Applied Clay Science 6768 (2012) 99105

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Applied Clay Science

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Research paper

Inuence of iron removal on the synthesis of pillared clays: A surface study by

nitrogen adsorption, XRD and EPR
J.G. Carriazo
Chemistry Department, Science Faculty, Universidad Nacional de Colombia, Carrera 30 # 45-03, Bogot, Colombia

a r t i c l e

i n f o

Article history:
Received 1 March 2011
Received in revised form 9 June 2012
Accepted 16 July 2012
Available online 5 September 2012
Keywords:
Pillared clays
Characterisation of pillared clays
Iron-oxide removal
Surface study of pillared clays

a b s t r a c t
The present paper reports a surface study on the synthesis of pillared clays before and after removal of iron
oxides (with sodium dithionite) from the clay used as starting material. Four pillared clays were synthesised
with Al- or Al-Fe-polyhydroxocationic solutions: two solids were prepared from the iron-removed clay and
the others from the non-pre-treated clay. All the solids were characterised by X-ray diffraction (XRD), electron paramagnetic resonance (EPR), differential adsorption potential distributions (DAPDs) and fractal
dimension from nitrogen adsorption. The natural clay was also analysed by transmission electron microscopy
(TEM) to verify iron oxide clusters. XRD and EPR analyses revealed that iron-reduction with sodium
dithionite, under the studied conditions, did not affect the clay mineral structure and the clay became successfully pillared in all cases; however, nitrogen adsorption showed a decrease of external surface areas
and an increase of micropore areas and volumes as a consequence of chemical pre-treatment. DAPDs indicated that iron-oxide removal reduced the surface heterogeneity of the pillared clays but enhanced the micropore fraction in the solids.
2012 Elsevier B.V. All rights reserved.

1. Introduction
Modifying clay minerals via pillaring currently constitutes an important and broad eld of materials and surface science research.
Pillared clays are complex microporous systems, having enormous
potential for application in adsorption and catalytic processes
(Carriazo et al., 2008, 2010). Many researchers thus show interest in
clays which have been modied through pillaring and their application as catalysts in a wide range of reactions (Carriazo et al., 2005,
2007a, 2007b; Centi and Perathoner, 2008; De Stefanis and
Tomlinson, 2006; Ding et al., 2001; Gil et al., 2000, 2008; Serwicka
and Bahranowski, 2004). Introducing inorganic pillars, in addition to
improving clay mineral strength and stability, increases microporosity and provides greater surface area on the solid, thereby facilitating
reagents access to potentially active sites for the catalysis of some reactions (Barrera-Vargas et al., 2007). The synthesis of pillared clays
has been widely described in the literature (Aouad et al., 2005;
Carriazo et al., 2009; Gil et al., 2000; Vicente and Lambert, 2003)
and characterising their porous structure has been recently reviewed
(Gil et al., 2008).
However, the synthesis of pillared clays requires several optimisations to enable such a procedure to be applied at industrial level and
marketing them in the future. One such improvement is to reduce

Tel.: +57 1 3165000x14403; fax: +57 1 3165220.

E-mail address: jcarriazog@unal.edu.co.
0169-1317/$ see front matter 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.clay.2012.07.010

previous purication treatments (minimal rening) of natural clays

(Storaro et al., 1996; Vaughan, 1998), such as eliminating organic
matter traces, soluble salts and iron oxides. Surface iron oxides are
commonly removed from some natural clays before pillaring because
it is considered that they affect the synthesis and textural properties
of the nal product (pillared clay), but a systematic study have not
been reported in the literature. Previous works use puried clays for
both lab synthesis and preliminary studies of the properties of the resultant solids; however, using raw clays is preferred for scaling-up
the process. Excessive content of iron oxides in natural clays may interfere on both the preparation procedures and the performance
of the nal solids synthesised from these clays, because high ironoxide content may modify the colloidal and rheological behaviour
of clay suspensions as well as the cation exchange capacity of the
clay mineral present. For more advanced processes, such as catalyst
manufacturing, some good properties of shaped macro-structures
(extruded solids, pellets, agglomerates, monoliths, etc) are desired,
but the high iron content may decrease the mechanical and thermal
stability of the nal products. Furthermore, both the acidic and
redox properties of nal pillared clays could be modied because of
the high iron content in the starting natural clay.
Iron oxides are usually eliminated from clay minerals by reducing
Fe 3+ to Fe 2+ by sodium dithionite (Na2S2O4) (Bertolino et al., 2010;
Drits and Manceau, 2000; Kunze, 1965), but this process can modify
natural clays' structural and surface properties. In fact, redox reactions
modify the chemical and physical properties of iron-containing smectites, such as cation exchange capacity, specic surface area, swelling
behaviour and ability to x interlayer cations (Drits and Manceau,

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J.G. Carriazo / Applied Clay Science 6768 (2012) 99105

2000; Komadel et al., 2006; Stucki et al., 2002). Consequently the texture of iron-removed clays and that of pillared clays synthesised from
these minerals may change. However, most of the studies on the reducing effect of sodium dithionite on clay minerals have been carried
out under inert conditions (using N2 atmosphere) (Anastcio et al.,
2008; Fialips et al., 2002; Komadel et al., 1999; Neumann et al.,
2011; Stucki et al., 1984), and the extent of iron reduction is not
completely understood. So, the effect of sodium dithionite on the
structure and texture of clay minerals under atmospheric air conditions is less known. On the other hand, some models about the reduction mechanism of iron (III) to iron(II) under inert atmosphere have
been proposed (Drits and Manceau, 2000; Manceau et al., 2000).
Most of the rst models assumed that Fe(II) in reduced dioctahedral
smectites was ve-coordinated, but Manceau et al. (2000) revealed
that iron is much more likely to maintain six-fold coordination after
complete reduction, with possible migration of some of the iron
atoms from cis- to trans-sites during the reduction reaction, and creating defects (vacant sites) in the octahedral sheets (Drits and Manceau,
2000; Komadel et al., 2006; Manceau et al., 2000; Stucki et al., 2002).
Recently Neumann et al. (2011) showed that reactions of Fe(II)/
Fe(III) in clay minerals depend on a variety of mineralogical and environmental factors, and that iron content, the overall cationic composition and the location of the negative excess charge determine which
structural Fe(II) arrangement forms during Fe reduction using sodium
dithionite. Furthermore, they suggest that these observations can be
used to rene the current model for structural Fe reduction proposed
by Drits and Manceau (2000). Thus, a model for reduction of iron in an
iron-bearing smectite under air atmosphere is not discussed in the literature, which makes difcult to predict the extent to which the structure of this mineral can be altered through the pre-treatment with
sodium dithionite to remove iron oxides before a pillaring process,
since the synthesis of pillared clays, as in the present work, is developed under atmospheric pressure.
Al- and mixed Al\Fe pillared clays showing an excellent catalytic
activity in environmental oxidation reactions have recently been
synthesised from an iron oxide-rich smectite-type clay (Carriazo et
al., 2005, 2007a); however, for optimising the synthesis, it should
be determined whether removing the natural iron oxides contained
on the surface of this raw clay can enhance or reduce the nal pillared
clays textural properties. The aim of this paper has thus been to present a study of the effect of removing iron-oxides from a clay (under
atmospheric air conditions) on the synthesised pillared-clays surface
and textural properties.

(Kunze, 1965). The resultant solid was centrifuged at 2200 rpm and
the supernatant extracted, and then washed several times up to the
conductivity of supernatant was closed to that of distilled water. This
procedure of removing iron oxides was repeated on the solid.
2.2. Characterising solids
Transmission electron microscopy (TEM) analysis of the naturalclay samples was performed using a Philips CM 120 (at 120 kV)
transmission microscope with EDX analyser. The clay samples were
dispersed in ethanol and then placed on a small copper grid covered
with a carbon lm. The EPR spectra were obtained on an X-Band
ESP 300 BRUKER spectrometer at 77 K, 100 kHz eld modulation
and 9.44 GHz frequency; 10 mW microwave power, 8000 swept
width, 10.25 G modulation amplitude, 40.96 ms time constant and
2 10 3 gain were used.
Powder X-ray diffraction (XRD) analysis was carried out in an
X-Pert Pro MPD PANalytical equipment using 2 geometry and a
Bragg-Brentano conguration at room temperature and using a 0.01
step size and 5 s step time. Nitrogen adsorption isotherms were
taken at 77 K using a Micromeritic TriStar 3000 adsorption analyser
in the 10 4 to 0.99 P/P0 range. The samples were outgassed at
90 C for 1 h and then at 350 C for 8 h. All calculations were developed assuming both a 16.2 2 area for covering a nitrogen molecule
(N2) and = 0.81 g/cm3 as density of nitrogen condensed in the
pores. -Curves and t-plots were used to verify the micropore formation: -curves were made using a non-porous silica as reference
(Gregg and Sing, 1982), = Vads/V(0.4), and t-values (thickness of
multimolecular layer) were calculated from Halsey equation:
0
11 =
3
B 5 C
B
C
. Micropore areas and volumes were obtained
t 3:54@
PA
Ln
P0
from t-plots. Adsorption potential distribution functions X(A) and the
characteristic adsorption curves v(A) were used for evaluating the
solids energetic heterogeneity (Carriazo et al., 2008; Jaroniec et al.,
1991, 1996). Total energetic heterogeneity results from both the contribution of functional groups on the surface, impurities and defects, and
the contribution of microporosity (Carriazo et al., 2008; Jaroniec et al.,
1991, 1996). X(A) was expressed as a differential potential distribution
function (Carriazo et al., 2008):
X A

dvA
dA

2. Experimental
2.1. Pillared clay synthesis
Two pillared clays were synthesised from a bentonite from Valle
del Cauca-Colombia and polyhydroxocationic aqueous solutions of
Al or Al\Fe(10%), as described elsewhere (Carriazo et al., 2005,
2008): Al-Pilc and Al\Fe(10%)-Pilc, labelled here as B-AlNR and
B-AlFeNR respectively. Additionally, the same solids were synthesised
by an identical method but after chemical pre-treatment with sodium
citrate, sodium bicarbonate and sodium dithionite (Na2S2O4) to remove the iron oxides from the clay surface, as described in the literature (Kunze, 1965). These pillared clays are named B-AlR and B-AlFeR
(characters NR and R respectively indicate non-removed ironoxides or removed iron-oxides).
To remove the iron oxides from the clay surface, 10 g of clay was
added to a mixture of 400 mL of 0.3 M sodium citrate solution with
50 mL of 1 N sodium bicarbonate solution (Kunze, 1965). The resultant suspension was heated to 80 C, and then 10 g of sodium
dithionite was added, maintaining this temperature and a continuous
stirring during 15 min. After this digestion period a volume of 100 mL
of a NaCl saturated solution was added to occulate the suspension

Fractal dimension (D) was determined from adsorption data (P/P0

between 0.08 and 0.2 (Carriazo et al., 2008; Gil et al., 2004), using the
Avnir and Jaroniec equation (Avnir and Jaroniec, 1989; Jaroniec,
1995):
Lnx K3DLnA
where x is the adsorbed amount, K is a constant and A is the adsorption potential.
A G RTLn

 
P0
P

R is the universal gas constant, T is the absolute temperature and

P0 and P are, respectively, the saturation and equilibrium pressures
during gas adsorption.
3. Results and discussion
Microscopic observation (TEM images) showed the existence of
iron-oxide particles on the surface of the natural bentonite-clay

J.G. Carriazo / Applied Clay Science 6768 (2012) 99105

101

Iron oxide particles

200 nm

100 nm

Bentonite

Bentonite

Si

Intensity

Al

Fe

Fe

1.0

2.0

5.0

6.0

7.0

Energy (keV)
Fig. 1. TEM micrographs of iron oxide particles observed on the natural clay (bentonite), and EDX spectrum of the sample.

150

Intensity

100

g = 4.3
g = 9.3

g = 2.0

50
B-AlR

0
B-AlNR

-50
-100
-150
1000

3000

5000

7000

Magnetic field (Gauss)

150
100

g = 4.3
g = 9.3

g = 2.0

50

Intensity

(Fig. 1). These iron oxides or oxyhydroxides might be hematite, goethite or magnetite (Bertolino et al., 2010) or mixed aluminium-iron
oxide nanoparticles (Schwertmann et al., 2000) supported on the
clay surface. In the present case iron oxide (or mixed aluminiumiron oxide) clusters were considered.
Typical values of g = 2.0, g = 4.3 and g = 9.3 for iron paramagnetic
species were observed from EPR analysis (Fig. 2). The rst value (g =
2.0) was attributed to iron oxides in cluster form, while g = 4.3 and
g = 9.3 were assigned to Fe 3+ in octahedral or tetrahedral chemical
environments (Bertolino et al., 2010; Carriazo et al., 2005). The last
two values could be interpreted as being iron ions in the octahedral
sheets (Fe 3+ replacing Al 3+) of the clay mineral (Bertolino et al.,
2010; Carriazo et al., 2005) plus iron ions contained in mixed
aluminium-iron oxides deposited on the clay surface. An important
EPR result was the signicant decrease of signal intensity (decrease
of area under curve) for the B-AlR and B-AlFeR solids due to clay mineral treatment with sodium dithionite. This conrmed an effective removal of iron oxides before synthesis of pillared clay. However, the
smaller reduction of signal intensity for the B-AlFeR sample resulted
from iron introduction during the course of this solid's synthesis.
Moreover, the EPR spectra indicated that clay mineral structural features were maintained and, therefore, the chemical treatment for
iron removal, under these conditions, did not have an apparent effect
on the clay mineral structure of the smectite.
XRD analysis revealed the successful synthesis of pillared clay in
all cases. The shift of the 001 diffraction maximum (d001 basal spacing) from 14.7 (natural clay) to 17.3 for all the modied solids
(Fig. 3a) clearly indicated that the smectite was pillared with the
polyoxocationic species (Carriazo et al., 2005, 2007a, 2009). The complete XRD traces (Fig. 3b) did not show other modications in these
solids structure, revealing similar XRD patterns for the pillared
clays synthesised with or without iron removal. Only slightly higher

B-AlFeR

B-AlFeNR

-50
-100
-150
1000

3000

5000

Magnetic field (Gauss)

Fig. 2. EPR spectra for the pillared clays.

7000

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J.G. Carriazo / Applied Clay Science 6768 (2012) 99105

55

(a)

Volume adsorbed (cm3/g), STP

d=17.3

Intensity (a. u.)

B-AlFeR

B-AlFeNR

B-AlR

B-AlNR

d=14.7

50

B-AlNR

45

B-AlR

40

Natural clay

35
30
25
20
15
10
5
0

Natural clay

0
0

10

12

14

Volume adsorbed (cm3/g), STP

(b)
B-AlNR - (1)
B-AlR - (2)
B-AlFeNR - (3)

Intensity (a. u.)

B-AlFeR - (4)

(4)
(3)
(2)
(1)

10

20

30

40

50

0.2

60

0.3

0.4

0.5

0.6

0.7

0.8

0.9

0.8

0.9

Relative pressure (P/P0)

2 theta, CuK

0.1

70

65
60
55
50
45
40
35
30
25
20
15
10
5
0

B-AlFeNR
B-AlFeR
Natural clay

80

0.1

0.2

2 theta, CuK

0.5

0.6

0.7

(a)
Volume adsorbed (cm3/g; STP)

intensity of peaks at ~ 2 = 21, 2 = 26 and 2 = 28 for the ironremoved samples was observed, which correspond to quartz and
feldspar impurities in the natural clay. The intensity of the diffraction
maxima of these minerals increases because their surfaces are
cleaned by iron-oxide elimination. This result conrmed that chemical treatment with sodium dithionite did not affect the smectite
structure. The iron oxide species in the materials were not detected
by XRD because they were present in small quantities and had poor
crystallinity.
The nitrogen adsorption isotherms for the natural and pillared
clays are shown in Fig. 4. The isotherms display H3 type hysteresis
(IUPAC classication), characteristic of slit shape pores, indicating
that the conguration of parallel plates of clay minerals was
maintained (Carriazo et al., 2008). The adsorption capacity of pillared
clays was higher than that of natural clay, due to the formation of micropores by the effective pillaring. Moreover, a slight difference in
adsorbed volumes was observed between pillared clays synthesised
with or without iron-oxide removal; the volume adsorbed by BAlNR was higher than that adsorbed by B-AlR and that of B-AlFeNR
was higher than B-AlFeR. The -curves (taking a nonporous silica as
reference) and t-plots (Fig. 5) conrmed the increase of microporosity of the synthesised solids: when micropores were introduced into
the solids, adsorption in the low-pressure region was enhanced and
the (- or t-) plots were bent, in accordance with previous reports
(Gregg and Sing, 1982). Pillared clays synthesised after iron-oxide
elimination thus showed lower nitrogen uptake than their natural
counterparts; B-AlFeNR was the material having higher apparent
complexity (Fig. 5a).
Table 1 shows the textural properties of the solids. Specic surface
areas and pore volumes for all the pillared clays increased compared
to the initial natural clay values; BET and external surface areas of

0.4

Fig. 4. Nitrogen adsorption isotherms for the natural clay and pillared solids.

Natural clay

60

B-AlNR

50

B-AlR
B-AlFeNR

40

B-AlFeR

30

nonporous silica
(reference)

20
10
0

0.5

1.5

2.5

3.5

(Vads/V(0.4))

(b)
Volume adsorbed (liquid) (cm3g-1)

Fig. 3. XRD patterns for the pillared clays. a) Amplifying the d001 peak. b) Complete
diffractograms.

0.3

Relative pressure (P/P0)

0.1
0.09
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
0

Natural clay
B-AlNR
B-AlR
B-AlFeNR
B-AlFeR

10

12

14

16

18

20

t value ()
Fig. 5. -curves (a), and t-plots (b) for the pillared solids and the natural clay.

J.G. Carriazo / Applied Clay Science 6768 (2012) 99105

103

Table 1
Textural properties of natural and pillared clays.
Solid

BET surface area

(m2g1)

Micropore area, Smp

(m2g1), from t-plot

External surface area,

Sext (m2g1)

Micropore volume, Vmp

(cm3g1), from t-plot

Total pore volume (cm3g1)

from Gurvitsch's method

Natural clay
B-AlNR
B-AlR
B-AlFeNR
B-AlFeR

42.8
72.1
66.6
76.8
69.3

3.4
74.0
74.6
38.2
60.5

35
18
13
44
25

0.0012
0.0262
0.0264
0.0135
0.0214

0.0470
0.0829
0.0704
0.1032
0.0866

B-AlR and B-AlFeR were lower than those of B-AlNR and B-AlFeNR as
a consequence of previous treatment for iron removal, which indicates that treatment with sodium dithionite, under this conditions,
allowed reduction of the free iron-oxides to decrease the number of
adsorption sites on outer smectite surface. Moreover, increase of micropore areas and volumes were observed for B-AlR and B-AlFeR
regarding B-AlNR and B-AlFeNR, although this result was more evident between B-AlFeR and B-AlFeNR. Removing iron oxides from
clay surface allowed access of N2 molecules to micropores generated
by the pillaring. Difference between B-AlFeR and B-AlFeNR micropore
areas indicates a higher effect of pore blocking because introducing
iron oxides in the synthesis of pillared clays. The adverse inuence
of natural iron-oxide particles on the pillaring with iron species probably is related to the nucleation of larger iron polyoxocations yielding
larger nanoparticles than those of aluminium oxide, since hydrolysis
of iron cations forms colloidal species with much higher degree of
condensation (Jolivet et al., 2000). On the other hand, the total specific surface area of the pillared clays is given as the sum of micropore
area plus external surface area (Stotal = Smp + Sext); therefore the
total specic surface area is higher than BET area for all the pillared
clays.
Important differences were observed in the characteristic adsorption curves for the solids (Fig. 6), indicating a possible surface

energetic variation. Pillared clays showed higher gas adsorption volumes than the natural clay throughout the adsorption potential
values as a consequence of their microporous structure, whilst solids
obtained after iron removal showed lower gas adsorption volumes
than clays pillared without such a chemical treatment probably because the external specic surface area of former materials was
reduced.
Differential adsorption potential distributions for the pillared
solids (Fig. 7) clearly revealed a shift of the maximum of the curves
to higher adsorption potential values compared to the natural clay
(from 3.3 to 4.05.0 kJ/mol), indicating effective formation of micropore structures in the solids. However, the highest derivative values
for B-AlNR and B-AlR in the low pressure region (high adsorption potential values: 4.05.0 kJ/mol) suggest the formation of a higher fraction of micropore in these solids than for Al\Fe pillared clays.
Pillaring with iron or aluminiumiron aqueous solutions leads to
the formation of iron oxide nanoclusters on the pillared clays
(Carriazo et al., 2005) which are able to partly block microporosity.
Furthermore, an additional complexity in the high adsorption potential region was observed for non-pre-treated solid curves (B-AlNR
and B-AlFeNR) (Fig. 7b) showing multimodal functions due to higher

(a)

Natural Clay
B-AlNR
B-AlR

0.04
0.03
0.02

Natural clay
B-AlNR
B-AlR
B-AlFeNR
B-AlFeR

0.012
0.010
0.008
0.006
0.004

0.01
0.002
0
1

Adsorption potential (A) (kJ mol-1)

(b)
0.009

0.05
Natural clay
B-AlFeNR

0.04

Adsorption potential (A) (kJ mol-1)

0.00
0

Volume adsorbed (liquid) (cm3g-1)

-dV/dA (mol cm3g-1kJ-1)

0.05

B-AlFeR

0.03
0.02
0.01

-dV/dA (mol cm3g-1kJ-1)

Volume adsorbed (liquid ) (cm3g-1)

0.014

B-AlNR

0.008

B-AlFeNR

0.007
0.006
0.005
0.004
0.003

Adsorption potential (A) (kJ mol-1)

0.00
0

Adsorption potential (A) (kJ mol-1)

Fig. 6. Characteristic adsorption curves for the solids (natural and pillared clays).

h
i
A
Fig. 7. Differential adsorption potential distributions dvdA
for the natural and pillared
clays. a) Complete curves and b) Expansion of an interval for non-pre-treated synthesised
solids.

104

J.G. Carriazo / Applied Clay Science 6768 (2012) 99105

Natural clay

3.5

B-AlNR

Ln (V)

Ln (V)

B-AlR

2.9

B-AlFeR

3.1
2.9
2.7

2.7
2.5
6.7

B-AlFeNR

3.3

3.3
3.1

Natural clay

3.5

6.9

7.1

7.3

7.5

2.5
6.7

Ln (A)

6.9

7.1

7.3

7.5

Ln (A)

Fig. 8. Linear relationship (AvnirJaroniec equation) for determining the fractal dimension of pillared clays by nitrogen adsorption.

heterogeneity on their surface. In this way, lack of removal of iron oxides contributed to higher surface heterogeneity of the pillared clays,
but it reduced the micropore fraction in the as-synthesised solids.
This effect was associated with a variation in the external and
microporo surface areas (Table 1). On the other hand, the rise in adsorption potential distribution functions at low adsorption potential
values (high relative pressures) revealed the multilayer adsorption
and capillary condensation (Carriazo et al., 2008) which was more
important on the natural and Al\Fe pillared clays due to their higher
external surface areas (Table 1).
The fractal dimension (D) determined for the solids (Fig. 8 and
Table 2) showed an increase in surface roughness as a result of the
successful pillaring of the natural clay to produce microporous structures (D from 2.6941 to 2.8583). In general, D value may vary from 2
to 3, with the lowest value (2) corresponding to a perfectly smooth
surface, and the upper limit (3) corresponding to a totally irregular
or rough surface (Avnir and Jaroniec, 1989; Jaroniec, 1995). D values
for B-AlNR and B-AlR were higher than those for Al-Fe pillared clays,
conrming the higher microporosity of the former solids. Although
these differences in D parameter were important, the fractal dimension could not verify any variation induced by the iron-oxide removal
pre-treatments, probably because all the synthesised solids have high
microporosity and therefore elevated roughness.
4. Conclusions
In this work, XRD and nitrogen adsorption analyses conrmed the
successful pillaring-intercalation of a Colombian bentonite, which
yielded similar microporous structures with or without previous
chemical treatment with sodium dithionite to remove iron oxides.
The pre-treatment with sodium dithionite did not affect the structure
of smectites in the bentonite. Removal of iron oxides from the clay reduced the external surface area and increased the micropore area and
volumes for Al- and Al-Fe-pillared clays (this effect being higher in
the Al-Fe-pillared clay) compared to the solids prepared without
such a treatment. Differential adsorption potential distributions and
the characteristic adsorption curves revealed some variations in energetic terms, indicating that eliminating iron oxides in this bentonite
contributed to a lower surface heterogeneity of pillared clays and increased the fraction of micropores in the solids. These results contribute in understanding some chemical pre-treatments and optimisation
procedures required for the pillaring of this Colombian bentonite.
Table 2
Fractal dimension (AvnirJaroniec equation) of solids studied here.
Solid

Equation

Fractal dimension (D)

Natural clay
B-AlNR
B-AlR
B-AlFeNR
B-AlFeR

y = 0.3059x + 4.9799
y = 0.1417x + 4.1129
y = 0.1464x + 4.0682
y = 0.2261x + 4.7293
y = 0.2086x + 4.5119

2.6941
2.8583
2.8536
2.7739
2.7914

0.9998
0.9988
0.9987
0.9997
0.9995

Correlation coefcient.

Acknowledgments
The author gratefully wishes to acknowledge the Universidad
Nacional de Colombia (Bogot) for supplying the resources for this
scientic investigation.
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