Carbon 41 (2003) 10091016

A study of the characteristics of activated carbons produced by

steam and carbon dioxide activation of waste tyre rubber
Guillermo San Miguel,, Geoffrey D. Fowler, Christopher J. Sollars*
Centre for Environmental Control and Waste Management, Department of Civil and Environmental Engineering,
Imperial College of Science, Technology and Medicine, London SW7 2 BU, UK
Received 21 December 2001; accepted 9 December 2002

Abstract
This paper presents a study into the effect of different activation conditions on the porosity and adsorption characteristics
of carbon adsorbents produced from waste tyre rubber. For the purpose of this work, three carbon series were produced using
different activation temperatures (between 925 and 1100 8C) and oxidising agents (steam or carbon dioxide). Carbons
produced to different degrees of burn off were characterised using gas (nitrogen) and liquid phase (phenol, methylene blue
and Procion Red H-E2B) adsorption. Total micropore volumes and BET surface areas increased almost linearly with the
degree of activation to 0.554 ml / g and 1070 m 2 / g, respectively, while the development of external surface area was
particularly rapid at degrees of activation above 50 wt% burn off. Steam was observed to generate a narrower but more
extensive microporosity than carbon dioxide. However, carbon dioxide produced carbons of slightly larger external surface
areas. Activation at higher temperatures resulted in pores of slightly larger dimensions, although this was only evident in
highly activated samples. Porosity characteristics were reflected in the capacity of the carbons to adsorb species of different
molecular size from solution. In this respect, steam-activated carbons presented greater capacities for the adsorption of
smaller molecular size compounds (phenol), while carbon dioxide-activated carbons adsorbed larger textile dyes more
effectively.
2003 Elsevier Science Ltd. All rights reserved.
Keywords: A. Activated carbons; B. Activation; C. Adsorption; D. Adsorption properties; Porosity

1. Introduction
Increasing demand for adsorption processes in the water
treatment industry is encouraging research into the production of activated carbon from alternative precursors
including industrial wastes and agricultural by-products
[13]. The production of carbon adsorbents from waste
tyre rubber has been investigated by several authors, with
marked differences in the porosity of the final products
[410]. This variability has been attributed primarily to
differences in the pyrolysis and activation conditions
employed but also to the characteristics of the rubber feed,
including particle size and composition [10].
*Corresponding author. Present address: Royal Holloway
Institute for Environmental Research, Huntersdale, Callow Hill,
Virginia Water, Surrey GU25 4LN, UK. Fax: 144-1784-477-427.
E-mail address: chris.sollars@rhul.ac.uk (C.J. Sollars).

The production of tyre rubber-derived activated carbons

requires the initial pyrolysis of the rubber followed by a
controlled oxidation (activation) of the carbonised char.
The pyrolysis process also generates a volatile fraction that
can be separated into a condensable hydrocarbon oil and a
gas, with industrial applications such as energy generation
and the production of refined chemicals [1113].
Commercial activation of carbon is usually conducted at
temperatures above 800 8C in a mixture of steam and
carbon dioxide. There is general agreement that steam is a
more reactive agent than carbon dioxide and, therefore,
requires the application of lower temperatures [1416].
However, contradictory information has been published
regarding the type of porosity generated by each activation
agent. In this respect, some authors have reported that
steam activation produced carbons with a narrower and
more extensive micropore structure than carbon dioxide
activation [1720]. This effect was attributed to the higher

0008-6223 / 03 / $ see front matter 2003 Elsevier Science Ltd. All rights reserved.
doi:10.1016 / S0008-6223(02)00449-9

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G. San Miguel, et al. / Carbon 41 (2003) 10091016

diffusion rates and greater accessibility to small pores of

the water molecule due to its smaller size. The opposite
was observed by other authors who found comparatively
lower micropore volumes but larger external surface areas
in steam-activated carbons [14,15,21,22].
This paper is aimed at bringing further understanding to
the effect of atmospheric conditions on the characteristics
of activated carbons. The work concentrates on the differences in the use of steam or carbon dioxide as activating
agents and different activation temperatures over a wide
range of degrees of activation. For the purpose of this
work, three series of carbons were produced using waste
tyre rubber as a precursor. The rubber was pyrolysed and
subsequently activated in carbon dioxide (950 and
1100 8C) or steam (925 8C), and the resulting carbons were
investigated for their porosity and surface area using
nitrogen gas adsorption. Aqueous adsorption tests (using
phenol, methylene blue and the textile dye Procion Red
H-E2B) were also conducted to determine the extent to
which differences in pore structure affected the capacity of
the carbons to adsorb species of different molecular size.

2. Experimental

2.1. Tyre rubber

The tyre rubber employed in this work was supplied by
Duralay (UK) as a powdered material of particle size
,0.42 mm.

2.2. Production of rubber-derived activated carbons

Tyre carbons were produced using a Carbolite HTR
11 / 150 laboratory scale rotary furnace, which allowed
pyrolysis and activation to be conducted consecutively
[10]. For the production of each sample, 200 g of rubber
were loaded into the furnace and heated at 5 8C / min to
700 8C under a flowing (500 ml / min) nitrogen atmosphere.
Volatile species generated at this stage were purged out of
the furnace while the carbonised char remained inside the
reaction vessel. When 700 8C was reached, the inert
atmosphere was rapidly substituted by either flowing (500
ml / min) carbon dioxide or steam / nitrogen (80:20, v / v).
The furnace was then heated (5 8C / min) to a target
temperature of between 925 and 1100 8C. Different reaction times were then applied for the generation of each
sample.
The resulting carbons were ground and sieved to a
particle size ,150 mm. The carbon series activated in
carbon dioxide at 950 and 1100 8C are referred to in this
paper as P 950 and P 1100, respectively. Steam-activated
]
]
carbons produced at 925 8C are referred to as SP]925.
Individual samples are designated using their series code
followed by their activation time (in minutes).

2.3. Characterisation of activated carbons by nitrogen

gas adsorption
Carbon samples were characterised for their surface and
pore characteristics using continuous volumetric nitrogen
gas adsorption at liquid nitrogen temperature. Analyses
were conducted in a Beckman Coulter Omnisorp M100
automatic adsorption analyser (Beckman Coulter, High
Wycombe, UK). Total surface areas were determined by
application of the BET equation [23,24] to the adsorption
data in the p /p8 range 0.0150.15, which generated
correlation coefficients r 2 .0.9999. External surface areas
were determined by application of the t-plot model in the
[2426], which generated correlation corange 79 A
efficients r 2 .0.9995. The DubininAstakhov (DA)
model was employed to characterise carbon microporosity
[2729]. The DA equation was applied in the pressure
range p /p8 0.00050.1 and generated correlation coefficients r 2 .0.9995.

2.4. Aqueous adsorption characteristics

Selected carbons were investigated for their aqueous
adsorption characteristics using phenol, methylene blue
and the textile dye Procion Red H-E2B. Adsorption
isotherms for Procion Red were produced by contacting
100 mg of carbon with 100 ml of solutions containing
1001000 mg / l of dye. For the other two compounds the
isotherms were produced by contacting different masses of
carbon (25600 mg) with 100 ml of phenol (235 mg / l) or
methylene blue (561 mg / l) solution. In order to minimise
the effect of pH on the adsorption determinations, stock
solutions contained 500 mg / l of sodium bicarbonate and
its pH adjusted to pH 6.860.2 by addition of concentrated
hydrochloric acid.
Carbon mixtures were end-over-end shaken for 24 h in a
temperature-controlled room at 20 8C and filtered through
Whatman WCN 0.45-mm membranes (textile dyes) or
Whatman No. 1 (phenol and methylene blue) filter-papers.
Residual concentrations were determined using a PerkinElmer Lambda 3 UVVis spectrophotometer at 265 nm
(phenol), 661 nm (methylene blue) and 510 nm (Procion
Red). Adsorption results were modelled according to the
Langmuir equation [30] to determine adsorption parameters Xm and b.

3. Results and discussion

3.1. Product yields

The first stage in the carbon production process involved
heating the tyre rubber to 700 8C under inert atmospheric
conditions. Work reported elsewhere had shown that, under
similar conditions, the rubber decomposed at temperatures
between 300 and 500 8C [10], while the application of

G. San Miguel, et al. / Carbon 41 (2003) 10091016

1011

respectively, and produced correlation coefficients (r 2 )

above 0.99.
The temperature employed for steam activation (925 8C
in series SP 925) was such that it resulted in a reaction rate
]
of 4.5 g / h, comparable to that of carbon dioxide at 950 8C.
Hence, differences in the characteristics of series SP 925
]
and P]950 can only be attributed to the nature of the
activation agent.

3.2. Porosity and surface area characteristics

Fig. 1. Product yields observed during the activation of rubber

carbon using steam (SP 925) and carbon dioxide (P 950 and
]
]
P 1100) at different temperatures.
]

higher temperatures did not affect the mass of residual char

significantly. Hence, the application of 700 8C was sufficient to ensure complete rubber pyrolysis and elimination
of derived volatile products, while the application of inert
conditions (nitrogen) ensured that no oxidation of the
carbon took place at this stage. The process generated 40.5
wt% of solid char, which remained inside the reaction
vessel, and a volatile fraction that accounted for the
remaining 59.5 wt%.
As illustrated in Fig. 1, activation of the chars at higher
temperatures under oxidising conditions resulted in a
progressive reduction of the carbon yield, which followed
a linear relationship with the reaction time. Reaction rates
in carbon dioxide at 950 8C (series P 950) and 1100 8C
]
(series P]1100) were calculated at 4.6 and 14.4 g / h,

Fig. 2 illustrates the adsorptiondesorption nitrogen

isotherms exhibited by pyrolytic char generated at 700 8C
(Pyro) and two activated samples (SP]925]400 and
P]950]400). The two activated carbons were produced to
degrees of activation similar to each other (45.3 wt% burn
off) so that their isotherms could be compared. The figure
indicates that steam produced a slightly higher N 2 adsorption than CO 2 activation, illustrating that it is more
aggressive than CO 2 .
The inactive carbon (Pyro) exhibited an isotherm of type
VI, characteristic of mesoporous materials [24]. The
activated samples presented greater adsorption capacities at
low relative pressures, indicating the presence of a more
developed micropore structure. The shapes of these isotherms are of mixed type Itype IV [24], characteristic of
microporous materials containing a well developed mesopore structure. Differences in the shape of the three
isotherms are not very significant, evidencing general
similarities in the pore structure of the activated samples.
Figs. 36 illustrate the evolution of various aspects of
the carbon porosity represented against their degree of

Fig. 2. Nitrogen gas adsorptiondesorption isotherms exhibited by tyre rubber pyrolytic char (Pyro) and carbons activated in steam
(SP 925 400) and carbon dioxide (P 950 400) to a similar degree of burn off.
]
]
]
]

1012

G. San Miguel, et al. / Carbon 41 (2003) 10091016

Fig. 3. Effect of activation on the BET surface area of rubberderived carbons.

Fig. 4. Effect of activation on the DA micropore volume of

rubber-derived carbons.

activation (carbon burn off). The results in Fig. 3 show a

progressive increase in the BET surface area with the
2
degree of activation to a maximum of 1070 m / g. It
should be noted that, owing to the microporous nature of
the carbons, the BET values reported do not represent true
surface areas but an indication of the nitrogen adsorption
capacity of the carbon under the conditions indicated
[17,24]. Comparison of results from series P]950 and
SP]925 shows that steam produced larger BET surface

Fig. 5. Effect of activation on the DA exponential value (n) of

rubber-derived carbons.

Fig. 6. Effect of activation on the t-plot external surface area of

rubber-derived carbons.

areas than carbon dioxide. Differences ranged between 3

and 28% and were more pronounced in samples produced
to high degrees of activation, which was attributed to the
additive effect of the activation process on the porous
structure.
Comparison of results from series P 950 and P 1100 in
]
]
Fig. 3 also show small differences in the characteristics of
carbons produced at different temperatures (950 or
1100 8C). It has been suggested that the diffusion of gas
molecules to the interior of the carbon particle may be
limited at higher reaction rates [17]. When this happens,
activation of the carbon particle takes part primarily in
areas readily accessible to the oxidising agent (external
surface and large pores). It has also been suggested that
temperature may influence the formation and diffusion of
hydrogen and carbon monoxide, two by-products of the
activation reaction with inhibiting properties [14]. Accumulation of these species inside the particle occurs more
effectively in narrow cavities favouring the development of
larger pores.
Fig. 4 illustrates the evolution in total micropore volume, as determined by application of the DubininAstakhov (DA) equation. Results followed a similar pattern
to that described for the BET surface area. Maximum
values were exhibited by highly activated carbons produced using steam activation (up to 0.554 ml / g). Carbon
dioxide-activated samples exhibited lower micropore volumes with differences being significant only at higher
degrees of activation.
Qualitative information about the relative size of micropores can be obtained from the analysis of the DA
exponential value (n), as illustrated in Fig. 5. This parameter has been associated with the width of the energy
distribution in the microporosity of the carbons. Thus,
molecular sieve carbons presenting a narrow distribution of
small micropores have been reported to produce n values
close to 3 while strongly activated carbons containing a
more heterogeneous distribution of micropores exhibit n
values below 2 [27,28].

G. San Miguel, et al. / Carbon 41 (2003) 10091016

The results in Fig. 5 for series P]950 and SP]925 suggest

that steam activation produced micropores of smaller
dimensions than carbon dioxide. Comparison of results for
series P 950 and P 1100 also show that activation at lower
]
]
temperatures (950 instead of 1100 8C) resulted in the
formation of narrower micropores. It should be noted that,
owing to molecular sieve effects associated with the
nitrogen molecule, the results presented in this work may
not be accurate for very narrow micropores like the ones
formed during the initial stages of the activation process
[31,32]. The use of carbon dioxide adsorption has been
suggested for the analysis of these pores [31].
Fig. 6 shows a progressive increase in the external
surface area during the initial stages of the activation
process. This increase becomes more rapid as activation
proceeds to values in excess of 50 wt% burn off, which has
been attributed to the burn out of pore walls and the
subsequent transformation of large micropores into mesopores. Experimental results showed very small differences
in the external surface areas of samples produced using
different atmospheric conditions.

3.3. Aqueous adsorption characteristics

Aqueous adsorption tests were conducted on selected
tyre rubber carbon with the aim of producing further
evidence about their porous structure and also for assessing
potential applications in the water treatment industry. The
three adsorbate compounds employed in this work cover a
range of molecular sizes, which makes them useful for the
investigation of adsorption in pores of different dimensions. Phenol (94 MW) is preferentially adsorbed in small
and medium sized micropores while methylene blue (394
MW) is mainly adsorbed in medium and large micropores

1013

[30,33]. Owing to its larger molecular dimensions, textile

dye Procion Red H-E2B (1300 MW) does not have access
to small micropores and adsorption of this compound takes
place preferentially in large micropores and small mesopores [33].
Adsorption capacity (Xm ) and affinity values (b), as
determined using the Langmuir equation, are presented in
Table 1 for all the samples analysed. For illustration, Fig. 7
presents the adsorption isotherms in more detail for phenol
(left), methylene blue (middle) and Procion Red (right)
produced by carbons from series SP 925 (steam activated
]
at 925 8C). Individual isotherms are identified by the
activation time (in minutes) of the sample from which they
originate.
Table 1 shows that adsorption of phenol by carbons
from series P 950, SP 925 and P 1100 increased rapidly
]
]
]
during the initial stages of the activation process to reach
values around 100 mg / l. This observation can be correlated with the rapid formation of narrow micropores, as
illustrated in Figs. 35. However, activation in excess of
3040 wt% (carbon burn off) produced a less significant
variation in the adsorption capacity for this compound.
During this stage it is believed that the increase in total
micropore volume is counteracted by the destruction of
micropores of smaller dimensions, where phenol is adsorbed preferentially.
Table 1 also shows a progressive increase in the
adsorption of methylene blue with the degree of carbon
burn off, even at higher degrees of activation. This pattern,
similar to that observed for DA micropore volume BET
surface area, provides further evidence of the adsorption of
this compound in pores of larger dimensions than phenol.
Highly activated carbons presented adsorption capacities
for this compound of up to 360 mg / g.

Table 1
Langmuir parameters determined for the adsorption of phenol, methylene blue and Procion Red by tyre rubber-derived carbons produced
under different activation conditions
Carbon
burn off
(wt%)

Phenol
Xm
(mg / g)

Methylene blue
b

Xm
(mg / g)

P 950 80
12.5
53
0.07
0.99
74
0.450
]
]
P 950 240
31.6
89
0.13
0.99
196
0.708
]
]
P 950 400
45.3
97
0.11
0.95
254
0.876
]
]
P 950 480
52.5
99
0.01
0.96
292
0.762
]
]
P 950 640
65.4
94
0.01
0.98
352
1.085
]
]
SP 925 80
12.5
64
0.06
0.99
125
0.06
]
]
SP 925 240
30.1
93
0.09
0.97
236
0.52
]
]
SP 925 400
45.3
92
0.11
0.96
296
0.19
]
]
SP 925 480
49.8
105
0.07
0.98
325
0.37
]
]
SP 925 640
63.2
106
0.06
0.99
360
0.57
]
]
P 1100 60
31.1
85
0.12
0.98
189
0.403
]
]
P 1100 120
46.5
89
0.07
0.98
287
0.513
]
]
P 1100 180
66.2
76
0.07
0.97
327
0.772
]
]
Values determined by application of the Langmuir equation to the adsorption data.

Procion Red
r

0.87
0.95
0.89
0.98
0.87
0.90
0.87
0.94
0.99
0.99
0.88
0.94
0.88

Xm
(mg / g)

r2

67
99
145
237
385
67
104
139
211
333
105
188
n/a

0.489
0.260
1.230
0.279
0.383
0.204
0.138
0.479
0.179
0.345
0.418
0.418
n/a

0.96
0.99
0.91
0.93
0.97
0.98
0.99
0.92
0.98
0.99
0.94
0.94
n/a

1014

G. San Miguel, et al. / Carbon 41 (2003) 10091016

Fig. 7. Adsorption isotherms for phenol (left), methylene blue (middle) and Procion Red (right) exhibited by tyre rubber carbons from series
SP 925.
]

Adsorption of Procion Red increased slowly during the

initial stages of the activation process and more rapidly at
higher degrees of activation, as shown in Table 1. This
pattern, which resembles that of the external surface area
in Fig. 6, has been attributed to the adsorption of this
compound in pores of large dimensions (large micropores
and mesopores) and the occurrence of molecular sieve
effects [33].
The adsorption characteristics of carbons from different
series produced to similar degrees of activation (burn off)
can be compared to assess the effect of activating agent
(steam or carbon dioxide) and temperature (9501100 8C).
Experimental results in Table 1 show that steam (series
SP 925) produced carbons of higher adsorption capacities
]
for both phenol and methylene blue than carbon dioxide
(series P 950). Differences ranged between 3 and 21% in
]
the case of phenol and between 3 and 70% in the case of
methylene blue, always in favour of the steam-activated
carbons. These results support the theory suggested from
the nitrogen gas adsorption test that steam activation
produces carbons with a narrower and more extensive
microporosity than carbon dioxide.
Contrary to that observed for the other two adsorbates,
samples activated in carbon dioxide (series P 950) ad]
sorbed Procion Red more efficiently than those activated in
steam (series SP 925) to a similar degree of burn off. This
]
observation has been associated with the larger dimensions
of the micropores formed by the carbon dioxide, as shown
in Fig. 4, and the development of a slightly more extensive
external surface area, as illustrated in Fig. 6.
Comparison of results in Table 1 also show that samples
activated at higher temperatures (series P 1100) exhibited
]
greater capacities for the adsorption of Procion Red but
lower for phenol and methylene blue than samples activated at lower temperatures (series P 950). Although
]
differences were not very significant, they are in line with

porosity and surface structure determinations presented

above.

4. Conclusions
Activation of pyrolytic chars from waste tyre rubber
resulted in a rapid development of their porosity, surface
area and capacity to adsorb organic species of different
molecular size. Results presented in this paper show that
carbon characteristics are primarily influenced by the
degree of activation of the carbons but also by the nature
of the activation agent (steam or carbon dioxide) and, to a
lesser extent, the process temperature.
The development of total micropore volume (DA) and
effective surface area (BET) followed a linear relationship
with the degree of activation while the formation of
mesopores was particularly extensive at degrees of activation above 50 wt%. Results presented in this paper show
that activated carbons produced in steam exhibited narrower micropores and larger BET surface areas and total
micropore volumes than those produced using carbon
dioxide. Differences in external surface areas were less
significant and usually in favour of the carbon dioxideactivated carbons. Activation at lower temperatures also
generated micropores of slightly narrower dimensions and
larger BET surface areas. However, these differences were
only significant in highly activated carbons.
Porosity characteristics were reflected in the capacity of
the rubber carbons to adsorb organic species of different
molecular sizes from solution. Thus, steam-activated carbons presented greater capacities for the adsorption of
small and medium size species (such as phenol and
methylene blue) while carbon dioxide-activated carbons
adsorbed larger molecular size compounds (textile dye
Procion Red) more effectively.

G. San Miguel, et al. / Carbon 41 (2003) 10091016

There is increasing pressure on industrial processes to

minimise the polluting nature of their discharges, and the
disposal of life-expired materials such as car tyres is being
more strictly regulated. The research described in this
paper demonstrates that a double benefit may be gained by
utilising waste car tyres as a feedstock for quality activated
carbon production, enabling both material recovery and
reuse and pollution abatement. Although the carbons
produced would not necessarily be appropriate for critical
applications such as potable water treatment, applications
related to the treatment of industrial and municipal wastewaters, and other adsorption processes requiring less
stringent quality standards, are potential beneficiaries.
Assuming that production cost advantages exist by using
rubber-derived carbons instead of currently available commercial activated carbons, there is potential to create new
demand for the rubber-derived adsorbents, thus stimulating
the market for them and widening their usage further.

[10]

[11]

[12]

[13]

[14]

[15]

[16]

Acknowledgements
One of the authors (Guillermo San Miguel) would like
Universidades e
to thank the Departmento de Educacion,
of the Basque Government (Spain) for
Investigacion
financial support in the form of a studentship.

[17]

[18]

[19]
[20]

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