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Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from

Anaerobically Digested Sewage Sludge

Conference Paper · April 2014

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 1042

Adsorption of Remazol Brilliant Blue R on

Adsorbents Obtained from Anaerobically
Digested Sewage Sludge
Didem Özçimen1, Tufan Salan2

Abstract
Because of its carbonaceous nature and organic materials, sewage sludge could be converted into the
porous adsorbents under controlled conditions using different processes and some chemical additives.In
this study, porous adsorbents were produced from sewage sludge via both chemical activation with
ZnCI2 and non-chemical activation in a split tubularfurnace. For both production processes, carbonization
experiments were carried out in optimum conditions of 20˚C/min heating rate, 550˚C reaction
temperature with 400 ml/min N2 flow rate for 1 hour residence time. Solid product yields were %70,25
and %71,25 for the chemical activation and only carbonization processes, respectively. Adsorbents
produced from carbonization processes were analyzed by SEM, BET, FTIR equipments and also thermal
characteristic of raw material was analyzed with a TGA equipment. The utility of adsorbents were
evaluated as activated carbon, and it is concluded that adsorbents have similar characteristic to activated
carbon.RemazolBrilliant Blue R (RBBR) dye adsorption experiments were performed for its different
concentrations.The maximum adsorption capacities of CSWS (carbonized sewage sludge) and ASWS
(activated sewage sludge) were 0.788 and 1.913 mg/g for 100 ppm RBBR dye concentration. The
concentrations of RBBR in the solution before and after the adsorption experiments were determined via
a UV-Vis spectrometer.Freundlich and Langmuir isotherms were used to analyze the equilibrium data.
Results indicated that dye removal efficiency of chemically activated adsorbent is better than that of
adsorbents produced via only carbonization process. As a result, this study demonstrated that sewage
sludge which is produced during waste water treatment process as secondary waste can be reused for the
treatment of waste water itself in an eco-friendly recycle.
Keywords: Remazol Brilliant Blue R, sewage sludge, carbonization, activated carbon, adsorption

1. INTRODUCTION
The synthetic dyes are broadly used in many industries mainly in the textile and other application areas such
as leather tanning, paper production, photography, rubber, plastics, cosmetics, pharmaceutical and food
industries [1], [2]. Dyes can be classified according to their structural compositions that divide cationic,
nonionic or anionic type. And anionic dyes are categorized as direct, acid and reactive dyes [3].

The structural diversity of synthetic dyes are originated from different azo-based chromophoric groups such
as azo, anthraquinone, triarylmethane and phthalocyanine; chromophores joined with diverse kind of reactive
groups such as vinyl sulfone, chlorotriazine, trichloropyrimidine, difluorochloro pyrimidine and different
applications such as reactive, direct, disperse and vat dyeing [4], [5]. Among these groups, reactive dyes are
the most common dyes used to dye cellulosic fibers in the textile industry. They are colored chemicals and

1
Correspondingauthor: Yıldız Technical University, Faculty of Chemical and Metallurgical Engineering, Department of
Bioengineering, Davutpasa Campus, 34220, Davutpaşa, Istanbul. ozcimen@yildiz.edu.tr
2
KahramanmarasSutcu Imam University, Department of Bioengineering and Sciences, Avsar Campus, 46100,
Kahramanmaraş. tufansalan@gmail.com
 1043

EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye
generally characterized by nitrogen to nitrogen double bonds (azo bonds). These azo bonds along with the
chromophores bring about colorful structure of azo dyes [6].

Almost 45% of textile dyes produced all over the world concerns the reactive group. Reactive dyes generally
used for cotton and other cellulosicshave very affirmative properties such as bright color, superior water-
fastness to the applied fabric, high photolytic stability, high solubility and resistance to microbial attack,
simple usage techniques and low energy consumption for textile applications [7], [8]. These dyes show a
broad range of different chemical structures, mainly based on substituted aromatic and heterocyclic groups
[9]. Chromophore and functional group bind the reactive dyes to the fibers. The functional groups also bind to
water and cause hydrolysis [10].

Dyes frequently cause pollution problems such as colored wastewater and drain into water environment due
to their large use. Because of their resistance disposition to conventional waste water treatment processes,
brightly colored and water soluble reactive and acid dyes are the most problematic ones [11].Pollution
problems of synthetic dyes arise due to their extensively use because of their easily usage, cheap synthesis
costs, stability and variety of color compared with natural dye. During the dye production and dye application
processes, up to 15% of the used materials are discharged into the wastewater stream therefore the residual
process waters from these industries are highly colored [12]. Furthermore synthetic dyes are not easily
biodegradable, therefore, even after broad treatment applications colors can still stay in the wastewater
stream. On the other hand, extensive use of azo-based dyes and their reaction outcomes such as aromatic
amines are an extremely cancer-causing agent. The release of dye processing wastewaters into natural water
environments streams threatens to aquatic life and mankind indirectly due to their high chemical oxygen
demands (CODs)/biological oxygen demands (BODs), toxic, allergic dermatitis, skin irritation, mutagenic
and carcinogenic features [9], [13]- [16].

Because of above mentioned problems, removal of dye color from industrial effluents has become more
important in recent years. However, due to high solubility, low biodegradability and chemical stability of
reactive dyes and their large amounts in the wastewater stream than other dye classes primarily in their spent,
hydrolyzed form, conventional treatment applications are usually cannot remove completely color of dyestuff
from effluent [6], [18]. Thus, scientists investigate many physical and chemical effective treatment methods
including adsorption, chemical coagulation, precipitation, ultra-filtration, electro-dialysis, ionizing radiation
and oxidation by ozone have been used for the treatment of dye-containing effluents [12].And alternatively,
biological materials such as algae, fungi, bacteria and yeast have been used for the dye removal as a
wastewater treatment method [19]. Among these methods adsorption process has been found to be excellent
compared to other techniques due to its easy design and operation and high yield. Adsorption is an effective
treatment procedure and it can be used widely to remove various contaminants such as coloring dye stuffs
from wastewater streams [20]-[22].

So far, many scientists have used different adsorbents particularly activated carbon to remove the reactive
dyes from wastewater environments. Activated carbon (AC) is one of the most efficient and important
adsorbents, which has been investigated with superb achievement for the treatment of wastewaters on not
only laboratory scales but also industrial applications [6]. The AC has significant properties like high internal
surface area, greatly advanced internal pore structure and the availability of abroad range surface functional
groups. These features make AC one of the most popular adsorbents [9], [23].

However, despite these superb features use of the commercial activated carbons are sometimes restricted due
to their quite expensive starting raw material and therefore higher application cost. Furthermore, following its
a few applications an activated carbon system become saturated and after this it couldn't adsorb any more
dyes from wastewater. When AC is saturated, a regeneration step is required for further application to purify
waste water effluent. Up to now, several techniques such as most commonly chemical [24], electrochemical
[25], oxidation [26], thermal [27] are used to regenerate saturated AC. But, regeneration of activated carbon
brings some problems along such as additional operation cost, decrease of carbon content and loss of
adsorption capacity in comparison with the parent activated carbon. Thus, in recent years many scientists
have been attempted to produce low-cost alternative carbon-based adsorbents from a range of wastes like
industrial or agricultural by-products which may substitute commercial activated carbons in wastewater
treatment via adsorption methods [28], [29].

Evaluation of wastes for the production of low-cost adsorbent can balance increasing waste disposal costs of
waste producers against the cost of activated carbon manufacturing; on the other hand, this kind of approach
recovers non-renewable natural resources and allows obtaining value-added products which may be used in
pollution control [30]. Agricultural wastes and industrial by-products are considered being a very important
feedstock for the activated carbon preparation, since they are renewable sources and low-cost alternative
materials. The agricultural feedstock such as banana peel [31], rice husk [32], bagasse [33], corncob [34],
 1044

Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan
loofah plant [35], nutshells [36], peanut hull [37], silk cotton hull [37], barley husk [38],wheat straw [39],
barley straw [40], coir pith [41], fruit stones [42], bamboo [43], date pits [44], wood sawdust [45], chestnut
shell [46],grape seed [47], straw [48], pine fruit shell [49], cassava peel [50], orange peel [51], olive stones
[52]and industrial by-products such as waste newspaper [53], solid wastes like waste tires, PET bottles [54],
blast furnace slag [55], scrap tire rubbers [56] and sewage sludge [57] have been used to produce adsorbents
for the adsorption of various pollutants. So far, several studies have been done to remove RBBR with above
mentioned alternative adsorbents. Related works about treatment of the RBBR with low-cost adsorbents and
other alternative adsorption techniques are summarized at the Table 1.

Table 1.Comparison of adsorption capacity of various adsorbents for RBBR

Adsorbent Adsorption pH Ref.

Capacity
(mg/g or %)
ImmobilizedScenedesmusquadricauda 48.3 mg/g 2 [1]
Peanut hull based activated carbon 149.25 mg/g - [58]
ZnO fine powder 345 mg/g 4 [16]
Sawdust based activated carbon 368.5 mg/g 10.7 [6]
MgO nanoparticles 166.7 mg/g 8 [59]
Polyaniline/bacterial extracellular 361.82 mg/g 3 [60]
polysaccharides composite
Jatrophacurcaspods based activated carbon 95%; 50 mg/L-25mL dye : 0.2 g 3 [10]
A.C.
Mangosteen peel based activated carbon 80.35% ; 100 mg/L-200mL dye : natural [61]
0.3 g A.C.
Rambutan peel based activated carbon 78.38% ; 100mg/L-200 mL : 0.3 - [22]
g A.C.
Pine cone based activated carbon >98%; different initial dye [62]
concentration/0.1 g A.C. 2 and 11
Polyurethane-Type Foam 5 mg/g 3 [63]
Prepared from Peanut Shell

Sewage sludge is the waste material produced as a result of urban and industrial wastewater treatment plants
processes. Nowadays, its production was increased rapidly and will rise as more municipal wastewater is
treated due to environmental necessity and legal requirements to reach better standards for wastewater
treatment along with the urbanization and industrial development [64], [65]. It is a very complex material
consisted of biological, organic and inorganic components and water. Undigested organic components are a
mixture of proteins and peptides, lipids, polysaccharides, plant macromolecules and aliphatic structures [66].

Average production of sewage sludge is around 40–60 g dry matter per resident per day for both urban
sewage plants and industrial sewage plants and its generation is expected to reach higher amounts. The
suitable progress in the environmental impact of water resources is probably to be responded by a clear rise in
sewage sludge volumes generated. For the present and estimated situations, when considering the high
production amounts, an appropriate handling of sewage sludge is a crucial necessary [67], [68]. Particularly,
in the EU more than 10 million tons (dry solids) of sewage sludge are produced annually. Germany which
generates 2 million tons per year (dry solid) located at the top on the sludge production, it is followed by the
UK, France, Italy and Spain produce over 1 million tons respectively [69]. On the other hand, for Turkey
there is no precise data available about total sewage sludge generation, but according to most recent press
release of TUIK (Turkish Statistical Institute), in the year of 2010,39640 tons of hazardous wastes brought to
incineration plants,was consisted of 779 tons of industrialsewage sludge and 741 tons of sludge and leachate
resulted from waste processing and disposal. And 56241 tons hazardous waste disposed/recycled in landfill
sites was consisted of 586 tons of sludge and leachate resulted from waste processing and disposal and 181
tons of industrial sewage sludge. And finally, 14320433 tons of non-hazardous waste brought to landfill sites
was consisted of 52992 tons of industrial wastewater treatment sludge, 724 tons sludge and leachate resulted
from waste processing and disposal, 182069 tones domestic waste water treatment sludge and 1848 tons
drinking water treatment sludge [70].Furthermore in the year of 2012, in Istanbul which is the largest
metropolitan of Turkey, where the over 13 million inhabitant that is about one over six of entire population of
country lives, waste water treatment plants produced over 40000 tons (dry solids) of sewage sludge. It is
expected that this amount will be 140000 tons/year by the year of 2020 [71].

An adequate management of sewage sludge is a fundamental step of waste water treatment applications as
mentioned above. Because, sewage sludge is it is mostly composed of unwanted pollutants heavy metals such
as Zn, Pb which are range of 1-1000 ppm, Polycyclic Aromatic Hydrocarbons (PAHs), Polychlorinated
 1045

EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye
Biphenyls (PCBs), dioxins, pesticides, linear alkyl sulfonates, phenols, pathogens like spores of
Cryptosporidium, Giardia and viruses which are considered to be extremely dangerous to environment and all
living organisms. If the sewage sludge is not disposed in a sustainable manner, serious pollution problems can
occur [72]-[74].

Sewage sludge disposal is a primary problem associated with these negative features. Considering that sludge
reduction is restricted due to sustainability of waste water treatment according to strict regulations; it would
be desirable to develop new ways for the valorization of this “waste of the waste” so sewage sludge would
turn into a useful feedstock [75], [76]. Until now, different handling methods have been developed for sewage
sludge which can be categorized in two main strategies: traditional disposal or reuse and energy applications.
Traditional disposal methods include agricultural applications such as fertilizer, composting placing landfill
sites, sea dumping and disposal on land by placing it in a surface disposal site [72], [77].

Because of problematic nature of sewage sludge countries have been developed regulations to protect the
public health and the environment when sewage sludge is disposed by these methods. Especially spreading
the sludge on land is an inexpensive solution, but, it has some limitations due to limited suitable areas and
unfavorable impacts to environment such as contamination of watercourses and groundwater resources [78].
Strict regulations set for environmental protection forbid sea dumping in due to protect the marine
environment and landfill due to limited landfill space, rising costs of lands, leachate and uncontrolled landfill
gases such as methane. And except the agricultural applications other methods aren’t permitted any more in
the EU. Without proper treatment and disposal, these methods may cause serious secondary pollution
problems in the environment [74], [79], [80]. For these reasons agricultural applications has become the most
attractive investigation area particularly as soil conditioner compost or organic fertilizer [81], [82].

The sewage sludge includes important nutrients essential to plant growth such as nitrogen, phosphorus
addition some valuable trace elements such as copper and selenium [83]. This practice is a very simple and
ecological alternative; however, itis not always possible due to the sludge quality, appropriateland presence,
and the difficultiescome across for its application, management and tracking [64], [68], [67], [75]. Moreover
odor, water pollution and heavy metals are the most important drawbacks for the agricultural usage [84].
Adequate concentrations of some trace elements present in sewage sludge applied to land, are potentially
phyto-toxic and zoo-toxic [85].

Because of all above mentioned problems of the traditional ways for sludge disposal, it is necessary to
investigate possible innovative, eco-friendly and effective routes to make sewage sludge more valuable raw
material [86]. Thus, sewage sludge can be used as a renewable feedstock to produce energy via anaerobic
digestion, combustion, gasification, pyrolysis/carbonization and novel technologies such as wet oxidation and
super critical water oxidation. Sewage sludge is a type of biomass and its calorific value is almost equal to
coal range of 9-29 MJ/Kg of dried solid [87]-[91].The main target of these methods is exposing of the stored
energy in sludge together with reducing environmental impacts and amount of sludge lowest level, so that
fulfill the increasingly stringent regulations and standards [77]. Except the anaerobic digestion thermal
methods include clearing of the organic content of the sewage sludge and as a by-product only the ash
component or char remains for final disposal. However there are some significant problems about thermal
processes such as need a lot of energy to reach high temperatures, high installation costs and broad air
pollution equipment necessary [92].

Especially, combustion processes causes emissions into the air like greenhouse gases, particulate matter, acid
gases, heavy metals and dioxins and furans such as volatile organic compounds (NO x, N2O, SO2, HCl, HF,
and CxHy) which are extremely dangerous to public health. From this aspect of view, sewage sludge
combustion must be controlled in a very good sustainable way [93].

Anaerobic digestion, one of the oldest methods for sludge stabilization processes which is very advantageous
compared to other ones.Biogas production is the one of the these advantages, because after purification of
impurities such as H2S, CO2 and water it can be used in combined heat and power (CHP) systems or to
supply energy to many process facilities of waste water treatment plant.Furthermore anaerobic digestion
reduces the solids content ofsludge to 25-50%, this decreases costs of its transport for disposal, eliminate
pathogens and as by-product generates a voluble fermented waste. This fermented solid waste can be used as
raw material for all of the above mentioned disposal and energy routes [94], [95].

On the other hand, pyrolysis is the thermal destruction of biomass in the absence of oxygen or airunder inert
atmosphere producing solid char, non-condensable gases and a liquid called bio-oil rich in oxygenated
compounds. Depending on the process conditions, the proportion of these fractions varies significantly [96].
So far, numerous studies have been done about the pyrolysis of sewage sludge with different purposes like
thermogravimetric studies dealing reaction kinetics and composition of the non-condensable gases obtained,
 1046

Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan
analytical investigations aimed on the characterization of the sewage sludge composition, and adsorbent, syn-
gas and liquid bio-oil production [97].Furthermore several commercial technologies have been developed for
pyrolysis of sewage sludge. For example EnerSludgeTMTechnology of Australia Environmental Clean
Technologies (ESI) Company and SlurryCarbTM Process of United States EnerTech Environmental Company
deal with only sewage sludge pyrolysis. Apart from this, particularly in France, Germany and Japan there are
the major technologies. In Germany Schwel–Brenn Process of Siemens AG Company, Recycled Clean
Products (RCP) Process of Von Roll Company includes sewage sludge pyrolysis and combustion process
together, Noell Conversion Process and Thermoselect Process includes a combination of pyrolysis and
gasification processes.

According to basic parameters of the pyrolysis process broadly classified as slow pyrolysis and fast pyrolysis.
Slow pyrolysis is a conventional method in which biomass is heated slowly to a final temperature. This
process is used primarily for char/charcoal (conventional) or activated carbon (carbonization) production
[98]. Because of carbonaceous structure and plenty organic compositions and volatile components, sewage
sludge is reasonably suitable for the production of porous adsorbents. It can be used as a raw material to
manufacture activated carbon via carbonization process under controlled treatment conditions with chemical
activation, physical activation such as steam or combination of both of these activation methods [72], [99],
[100]. This strategy would not only solve sewage sludge pollution and disposal problems but also offer the
possibility of producing a useful material which could be used for advanced treatment wastewater that caused
the sewage sludge generation. Thus, an alternative way essentially incorporates the disposal and recycling
applications of this waste is developed [80].

Carbonization is an innovative option allows utilization of sewage sludge in the production of a valuable
material. Activated carbon production from sewage sludge would mean both a considerable saving in starting
material costs, reducing sludge volume generated in wastewater treatment plants and a way of making use of
a waste material economically valuable [64], [75], [86]. In a waste water treatment plant dealing with sludge
represents an important percentage of total operating costs. Handling, treatment and disposal of sewage
sludge account for 25–65% of the total process expense. But, use of sewage sludge in the form of activated
carbon for treatment of waste water the plant itself would reduce costs [68], [75], [99].

Until now, sewage sludge has been demonstrated as a great in-expensive and easy accessible feedstock
candidate by many scientists for the production of activated carbon [101]. Many of these studies have been
concerned performance of adsorbent about their aqueous adsorption of organic phenol and phenolic
compounds, heavy metals, gaseous and dyes [102]-[104]. There have been many studies to uptake of dyes by
sewage sludge based adsorbents. Methylene blue is a commonly used adsorbate for assessing the dye uptake
of adsorbents. Table 2 summarizes the important points of the related works.
 Table 2. Various dye uptake data of sewage sludge based adsorbents.

Carbonization/Activation Conditions Maximum Adsorption

Dye pHsol. capacity (mg/g or %) Ref.
Sludge type Temperature (˚C) Time (h) Reagent

- - - Meth B N/A 95.9 (1000mg/L-0.1L sol.: 1g AC)

AD U WWTP [105]
Meth B N/A 20 (1000mg/L-0.1L sol.:1g AC)
625 0.5 H2SO4
Dr AD M WWTP - - - R Blue ED 0.5 117.1 (Langm) [106]

DrWRP 700 2 - Meth B 3-12 %95 (10 µmol/L) [107]

Vat B4 9.2 248.3 (Langm) [108]

Dh U WWTP - - - Direct R79 6.4 19.6 (Langm)

1047

Indigo 12.3 8.1 (Langm)

Dh IWWTP 600 N/A - 1,2,4-Acid 5 95.1 (Langm) [80]
%95 (100 mg/L-50 mL : 0.25%wt AC) [100]
AD U WWTP 500 3 - Alka B 1

Dh U WWTP - - - Vat Red 10 11.7 77.65 [76]

(Langm)
Vat Org 11 12.1 59.55 (Langm)
Dh M WWTP 450 0.5 ZnCl2 R B R X-3B N/A 144.9 (Langm) [109]
H2SO4
A.Yel 49 5.98 71.43 (Langm)
M WWTP 750 0.5 - B.Blue 41 5.45 416.67 (Langm)
R. Red 149 5.36 18.93 (Langm) [74]
A.Yel 49 5.98 116.28 (Langm)
B.Blue 41 5.45 588.24 (Langm)
 Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan

750 0.5 CO2 R. Red 149 5.36 25.06 (Langm)

PM WWTP 300 1 Steam Meth B Nat. 103.58 (100 mg/L sol: 0.5 g AC) [110]
850 ˚C
0.66 h RR24 15.68 (50 mg/L sol: 0.5 g AC)

AD U WWTP B. Red 46 188 (Langm) [30]

700 0.5 H2SO4 A. Brow. 283 Nat. 20.5 (Langm)
D. Red 89 49.2 (Langm)
D. Bla. 168 28.9 (Langm)
- - - 106.628 (1500mg/L-0.1L sol.: 1g AC)

AD U WWTP Meth B 31.604 (1500mg/L-0.1L sol.: 1g AC)

625 0.5 -

24.093 (1500mg/L-0.1L sol.: 1g AC)

625 0.5 H2SO4 N/A
1048

74.403 (1500mg/L-0.1L sol.: 1g AC) [67]

- - -
28.364 (1500mg/L-0.1L sol.: 1g AC)
PCT AI WWTP 550 0.5 - Meth B

22.935 (1500mg/L-0.1L sol.: 1g AC)

550 0.5 H2SO4

AD U WWTP 625 0.5 H2SO4 Meth B 5 194.3(Langm) [75]

Saphr 9.22 250.2(Langm)
AD U WWTP - - - Indi Carm 30.82 (Langm) [68]
CrystVio 184.68 (Langm)
625 0.5 H2SO4 Indi Carm 60.04 (Langm)
CrystVio 270.88 (Langm)
N/A
Dh WWTP 550 1 ZnCl2 DD Brow M 502 (Langm) [111]
EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye

AM Brow Rh 329.7 (Langm)

3
600 1 - Acid R18 8 58
780 65 min. Steam (30 mg/L-1L sol: 0.5 g AC) [86]
VLS M WWTP 600 1 - B Vio4 8 81
780 65 min. Steam (50 mg/L-1L sol: 0.5 g AC)
WWTP 600 1 KOH A B S GR 6.4 %99.7 (300 mg / L: 20g AC) [112]
50 wt% IOS 950 0.5 - Acid R1 10.7 72.8 (Langm–Freun)
50wt% WWTP Bas Fuc 68.4 (Langm–Freun) [113]
650 0.5 - Acid R1 10.7 126.9 (Langm–Freun)
Bas Fuc 105.9 (Langm–Freun)

Abbreviations: AD: Anaerobically Digested, U: Urban, M: Municipal, WWTP: Waste Water Treatment Plant, N/A: Data Not Available in the Paper, Meth B: Methylene Blue, Vat B4:
Vat Blue 4, Direct R79: Direct Red 79, Langm: Adsorption value calculated from Langmuir equation adsorption isotherm, Dh: Dehydrated, Alka B: Alkalin Black, AC: Activated
Carbon, A.Yel 49: Acid Yellow 49, B.Blue 41: Basic Bleu 41, R. Red 149: Reactive Red 149,sol.: Solution, Nat.: Natural, B. Red 46: Basic Red 46, A. Brow. 283: Acid Brown 283, D.Red
89: Direct Red 89, D. Bla. 168: Direct Black 168,PCT: Treated by Physico-Chemical Process, AI : Agrofood Industrial, Indi Carm: Indigo Carmine, CrystVio:Crystal Violet, Acid R18:
Acid Red 18, B Vio4: Basic Violet 4, IOS: Industrial oil sludge,Acid R1: Acid Red1, Bas Fuc: Basic Fuchsin, Langm–Freun: Uptake calculated from the adsorption isotherm with the
Langmuir–Freundlich equation, Dr: Dried, B Blue ED: Burazol Blue ED, WRP: Water Reclamation Plant, IWWTP: Industrial Waste Water Treatment Plant,1,2,4-Acid: 1-diazo-2-
1049

naphthol-4-sulfonic acid, Vat Org 11: Vat Orange 11,R B R X-3B: Reactive Brilliant Red X-3B, RR24: Reactive Red 24, PM: Paper Mill, Saphr:Saphranine, A B S GR: Acid Brilliant
Scarlet GR, DD Brow M: Direct Dark Brown M, AM Brow Rh: Acid Mordant Brown R
 1050

The usage of a waste material generated from one industrial activity for treatment the wastewater of another
one or itself, is eco-friendly and attractive especially if the used material is cost free [76].For this reason this
paper deals with feasible utilization of sewage sludge for the production of low-cost adsorbents that can be
used for the adsorption of dyeing pollutants present in wastewater. Although several studies have been
reported in the literature on the RBBR adsorption by activated carbons produced from different feedstock,
any study on the adsorption of RBBR by activated carbons produced from sewage sludge does not exist. The
goal of this study was to investigate the RBBR removal efficiencies of an economical and eco-friendly
activated carbon produced from sewage sludge by the chemical activation method. The adsorption of RBBR
dye onto activated carbons was studied in batch equilibrium conditions. Freundlich and Langmuir isotherms
were used to analyze the equilibrium data.

2. EXPERIMENTAL

2.1. Materials
The sewage sludge samples used in this work obtained from Atakoy Advanced Biological Wastewater
Treatment Plant which is an urban treatment plant located in Istanbul, Turkey.The sludge was anaerobically
stabilized via biogas production processfollowing activated sludge biological treatment and it was dewatered
by centrifugation and dried by the rotary disc driers at the plant with an average dry solid content of 90%.As a
chemical activation reagent ZnCl2 (Merck) was used in the activated carbon production experiments. For the
adsorption studies a stock solution of Remazol Brilliant Blue R (Sigma-Aldrich) anthraquinone-baseddyewas
used.Remazol Brilliant Blue R dye (RBBR) is one of the most important reactive dyes in the textile industry.
RBBR is an anthracene derivative and represents an important class of toxic and recalcitrant organo-
pollutants. The general characteristics of RBBR are summarized below in Table 3. Remazol Brilliant Blue R
(RBBR) is frequently used as a starting material in the production of polymeric dyes [10], [17].

Table 3. General characteristics of Remazol Brilliant Blue R

Molecular
Formula and Color λmax Molecular Structure
Molecular Class Index (nm)
Weight Number

C22H16N2O11S3 Anthraquinone 61200 592

626.54

2.2. Preparation of the adsorbents

Before the carbonization and activation experiments, raw powder sewage sludge was dried at 105 °C in an
oven for 24 h. It wasn't ground and sieved due to its uniform particle size distribution. For the determination
of thermal properties of sewage sludge, thermogravimetric analysis (TGA) was used. Thermal analysis of
sewage sludge was conducted at a heating rate of 10 °C/min from 25 °C to 750 °C 100 mL/min N 2
atmosphere, using Shimadzu TGA-50 equipment.For the production of adsorbents two different methods
were used. In the first method, dried sewage sludge samples were physically impregnated with
ZnCl2employing a mass ratio of ZnCl2 to raw material of 1:1 andthen, they were activatedin a quartz pipe
inserted in a horizontal split tubular furnace (Protherm ASP)in nitrogen atmosphere with a 400 ml/min flow
rate. The heating rate of the furnace was 20 °C/min and the reaction carried out at a final temperature of 550
°C for 1 h. The adsorbents produced via this method are referred to asASWS (activated sewage sludge). On
the other hand in the second method, dried sewage sludge was only carbonized without activation agent at the
same reaction conditions. And the adsorbents produced via this method are referred to as CSWS (carbonized
sewage sludge).After completion of experiments, these carbonized materialswere used as activated carbons
after washing several times withdilutedHCl solution and hot distilled water and drying at 105 °C for24 h.

2.3. Characterization of the adsorbents

Characterization of the adsorbents thereby produced was performed via various analysis techniques. Thus, the
some physical properties of the activated carbons, porosity, surface area and functional groups were
determined. The SEM micrographs of the activated carbons were compared using Jeol JSM 5410 LVmodel
scanning electron microscope equipment.Fourier-transforminfrared(FT-IR) spectroscopic analysis of theboth
of the raw material and activated carbons was performed using Agilent Cary 630 model ATR (Attenuated
total reflectance)/FTIRinstrument with Spectra were recorded between 4000 and 650 cm-1 wave number
 1051

EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye
region for all samples.TheBrunauer–Emmett–Teller (BET) surface analysis of both of the sewage sludge and
activated carbons determined using Micromeritics TriStar II 320 equipment after degassing process of
samples which is carried out at 110 °C for 1 hour.

2.4. Adsorption experiments

For the adsorption experiments,1000 ppm stock dye solution was preparedby dissolving Remazol Brilliant
Blue Rin distilled water.Then this stock solution was diluted to obtain the working standard concentrations of
20, 40, 60, 80 and 100 ppm. The pH values of the standard solutions were adjusted to a fixed value of 3in all
cases employing HCl/NaOH solutions.At the first stage an initial kinetic experiment was conducted in which
the optimum adsorption time (equilibrium time) for the adsorbents wasdetermined using dye solution which
had concentration of 100 ppm. This experiment was carried out for 120 minutes and amount of the adsorbed
dyestuff at 5th, 15th, 30th, 60th, 90th, 120th minutes of adsorption process determined via Scinco S-3100 model
UV-Vis equipment at 593 nm which is maximum absorbance value of RBBR. This optimum time was
subsequently employed in studies of other dye concentrations for both adsorbents (ASWS and CSWS). In
batch adsorption experiments 40 mg adsorbent was thoroughly mixed with the 5 ml aqueous solutions having
these dye concentrations in sealed conical centrifuge tubes placed in a tube rack. This rack was placed in a
thermo stated water bath shaker at a rolling speed of 200 rpm at a constant temperature of 25°C for 60
minutes of optimum time. At the end of the equilibrium period, the supernatant part of the tubes was
subsequently analyzed for residual concentration of RBBR via UV/Vis spectrophotometer and the adsorption
capacity of adsorbents was calculated. The RBBR amount remained after the adsorption process determined
from a calibration curve obtained according to concentration-absorbance chart of parent standard solutions.
And finallythe amount of dyestuffabsorbedbyper unit weight of the adsorbents (ASWS and CSWS) was
calculated following equation:
Q = (C0 – Ce ).V/W (mg/g) (1)
whereC0 and Ce(milligrams per liter), are the amount of initial and remainingRBBRin the solution at time of
equilibrium respectively,V is the volume of the solution, and W is the weight ofadsorbent (grams).

Attempts were made to fit these kinetic data employing the pseudo-first-order [117] and pseudo-second-order
[118] models, as expressed by equations and, respectively:
Pseudo-first-order equation:ln (Qe-Qt) = ln Qe – (k1.t) (2)
Pseudo-second-order equation:t/Qt = (1/k2 .Qe2) + t/Qe (3)
where Qe and Qt are the amounts (mg/g) of metal ions adsorbed onto the activated carbon at equilibrium and
at time t, respectively, while k1 and k2 are the kinetic rate constants for the pseudo-first-order (1/min) and the
pseudo-second-order [g/(mg min)] adsorption processes, respectively.

After determination of Q values for all solutions, in order to develop the quantitative data further, the
experimental data obtained for the equilibrium adsorption of RBBR onto the adsorbents were analyzed
employing the Langmuir [114] and Freundlich[115] isotherm equations given below:
Freundlich isotherm equation:logQe = log KF + (1/n) log Ce (4)
Langmuir isotherm equation: 1/Qe= (1/Qmaxb).(1/Ce) + 1/Qmax (5)
whereQe (mg/g) and Ce (mg/L) are the equilibrium concentrations of RBBR dye in the solid andliquid phases,
respectively, while KF [(mg/g)/(mg/L)1/n] and n are the Freundlich constants relatedto the adsorption capacity
and intensity, respectively. Similarly, Qmax (mg/g) and b (L/g) are the Langmuir constants related to the
adsorption capacity.

3. RESULTS AND DISCUSSION

The result of thermal analysis (TGA) of raw sewage sludge without ZnCl2activation is shown in Figure 1. As
can be seen from the Figure 1, weight loss of sludge was separated into three discrete between 25°C and 750
°C temperature range. The first step occurs at 25-200 °C with a weight loss of 3.33% which was caused by
the evaporation of adsorbed and bound moisture content in the structure of sludge. In the second steps
between 200 and 600 °C a weight loss of 23.2% occurred. This important weight loss can be explained due to
decompositionvolatile organic constituent that forms a significant part of sewage sludge. Finally, at the third
step over 600 °C a weight loss of 8.5% was observed. This can be associated with thermal decomposition of
inorganic compound such as ash which is another important content in the structure of sewage sludge.
 1052

Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan

Figure 1 TGA curve of the raw sewage sludge

The Fig. 2 illustrated the FT-IR spectrum of sewage sludge (SWS), carbonized sewage sludge (CSWS) and
activated sewage sludge (ASWS). As seen from the figure SWS and CSWS had very close infrared spectra
with the exception of a few peaks at around 2900 cm-1, 1500 cm-1 and, between 650 and 800 cm-1
wavenumber due to thermal destruction of some chemical functional groups. But for the ASWS some peaks
and bands were differ significantly due to both chemical and thermal decomposition of sewage sludge
samples during activation process. It can be seen from the Figure 2 for all samples broad band between 3100
and 3600 cm-1 is associated with O-H stretching groups which are hydroxyl containing compounds such as
water and alcohol. Moreover it can be due to N-H stretching vibrations of amine and amide containing
compounds. In FTIR spectra of SWS the most characteristic bands at 2851 cm-1 and 2922 cm-1 are due to
stretching vibrations of aliphatic C-H bonds. These bonds can be ascribed to methylene groups and lipid
content of SWS. These bands were disappeared for sewage sludge based adsorbents after thermal (CSWS)
and chemically activated (ASWS) thermal treatment. The weak broad peaks of 2106 cm-1 and 1995 cm-1 may
correspond to C≡C and C=C=C stretch, respectively.For SWS,medium broad band at 1633 cm-1 could be
related to C=O (Amide I band) stretching vibration of carbonyl groups owing to carboxylic acids and its
derivatives or C=C stretching due to alkenes content of SWS. It is very obvious form the Figure 2 for CSWS
and ASWS, this band quite shifted toward a lower wavenumber of 1620 cm-1 and 1584 cm-1, respectively.
This might be caused some changes in the functional groups due to thermal and chemical interactions during
adsorbent production processes.The week absorption peak at 1520 cm-1shows the presence of protein content
(Amide II band) of SWS like Amide I band. In the Figure 2 it can be seen clearly this N-H bending derived
band disappeared at spectra of CSWS and ASWS. At 1422 cm-1, medium broad band probably caused by C-H
and carboxyl O-H vibrations because of amine and hydroxyl compounds. This band completely was disposed
after ZnCl2 activation of SWS. In the fingerprint region, the strong narrow bands between 1000 cm-1and 1100
cm-1 could indicate two different chemical groups. One of them is C-O stretching vibrations of alcohols and
phenol compounds, the other one is Si-O-C or Si-O-Si stretching vibrations which are incorporated with
silicon components in sewage sludge and adsorbents. As a result of plenty organic and inorganic content
ofsewage sludge, FTIR spectra of raw material and adsorbentsdemonstrate presence of different functional
groups such as aliphatic, carboxylic, aromatic, silicon and phosphorous which are based on various
components of bacterial residues, carbohydrates, proteins, lipids and ashes.

Figure 2 FT-IR spectra of sewage sludge and sewage sludge derived adsorbents
 1053

EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye
The surface properties of raw sewage sludge, carbonized sewage sludge and activated sewage sludge were
investigated by SEM and the micrographs are presented in following Fig. 3 in 1000 times magnification.The
structure of raw sludge (Fig. 3a) is dense and there arealmost no pores on it. Following the carbonization and
activationprocess, the structure became different due to the decomposition of organic matters. It can easily be
seen from the micrographs that the surface of carbonized product (Fig. 3b) was loose, collapsed and some
pores structures appeared. On the other hand, when ZnCl2 was used for chemical activation pores in various
shapes and sizes (Fig. 3c) occurred because of some ZnCl2evaporationand interaction between other
compounds (e.g. H2O) of sludge during activation process and leaving the space formerly closed by this
chemical activation agent. The BET analysis has strongly supported the SEM micrographs. According to
BET results surface area has significantly raised from raw sewage sludge to chemically activated sewage
sludge. BET surface area values of SWS, CSWS and ASWS were 0.9350 m2/g, 19.1925 m2/g and 348.9273
m2/g, respectively. It is very clear chemical activation method is the best option for the production of high
surface area adsorbents. The value 348.9273 m2/g is very notable when it compared with literature. There are
a lot of investigations on sewage sludge based adsorbents and BET values differ in a wide range of 7-1705
m2/g [105].

(a) (b) (c)

Figure 3 SEM images of SWS (a), CSWS(b) and ASWS(c)

Before the batch adsorption experiments, in order to determine the optimum adsorption time and determine
the adsorption kinetics for theadsorbents used in this study the effect of contact time onadsorption was
determined at 25 ˚C by using the stock solutionwhich has the RBBR concentration of 100ppm.As can be
seenfrom Fig. 4, the RBBR removal increased rapidly at the beginningof adsorption with increasing contact
time and thereafter attainedto the equilibrium. The minimum contact time required to reach tothe equilibrium
is found as 60 min for both of CSWS and ASWS adsorbents. Thus for the following batch
adsorptionexperiments the contact timewas fixed at this value to make sure that equilibrium was
established.This figure indicates that the extent of adsorption increased with increasing time up to a particular
value, after which no further increase in the adsorption of RBBR occurred. Furthermore, when adsorbents
have been saturatedby RBBR after about 70 min, a desorption process started.

2,5

1,5 CSWS
Q (mg/g)

1 ASWS

0,5

0
0 20 40 60 80 100 120 140
Time (s)

Figure 4 Effect of contact time on the amount of RBBR adsorbed by adsorbent

The calculated kinetic parameters for the adsorption of RBBR onto adsorbents are listed in Table 4. The
findings showed that, in both cases, theadsorption process was better fitted by the pseudo-second-order
kinetic model. The calculatedvalues of Qe for the pseudo-second-order kinetic model agreed well with the
 1054

Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan
experimental data, while the correlation coefficients for the pseudo-second-order kinetic model were
alsohigher than the corresponding values for the pseudo-first-order kinetic model. As can be seen from the
Table 4, Qevalues from pseudo-first order kinetic model is not in agreementwith experimental data Qexp,
although the correlationcoefficients have pretty high values, the adsorption processdidn'tcomply with this
model. According to these results adsorption of RBBR onto adsorbents is based on chemisorptionsmechanism
with a rate-limiting exchange reaction step which controls adsorption process due to inter particular diffusion
[58], [119], [120].

Table 4 Pseudo-first-order and Pseudo-second-order kinetic model constants for the adsorption of RBBR onto adsorbents

Pseudo-first-order Pseudo-second-order
Adsorbents
Qe(exp) Qcal k1 R2 Qcal k2 R2
(mg/g) (mg/g) (1/min) (mg/g) [(g/(mg min)])

CSWS 0.788 0.449 0.029 0.932 0.837 0.138 0.994

ASWS 1.913 0.479 0.021 0.826 1.919 0.205 0.999

The following Fig. 5 shows the amount of adsorbed RBBR onto the adsorbents at equilibriumwere studied
and plotted as a functionof the initial concentration of the standard solutions RBBR dye. As shown in Fig. 5
theadsorption capacity of ASWS increased reasonably linear with increasing initial concentration of RBBR at
equilibrium time of 60 min.However, for CSWS,uptake dye amount has entered into a negative increase stage
after 60 ppm initial dye concentration unlike ASWS. The reason of this situation is due to limited pore
structure devoid of mesopore and micropore formations and quite low surface are of CSWS which treated
only thermal process. According to the data obtained both of the adsorbents CSWS and ASWS had a
maximum value of dye adsorption percentage of %10.38 and %21.14 respectively at 20 ppm dye
concentration. These values were lower at other initial dye concentrations because of rapidly increasing pore
saturation with increasing concentrations. On the contrary uptake amount of RBBR increased with increasing
concentrations and theadsorption capacities of CSWS and SWSW are 7.416 and16.652 mg/gat 100 ppm
RBBR initial concentration, respectively.

2,5

1,5
Qe (mg/g)

CSWS
1 ASWS

0,5

0
0 20 40 60 80 100 120
Co (mg/L)

Figure 5 Amount of dye stuff absorbed by per unit weight of the adsorbents at different standard solution concentrations

Adsorption isotherms are very important for the design ofadsorption systems since they represent how the dye
molecules arepartitioned between the adsorbent and liquid phases at equilibriumas a function of RBBR
concentration. Inthis study the equilibrium data obtained for the adsorption of RBBR onto adsorbents were
analyzed by considering theFreundlich and Langmuir isotherm model equations.The Freundlich and
Langmuir isotherms obtained fromthe equilibriumadsorption data of CSWS and ASWS were given in Fig. 6-
Fig. 9, respectively.
 1055

EurAsia Waste Management Symposium, 28-30April 2014, YTU 2010 Congress Center, İstanbul/Türkiye

0 1 2 3
0 0,4
y = 0,827x - 1,340
-0,2 0,2 R² = 0,935
y = 0,898x - 1,838

Log Qe
Log Qe

R² = 0,957 0
-0,4
0 1 2 3
-0,6 -0,2

-0,4
-0,8 CSWS Log Ce ASWS
Log Ce
Figure 6 Freundlich adsorption isotherm for the adsorption Figure 7 Freundlich adsorption isotherm for the adsorption
of RBBR onto CSWS of RBBR onto ASWS

6 2,5 y = 27,38x + 0,334

y = 83,66x + 0,378
5 R² = 0,953 2 R² = 0,888
4
1,5
1/Qe

1/Qe

3
1
2
1 CSWS 0,5 ASWS
0 0
0 0,02 0,04 0,06 0 0,05 0,1
1/Ce 1/Ce

Figure 8 Langmuir adsorption isotherm for the adsorption Figure 9 Langmuir adsorption isotherm for the adsorption
of RBBR onto CSWS of RBBR onto ASWS

It is observedfrom isotherms given in Figs. 6–9 that both models indicate agood representation of the
experimental results by linear Langmuiror Freundlich isotherm equations. But from the calculatedregression
coefficients (R2), it can be seen that Freundlichisotherm provided better fit to the equilibrium data than
Langmuirisotherm.The Freundlich and Langmuir isotherm constants obtained from the data for the batch
adsorption experiments conducted in the present study are listed in Table 5.
Table 5 Calculated Freundlich and Langmuir constants and correlation coefficients for the adsorption of RBBR onto
CSWS and ASWS

Freundlich constants Langmuir constants

Adsorbents
Kf (mg/g) n R2 Qmax b R2
(mg/g) (L/g)

CSWS 5.44 1.11 0.957 2.65 4.51x10-3 0.953

ASWS 7.46 1.21 0.935 2.99 12.20x10-3 0,888

As can be seen from Table 6, the Kf and Qmax values of ASWS which areindicating the adsorption capacity
were found higher than CSWS for the adsorption of RBBR onto adsorbents. However, these values were
significantly higher for experimental studies. Furthermore, n and b values indicated ASWS has a higher
sorption intensity and affinity energy than that of CSWS.These n values indicated that adsorption process is
very favorable because of n value between 1 and 10, and moreover very close to value of 1.The isotherm
plots (Figs.6-9) showed thatFreundlich isotherm presented the best harmony with a correlation coefficient of
0.957 for CSWS. But the correlation value of Langmuir isotherm (0.953) was quite close to this value. So,
adsorption characteristics of CSWS can be explained with both of Langmuir and Freundlich isotherms as
homogeneous surface and monomolecular or heterogeneous surface adsorption mechanisms, respectively.
However, if a system is explained withLangmuir isotherm, it is very important to determine dimensionless
separation factor called equilibrium parameter, RL which represented following equation [116]:
 1056

Adsorption of Remazol Brilliant Blue R on Adsorbents Obtained from Anaerobically Digested Sewage Sludge
D. Özçimen, T. Salan
RL = 1/(1+b.C0) (4)
where b(mg/L) is the Langmuir constant and C0 (mg/L) is the initial dye concentration.The value of RL shows
the kind of the Langmuir isotherm to be unfavorable (RL > 1), linear (RL = 1), favorable (0 < RL< 1) or
irreversible (RL = 0). Fig.10 presents the values of RL for the CSWS at different initial dye concentrations.As
can be seen in the figure all RL values are between 0 and 1, it decreases due to increasing RBBR dye
concentration from one to zero. These RL values indicated the adsorption behaviors of RBBR dye onto CSWS
were significantly favorable and disposed to a little irreversible with the rising concentration of adsorbate.

0,9
0,8
0,7
0,6
0,5
RL

0,4
0,3
0,2
0,1
0
0 20 40 60 80 100 120
C0 (ppm)

Figure 10Dimensionless separation factor of RBBR adsorbent onto CSWS

On the other hand, it was very clear from Table 4 for ASWS adsorption was in a quite low harmony with
Langmuir isotherm for relatively lower regression coefficient of 0.888. Therefore, it would be a rational
approach to explain the characteristics of ASWS adsorption as a heterogeneous surface system with
interactionbetween the molecules adsorbed and an exponential distribution of active centers in the adsorbent
due toFreundlich isotherm which has a higher regression coefficient of 0.935. Negatively charged reactive
RBBR dye compounds in the solution, is affected with an electrostatic attraction towards positively charged
adsorbent surface and thereby this mentioned adsorption phenomena occurs.

4. CONCLUSIONS
This study has shown that adsorbents prepared from ASWS rather than CSWS can beemployed as effective
activated carbon for the removal of reactive RBBR dye from waste water streams.SEM micrographs of
produced adsorbents proved that chemical activation is an effective way to manufacture useful high porosity
activated carbons. Chemical analysis of adsorbents via FTIR showed there are a lot of functional groups
which are very important for the nature of adsorption process on the surface of adsorbents and these
compounds vary due to raw material used to produce adsorbents. Moreover, chemical activation results in
significant changes in the structure and number of the functional groups. The calculated adsorption capacity
from kinetic models was quite closer to theexperimental datawhich indicated that the pseudo first-orderis a
very proper model to explain the RBBR adsorption kinetics. On the other hand, R2 values obtained from plots
of Langmuir and Freundlichmodels indicated that Freundlich is more suitable model to describe the RBBR
dye adsorption isotherm. In all cases, ASWS showed better performance than that of CSWS due to its well
porous structure and high surface area. As a result, current study proved that, sewage sludge which is a
problematic by-product of waste water treatment plant can be effectively used for the treatment of same waste
water stream from which is originated after it is processed thermally and chemically via carbonization
method.

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BIOGRAPHY
Dr. Didem ÖZÇİMEN works as assistant professor doctor atYıldız Technical University Bioengineering
Department.Özçimenwas graduated from Istanbul Technical University in 1998. She finished Ph.D study on the biomass
energy technologies in Istanbul Technical University, at Chemical Engineering Department in 2007. She is interested in
the renewable energy sources, thermal conversion technologies, energy and environment, activated carbon, adsorption
technologies and renewable biomaterials. She may be contacted atozcimen@yildiz.edu.tr

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