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A Comprehensive Guide For Characterization of Adsorbent Materials
A Comprehensive Guide For Characterization of Adsorbent Materials
A R T I C L E I N F O A B S T R A C T
Keywords: Given the great relevance that adsorption processes have for many applications, especially for the water and
Microscopy wastewater treatment, the development and improvement adsorbent materials is a key research topic. When a
Spectroscopy new adsorbent is proposed, a good characterization of the material is fundamental to in order to know its
Physicochemical characterization
properties, support its application and understand its performance in the desired process. There is a variety of
Surface analysis
Adsorption
physical and chemical information that can obtained by different techniques, whose choice depends on the type
of material to be studied and on the available instrumentation. The available techniques include UV–vis, FTIR,
Raman, XPS, EDX, zeta potential, XRD, SEM/FESEM, TEM, AFM, surface area and porosimetry, VSM, DLS,
thermoanalytical analysis (TG, DTA, DSC and DTG), among several others. These techniques enable the iden
tification, location and quantification of chemical constituents, like elements, functional groups and molecules,
as well as the study of the structure, topography, morphology, magnetic properties, and size, among other
physical properties of materials. This information can provide great support for the assessment of the synthesis/
functionalization of adsorbent materials as well as in the study of the adsorption process by the interactions
between adsorbent and adsorbate. In the face of that, this review intends to be a comprehensive and concise
guide for researchers that study adsorbent materials to consult the available characterization techniques and
choose the most suitable ones for their specific needs.
* Corresponding author.
** Corresponding author.
E-mail addresses: leandro.pellenz@posgrad.ufsc.br (L. Pellenz), adriano.silva@ufsc.br (A. da Silva).
https://doi.org/10.1016/j.seppur.2022.122435
Received 10 August 2022; Received in revised form 21 September 2022; Accepted 18 October 2022
Available online 22 October 2022
1383-5866/© 2022 Elsevier B.V. All rights reserved.
L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
2.1. UV–vis
2. Chemical characterization
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2.2. FTIR Fig. 3. FTIR analysis. (a) - Schematic illustration of the FTIR technique working
principle; (b) - FTIR spectra showing absorption peaks related to several
Infrared spectroscopy (IR) is a technique based on the vibrations of chemical bonds of Cymbopogon flexuosus biomass immobilized on sodium
atoms in organic or inorganic materials. The IR spectrum of a material is alginate beads before (black line) and after adsorption of Cr(III) (red line)
sensitive to its chemical composition, isomorphic substitution, layer [Copyright 2021, Elsevier, [38]; reproduced with permission]. (For interpre
stacking order, or structural modifications. This makes FTIR the most tation of the references to color in this figure legend, the reader is referred to
informative technique, not only for determining functional groups, but the web version of this article.)
also for determining different interactions between materials. The
principle of this technique is the excitation of a molecule by IR radiation, FTIR transmission spectrum. Some radiation is reflected, some passes
which results in vibrations of its molecular bonds at different fre through, and some is absorbed by the sample by causing stretching and
quencies in the IR region [36]. The currently used FTIR spectrometers bending vibrations in the molecular bonds. The absorption peaks at
are typically equipped with a Michelson interferometer. A source emits a given wavenumber ranges are fingerprints of specific functional groups
beam of infrared radiation into the interferometer, where it hits a [36,37].
beamsplitter that splits the beam into two. The two beams are then The functional groups present on the surface of an adsorbent play an
redirected to the beamsplitter, recombined with interference and important role in the adsorption process, providing interaction sites for
directed to the sample, that precedes a detector (Fig. 3a). The raw signal the fixation of the target adsorbates. Thus, FTIR can be used in the
provided by the detector is then mathematically converted by Fourier characterization of materials by identifying the functional groups pre
transform into a plot of intensity (transmittance or absorbance) versus sent in the adsorbent material. Likewise, the presence of adsorbate in the
wavenumber, based on the movable mirror position. The division of the adsorbent can be confirmed and investigated by determining the sites of
sample spectrum by the reference spectrum (no sample) results in the
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
cm− 1), S–H stretching (2550–2600 cm− 1) (Fig. 3b) [40–45]. In acti
vated carbon, a widely used adsorbent, researchers have identified via
FTIR the presence of carboxylic acids, quinones, phenolic groups, lac
tones, ketones, ethers, pyridine-like groups, amides, and amines, among
others [40]. Furthermore, the functionalization of adsorbents in order to
increase their adsorption sites is often performed with oxygen, nitrogen
and sulfur-containing groups. The insertion of these new groups can be
verified and relatively quantified with FTIR analysis [46,47]. FTIR is a
qualitative technique, but the comparison between signal strengths of
different groups can be used to quantify the formation of certain func
tional groups. Yet, it is important to note that some are formed by the
sum of signals of more than one bond [40]. Additionally, when the FTIR
analysis is carried out in a loaded adsorbent, slight shifts in the peaks
and changes in intensity indicate that the respective functional groups
are involved in the adsorption process [48–50].
2.3. Raman
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2.5. EDX
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Fig. 6. EDX analysis. (a) - Schematic illustration of the EDX technique working principle; (b) EDX results obtained in a SEM-EDX equipment showing the C, N, O, Al,
and Co percentage in a zeolitic imidazolate framework-molecularly imprinted composite and the mapping of C, N, O and Co along the surface of a region of the
material [Copyright 2013, Elsevier, [78]; reproduced with permission].
Increasing the pH of a solution causes deprotonation of the adsor suitable zeta potential value tend to perform better in separating ionic
bents and reduces their zeta potential. A simple and frequently applied adsorbates [83,94]. It has been reported that functionalization and
measurement in adsorbent material is the isoelectric point, commonly chemical modifications of the surface of materials typically change their
known as point of zero charge (PzC), which identifies the pH value under Zeta potential, making it a parameter worth investigating in adsorbent
which the zeta potential is zero. The method consists in adding the synthesis processes [92,94,95,97].
adsorbent to solutions within a range of pH values in order to verify the
point (pH value) at which there is no change in the solution pH caused 3. Physical characterization
by the material (Fig. 7b) [16,93]. The presence of functional groups on
the adsorbent that can be protonated and deprotonated, like carboxyl The structure, topography, morphology, magnetic properties and
and amine, enhances the variation of the zeta potential with the change size are some of the most important physical features to consider in
of the solution pH [92,94]. The charge of the adsorbent is especially evaluating an adsorbent material. These studies can be carried out by X-
relevant in the adsorption of charged molecules, such as metals and ionic ray diffraction analysis (XRD), scanning electron microscopy (SEM),
forms of organic compounds, since it can be favored or hindered by field emission scanning electron microscopy (FESEM), transmission
electrostatic interactions and complexation reactions between adsorbent electron microscopy (TEM), atomic force microscopy (AFM), surface
and adsorbate [95,96]. Thus, considering the electrostatic interactions area and porosimetry analysis, vibrating sample magnetometry (VSM),
mechanism, negatively charged adsorbents have more affinity for and dynamic light scattering (DLS), among other techniques.
positively charged adsorbates, and vice versa [83]. This becomes more
relevant when adsorbents are designed for real applications where the
pH cannot be adjusted for adsorption. In these cases, adsorbents with a
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
Fig. 7. Zeta potential analysis. (a) - Schematic illustration of the Zeta potential technique working principle; (b) – Zeta potential profiles of GO and Fe3O4-SiO2-NH2,
Fe3O4-SiO2-GO and Fe3O4-SiO2-GO-2-phenylethyl amine in suspensions of 300 mg/L in the pH range from 2 to 12 [Copyright 2018, Elsevier, [92]; reproduced
with permission].
XRD is widely used to study the crystal properties of materials, SEM is a widely applied technique for microstructural analysis of
assessing the atomic arrangement, crystal size, lattice parameters, and adsorbent materials. It provides information about morphology, topo
imperfections. Therefore, a laser beam of X-rays is emitted at a certain graphic features, crystal structure and orientation, variation of the
angle toward a sample placed on a solid surface. At certain angles of composition, phase distribution, and the location of electrical defects in
incidence of the beam, the atoms present on the material diffract it with the material [104]. The technique consists of the excitation of the
constructive interference (amplification). A detector, that moves at the sample by an electron beam that is generated by an electron gun and
same angle as the laser on the opposite side, captures these diffraction crosses a set of electromagnetic lenses inside a vacuum chamber. The
peaks identifying the angle on which they occurred (Fig. 8a). Based on beam hits the sample releasing secondary electrons that are captured by
the diffraction angle, it is possible to determine spacing between ordered detectors, which convert this information into a scanning image
atoms of a sample using Bragg’s law [98]. (Fig. 9a). Nonconductive samples are coated with an ultrathin film of a
Crystalline adsorbent materials have distinctive diffraction peaks at conductive metal, frequently gold, in order to enhance the signal.
specific angles, and some of these appear with more intensity, such as 2θ [104,105]. As an enhanced version of SEM, FESEM produces a narrower
of 26.0–27.0◦ for pristine graphene/graphite, ~10.0◦ for GO [56,72], electron beam and generates images with improved spatial resolution,
12.0◦ and 25.0◦ for kaolinite [99], 10.4◦ and 20.0–21.0◦ for chitosan sub-nanometer in some cases. SEM/FESEM can also be equipped with an
[81,100], 22.0◦ for SiO2 and 26.0◦ for TiO2 [81]. Furthermore, XRD EDS detector, which is performs an elemental analysis on the surface of
broad peaks indicate amorphous structure, while sharp peaks evidence the material [105].
crystalline arrangement. Chemical modifications often change the ma SEM/FESEM is one of the most applied characterization techniques,
terial structure, which can be observed by the change in intensity, whether just to present an image of a particular adsorbent material and
breadth, and angle shift of the peaks, as well emergence of new XRD observe its features or to visualize modifications of its structure by
peaks [56,71,100–103]. XRD has been applied to assess the synthesis of physical/chemical treatments or functionalization/decoration of its
some adsorbents which can be verified, for example, with the combi surface [82,84,107–109]. Furthermore, some researchers have also
nation of the XRD peaks in the formation of a binary or multicomponent applied SEM/FESEM to observe the saturation of the surface and pores
material (Fig. 8b) [71,81,100,103]. Another application has been in of adsorbents with the target adsorbate [110–112]. The analysis can be
evaluation of GO, an increasingly studied adsorbent in recent years that carried out in relatively low magnification (<1000 times) to visualize
is often synthesized from the oxidative exfoliation of graphite. While, the shape and porous structure of micro size adsorbents, such as acti
according to the literature, graphite presents a sharp peak with inter vated carbon [113,114], mineral [115,116] biomass [82,107,117,118]
planar distance of 0.33–0.34 nm, graphene shows a broader peak with and synthetic-based [119] materials (Fig. 9b), or in higher magnifica
an interplanar distance between 0.77 and 0.95 nm, which indicates the tions (>30,000 times) to observe nano size adsorbents, like the forma
insertion of oxygen functional groups and a potential improvement as tion of aggregates in metal organic frameworks (MOF) [108], dispersion
adsorbent [16,56]. of metals in supporting materials [109,113], or the arrangement/shape
of nanocomposites such as graphene and CNT-based adsorbents
[120–122]. Also, SEM/FESEM analysis could be used strategically to
evaluate the adsorbent after the process, as well as after adsorption/
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
Fig. 8. XRD analysis. (a) - Schematic illustration of the XRD technique working
principle; (b) – XRD spectra of MnFe2O4/Bi2MoO6/PPy and MnFe2O4/Bi2MoO6
composites and of single Bi2MoO6 and MnFe2O4, presenting 2θ peaks at 23.6◦ ,
28.3◦ , 32.7◦ , 33.2◦ , 36.1◦ , 47.2◦ , 55.7◦ , 56.3◦ and 58.5◦ for Bi2MoO6; at 30.1◦ ,
35.4◦ , 43.1◦ , 56.8◦ and 62.4◦ for MnFe2O4 and 10.9◦ ; and the combination of
these set of peaks in the composites with the two components [Copyright 2022,
Elsevier, [71]; reproduced with permission]. Fig. 9. SEM/FESEM analysis. (a) - Schematic illustration of the SEM/FESEM
technique working principle; (b) – SEM images of peach stone activated carbon
impregnated with H3PO4 and modified with HNO3 showing the morphology of
desorption cycles to verify the stability of the material. Activated car
the material obtained with a magnification of 600 times with an accelerating
bons typically have porous structures that make them good adsorbents voltage of 20 kV [Copyright 2020, Elsevier, [106]; reproduced
in general, like the SEM image presented in Fig. 7b, where mesopores with permission].
(2–50 nm) can be visualized with micropores (<2 mm) inside them
[106]. Thermal and chemical activation of materials to produce adsor
the emission of an electron beam with uniform current density towards
bents can also be clearly visualized using SEM, with changes like the
an ultrathin sample. The beam crosses a set of lenses that allow the
destruction of its original structure and the formation of pores [119].
variation in the illuminated area of the sample. The irradiated sample
Other modifications in adsorbents may cause morphological changes
suffers different types of scattering according to the material, and the
that are visible in SEM images, such as a rough and edgy sand that be
scattered electrons behind the sample are imaged through a lens system
comes smoother and covered with iron-oxide spherical particles [109],
(Fig. 10a) [124].
or the filling some activated carbon pores with metal nano-particles
Unlike SEM, in the TEM analysis, the electron beam has to cross the
[111,113], or even the filling of pores with adsorbate [112]. In some
sample; therefore, it is commonly applied to characterize very small-size
cases, high-resolution FESEM can also show textural changes in the
adsorbents, often nanocomposites. In graphene-based adsorbents TEM is
adsorbent surface when saturated with the adsorbate [110,112].
used to observe defects, thickness, arrangement, agglomeration of the
nanosheets and size of particles, before and after functionalization/
3.3. TEM modification processes [16,72]. Polymeric adsorbents have also been
characterized by TEM to determine particle size, stacking and arrange
TEM is applied to analyze the chemical and electronic structures of ment of fibers [71,126,127]. Mineral and metal-based nano adsorbents
materials and identify defects, such as vacancy and dislocations, but it and carbonaceous materials decorated with metals are also often
can also provide information about the shape, thickness and approxi analyzed by TEM to observe the crystal and particle size, shape and
mate sizes of particles [123]. Conventional TEM apparatus consists of
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
3.4. AFM
Fig. 10. TEM analysis. (a) - Schematic illustration of the TEM technique
working principle; (b) – TEM image of commercial kaolinite (Saca-B®) showing
its pseudo-hexagonal shape in the basal plane, overlapping of layers, and
approximate size [Copyright 2021, Elsevier, [125]; reproduced
with permission].
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
used to estimate the particle size of nano adsorbents such as MgO and condensation; Isotherm type VI – formation of layers on an uniform and
ZnO and the lateral dimension of graphene nanosheets [139–141]. Re nonporous surface (Fig. 12b) [145].
searchers often apply AFM to determine sheet thickness and height The specific surface area is directly related to fundamental physical
fluctuation of sheet-like and membrane adsorbents. Usually, the func properties of particle size, porosity, surface energy, and uniformity of
tionalization or the saturation of an adsorbent with an adsorbate in the material. Since the surface area and porosity greatly influence in the
creases its sheet thickness and the roughness of its surface. It has been adsorption capacity, porous adsorbents, like carbonaceous materials,
measured via AFM that a specific pure GO sheet has a thickness of ~0.8 porous minerals and polymers, are often characterized by BET analysis
nm and a height fluctuation of ~0.1 nm, and after adsorption of MB the [6,147–151]. Their properties may vary significantly depending on the
thickness increases to ~ 0.9 and the height fluctuation to ~ 0.4 nm raw material and the physical/chemical processes applied to their pro
[142], and functionalized GO sheet can present increased sheet thick duction. Researchers have reported activated carbons with BET surface
ness, up to 2.5 nm [16,141]. An amine-functionalized sodium alginate areas up to 2630 m2/g and pore volume up to 1.91 m3/g with varied
membrane described in the literature presented a roughness average of sizes of pores (micro, meso, and macropores (>50 nm)) [147–149,152].
8.2 nm before adsorption, and 27.6 nm after the adsorption of Cr(III) As for zeolites, authors have observed surface areas up to 2300 m2/g
(Fig. 11b) [136]. The differences in the surface roughness upon with predominance of micropores [150,151,153]. Graphene and CNT-
adsorption/functionalization can also often be visually observed in the based materials have gained importance as adsorbents due to its possi
3-dimensional AFM images [136,137,141,142]. bilities of modification/functionalization and relatively high surface
area with reported values up to 1000 m2/g, depending on the synthesis
method, and varied pore sizes, depending on the composite
3.5. Surface area and porosimetry [16,46,72,154,155]. Polymeric adsorbents usually present a smaller
surface area when compared with the above and a varied porosity,
BET is one of the most widely applied surface area analyses in porous depending on the polymerization conditions [71,146,156]. Although
materials, including many adsorbents. The analysis starts with the the pore size is inversely proportional to the surface area, it also matters
sample being degassed and placed under a vacuum. Then it is exposed to in assessing an adsorbent since the pores can allow more or less diffusion
an inert gas, typically nitrogen, at constant temperature (77 K for ni of the adsorbate inside the adsorbent. Large molecules of organic com
trogen) and increasing relative pressure, from 0 to 1. The gas molecules pounds are normally trapped inside macropores, while small inorganic
are adsorbed by the material and cover first the micropores, then mes species can enter in micropores [157]. Macropores (>50 nm) allow a
opores and macropores, and ultimately, form a monolayer of molecules wide range of adsorbates to diffuse rapidly inside adsorbents, besides
over the whole area of the sample. Furthermore, more layers of mole facilitating adsorbent recycling by allowing eluting agents to diffuse
cules can be formed, as the gas pressure increases. The amount of gas through the material [46,157].
adsorbed as a function of the pressure, as well as the reverse process
(desorption), can be measured (Fig. 12a) [143]. With this data, the BET 3.6. VSM
model, as well as other derived models such as Barrett-Joyner-Halenda
(BJH) and Dollimore-Heal (DH) models are able to estimate the specific VSM is a technique that provides information about the magnetiza
surface area, pore volume, and area, as well as the pore size distribution tion of a material. In adsorbents it can be applied to evaluate magnetic
of the material [144]. Additionally, based on the gas adsorption and composites to evaluate their suitability for magnetic separation when
desorption isotherms, the International Union of Pure and Applied dispersed in a liquid media [158]. The VSM apparatus consists of a
Chemistry (IUPAC) classifies materials into six groups: Isotherm types I – magnetic field that first magnetizes the sample and then is removed. The
mostly micropores (< ~2.5 nm); Isotherm type II – absence of micro magnetized sample then generates its own magnetic field and is vibrated
pores; Isotherm type III – weak adsorbent-adsorbate interactions; by the equipment, generating an electric field proportional to the
Isotherm type IV – mesopores (2 – 50 nm)/capillary condensation; magnetic field applied to the sample, which is captured by a set of coils
Isotherm type V – weak adsorbent-adsorbate interactions/capillary and provides data about the magnetization of the material (magnetiza
tion curve and magnetic saturation) (Fig. 13a) [159].
In magnetic adsorbent characterization, VSM analysis is normally
carried out with the application of a magnetic field range from − 20 to
20 kOe and the results are expressed in terms of saturation magnetiza
tion (emu/g) in curves (Fig. 13b) [71,128,158]. The necessary magne
tization for separating a dispersed adsorbent material from a solution
may vary depending on several factors, like its morphology, size and
shape, as well as the external magnetic field strength and the layout of
the system [161]. Authors have reported that saturation magnetization
values of ~ 15.0 emu/g for MnFe2O4/Bi2MoO6/Polypyrrole [71], 23.6
emu/g for L-cystine/Sodium alginate/Fe3O4 [162], 35.0 emu/g for MOF-
Fe3O4/potassium nickel hexacyanoferrate [163], 29.3 emu/g for amine/
Fe/GO [75], 22.2 emu/g for Fe3O4/cyclodextrin/chitosan/GO [158],
16.9 emu/g for Reduced GO/Fe3O4/polydopamine [85], and 33.0 emu/
g for Fe3O4/SiO2/GO/2-phenylethyl amine [92] were sufficient for easy
magnetic separation of the composite from aqueous media in batch
systems. Currently, magnetic separation is more often applied to cata
lysts, but it could be an alternative for separating of powder-like ad
sorbents that are being increasingly developed and studied, like carbon
nanomaterials, metal oxides and nanocomposites [161,164].
Fig. 12. BET analysis. (a) - Schematic illustration of the BET technique working
principle; (b) – BET curve chart where it is possible to visualize nitrogen
adsorption and desorption profile as a function of the relative pressure in a 3.7. DLS
sample of kaolin-based geopolymer, which presented a specific surface area of
26.60 m2/g and a total pore volume of 0.24 cm3/g [Copyright 2022, Elsevier, DLS, also called Photon Correlation Spectroscopy (PCS), is widely
[146]; reproduced with permission]. applied to evaluate the dimensions of suspended particles [165]. When
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4. Thermal characterization
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
Fig. 14. DLS analysis. (a) - Schematic illustration of the DLS technique working principle; (b) DLS result presenting the particle size distribution of lepidocrocite and
goethite nanoparticles in a sample containing 5 % W/V (nanoparticle/water), with an average particle size of 268.8 nm for lepidocrocite and 145.6 for goethite
[Copyright 2015, Elsevier, [168]; reproduced with permission].
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L. Pellenz et al. Separation and Purification Technology 305 (2023) 122435
temperatures and ascribe them to the loss of specific constituents of the Another characterization method that can be applied in adsorbents
material. The first degradation peak normally occurs at 100 ◦ C, in which available is temperature programmed desorption (TPD). This technique
the adsorbents lose their moisture, since water molecules are adsorbed can be applied to study the kinetics and thermodynamics of the
physically by weak hydrogen bonds. This can be clearly observed in desorption process, as well as the surface chemistry of the adsorbent
Fig. 15b by a mass loss in the TGA analysis and an endothermic peak in material [100,202]. TPD consists of heating the adsorbent-adsorbate
the DSC chart, both around 100 ◦ C [81,182]. Other degradation peaks with a linear temperature increase and simultaneously measuring the
can be related to the elimination of volatile organic compounds amount of adsorbate that is transferred to the gas phase, typically by gas
(250–480 ◦ C) and amines (250–350 ◦ C) [100,182]. Functionalized ad chromatography or mass spectrometry, obtaining a desorption profile as
sorbents normally have less thermal stability in comparison with non- a function of temperature [202].
functionalized material. This occurs because the functional groups on Depending on the conditions of applications, some adsorbents like
the surface are degraded at lower temperature than the material itself. membranes can be also subjected to mechanical characterization,
However, the thermal removal of functional groups normally starts at including tension, compression, shear, bending and indentation tests to
temperatures higher than 200 ◦ C, and most adsorbent applications occur measure deformation as a function of the force under different condi
at mild conditions, often at ambient temperature [59,100]. No signifi tions (temperature, pressure, humidity, etc.) [203].
cant mass losses are observed beyond a certain temperature, 550 –
900 ◦ C, depending on the material, and the remaining mas is related to 6. Conclusion and future outlook
the inorganic contents of the adsorbent [81,100,182].
There is a great variety of characterization techniques that can be
5. Additional techniques applied to study adsorbent materials and enable researchers to assess
several physical, chemical, and thermal features of a sample in various
Here we present briefly a few physical and chemical characterization ways and levels of detail. Normally, researchers apply at least one
techniques that are not frequently used in the characterization of ad chemical characterization technique and one physical to provide basic
sorbents but could be alternatives for researchers to obtain more infor information about the material. However, the future perspectives lie in
mation about these materials. the improvement of the quality of these techniques and especially in
X-ray absorption fine structure (XAFS) techniques, which include X- their effective use. Much of the literature on new adsorbent materials, in
ray absorption near-edge structure (XANES) and extended X-ray ab our opinion, does not present enough characterizations or presents
sorption fine structure (EXAFS), can be applied to study the adsorption incomplete analyses. Characterization can be carried out in (i) raw
mechanism of metals into nano adsorbents since they can provide in materials or precursors, (ii) synthesized/composite or functionalized/
formation on the oxidation state and coordination geometry of a metal modified adsorbents, (iii) adsorbents loaded with the adsorbate, and (iv)
in on the adsorbent, coordination number and distance of a metal atom adsorbent after adsorption/desorption cycles, in order to study the
with neighbors atoms, coordination type and bond length [187,188]. material, to identify/confirm modifications, to identify/confirm
In the analysis of biomass-based, such as activated carbons, rapid adsorption, and to study stability and reusability of the material,
analysis of carbon, hydrogen, nitrogen, and sulfur (CHNS) contents can respectively. The choice of the techniques to be employed depends
be carried out in automated analyzers. These analyzers perform com primarily on the type of material, type of adsorbate, media to be applied,
bustion of the sample, converting carbon into carbon dioxide, hydrogen and inevitably, on the available resources. It is expected that with
into water, nitrogen into nitrogen gas/ oxides and sulfur into sulfur di technological development these techniques will become, in general,
oxide, which can be further separated and quantified via thermal con more affordable and with results of ever-increasing quality and accu
ductivity [86,189,190]. racy. This improvement is extremely positive for the research on ad
Chemical titration is another alternative method that can be applied sorbents, and can help to address a well-known challenge in laboratory
to quantify acidic (lactonic, carboxylic, phenolic and carbonyl) as well studies of new materials, which is the scale-up from controlled bench
as alkaline (pyrone, chromene) functional groups present on the surface conditions to real applications. An extensively studied and well-
of an adsorbent based on selective neutralization of these groups and characterized new material provides to the scientific community and
measurement of the amount of acid/base necessary to neutralize them industry quality information, potentializing future improvements and
[191–193]. application steps.
Solid-state nuclear magnetic resonance (ss NMR) is another available
chemical characterization technique that can be applied to study the Declaration of Competing Interest
atomic level structure of an adsorbent material and to investigate the
molecular level interaction between the adsorbate with the adsorbent The authors declare the following financial interests/personal re
[194,195]. In this technique, the sample is subjected to an external lationships which may be considered as potential competing interests:
magnetic field, which makes the atom nuclear spins, that are random in Leandro Pellenz reports financial support was provided by National
natural conditions, to align with the magnetic field. A coil sends radio Council for Scientific and Technological Development.
frequency pulses into the sample and perturbation of the aligned spins,
that further return to the original state producing a signal that is Data availability
detected and recorded. This data is processed as resonance frequencies
of a specific atom, compared to a reference, that varies depending on the No data was used for the research described in the article.
electronic environment in which it is located [196].
Scanning transmission electron microscopy (STEM) is a variation of Acknowledgments
TEM in which the electrons beam is focused towards de sample at an
angle and allows observing with higher contrast individual atoms, like The authors wish to thank Conselho Nacional de Desenvolvimento
metals, inside the adsorbent framework, as well as analyzing particle Científico e Tecnológico – CNPq for the financial support.
size, defects, and crustal morphology. Furthermore, STEM microscopes The authors are grateful to the Laboratory of Mass Transfer (LAB
can be equipped with an electron energy loss spectroscopy (EELS) de MASSA-UFSC) for the available infrastructure.
tector that performs an elemental identification similar to EDX
[197,198]. In adsorbents, some researchers have used STEM to visualize
the distribution of high-density elements on the surface of the material
[199–201].
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