SCIENCE CHINA

Technological Sciences
• RESEARCH PAPER • September 2010 Vol.53 No.9: 2515–2520
doi: 10.1007/s11431-010-4058-5

Effect of activation agents on the surface chemical properties and

desulphurization performance of activated carbon
ZHANG XiangLan*, ZHANG Yan, WANG ShuangSheng, ZHANG JingJing & ZHOU Wei
School of Chemical and Environmental Engineering, China University of Mining and Technology (Beijing), Beijing 100083, China

Received March 19, 2010; accepted May 20, 2010

Flue gas pollution is a serious environmental problem that needs to be solved for the sustainable development of China. The
surface chemical properties of carbon have great influence on its desulphurization performance. A series of activated carbons
(ACs) were prepared using HNO3, H2O2, NH3·H2O and steam as activation agents with the aim to introduce functional groups
to carbon surface in the ACs preparation process. The ACs were physically and chemically characterized by iodine and SO2
adsorption, ultimate analysis, Boehm titration, and temperature-programmed reduction (TPR). Results showed that the iodine
number and desulphurization capacity of NH3·H2O activated carbon (AC-NH3) increase with both activation time, and its
desulphurization capacity also increases with the concentration of activation agent. However, HNO3 activated carbon
(AC-HNO3) and H2O2 activated carbon (AC-H2O2) exhibit more complex behavior. Only their iodine numbers increase mo-
notonously with activation time. Compared with steam activated AC (AC-H2O), the nitrogen content increases 0.232% in
AC-NH3 and 0.077% in AC-HNO3. The amount of total basic site on AC-HNO3 is 0.19 mmol·g−1 higher than that on AC-H2O.
H2O2 activation introduces an additional 0.08 mmol·g−1 carboxyl groups to AC surface than that introduced by steam activation.
The desulphurization capacity of ACs in simulate flue gas desulphurization decreases as follows: AC-NH3 > AC-HNO3 >
AC-H2O2 > AC-H2O. This sequence is in accord with the SO2 catalytic oxidation/oxidation ratio in the absence of oxygen and
the oxidation property reflected by TPR. In the presence of oxygen, all adsorbed SO2 on ACs can be oxidized into SO3. The
desulphurization capacity increases differently according to the activation agents; the desulphurization capacity of AC-NH3
and AC-HNO3 improves by 4.8 times, yet AC-H2O increases only by 2.62 as compared with the desulphurization of corre-
sponding ACs in absence of oxygen.

activated carbon, activation agent, surface chemical property, desulphurization, TPR

Citation: Zhang X L, Zhang Y, Wang S S, et al. Effect of activation agents on the surface chemical properties and desulphurization performance of activated
carbon. Sci China Tech Sci, 2010, 53: 2515−2520, doi: 10.1007/s11431-010-4058-5

1 Introduction terials can be applied to simultaneous removal of NOx and

Flue gas pollution is a serious environmental problem that
needs to be addressed for the sustainable development of
China. Carbon materials (activated carbon, activated coke,
carbon fiber, etc.) have been shown to be potential desul-
phurization adsorbents/catalysts for the flue gas desulphuri-
zation process at low temperature. Furthermore, carbon ma-
*Corresponding author (email: zxl311@sohu.com)
mercury [1–3]. To improve the desulphurization perform-
ance at the exhaust gas temperature, various carbon-based
materials have been studied extensively and the results have
shown that the surface chemical properties of carbon have
great influence on its desulphurization performance [4–7].
Activated carbons (ACs) are usually modified to obtain
different surface chemical properties: H2, O2, and NH3 are
mainly used as gas modification agents [8–10], while HNO3,
and H2O2 are used as liquid modification agents[5, 11, 12].

© Science China Press and Springer-Verlag Berlin Heidelberg 2010 tech.scichina.com www.springerlink.com
2516 ZHANG XiangLan, et al.
The modification process increases the preparation steps of
AC used as desulphurization materials. In this paper, the
activation and modification of carbon precursor are carried
out simultaneously, using HNO3, H2O2, and NH3·H2O as the
activation agents. The relations between desulphurization
performance and the AC surface properties are also exam-
ined. Our results will help further research in improving the
performance of desulphurization and reducing the prepara-
tion cost of ACs
2 Experimental
2.1 Preparation of activated carbon
Datong bituminous coal was used as the precursor, and the
proximate analysis is shown in Table 1. A series of ACs
were prepared following the procedures: crushing and siev-
ing the raw coal to 0.074 mm, and then molding, carboniza-
tion and activation.
The molding coal was heated to 600°C at a heating rate
of 10°C/min in flowing N2 (0.16 L/min) and was kept at
600°C for 30 min. After that the temperature was raised to
850°C at a heating rate of 10°C/min.
The activation process was initiated when the tempera-
ture reached 850°C. The activation time was 20, 40, 60,
80 min, respectively. The flow rates of activation agent and
nitrogen were 1.6 mL/min and 0.16 L/min, respectively.
HNO3, NH3·H2O and H2O2 were selected as activation
agents. The concentration of HNO3 was 2 mol/L, 4 mol/L
and 6 mol/L. The concentration of NH3·H2O was 2.2 mol/L,
4.4 mol/L, 6.6 mol/L and 13.4 mol/L. H2O2 concentration
was 3.0 mol/L, 6.3 mol/L and 9.8 mol/L.
For comparison, steam was used as the activation agent
and the corresponding activated carbon (AC-H2O) was pre-
pared under the same activation conditions above. The acti-
vation time was 40 min.
2.2 Characterization of activated carbon
2.2.1 Iodine adsorption number
The iodine adsorption number (iodine number) of activated
carbon was determined according to GB/T7702.7-87.
2.2.2 The measurement of acid and basic functional
groups of ACs (Boehm titration [13])
The surface functional groups containing oxygen were de-
termined using Boehm titration. One gram of ACs with par-
ticle size < 0.074 mm was placed in 25 mL of the following
solutions (0.1 mol/L): NaOH, Na2CO3, NaHCO3 and HCl.
Table 1 Proximate analysis of raw coal (%)
Raw material Vad Aad Mad
Bituminous coal 30.45 3.05 4.33
Sci China Tech Sci September (2010) Vol.53 No.9
The conical flasks were sealed and shaken for 24 h and then
filtered. Afterward, 50 mL of 0.1 mol/L HCl was added to
each filtrate. The Na2CO3 and NaHCO3 filtrate were heated
for 30 min to remove the CO2, and 5 mL of the filtrate was
pipetted and the excess base or acid was titrated with HCl or
NaOH respectively. The number of acid sites was deter-
mined under the assumption that NaOH neutralizes carbox-
ylic, lactonic, and phenolic groups; Na2CO3 neutralizes car-
boxylic and lactonic groups; NaHCO3 neutralizes only car-
boxylic groups. The number of basic sites was calculated
from the amount of HCl that reacted with the carbon.
2.2.3 TPR
Temperature-programmed reduction (TPR) was performed
using TP-5000 (II) adsorption instrument produced by Tian-
jin Xianquan Co. Ltd. (China). H2 was used as the reduction
gas, and N2 was used as the carrying gas. The flow rates of
N2 and H2 were 36 mL/min and 4 mL/min, respectively.
These two gases were mixed and heated to 800°C at the rate
of 20°C/min.
2.2.4 Desulphurization performance of activated carbon
The desulphurization capacity and SO2 catalytic oxidation/
oxidation ratio (CAT-SO2) were used to measure the desul-
phurization performance. A gas mixture in the absence of
oxygen which contained 0.2% (volume percent, the same
for the others) SO2, 10% H2O, and 89.8% N2, and a simu-
lated flue gas containing 0.2% SO2, 10% H2O, 6% O2, and
83.8% N2 were used.
The desulphurization performance of AC in the absence
of oxygen mainly reflects the surface chemical properties of
AC. CAT-SO2 may reveal the catalytic oxidation/oxidation
ability of carbon. The desulphurization performance of AC
in the simulated flue gas presents the desulphurization ca-
pacity of AC and the role of oxygen in the desulphurization
process.
5 g AC was filled in the middle of a fixed-bed reactor
(Φ 13 mm×600 mm) and the bed temperature was raised to
110°C. Mixed gas flowed through the bed and SO2 concen-
tration in the outlet gas was measured [14]. When the SO2
concentration reached 1000 mg·g−1 in the outlet, the adsorp-
tion process stopped, and the AC sample was removed from
the reactor and immersed into distillation water for 24 h and
filtered. The filtrate was separated into two portions. One
portion was oxidized by H2O2 in order to make sure all the
H2SO3 was converted to H2SO4 and precipitated by adding
sufficient BaCl2 solution. The total resulting H2SO4, which
represents the desulphurization capacity, was calculated
according to the amount of precipitation. Another portion
was titrated by standard iodine solution and the resultant
H2SO3 representing the physical adsorbed SO2 on the ACs
was calculated according to the assumption of iodine
amount. The difference between total amount of H2SO4 and
FCad
the amount of H2SO3 is the amount of SO2 catalytic oxi-
62.17
dized or oxidized by ACs. The percentage of SO2 catalytic
 ZHANG XiangLan, et al. Sci China Tech Sci
oxidized or oxidized amount to desulphurization capacity
on the ACs represents CAT-SO2.
3 Results and discussion
3.1 Effect of activation conditions on the iodine num-
ber of ACs
Figures 1 and 2 illustrate the effects of activation time and
concentration of activation agents on the iodine number.
The iodine numbers of ACs prepared from all three activa-
tion agents increase similarly with the activation time.
However, the influence of concentration on iodine number
of ACs is more complicated. With the increase of NH3·H2O
concentration, the variation of iodine number of AC-NH3
was less than 10 mg·g−1 with the exception of the AC pre-
pared using 4.4 mol/L NH3·H2O. The iodine number of
AC-HNO3 decreases at moderately higher activation agent
concentration, while that of AC-H2O2 exhibites a monoto-
nous decreasing function with activation agent concentra-
tion. The different variation of iodine number between the
AC-HNO3, AC-H2O2 and the AC-NH3 is due to the differ-
ent influences of surface oxygen groups and nitrogen func-
tional groups on the carbon reaction rate. Some kinds of
introduced surface oxygen groups inhibite carbon reaction
Figure 1 Effects of activation time on iodine number of activated
carbon.
Figure 2 Effects of concentration of activation agents on the iodine num-
ber of activated carbon (activation time 40 min).
September (2010) Vol.53 No.9 2517
rate, and the introduced nitrogen groups have no significant
effect on carbon reaction rate.
3.2 Effect of activation conditions on desulphurization
performance of ACs
3.2.1 Effect of activation conditions on the desulphuriza-
tion capacity in absence of oxygen
The effects of activation time and activation concentration
on the desulphurization capacity in the absence of oxygen
are shown in Figures 3 and 4, respectively. At an activation
time of 40 min, AC-HNO3 and AC-H2O2 exhibit the largest
desulphurization capacity, but both of their desulphurization
capacity declines after that. Compared with Figure 1, the
surface properties of AC have a greater influence on the
desulphurization capacity than the effect of pore structure
reflected by the iodine number on it. Furthermore, some
kinds of oxygen groups introduced to the carbon surface
have a negative effect on desulphurization as the activation
time increases.
Only AC-NH3 exhibits a monotonously increasing func-
tion with activation time, as with its iodine number. It indi-
cates that the introduction of nitrogen groups to carbon sur-
face is always favorable to the desulphurization perform-
ance of activated carbon [5–10].
Figure 3 Effects of activation time on the desulphurization capacity of
activated carbon in the absence of oxygen.
Figure 4 Effects of activation agents concentration on the desulphuriza-
tion capacity of activated carbon in absence of oxygen.
2518 ZHANG XiangLan, et al.
Figure 4 shows that the desulphurization capacity of
AC-NH3 increases monotonously with the NH3·H2O con-
centration. Again, while AC-HNO3 and AC-H2O2 have
higher desulphurization capacity when the concentrations of
activation agent are 4 mol/L and 6.6 mol/L, respectively,
their desulphurization capacities decline with higher con-
centration of activation agents. Both the activation time and
concentration of activation agent have influences on the
species and amount of oxygen functional groups introduced
to the AC surface and these groups influence the further
desulphurization capacity of ACs.
3.2.2 Effect of activation conditions on CAT-SO2
The effects of activation time and concentration of activa-
tion agents on CAT-SO2 are shown in Figures 5 and 6,
respectively. The AC-HNO3 and AC-H2O2 exhibited the
highest CAT-SO2 when activation time was 40 min and
the concentrations of HNO3 and H2O2 were 4 mol/L and
6.6 mol/L, respectively. The CAT-SO2 of AC-NH3 in-
creased with the NH3·H2O concentration. However, the
CAT-SO2 increased with the NH3·H2O activation time and
reached a peak when the activation time was 60 min; after-
ward, its CAT-SO2 decreased.
The effects of concentration and activation time of
NH3·H2O on the properties of ACs are obviously different
Figure 5 Effects of activation time on CAT-SO2.
Figure 6 Effects of concentration of activation agents on CAT-SO2.
Sci China Tech Sci September (2010) Vol.53 No.9
from those of HNO3 and H2O2 on ACs as shown in Figures 1
to 6. This difference can be attributed to that the introduced
nitrogen functional groups and oxygen functional groups
have different influences on the carbon reaction rate and the
interaction of SO2 with the carbon surface.
3.3 Effect of activation agents on the properties of ACs
To study the surface chemical properties of carbon, ACs
with similar iodine number were prepared using different
activation agents in order to exclude the influence of pore
structure as much as possible. The iodine numbers and ac-
tivation agents are listed in Table 2. The iodine number in-
creases as follows: AC-NH3<AC-HNO3<AC-H2O2<AC-H2O.
However, the difference between the lowest value of 513
mg·g−1 and the largest one at 570 mg·g−1 is only 57 mg·g−1.
The difference of the iodine numbers with these ACs is not
significant.
3.3.1 Oxygen functional groups and nitrogen on activated
carbon
Boehm titration results of ACs are shown in Table 3.
AC-H2O has relative higher surface carboxylic groups
while the acidic functional groups and total basic sites are
the lowest. Compared with AC-H2O, the lactonic groups
on AC-HNO3 and AC-H2O2 increase 0.02 mmol·g−1 and
0.06 mmol·g−1, respectively, and no changes on AC-NH3
were observed. The decrease of carboxylic groups on
AC-HNO3 and AC-NH3 indicates that the formation of car-
boxyl functional groups was inhibited when HNO3 and
NH3·H2O were used as the activation agents. However,
0.03 mmol·g−1 and 0.05 mmol·g−1 phenolic groups were in-
troduced to AC-HNO3 and AC-NH3, respectively. The basic
sites on AC-HNO 3 , AC-H 2 O 2 and AC-NH 3 increase
0.19 mmol·g−1, 0.15 mmol·g−1, and 0.07 mmol·g−1, respec-
tively. It is suggested that the activation of ACs with both
NH3·H2O and HNO3, H2O2 created basic functional groups
on AC surface and led to an increase of total basic sites of
AC. The sum of lactonic and phenolic groups is the same as
the order of the total basic sites, i.e., AC-HNO3>AC-NH3>
AC-H2O2>AC-H2O.
Ultimate analysis of AC-HNO3 and AC-NH3 was meas-
ured in order to determine the amount of nitrogen intro-
duced into the ACs by different activation agents. For com-
parison, the nitrogen content of AC-H2O was also measured,
and the results are shown in Table 4. The nitrogen content
Table 2 Iodine numbers and activation conditions of different activated
carbons
Symbol Activation time and concentration Iodine number
of carbons of activation agents (mg·g−1)
AC-NH3 NH3·H2O, 13.4 mol/L, 40 min 513
AC-H2O2 H2O2, 6.3 mol/L, 40 min 567
AC-H2O Steam, 40 min 570
AC-HNO3 HNO3, 4 mol/L, 40 min 529
 ZHANG XiangLan, et al. Sci China Tech Sci September (2010) Vol.53 No.9 2519

Table 3 Boehm titration results of activated carbons (unit: mmol·g−1)

Samples Carboxylic group Phenolic group Lactonic group Acidic functional groups Basic sites
AC-H2O 0.12 0.11 0.12 0.35 0.93
AC-H2O2 0.2 0.10 0.14 0.44 1.08
AC-HNO3 0.09 0.14 0.18 0.41 1.12
AC-NH3 0.07 0.16 0.12 0.35 1.1

Table 4 Ultimate analysis of activated carbon (%)

Samples Nad Cad Sad Had Others

AC-H2O 0.997 92.74 0.825 0.983 4.455
AC-HNO3 1.074 88.71 0.815 1.014 8.387
AC-NH3 1.229 89.83 0.763 1.002 7.176

of AC-HNO3 and AC-NH3 is higher compared with

AC-H2O. The nitrogen content of AC-HNO3 and AC-NH3
increase 0.232% and 0.077%, respectively. It indicates that
NH3·H2O activation has introduced much more nitrogen to
the surface of AC; the high nitrogen content causes the in-
creasing of basic sites.

3.3.2 TPR analysis

The temperature-programmed reduction (TPR) curves of
ACs are shown in Figure 7. There is a prominent peak dis-
played around 400–750°C for all ACs. AC began to react
with H2 at about 400°C. With increasing temperature, the
H2 consumption increased rapidly with temperature. The
consumption of H2 can attribute to chemisorbing of H2 on
reactive nascent sites created by the decomposition of oxy-
gen-containing groups, and H2 can react with oxidized car-
bons during thermal desorption of oxygen surface com-
plexes [15, 16]. The oxidation ability of AC surface can be
revealed through comparing the peak area of various ACs.
From Figure 7, the oxidation ability of AC surface revealed
by TPR is in the following order: AC-NH3 > AC-HNO3 >
AC-H2O2>AC-H2O. This sequence is in accord with the
CAT-SO2 in the absence of oxygen.
3.3.3 Effect of activation agents on desulphurization per-
formance of subsequent AC
The desulphurization performance of ACs prepared by dif-
ferent activation agents is summarized in Table 5.
Figure 7 TPR profiles of activated carbon samples.
The desulphurization capacity of AC prepared by differ-
ent activation agents is roughly the same in the absence of
oxygen, but the CAT-SO 2 increases from 20% with
AC-H2O to 60% with AC-NH3. The iodine number of ACs
has no substantial difference as indicated in Table 2, which
indicates that the desulphurization capacity in the absence
of oxygen mainly depends on the pore structure reflected by
iodine number. The variation in CAT-SO2 reflects the dif-
ference of surface properties caused by different activation
agents. The CAT-SO2 of ACs in the absence of oxygen is
AC-NH3 > AC-HNO3 > AC-H2O2 > AC-H2O. The orders of
AC-NH3 and AC-HNO3 are different from the order of basic

Table 5 The desulphurization performance of activated carbon under different conditions

Adsorbed gas in the absence of O2 Simulate flue gas Ratio of desulphurization

Samples Desulphurization capacity CAT-SO2 Desulphurization capacity CAT-SO2 capacity under different
(mmol·g−1) (%) (mmol·g−1) (%) adsorption conditions
AC-H2O 0.1402 17.33 0.3682 100 2.62
AC-H2O2 0.1667 43.53 0.4973 100 3.0
AC-HNO3 0.1668 48.98 0.8003 100 4.8
AC-NH3 0.1688 59.8 0.8143 100 4.82
2520 ZHANG XiangLan, et al. Sci China Tech Sci
sites on these two carbons. This difference can be attributed
to the higher nitrogen content of AC-NH3. The effect of
nitrogen functional groups on SO2 catalytic oxidation/oxi-
dation ability is greater than the effect of oxygen functional
groups on it. This is in accord with the increasing of desul-
phurization capacity and CAT-SO2 with NH3·H2O concen-
tration and activated time.
The CAT-SO2 of all ACs reaches 100% in the presence
of oxygen. The desulphurization capacity of various ACs
has a substantial increase; furthermore, the increased
amount is related to the activation agents: AC-NH3 and
AC-HNO3 improves by 4.8 times; yet the AC-H2O increases
only 2.62 times. It reveals that the desulphurization capacity
in the presence of oxygen depends on the specific surface
area and surface chemical properties. Moreover, the surface
chemical property is a more influential parameter.
Some active sites on ACs interact with oxygen at the
presence of oxygen, then catalytically oxidize adsorbed SO2
into SO3. SO3 is more soluble in water than SO2 and is easy
desorbed from active sites; the renascent active sites adsorb
more SO2 and thus enhance the desulphurization capacity.
The order of desulphurization capacity of various ACs is
AC-NH3 > AC-HNO3 > AC-H2O2 > AC-H2O, and this order
is in accord with the CAT-SO2 in the absence of oxygen and
with the oxidation ability reflected by TPR.
4 Conclusions
It has been shown that applying different kinds of activation
agents to the activation process can lead to ACs with dif-
ferent chemical characteristics. Activation by HNO3 and
NH3·H2O lead to the fixation of nitrogen functional groups
as indicated by the ultimate analysis. Meanwhile, different
kinds of oxygen functional groups can be introduced to the
AC-HNO3 surface as indicated by Boehm titration. The
nitrogen content of AC-NH3 is significantly higher than that
in AC-HNO3, which indicates that NH3·H2O activation is an
effective way to introduce nitrogen to the AC surface. The
introduced functional groups can enhance the amount of
both H2 and SO2 adsorbed, and also the SO2 catalytic oxida-
tion/oxidation ability of ACs. Furthermore, the active sites
which have adsorbed H2 chemically are related to the active
site for catalytic oxidation/oxidation of SO2.
CAT-SO2 of ACs reaches 100% and the desulphuriza-
tion capacity increases significantly when simulated flue
gas is used. In the presence of oxygen, CAT-SO2 has noth-
ing to do with the activation agents, but the activation
agents obviously influence the increasing of desulphuriza-
tion capacity: The desulphurization capacity of AC-NH3
and AC-HNO3 improves by 4.8 times, yet the AC-H2O only
September (2010) Vol.53 No.9
increases by 2.62 times compared with the desulphurization
capacity of corresponding ACs in absence of oxygen. The
desulphurization capacity of ACs in the presence of oxygen
is related to its SO2 catalytic oxidation or oxidation ability
in absence of oxygen in this study.
This work was supported by the National Natural Science Foundation of
China (Grant No. 50204011) and the Chemical and Environmental Engi-
neering Lab for the TP-5000(II) adsorption instrument. The authors wish
to thank Professor Pao in University of California, San Diego, for his
timely assistance with the English language correction in the final paper.
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