adsorption kinetics.
 Microporous pore size leads to a slower kinetic constant.
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Veriﬁcation of Pore Size Effect on Aqueous-Phase Adsorption Kinetics: A Case

Article in Colloids and Surfaces A Physicochemical and Engineering Aspects · July 2021

Joshua O. Ighalo Kingsley O. Iwuozor

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Chinenye Adaobi Igwegbe Adewale George Adeniyi

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The user has requested enhancement of the downloaded file.

Verification of Pore Size Effect on Aqueous-Phase

Joshua O. Ighalo, Kingsley O. Iwuozor, Chinenye

To appear in: Colloids and Surfaces A: Physicochemical and Engineering

Joshua O. Ighalo1, 2*, Kingsley O. Iwuozor3, 4, Chinenye Adaobi Igwegbe1**, Adewale

Adewale George Adeniyi, https://orcid.org/0000-0001-6615-5361

Figure 1. Chemical structure of Methylene Blue (MB)

2.1 Data collection and description

2.2 Research problem

Adsorbent name Average

Graphene alginate nanocomposite 55.70 - - - 0.998 L [55]

Fe3O4/ Montmorillonite 46.39 - - 0.011 0.9999 L [57]

Hydroxyapatite/ 5% sodium alginate 35.73 - - 0.026 0.9990 NL [59]

Porous PVA/Zn-Fe-Mn oxide nanocomposite 26.00 - - 1.8500 0.9485 L [61]

Commercial AC/AgCl 7.477 - - 0.0267 0.9999 - [96]

Magnesium silicate/AC 6.510 - - 22.76 0.9970 L [99]

AC from tomato waste 5.916 - - - - - [101]

AC from Coconut leaf 3.650 - - 0.0470 1.0000 NL [141]

AC from olive ash 3.560 0.0976 0.9900 0.04738 0.9900 NL [143]

Lacosperma secundiflorum hydrochar 3.550 0.1730 0.9900 0.01880 0.9900 NL [144]

Macrogel polyvinyl alcohol 3.400 - - 0.00292 0.9991 L [111]

AC from Acacia mangium using CO2/ CaO 2.250 - - - - - [145]

AC from Acacia mangium using N2/ KOH 2.170 - - - - - [145]

AC from Mangosteen peel 2.137 - - 0.001388 1.0000 L [180]

BC from hickory chips 2.090 - - 0.00005117 0.9670 NL [132]

AC from sugarcane bagasse/ 10% nano-TiO2 1.159 - - 0.0081 0.9988 L [200]

Biochar/ 10 mg/L SDS 1.149 - - 0.000270 0.9361 NL [207]

Commercial AC (PAC 200) 1.144 - - - - - [164]

Posidonia oceanica leaves/ Acetic acid 0.740 - - 0.000068 1.0000 L [205]

3. Results and Discussion

Figure 2. Dimensions of the MB molecule and its preference for mesopores

Table 3. Variation of pore size with mean values

3.2 Kinetics models and MB adsorption

3.3 Modelling technique for MB adsorption

macroporous to the mesoporous range suggesting an increase in uptake rapidity. However, MB

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equilibrium, mechanism, thermodynamic and process design. Desalination and Water