Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259

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Journal of Analytical and Applied Pyrolysis

journal homepage: www.elsevier.com/locate/jaap

Physicochemical characteristics of a novel activated carbon produced

from tea industry waste
Ali Gundogdu a,∗ , Celal Duran b , H. Basri Senturk b , Mustafa Soylak c ,
Mustafa Imamoglu d , Yunus Onal e
a
Department of Food Engineering, Faculty of Engineering and Natural Sciences, Gumushane University, 29100 Gumushane, Turkey
b
Department of Chemistry, Faculty of Sciences, Karadeniz Technical University, 61080 Trabzon, Turkey
c
Department of Chemistry, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey
d
Department of Chemistry, Faculty of Arts & Sciences, Sakarya University, 54187 Sakarya, Turkey
e
Department of Chemical Engineering, Faculty of Engineering, Inonu University, 44280 Malatya, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: Tonnes of waste are generated during tea production in Turkey, one of the black tea producing countries
Received 30 March 2013 in the world. These wastes are not used for any purposes throughout industrial sector. The objective of
Accepted 19 July 2013 this study is to bring in economic value to waste materials by producing activated carbons from wastes
Available online 29 July 2013
of a tea plant and to characterize their physicochemical properties. Three types of activated carbons
were produced by chemical activation using zinc chloride from tea industry wastes (TIW). Mesoporous
Keywords:
structure and surface area rise as the ratio of ZnCl2 /TIW increases. When the ratios of ZnCl2 /TIW were
Activated carbon
selected as ½:1, 1:1, and 2:1, mesoporous activated carbons are found in the percentages of 10.9%, 39.9%
Tea industry waste
Chemical activation
and 77.7% with BET surface areas of 706, 1066 and 1141 m2 g−1 , respectively. The resultant activated
Zinc chloride carbons were characterized by analyses of proximate–ultimate, FT-IR, SEM, TGA, methylene blue-iodine
Characterization numbers, and surface functional groups.
© 2013 Elsevier B.V. All rights reserved.

1. Introduction Large quantities of readily available and low-cost solid raw

Activated carbon (AC) is a well-known material used in
various environmental applications for water and wastewater
treatment, gas filters, etc. ACs are also used as solid-phase
extractors for removal, separation and preconcentration of some
metallic–nonmetallic species from aqueous solutions [1–3]. ACs
can be prepared from a wide range of raw materials with high
carbon content and low levels of inorganic compounds [4]. ACs
are known as very effective and particularly favorable adsorbents
due to their highly developed porosity, large surface area, variable
characteristics of surface chemistry, and high degree of surface
reactivity. These unique characteristics make ACs very versatile
materials. However, due to their high production costs, these mate-
rials tend to be more expensive than other adsorbents. Therefore,
many studies have been performed on the development of low-cost
activated carbons from various agricultural byproducts or wastes
to remove some organic and inorganic compounds from liquid and
gas phases [5,6].
∗ Corresponding author. Tel.: +90 4562337425; fax: +90 4562337427.
E-mail addresses: aligundogdu@gumushane.edu.tr,
a.ramazan.gundogdu@gmail.com (A. Gundogdu).
materials containing sufficient amount of carbon in their struc-
ture can be used for the production of AC. In addition to commonly
used natural raw materials of coal, wood, pit shells, coconut and
nut shells, various synthetic polymer-based raw materials are used
for manufacturing AC. The physical and chemical structures and
adsorption properties of AC vary depending on initial material used
[7]. If materials having high lignin content, like grape and cherry
seeds, are used, then, mainly ACs with macroporous structure can
be produced. On the other hand, ACs with a high content of micro-
pores can be obtained from almond and apricot seeds, which have
high cellulose content. However, formation of pores is especially
affected by the type of activating agent used in chemical activation
[8].
Production of AC involves two main steps: (i) carbonization
of the raw material in an inert atmosphere and (ii) activation of
the carbonized product by physical or chemical treatment. During
carbonization, the raw material is first pyrolyzed to remove non-
carbon elements, then activation occurs at temperatures ranging
from 700 to 1100 ◦ C in order to develop the porosity of the car-
bonized material, and thus resulting in an increased adsorption
capacity [5]. Physical and/or chemical activation can be applied
to the precursor. Physical activation involves carbonization of a
carbonaceous material followed by activation in the presence of

0165-2370/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jaap.2013.07.008
250 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259
activating agents such as CO2 or steam. In chemical activation, car-
bonization and activation occurs simultaneously, and raw material
is impregnated with activating agents such as ZnCl2 , H3 PO4 , KOH,
K2 CO3 , then the impregnated material is heated in the absence of
oxygen [9].
ZnCl2 is one of the most widely used agents for the chemical acti-
vation of a carbonaceous material [10]. Chemical activation using
zinc chloride produces high surface area and more porous ACs, and
thus provides high adsorption capacity. ZnCl2 acts as a dehydrat-
ing agent promoting the decomposition of carbonaceous material
during the pyrolysis process, restricts the formation of tar, and
increases the carbon yield [11].
In this study, three different types of ACs are produced from tea
wastes of a plant by chemical activation using ZnCl2 . Tea industry
waste (TIW), produced in large amounts every year, is a byproduct
of tea industry representing a major sector in Turkey. According
to the reports of General Directorate of Tea Enterprises (Çaykur),
approximately more than 700,000 tons of fresh tea leaves per year
are used in black tea production and approximately 4% of this
amount is disposed of as tea fibers and stalks. These disposed
materials are only exploited as organic fertilizers. Considering the
approximately 30,000 tons of waste generated annually from tea
production in Çaykur facilities and those generated by private facil-
ities, it emerges that the amount of tea waste in Turkey is much
more than the figures given [12–14].
There are a number of academic studies concerning tea wastes
both in Turkey and worldwide; but their use in industry is hardly
known. There are also numerous studies regarding direct use of
tea wastes for removing various pollutants, whereas the studies
suggesting using tea leaves in AC production are rare. Yagmur
et al. reported obtaining AC from tea wastes by chemical acti-
vation using H3 PO4 in the presence of microwave energy [15].
Ahmaruzzaman and Gayatri produced AC from tea wastes by H3 PO4
activation for removing p-nitrophenol from water [16]. Recently,
Duran et al. gained AC from tea wastes by H2 SO4 activation for
co-determination of Cr(III) and Cr(VI) in various water and solid
samples [17], and also Gundogdu et al. produced AC from tea indus-
try wastes for removing phenol molecules from water [18].
In this study, three different ACs were generated from TIW by
zinc chloride activation. Produced ACs were characterized by vari-
ous analytical techniques such as analyses of proximate–ultimate,
FT-IR, SEM, TGA, methylene blue-iodine numbers, and surface func-
tional groups. The aim of this study was to prevent possible environ-
mental damage caused by these wastes, which bear the risk of cre-
ating an environmental concern due to their safely uncontrollable
nature, as well as giving them an economic value by producing AC.
2. Materials and methods
2.1. Preparation of AC
In this study, TIW used, as the starting material for AC produc-
tion, were supplied from green tea processing plant located in the
town of Of, Trabzon, Eastern Black Sea Region, Turkey. Before pro-
ducing AC, TIWs were first dried in an oven at 105 ◦ C for 20 h and
then ground and sieved to the particle size range of 125–300 ␮m
[18].
Three different types of ACs were produced by chemical activa-
tion with ZnCl2 depending on activating agent/TIW ratios selected
as ½:1, 1:1 and 2:1, respectively. Initially, 20 g of TIW in dimen-
sions of 125–300 ␮m was separately mixed with 10, 20 and 40 g
ZnCl2 . Then 150 mL of distilled water was added to the mixtures
and they were allowed to stand for 24 h. After excess solution was
removed, the solution was put into stainless steel reactor (Fig. 1),
with dimensions of 9.0 cm × 19.0 cm. The reactor was placed into
a cylindrical high temperature furnace (Nuve MF 100, Turkey) and
the mixture inside the reactor was carbonized at 700 ◦ C under N2
atmosphere at a flow rate of 100 mL/min for 4 h.
The resultant three types of ACs were boiled within 2 M HCl
to remove any impurities, filtrated through vacuum filtration
setup, and washed thoroughly with ultra-pure water. Then the ACs
obtained were dried at 105 ◦ C for 4 h [18–21].
The procedures for AC production explained above were also
repeated by only carbonization of TIW without using ZnCl2 . Within
the scope of this study, five different adsorbents were prepared,
namely (i) original TIW not subjected to any process, (ii) only car-
bonized tea industry waste (TIWC; tea industry waste carbon, char
product), (iii) AC obtained using ZnCl2 /TIW in the ratio of ½:1
(TIWAC-1; tea industry waste activated carbon), (iv) AC acquired
using ZnCl2 /TIW in the ratio of 1:1 (TIWAC-2) and (v) AC gained
using ZnCl2 /TIW in the ratio of 2:1 (TIWAC-3).
2.2. Characterization of adsorbents
The adsorbents obtained were characterized by several tech-
niques. Quantitative measurement of humidity, volatile matter,
fixed carbon and ash amount was defined by proximate analy-
sis. To determine C, H, N, S and O quantitatively ultimate analysis
(elemental analysis) was applied. Then, surface characterization
analyses were carried out. For this, BET (Brunauer, Emmett, Teller)
surface areas, micro-mesopore areas, pore volumes, pore distribu-
tions were determined. Furthermore, analyses such as iodine and
MB numbers, FT-IR (Fourier transform infrared), SEM (scanning
electron microscopy), TG (thermogravimetry), DTG (derivative
thermogravimetry) and DTA (differential thermal analysis) were
applied. Also to determine pH–pHpzc and surface acidic groups
Boehm titration were implemented.
Proximate analyses were performed according to ASTM D2854-
96(2004) and ASTM D5832-98(2003) [22,23], whereas ultimate
analyses were carried out by pyrolyzing samples in the elemental
analysis instrument (LECO CHNS-932, St. Joseph, USA) at around
950–1000 ◦ C and oxidizing them to N2 , CO2 , H2 O and SO2 gases.
Quantification of acidic surface oxide groups of the adsor-
bents (lactonic, phenolic and carboxylic groups) was performed by
Boehm titration. According to this, 1 g of each adsorbent was sep-
arately treated with 50 mL 0.1 M NaOH (for neutralization of total
surface acidic groups), NaHCO3 (for neutralization of lactonic and
carboxylic surface acidic groups) and Na2 CO3 (for neutralization of
only carboxylic surface acidic groups) for 24 h. After the mixtures
separated, the filtrates were titrated with 0.1 M HCl [24,25].
The pH value of each adsorbent was determined by first agitat-
ing 0.1 g of adsorbent with 10 mL of boiling ultra-distilled water,
followed by measuring pH of filtrate with a pH meter (Hanna pH
211 with glass electrode, Germany). To specify pHpzc values of the
adsorbents, a series of 0.1 M NaCl solutions with initial pH values
in the range of 2–10 were agitated with 0.1 g of each adsorbent for
24 h. After agitation, the adsorbent and the solution were separated
from each other by centrifuging, and equilibrium pH values of the
solutions were measured with a pH meter. A graph of pH (y-axis)
obtained by subtracting equilibrium pH values from initial pH val-
ues versus initial pH values (x-axis) was plotted. The point in which
the graph cuts x-axis, where the value of y is 0, was noted as pHpzc
value [26].
Scanning electron micrographs of 5 adsorbents (by JEOL/JSM-
6335F scanning electron microscope, Tokyo, Japan) were shot by
enlarging 500, 1000 and 2000 times. After carbonization and activa-
tion changes occurred, on the surface of the adsorbents and porous,
were compared.
For surface characterization analyses, about 0.1 g of dry
samples was measured on surface characterization instrument
(Micromeritics TriStar 3000, Norcross, USA) by N2 adsorption at
 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259
Fig. 1. AC production reactor.
77 K and at a relative pressure (P/Po ) in the range of 10−6 –1.
Before such measurements, the samples were degassed at 105 ◦ C
for 4 h. BET (Brunauer–Emmett–Teller) surface areas (SBET ), micro-
pore areas (Smicro ) and total pore volumes (Vtotal ) were obtained
from N2 adsorption isotherms plotted. Average pore diameters (Dp )
were calculated from volume and surface area data according to
4 Vtotal /SBET formula. Mesopore volumes and areas (Vmeso and Smeso )
were determined by subtracting micropore volumes and areas from
total pore volumes and areas. Distribution of pore dimensions was
found by DFT plus software application. Micropore volumes (Vmicro )
and mesopore volumes (Vmeso ) were calculated according to t-plot
method [27–30].
In order to plot TG, DTG and DTA curves for five adsorbents, a
few milligrams of precisely weighed sample were subjected to high
temperatures (Seiko II Exstar 6000 TG/DTA thermal gravimetric
analyzer, USA) both in N2 and O2 media and losses in its mass were
recorded. Heating procedures were started at room temperature
and reached up to 800 ◦ C by gradually increasing the temperature.
The heating process is allowed to continue at this temperature for a
while; when no change in mass observed, the process is terminated.
TG, DTG and DTA graphs were plotted as a function of changes
versus time and then construed.
For FT-IR analyses, 10–20 mg of samples was taken and
thoroughly mixed with 50–100 mg of spectroscopy-grade KBr,
compressed and turned into tablets. In case of grabbing moisture
from the air, after drying tablets completely, their spectra were
taken by the instrument of Perkin Elmer 1600 FTIR spectropho-
tometer in the range of 4000–400 cm−1 (MA, USA).
To specify MB numbers, 0.02 g of adsorbent was agitated
with 10 mL 1000 mg L−1 MB solutions for 12 h. Then, the mix-
ture was filtrated through 0.45 ␮m nitrocellulose membrane. MB
concentration left in the filtrate was determined by carrying out
measurements in UV–vis spectrophotometer (Unicam UV-2 spec-
trophotometer, England) at 668 nm [31]. Iodine numbers of 5
adsorbents were defined according to ASTM D4607-94(1999) [32].
3. Results and discussion
3.1. Characterization results
3.1.1. Proximate–ultimate analysis
Contents of moisture, volatile matter, fixed carbon and ash along
with AC production yields for TIW, TIWC, TIWAC-1, TIWAC-2 and
TIWAC-3 are given in Table 1.
It is evident from the table that the highest amount of volatile
matter determined for TIW belongs to the starting material since it
was not subjected to heat treatment as other absorbents were. Rel-
atively high amount of ash (4.7%) arises from its inorganic content.
251
When TIWC, the product obtained only by carbonization, is consid-
ered, it is apparent that it has a relatively low amount of volatile
matter (13.2%) due to being subjected to carbonization at 700 ◦ C
like the other ACs. Since it has not been activated with any agent,
an adsorbent with a low surface area but a high amount of fixed
carbon (74.2%) was obtained. The inorganic structure created as a
result of carbonization of TIW became relatively abundant in TIWC
and caused an increase in ash content (5.40%).
In the case of TIWAC-1, TIWAC-2 and TIWAC-3 ACs, availabil-
ity of the inorganic content in the structure weakens because of
increasing porous structure and a significant amount of ash is
removed from the medium during washing of ACs after produc-
tion. The production of activated carbons obtained by activation of
ZnCl2 almost have the same yield but increasing amount of ZnCl2
caused more fractures in the structure and so the productivity
has declined, hence causing an increase in mesoporous structure.
However, ZnCl2 , a Lewis acid, contributes to aromatization of the
structure as having only a dehydrating agent role in producing of
AC. ZnCl2 does not react with carbon, hence resultant yield is much
higher compared to activated carbons obtained by KOH activation
[10].
Carbon atoms play a major role in the organized structure and
aromatization [33]. When the results of ultimate analysis in Table 1
are considered, TIWAC-3 has the highest C content, whereas TIW
has the lowest, so the ratio of C/H has also increased by rising C
percentage. An increment in the ratio of C/H indicates an increase
of aromatization in the structure, hence formation of a regular
structure as well as an increase in graphitization. For 5 differ-
ent adsorbents, oxygen (O) amount decreases against increasing
amounts of C as expected. In 3 ACs, the amounts of N also increased
in parallel with increasing amounts of C. In contrast, reductions in
the amounts of H and O are observed. H and O atoms were gradually
removed from structure using zinc chloride being a dehydrating
agent [11].
3.1.2. SEM analysis of the adsorbents
SEM photographs of five types of adsorbents shot for visualizing
their surface structures are shown in Fig. 2. SEM photograph of TIW
used as starting material for AC production shows that the surface
of the material is very rough and has indents and protrusions, but
has no porous structure, channels or gaps (Fig. 2(a) and (b)). In the
product obtained only by carbonization without using activating
agents (TIWC), it can be seen that partial porous structures formed
as a result of high temperature in N2 environment (Fig. 2(c)).
When SEM images of three types of ACs obtained by activation
with different amounts of ZnCl2 are considered, it is apparent that
TIWAC-1 and TIWAC-2 ACs are relatively similar but TIWAC-3 AC
has a little more different surface structure (Fig. 2(d)–(f)). By SEM,
252 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259

Table 1
Contents of moisture, volatile matter, fixed carbon and ash along with AC production yields for the adsorbents.

Adsorbent Proximate analysis (%) Ultimate analysis (%)

Moisture Volatile matter Fixed carbon Ash AC yield C H N S Ob C/Hc

TIW 6.6 77.2 11.4 4.7 – 47.9 5.9 2.4 0.30 43.6 0.7
TIWC 7.3 13.2 74.2 5.4 43.1a 68.3 1.5 2.2 0.16 27.9 3.9
TIWAC-1 9.7 16.6 71.5 2.2 39.6 75.5 2.0 3.2 0.19 19.2 3.3
TIWAC-2 8.1 19.6 71.2 1.0 36.7 79.3 1.8 3.5 0.24 15.2 3.7
TIWAC-3 5.2 11.0 82.6 1.2 35.8 83.5 1.4 3.9 0.23 10.9 4.9

TIW, tea industry waste (original raw material, precursor); TIWC, tea industry waste carbon (only carbonized material); TIWAC-1, tea industry waste activated carbon
(produced with ½:1activating agent/precursor); TIWAC-2, tea industry waste activated carbon (produced with 1:1 activating agent/precursor); TIWAC-3, tea industry waste
activated carbon (produced with 2:1 activating agent/precursor).
a
Carbonization yield.
b
Calculated by difference.
c
Mole ratio.

only gaps, slits or channels can be seen, however, extremely useful
information can be obtained on the pore structure [34]. Although
information about the type of pores cannot be acquired by SEM,
porous structures of ACs can relatively be compared and the devel-
opment of porous structures can be monitored through [35]. When
SEM images magnified by a thousand times are examined, pore
sizes can be comparable. It can be said that pore dimensions of
TIWAC-1, shown in Fig. 2(d) is smaller than those of TIWAC-2 and
TIWAC-3, shown in Fig. 2(e) and (f). As a result, increasing amount
of activating agent causes a trend in the structure going from

Fig. 2. SEM micrographs for (a and b) TIW, (c) TIWC, (d) TIWAC-1, (e) TIWAC-2, and (f) TIWAC-3.
 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259 253

Table 2
BET surface areas and pore size distributions of the adsorbents.

Adsorbent SBET (m2 g−1 ) Smicro Smeso Vtotal (cm3 g−1 ) Vmicro Vmeso Dp a (nm)
2 −1 2 −1 3 −1 3 −1
m g % m g % cm g % cm g %

TIW 35.2 – – – – – – – – – –
TIWC 118.1 59.7 50.6 58.4 49.4 0.066 – – – – 2.25
TIWAC-1 706.0 629.0 89.1 77.0 10.9 0.369 0.324 87.8 0.045 12.2 2.09
TIWAC-2 1066.0 641.0 60.1 425.0 39.9 0.580 0.337 58.1 0.243 41.9 2.18
TIWAC-3 1141.0 254.0 22.3 886.0 77.7 0.806 0.130 16.1 0.676 83.9 2.83

SBET , BET surface area; Smicro , micropore surface area; Smeso , mesopore surface area; Vtotal , total pore volume; Vmicro , micropore volume; Vmeso , mesopore volume; Dp , average
pore diameter; –, not determined.
a
4 Vtotal /SBET .

microporosity toward mesoporosity. This situation is also discussed
at the analyses of surface characterization (Section 3.1.3).
3.1.3. BET surface areas and distribution of pore sizes
Surface areas of ACs and other adsorbents are extremely
important in terms of adsorption ability. Surface area and pore char-
acteristics changes depend on numerous factors such as starting
material and its structure, selected activation method and agents
used, temperature and duration of pyrolysis. Even though the start-
ing material is the same, ACs with very different characteristics can
be produced by any change in other parameters [24,36]. BET surface
areas (SBET ), t-plot micropore areas (Smicro ), mesopore areas (Smeso ),
total pore volumes (Vtotal ), micropore volumes (Vmicro ) and average
pore diameters (Dp ) for five adsorbents are given in Table 2.
As expected, TIW has a very small surface area (35.2 m2 g−1 ).
TIWC has a slightly higher surface area (118.1 m2 g−1 ). In the car-
bon produced by temperature rise in N2 atmosphere and removal
of volatile components, formation of pores can be seen although
they are in small numbers. These pores can also be seen in SEM
photographs (Fig. 2(c)). Temperature of the environment during
carbonization when no activating agent used, also contribute more
or less to pore formation. For example, in a study where AC was pro-
duced from lignite, improvement of porous system was observed by
increasing temperature [37]. Therefore, owing to developing pore
structure of TIWC by the effect of temperature, its surface area is
found larger than that of TIW.
As seen from Table 2, use of activating agent along with car-
bonization has increased surface area of the material and enhanced
porous structure. Surface areas and porous structures of all three
ACs have significantly developed in comparison to TIW and TIWC.
TIWAC-3, the AC obtained by using the highest amount of acti-
vating agent, has the highest surface area (1141 m2 g−1 ). Although
the starting material and activating agent are the same, ACs with
varying surface and porous structure can be produced by changing
ratios as observed in this study. For this purpose, when three ACs
obtained by activation with zinc chloride are compared with each
other, it is seen that surface area increases with rising ZnCl2 /TIW
ratio (Table 2). This proves that the activating agent enhances
surface area and hence has an extremely important role in pore
formation [36]. Increase in the amount of zinc chloride also led
to development of mesopores. While TIWAC-1, micropore area
(Smicro ) contains a large portion of total area (SBET ) (89.1%), TIWAC-2
and TIWAC-3, microporous areas are gradually decreased and thus
mesoporous areas have improved. Mesoporous areas in TIWAC-3
reached 77.7% of the total area. This case is also understood by an
increase in average pore diameters (Dp ) and mesopore volumes

Fig. 3. (a–c) N2 adsorption isotherms for TIWAC-1, TIWAC-2 and TIWAC-3, respectively. (d–f) Pore size distributions for TIWAC-1, TIWAC-2 and TIWAC-3, respectively.
254 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259

Table 3
Quantities of surface acidic functional groups and values of pH and pHpzc of the adsorbents.

Adsorbent Surface acidic functional groups (mmol g−1 ) pH pHpzc

Total acidic groups Carboxylic groups Phenolic groups Lactonic groups

TIW 2.47 1.03 0.98 0.46 5.32 4.90

TIWC 0.72 0.34 0.28 0.10 4.96 5.55
TIWAC-1 3.14 1.55 1.34 0.26 4.11 6.20
TIWAC-2 2.71 1.03 1.16 0.52 4.20 5.85
TIWAC-3 2.50 0.98 0.95 0.57 4.93 6.45

(Vmeso ) with increasing amount of zinc chloride. Since aromati-
zation takes place in activation mechanism of zinc chloride, the
sample with the highest ratio of C (TIWAC-3) has the highest sur-
face area. It can be said that as the percentage of zinc chloride is
increased structure began to deteriorate, in other words, micropo-
res undergo deformation and are transformed into mesopores.
In this study, from the data obtained as a result of N2 adsorp-
tion at 77 K on three ACs, a graph of N2 volume adsorbed (cm3 g−1 )
versus relative pressure (P/Po ) was plotted and gas adsorption
isotherms were obtained. Adsorption isotherms help determi-
nation of general characteristics of adsorbents such as surface
area, pore volume and porous structure [34]. Gas physisorption
isotherms are divided into six groups according to IUPAC classi-
fication (1985) and the first five types of the classification were
suggested by Brunauer et al. [38].
Adsorption isotherms obtained can be seen in Fig. 3. Diameter of
curvature at bending point of isotherms depending on increasing
P/Po values increases due to the increase in surface area of AC. When
these three ACs are analyzed diameter of curvature at bending point
of the curves plotted rises as a result of shrinking micropore surface
area with increasing amount of zinc chloride. Isotherms plotted
for TIWAC-1 and TIWAC-2 are similar to Type I isotherms indi-
cating mostly a microporous structure, however, since TIWAC-3
has mostly a mesoporous structure, its isotherm resembles Type IV
isotherm. Type IV isotherm shows that an adsorbent has a structure
of a mixture of micro and mesopores. However, the initial part of
the isotherm follows the same path with Type II isotherm. There-
fore, this isotherm type refers to single layer–multilayer adsorption
on mesopore walls of the adsorbent.
DFT plus software pore size distribution graphs of the adsor-
bents are given in Fig. 3(d)–(f). In parallel with the data in Table 2,
it is apparent that mesoporous structure increasingly with increas-
ing amount of zinc chloride. Distributions of porous structures for
TIWAC-1, TIWAC-2, and TIWAC-3 are in the range of 1–2.5 nm,
1–5 nm and 1–10 nm, respectively.
3.1.4. FT-IR analysis
Adsorption capacity of AC is defined not only by its pore struc-
ture but also by the chemical nature of its surface. In AC structure,
many heteroatoms (oxygen, hydrogen, nitrogen and others) exist as
single atoms and/or in the form of functional groups. Oxygen is the
most dominant heteroatom in the carbon matrix. Carbon–oxygen
surface compounds are the most important centers having an effect
on surface reactions and surface behaviors of activated carbon.
Table 4
SBET surface areas, and iodine and MBa numbers for the adsorbents.
Adsorbent SBET (m2 g−1 ) I2 number (mg g−1 ) MB number (mg g−1 )
TIW 35.2 253.0 153.0
TIWC 118 119.2 27.8
TIWAC-1 706 496.4 31.9
TIWAC-2 1066 605.8 100.2
TIWAC-3 1141 630.2 260.4
a
Methylene blue.
Adsorption properties of AC can be controlled by modification of
surface groups [39].
FT-IR spectrum for TIW is shown in Fig. 4. TIW, which was not
subjected to heat treatment and hence, contains especially volatile
compounds, is the richest in terms of functional groups compared
to other adsorbents. Slightly broad peak appearing at 3396 cm−1
is due to moisture as well as hydroxyl ( OH) groups present in
the sample. Structures containing hydroxile are phenols, alcohols
and carboxylic structures. The peak at 1454 cm−1 arises from the
phenolic OH group existing in the structure. Since at high tempera-
tures phenolic structures are decomposed, the peaks in this region
disappear. Three peaks at 2918, 2852 and 1372 cm−1 are aliphatic
C H peaks. The peak appearing at 1734 cm−1 is C O stretching
peak arising from carbonyl groups. While the peak at 1051 cm−1
points out to C C bonds, the peaks appearing between 1051 and
1237 cm−1 show existence of S O peaks in the structure. Relatively
long peaks at 1646 and 1051 cm−1 are C C and C O stretching
peaks. The peak at 892 cm−1 also indicates C O H group [40–43].
IR spectra of other carbons obtained by carbonization at high
temperatures are very much simpler and the peaks existing due to
the amorphous structure of carbon cover off each other well, thus it
becomes difficult to interpret. The most significant peaks for TIWC
with an extremely plain spectrum are at 3407 and 1021 cm−1 , and
these indicate the existence of OH and C O groups, respectively
(Fig. 4). IR spectra of TIWAC-1, TIWAC-2 and TIWAC-3 ACs are very
similar to each other. The spectrum obtained for TIWAC-2 is shown
in Fig. 4. There are four significant peaks in this spectrum and the
peak at 3372 cm−1 indicates OH stretching vibration peak and
those at 2056 and 1543 cm−1 point to the existence of carboxylic
acid and/or lactone group. The peak appearing at 1075 cm−1 is C O
stretching peak in heterocyclic rings.
3.1.5. pH and pHpzc determinations
pHpzc , is the pH value at the point where net surface charge of
the adsorbent is 0. pHpzc values for five adsorbents vary in the range
of 4.90–6.45 and their pH values ranged from 4.11 to 5.32 (Table 3).
The pH values of the adsorbents generally fall in the slightly acidic
region and values of pHpzc <7 show dominancy of acidic groups over
basic groups [44]. It is also evident from Boehm titration that the
surfaces of adsorbents are rich in acidic groups (Section 3.1.6). Net
charge of the adsorbent under pHpzc is positive, while it is negative
above pHpzc . Therefore, knowledge of this value helps deciding at
which pH value one should work during adsorption studies.
3.1.6. Boehm titration
As seen in Table 3, increased amount of ZnCl2 for three ACs
caused removal of more volatile compounds from the structure,
and so the amount of total acidic groups decreased. As increasing
amount of ZnCl2 affected carboxylic and phenolic groups, it had no
effect on lactonic groups. On the contrary, an increase was observed
in lactonic group and this is in compliance with AC studies carried
out by activation with ZnCl2 in the literature [33].
Activating agent has effects on enhancement of surface area and
hence, on the pore development as well as arrangement of sur-
face functional groups. In comparison to TIW, higher surface area
 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259
Fig. 4. FT-IR spectra of the adsorbents: (a) TIW, (b) TIWC, and (c) TIWAC-2.
of TIWC obtained without using any activating agent is only the
result of high temperature during carbonization. However, it is
evident that ACs obtained by using activating agent in the same
carbonization medium as TIWC has bigger amounts of surface
groups.
3.1.7. MB and iodine numbers
I2 is a small molecule with a size of 0.56 nm. I2 number can
give an idea about the micropore structure and, MB number about
the mesopore structure [32]. Increasing surface area and surface
active groups cause a rise in iodine and MB adsorption. I2 and MB
numbers are given in Table 4. I2 number gives information about
microporous structure lower than 1 nm, rather than about total sur-
face area [42]. Table 4 also shows changes in MB and I2 numbers
with increasing surface area. It is apparent that increase in iodine
and MB adsorption occurs with increasing surface area.
Surface functional groups are also effective on iodine and MB
adsorption, besides to the surface area. For example, both iodine
and MB numbers of TIW were higher than those of TIWC, although
surface area of TIW was smaller than TIWC. Therefore, adsorption
ability of TIW compared to iodine and MB is largely a result of
functional groups on its surface. While TIWC can adsorb a certain
amount of iodine by its existing micropores, it is not capable of
adsorbing MB, which is a larger molecule. Moreover, due to being
the poor absorbent in terms of surface functional groups, especially
its MB number is very low.
3.1.8. Results of TG, DTG and DTA analyses
Changes in structures of adsorbents obtained by applying heat
treatment in the presence of O2 and N2 were examined on graphs
plotted as TG, DTG and DTA versus temperature.
In Fig. 5, TG and DTG graphs of TIW, the starting material for
production of ACs, in the presence of O2 and N2 can be seen. In
O2 medium, TG and DTG graphs essentially show three different
temperature zones: (i) 0–150 ◦ C, (ii) 150–460 ◦ C, (iii) 460–600 ◦ C.
In the first stage (T1 = 75 ◦ C), moisture in the sample is removed. In
the second stage, (T2 = 316 ◦ C) hemicellulosic and cellulosic struc-
tures are removed from the medium in the form of CO2 [35]. At
255
this stage, a mass loss of 52.6%, excluding moisture, takes place. In
the last stage, lignin, the hardest component of the structure and
the remaining carbon skeleton dissociate as inorganic mass in O2
medium (T3 = 590 ◦ C). At this stage, despite a mass loss of 38.5%, a
total mass loss of 91.1% took place until ash formation from sample,
excluding moisture.
In order to observe how carbonization process took place,
in TG and DTG curves of TIW in N2 medium (Fig. 5(b)), the
presence of a significant single peak can be seen in the range
150–390 ◦ C (T2 = 346 ◦ C), except the small peak arising from mois-
ture [23,45,46]. As expressed above, this peak is the dissociation
peak of cellulose along with hemicellulose. This temperature
range is also caused by partial decomposition of lignin [47].
The trend in the range of 390–580 ◦ C corresponds possibly to
dissociation of lignin. The remaining is carbon skeleton. In N2
medium, total mass loss, excluding moisture until this stage
is 73.0%. This value more or less corresponds to the result in
Section 3.1.1.
When DTA curves of TIW are examined, essentially two peaks
in O2 medium and a broad single peak in N2 medium can be seen
in Fig. 5(c) and (d). In O2 medium, at a low temperature of 360 ◦ C,
firstly volatile components dissociate into CO2 and H2 O, then at
509 ◦ C, the carbon skeleton decomposes.
TG and DTG graphs for products carbonized are seen in Fig. 6. In
DTG curves, a single peak can be seen, except for the peak arising
from moisture. In O2 medium, dissociation percentages of the car-
bon skeleton, excluding moisture, TIWAC-1, TIWAC-2 and TIWAC-3
are 82.6%, 85.0% and 90.6%, respectively. The temperatures corre-
sponding to these dissociations can be seen from DTA curves in
Fig. 7.
Endothermic peaks around 100 ◦ C in the graphs are a result
of evaporation of water. In the case of exothermic peaks, they
may provide clues about the components of the organic struc-
ture depending generally on the arrangement. Decisive exothermic
peaks in DTA graphs show effective nature of impregnation of acti-
vation agent [33]. When DTA graphs are considered, peaks are very
significant in TIWC, TIWAC-1, TIWAC-2 and TIWAC-3. When tem-
perature values are considered, TIWAC-2 has the highest value
256 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259

Fig. 5. TG and DTG graphs for TIW (a) in O2 medium, (b) in N2 medium, (c) DTA graph in O2 medium and (d) DTA graph in N2 medium.

Fig. 6. TG and DTG graphs for carbonized products.

 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259 257

Fig. 7. DTA graphs for carbonized products.

Table 5
Comparison with other studies in the literature.

Starting material Activating BET surface area Total pore volume Iodine number MB number Total surface acidic References
agent (m2 g−1 ) (cm3 g−1 ) (mg g−1 ) (mg g−1 ) groups (mmol g−1 )

Pine cone H3 PO4 1597 – – 370.37 2.56 [24]

Pine cone ZnCl2 1806 – – 370.37 0.89 [24]
Olive bagasse Steam 1106 0.6067 ∼500 – 1.897 [48]
Brown seaweed ZnCl2 802 0.517 1041 – – [49]
Red seaweed ZnCl2 783 0.481 962 – – [49]
Wood powder KOH 733 0.359 – 130.81 – [50]
Cotton stalk ZnCl2 794.84 0.63 972.92 193.50 – [51]
Coconut coir ZnCl2 205.27 0.0246 – 15.59 – [52]
Cattle manure compost ZnCl2 2114 1.244 – 519 1.138 [53]
Rubber-seed shell Steam 948 0.988 1326 265 – [35]
Carbon aerogels CO2 654.4 1.410 ∼800 ∼150 – [54]
Tectona grandis sawdust ZnCl2 585 0.442 1036 362 – [55]
Almond shell CO2 1310 0.621 ∼1100 ∼400 2.606 [56]
Lotus stalk Guanidine phosphate 1503 1.08 – – 1.81 [57]
Tea industry waste ZnCl2 706 0.369 496.4 31.9 3.14 This study
Tea industry waste ZnCl2 1066 0.580 605.8 100.2 2.71 This study
Tea industry waste ZnCl2 1141 0.806 630.2 260.4 2.50 This study

(640 ◦ C), showing it is an adsorbent with the highest structural
stability.
4. Conclusions
In this study, three different kinds of AC were produced from
tea industry wastes by using ZnCl2 and the resultant ACs were
characterized by several methods.
The results obtained from this study can be summarized briefly
as follows: although both starting material and activating agent
are the same, ACs with three different kinds of characteristics and
porous structure were produced. It was observed that the surface
areas of ACs produced increased compared to the TIW. A surface
area of 35.2 m2 g−1 of TIW, the starting material, was increased to
1141 m2 g−1 by ZnCl2 at 700 ◦ C (TIWAC-3). It was observed that
percentage of C increased as well as mesoporous structure was
enhanced with augmenting amount of activating agent (ZnCl2 ).
While an increase in I2 and MB numbers with increasing surface
area was observed, the lowest performance was seen in TIWC. As
a result of DTA analysis, it was understood that the most stable
258 A. Gundogdu et al. / Journal of Analytical and Applied Pyrolysis 104 (2013) 249–259
AC was TIWAC-2 due to its high decomposition temperature. SEM
photographs of all ACs and the starting material were taken and the
development of porous structure was observed.
The results obtained from this study were also compared with
other studies in the literature in terms of BET surface area, pore
volume, iodine–MB numbers and surface acidic functional groups.
From Table 5, our results were comparable to those presented by
other studies described in the literature. The ACs produced in this
study have relatively high surface areas, iodine–MB numbers and
also quite rich acidic groups when compared with other studies.
By this study, it was proved that owing to the high lignocellu-
losic content of this type of agricultural wastes, TIW can be used for
high performance AC production. These wastes are either disposed
in nature or utilized as fertilizers at best in Turkey. Disposition
in nature of these wastes, which cause storage difficulties, is the
likely brings various environmental problems. Utilizing this type of
wastes in AC production may eliminate this burden. Besides, ensur-
ing that TIW, which has no economic value, is regained to economy
by its usage in AC production and helping resolution of an environ-
mental problem, especially using it as an adsorbent for waste water
treatments make this study extremely meaningful.
Acknowledgements
We would like to thank Central Laboratory of Middle East
Technical University, Ankara, Turkey for surface characterization
analyses of the adsorbents and TUBITAK Marmara Research Cen-
ter, Kocaeli, Turkey for SEM analyses. Our special thanks go to Dr.
Yaprak Uygur for his contributions.
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