REMOVAL OF IBUPROFEN FROM AQUEOUS SOLUTIONS BY ADSORPTION ON LENTIL AND RICE HUSK

1. GRADUATION THESIS
REMOVAL OF IBUPROFEN FROM AQUEOUS SOLUTIONS BY
ADSORPTION ON LENTIL AND RICE HUSK
Supervisor: Prof. Dr. Belma KIN ÖZBEK
10051042 Esra ALTUN
11051803 Ayşe ÇELİK

2. CONTENTS
Materials and Methods
Conclusions
Results and Discussions
Adsorption
Industrial Wastewater Treatment
Pharmaceuticals

3. PHARMACEUTICALS

4. These excreted wastes can easily metabolise by
microorganisms in sewage treatment plants.
Many human and veterinary pharmaceuticals aren’t
completely metabolized and excreted unchanged via urine
and feces.
Pharmaceuticals are organic compounds that are signing
anthropogenic origin, consumed, produced and/or excreted
by humans and animals, or used in household products.

5. Consume of Pharmaceutical in Public
30%
153%
0
20
40
60
80
100
120
140
160
180
Years
1994-2002 2002-2012
%Change

6. IBUPROFEN

7. Acidic drugs are ionic in neutral pH, which makes them an
interesting compound to study.
Ibuprofen is a non-steroidal acidic anti-inflammatory drug
which is largely used throughout the world (Lischman et al.,
2006).

8. Melting Point;
77-78 °C
Boiling Point ;
157 °C (4
mmHg)
Storage T ;
-20°C Freezer
Water
Solubulity;
Insoluble
UV
Spectrum;
220nm
Colourless,
Crystalline
Steam
Pressure;
1.86.10-4(mm
Hg)
pKa; 4.9
Henry Laws
Constant
1.50.10-7
(atm.m3/mole)

9. INDUSTRIAL WASTEWATER
TREATMENT

10. Industrial wastewater treatment includes the mechanisms and
processes used to treat waters which have been contaminated in
some way by anthropogenic industrial or commercial activities prior
to its release into the environment.
In the developed world, recent trends have been to minimize or
recycle waste inside the production process.
Sources of Industrial Wastewater;
Iron and steel industry
Mines and quarries
Food industry
Complex organic chemicals industry

11. Solid removal
• Most solids can be removed by using simple sedimentation
techniques with the solids recovered as sludge or slurry.
Oil and grease
removal
• Skimming devices can recover many oils from open water
surfaces.
Removal of
biodegradable
organics
• Biodegradable organic materials can be removed using
extended usual wastewater treatment processes such as
trickling filter or activated sludge.
Activated
sludge process
• Activated sludge is a biochemical process for treating sewage
and industrial wastewater by air (or oxygen) and
microorganisms.

12. Treatment of
acids and alkalies
• Alkalis and acids can usually be neutralized under controlled
conditions. Neutralization frequently produces sediment that will
require treatment as a solid residue that may also be toxic.
Treatment of toxic
materials
• Toxic materials (many organic materials, metals, acids, alkalis and
non-metallic elements) are generally resistant to biological processes
unless very dilute. Metals can often be precipitated out by changing
the pH or by treatment with other chemicals.
Trickling filter
process
• A trickling filter consists of a bed of rocks, slag, gravel, plastic media
or peat moss. The process involves adsorption of organic compounds
in the wastewater by the microbial slime layer covering the bed
media. Aerobic conditions are continued by forced air flowing
through the bed.

13. ADSORPTION

14. Adsorption is the adhesion of molecules, atoms or ions from a dissolved
solid, liquid or gas to a surface.
Adsorption is the binding of molecules or particles to a surface. It must
be distinguished from absorption by the filling of pores in a solid. The
surface binding is generally weak and reversible.
Types of Adsorption;
Physical adsorption or physisorption
Chemical adsorption or chemisorption

15. Physisorption
Low heat of adsorption
Van der Waal's forces
Takes place at low temperature
Its reversible
Related to the ease of liquefaction of
the gas
Not very specific
It forms multi-molecular layers
No requirement of activation energy
Chemisorption
High heat of adsorption
Chemical bond forces
Takes place at high temperature
It is irreversible
Extent of adsorption is generally not
related to liquefaction of the gas
Highly specific
Forms monomolecular layers
Requires activation energy

16. • Schematic representation of the adsorption
and possible subsequent reaction of carbon
monoxide on various solid surfaces

17. Most Important Adsorbents
Adsorbents are usually used in the form of rods, spherical pellets, monoliths or
moldings, with hydrodynamic diameters between 10 and 0.5 mm.
Adsorbents are mostly microporous and high specific surface materials (200 -
2000 m2/g)
The adsorbent is the separating agent which is used to express the difference
between molecules in a mixture: adsorption equilibrium or kinetics.

18. Activated
carbon
Silica gel
Alumina
Alumino
silicates
ZeoliteMordenite
Clays
Carbon
nanotubes
Red mud
Adsorbents

19. Factors Affecting Adsorption
• Surface area of adsorbent
• Particle size of adsorbent
• Contact time or residence time
• Solubility of solute (adsorbate) in liquid (wastewater)
• Affinity of the solute for the adsorbent (carbon)
• Number of carbon atoms
• Size of the molecule with respect to size of the pores
• Degree of ionization of the adsorbate molecule
• pH

20. Adsorption Isoterms
NAME ISOTHERM EQUATION APPLICABILITY
Langmuir
𝐪 =
𝐪 𝐦 𝐤 𝟏. 𝐂
𝟏 + 𝐤 𝟏 𝐂
Chemisorption and
physical adsorption
Freundlich 𝐪 = 𝐊 𝐅 𝐂 𝟏/𝐧 Chemisorption and
physical adsorption at low
coverages
Temkin
𝐪 𝐞 =
𝐑𝐓
𝐛
𝐥𝐧 𝐀 𝐓 𝐂 𝐞
Chemisorption

21. Langmuir isotherm vs. Freundlich
isotherm
Theoretical
justification
Assumes
reversible
adsorbtion
and
desorption
Represents
well data for
single
components
Represents an
empirical model
No
assumption
Used also for
mixtures of
compounds
LANGMUIR FREUNDLICH

22. Temkin Isotherm
Temkin isotherm comprises a factor that explicitly taking into the account of adsorbent–
adsorbate interactions.
The model assumes that heat of adsorption of all molecules in the layer would decrease
linearly rather than logarithmic with coverage by ignoring the extremely low and large
value of concentrations (Tempkin et al., 1940; Aharoni et al., 1977).
As denoted in the equation, its derivation is characterized by a uniform distribution of
binding energies.

23. Adsorption Kinetics
Pseudo-first order rate model 𝐥𝐨𝐠 𝐪 𝐞 − 𝐪𝐭 = 𝐥𝐨𝐠𝐪 𝐞 −
𝐤 𝐩
𝟐. 𝟑𝟎𝟑
𝐭
Pseudo-second order rate model 𝐭
𝐪𝐭
=
𝟏
𝐤 𝟐 𝐪 𝐞
𝟐
+
𝐭
𝐪 𝐞
Intraparticle diffusion model 𝐪𝐭 = 𝐤 𝐩 𝐭 𝟏/𝟐 + 𝐂
Elovich kinetic model 𝐪𝐭 = 𝛃 𝐥𝐧 𝛂𝛃 + 𝐥𝐧 𝐭

24. MATERIALS and METHODS

25. MATERİALS
Ibuprofen
•The chosen pharmaceutical ibuprofen was supplied from a
pharmaceutical factory and used as the single component
adsorbate in the present study. The concentration of
ibuprofen was used as 30 mg/L
Rice Husk
•Rice husk was supplied from Güven Rice Factory in Osmancık
Çorum. Rice husk’s outer surface area is around 4000 m2/
m3. The moisture of rice husk was obtained 7% in the
present study.
Lentil Husk
•Lentil husk was supplied from Arpacioglu lentil production
factory in Şehitkamil in Gaziantep. The moisture of lentil husk
was obtained 1%.

26. APARATUS
IKA KS
4000 IC
Shaker
Scale
SHIMADZU UV-
1800
spectrofotometer
Eutech pH
meter
Syringe
Filter

27. Experimental Methods
Several amounts of adsorbent were poured to
100 mL water and taken to the shaker for a
good mixing for an hour.
3 mg of ibuprofen was dissolved in 5 mL
methanol and it was added into the solution.
pH of the solutions were adjusted before the
adsorption experiments.
When the adsorption started, samples were
taken in defined time intervals.

28. Experimental Methods
During the adsorption experiments, the residual of the
ibuprofen amounts were examined for a time interval.
For determination ibuprofen amounts, the adsorbent
solution was filtrated by using the syringe filter and
absorbance values were measured.
By using the calibration curve, the concentration values were
calculated from absorbance values.
In the meantime, adsorbent solution without ibuprofen was
used as blank solution at defined pH and temperature values.
The absorbance values of the blank solution were measured.

29. Calibration curve of ibuprofen
σ=0.00384

30. RESULTS
and
DISCUSSIONS

31. pH Effect on Ibuprofen Adsorption
Concentrations (mg/L)
Time (h) pH 3 pH 4 pH 5
0 30.00 30.00 30.00
1 21.92 24.59 29.19
2 16.55 22.38 25.36
3 16.36 20.95 22.76
4 15.84 20.95 21.89
5 15.52 20.63 21.27
6 15.00 18.98 21.09
• The ibuprofen adsorption was
examined at various pH
values such as 3, 4 and 5,
respectively.
• The adsorbent concentration
was 10 g/L and ibuprofen
concentration was 30 mg/L at
temperature of 25 0C.
• The adsorption percentages
for pH 3, 4 and 5 were
obtained as 50.0 %, 36.7%
and 29.7%, respectively.

32. pH Effects on Ibuprofen Adsorption
0
5
10
15
20
25
30
35
0 1 2 3 4 5 6 7
Concentration(mg/L)
Time (h)
pH 3 pH 4 pH 5

33. Rice Husk Concentration Effect on
Ibuprofen Adsorption
• The ibuprofen adsorption
was examined at various
adsorbent concentration
values such as 5, 10, 20 and
40g/L, respectively.
• The pH value was 3 and
ibuprofen concentration was
30 mg/L at temperature of 25
0C.
• The adsorption percentages
for adsorbent concentrations
5, 10, 20 and 40g/L were
obtained as 10.17 %, 50.00
%, 53.73 % and 51.99 %,
respectively.
Concentrations (mg/L)
Time (h) 5 g/L 10 g/L 20 g/L 40 g/L
0 30.00 30.00 30.00 30.00
1 27.97 21.92 19.28 16.51
2 27.46 16.55 16.51 15.95
3 27.27 16.36 14.41 15.32
4 27.27 15.84 14.21 14.96
5 26.95 15.52 13.88 14.82
6 26.95 15.00 13.88 14.40

34. Rice Husk Concentration Effect on
Ibuprofen Adsorption
0
5
10
15
20
25
30
35
0 1 2 3 4 5 6 7
Concentration(mg/L)
Time (h)
5 g/L 10 g/L 20 g/L 40 g/L

35. Temperature Effect on Ibuprofen
Adsorption
Concentrations (mg/L)
Time (h) 25 ºC 30 ºC 40 ºC
0 30.00 30.00 30.00
1 19.28 18.96 19.49
2 16.51 16.83 17.36
3 14.41 14.70 15.23
4 14.21 14.17 14.90
5 13.88 13.84 14.70
6 13.88 13.84 14.57
• Ibuprofen adsorption was
examined for various
temperatures such as 25,
30 and 40 ºC, respectively.
• At pH 3, ibuprofen
concentration was 30 mg/L
and rice husk concentration
was 20 g/L.
• The adsorption
percentages for
temperatures 25, 30 and 40
ºC were obtained as
53.73%, 53.88% and
51.44%, respectively.

36. Temperature Effect on Ibuprofen
Adsorption
0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
0 1 2 3 4 5 6 7
Concentration(mg/L)
Time (h)
25 C 30 C 40 C

37. Ibuprofen Adsorption onto Lentil Husk for
Optimum Conditions
• The optimum conditions
were 20 g/ L adsorbent, 30
mg/ L ibuprofen, pH 3 and
room temperature.
• The removal percentage of
ibuprofen was 26.43%.
Time (h) Concentration (mg/ L)
0 30.00
1 26.45
2 24.85
3 23.67
4 22.84
5 22.49
6 22.07
0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
0 1 2 3 4 5 6 7
Concentration(mg/L)
Time (h)

38. Optimum data of adsorption onto
rice husk
• From 6 hours’ experiments, optimum conditions were; pH 3, room temperature
(25 ± 2 ºC), 180 rpm shaking velocity and 20 g/L adsorbent concentration.
Time (h) Adsorbed Concentration (mg/L) qt (mg/g)
0 0.00 0.00
1 10.72 0.54
2 13.49 0.67
3 15.59 0.78
4 15.79 0.79
5 16.12 0.81
6 16.12 0.81

39. Adsorption capacities (qe) of 20 g/L
rice husk against time
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
0 1 2 3 4 5 6 7
qt(mg/g)
Time (h)

40. Adsorption Isotherms

41. Langmuir Isotherm
• Ce was adsorbed ibuprofen concentration and qe was removed ibuprofen
per unit mass of adsorbent.
Time (h) Ce = C1-C2 (mg /L) Ce/ qe (g/L)
1 10.72 13.31
2 13.49 16.73
3 15.59 19.35
4 15.79 19.59
5 16.12 19.90

42. Langmuir Isotherm
y = 1.2322x + 0.1034
R² = 0.9998
13.00
14.00
15.00
16.00
17.00
18.00
19.00
20.00
10.50 11.50 12.50 13.50 14.50 15.50 16.50
Ce/q(g/L)
Ce (mg/L)

43. Langmuir Isotherm
• KL is the adsorption equilibrium constant which is related to
the energy of adsorption (L/mg).
• qmax (mg/g) is the maximum adsorption capacity.
Langmuir Equation qmax (mg/g) KL (L/mg) R2 σ
𝐂 𝐞
𝐪 𝐞
= 𝟏. 𝟐𝟑𝟐𝟐 ∙ 𝐂 𝐞 + 𝟎. 𝟏𝟎𝟑𝟒 0.812 11.92 0.9998 0.0471

44. Freundlich Isotherm
Time (h) Ln qt Ln Ce
1 -0.62 2.37
2 -0.39 2.60
3 -0.25 2.75
4 -0.24 2.76
5 -0.22 2.78

45. Freundlich Isotherm
y = 1x - 2.9957
R² = 1
-0.70
-0.60
-0.50
-0.40
-0.30
-0.20
-0.10
0.00
2.35 2.40 2.45 2.50 2.55 2.60 2.65 2.70 2.75 2.80 2.85
lnqt
ln Ce

46. Freundlich Isotherm
• K (mg/g) (L/g)1/n is the Freundlich constant
related to sorption capacity
• n is the heterogeneity factor.
Freundlich Equation KF (mg.L/g2) n R2 σ
Ln qe= -2.9957+ln Ce 0.05 1 1 0.0029

47. Temkin Isotherm
Time (h) qt (mg/g) Ln Ce
1 0.54 2.37
2 0.67 2.60
3 0.78 2.75
4 0.79 2.76
5 0.81 2.78

48. Temkin Isotherm
y = 0.6617x - 1.0377
R² = 0.9976
0.50
0.55
0.60
0.65
0.70
0.75
0.80
0.85
2.35 2.40 2.45 2.50 2.55 2.60 2.65 2.70 2.75 2.80 2.85
qt(mg/g)
ln Ce

49. Temkin Isotherm
• q 𝑒 =
𝑅𝑇
𝑏
ln 𝐴 +
𝑅𝑇
𝑏
ln 𝐶𝑒 = 𝐵 ln 𝐴 +
𝐵 ln 𝐶𝑒
• R is Gas constant (J/moleK).
• A and B are Temkin constants.
• B is written instead of RT/b.
Temkin Equation A B R2 σ
𝐪 𝐞 = −𝟏. 𝟎𝟑𝟕𝟕 + 𝟎. 𝟔𝟔𝟏𝟕 𝐥𝐧 𝐂 𝐞 0.208 0.6617 0.9976 0.0102

50. Adsorption Kinetics

51. Pseudo first order kinetic model
• qe is the adsorbed ibuprofen onto unit adsorbent in
equilibrium (mg/g).
• qt is the adsorbed ibuprofen onto unit adsorbent at
any time (mg/g).
• K1,ad is the pseudo first order kinetic constant (h-1)
Time (h) log(qe-qt)
0 -0.09
1 -0.57
2 -0.88
3 -1.58
4 -1.78

52. Pseudo first order kinetic model
y = -0.4391x - 0.1032
R² = 0.9787
-2.00
-1.80
-1.60
-1.40
-1.20
-1.00
-0.80
-0.60
-0.40
-0.20
0.00
0 0.5 1 1.5 2 2.5 3 3.5 4
log(qe-qt)
time (h)
Pseudo First Order Kinetic
Model Equation qe (mg/g) qe,h (mg/g) k1,ad(h-1) R2 σ
Log(qe-qt)= -0.439t-0.1032 0.810 0.788 1.011 0.9787 0.1197

53. Pseudo second order kinetic model
Time (h) t/qt (g.h/mg)
1 1.87
2 2.97
3 3.85
4 5.07
5 6.20
6 7.44
y = 1.1095x + 0.6825
R² = 0.9977
0.00
1.00
2.00
3.00
4.00
5.00
6.00
7.00
8.00
1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6
t/qt(g.h/mg)
time (h)

54. Pseudo second order kinetic model
Pseudo Second Order
Kinetic Model Equation
qe
(mg/g)
qe,h
(mg/g)
k2,ad(h-1) R2 σ
t/qt= 1.1095t+0.6825 0.810 0.901 1.803 0.9977 0.1119

55. Elovich kinetic model data
• α is the adsorption kinetic at the beginning (mg/g.h)
• β is the adsorption constant during the experiments
(g/mg).
qt (mg/g) ln t
0.54 0.00
0.67 0.69
0.78 1.10
0.79 1.39
0.81 1.61

56. Elovich kinetic model
y = 0.1747x + 0.5498
R² = 0.9561
0.50
0.55
0.60
0.65
0.70
0.75
0.80
0.85
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80
qt(mg/g)
ln t
Elovich Kinetic Model
Equation α (mg/g.h) β (g/mg) R2 σ
qt= 0.1747 ln t+0.5498 4.065 5.724 0.9561 0.0257

57. Intraparticle diffusion kinetic model
• ki is the intraparticle diffusion model kinetic constant
(mg/g.h0.5)
• Ci is a constant that gives information about the layer
thickness between the adsorbent and adsorbate.
qt (mg/g) t0.5 (h0.5)
0.54 1.00
0.67 1.41
0.78 1.73
0.79 2.00
0.81 2.24

58. Intraparticle diffusion kinetic model
y = 0.2219x + 0.3451
R² = 0.904
0.5
0.6
0.7
0.8
0.9
1 1.5 2
qt(mg/g)
t1/2 (h1/2)
Intraparticle Diffusion
Model Equation
ki (mg/g.h0.5) Ci (mg/g) R2 σ
qt= 0.2219 t0.5 +0.3451 0.2219 0.3451 0.904 0.0387

59. The comparison of studies about removal of
Ibuprofen by adsorption
Reference Adsorbent Parameters
Adsorbent
Cons.(g/L)
Working Cons.
(g/L)
Time (hour) Temperature
(°C)
pH Isotherm Model % Adsorption
The present
study, 2014
Rice husk 20 0.03 2 25 3 Freundlich 53.8 %
The present
study, 2014
Lentil husk 20 0.03 2 25 3 26.32 %
Guedidi et al.
2014
Activated carbon
cloth
0.1 0.01 16 25, 40, 55 3, 7 Freundlich
Langmuir
23 %
Connors et al.
2013
Filtrasorb 200 GAC,
PWA PAC, Purolite
A530E, Amberlite
XAD-4, Amberlite
XAD-7, and Optipore
L-493
0.0006 0.015 24 25 4, 5, 7 Freundlich
Langmuir
96 %
Behera et al.
2012
Kaolinite,
montmorillonite,
goethite, and
activated carbon
1 0.06 6 25 3-11 AC (90 %)
Diğerleri
(10 %)
Jodeh, 2012 Agriculture soil 20 0.05 2 25 1-4 Freundlich 88 %
Staiti, 2012 Soil 0.05 (20-50).10-6 10,30,60,120,1
80 min
15,25,35 1.5-7 Freundlich
Langmuir
92 %

60. The comparison of studies about removal of
Ibuprofen by adsorption
Reference Adsorbent Parameters
Adsorbent
Cons.(g/L)
Working Cons.
(g/L)
Time (hour) Temperature
(°C)
pH Isotherm Model % Adsorption
Almendra,
2011
Activated carbon
F400
0.01 100.10-6 2-24 23 4,5-8 Langmuir
Freundlich
80 %
Deng, 2010 Powdered
activated carbon
0.0005-0.07 100.10-6 2, 5, 10, 15,
30, 60 and
120 min
25 4-7 Freundlich 90 %
Serrano et
al. 2010
Activated sludge 0.01 0.1-1 48 25 2.5 Freundlich 90 %
Bui et al.
2009
SBA-15 1-2 0.1 24 25 3 Langmuir
Freundlich
94.3 %
Xu et al.
2009
Agricultural soils 0.001g/kg (0.5,1,2.5,5,
10).10-3
24 20 Freundlich 98 %
Säfström,
2008
Powdered
activated carbon
0.05 25.10-6 2 25 2.6 92 %
Kabak et al.
2008
Activated sludge 3 0.01-0.05 160min 25 7.5-8.3 Freundlich 79 %

61. CONCLUSIONS
• In previous study, ibuprofen which is mostly used by human being
was chosen as pollutant because of its common usage.
• For removing ibuprofen, rice husk and lentil husk were chosen as
bioadsorbent for the adsorption studies, since they were
agricultural residues and they weren’t harmful to the environment
and they are low-cost materials .
• Adsorption capacity was dependent on adsorbent amount, contact
time and pH value.
• To achieve these goals, different concentration, pH and
temperature values were studied.
• As a result of 6 hours experiments, optimum conditions were; pH 3,
room temperature (25 ± 2 ºC), 180 rpm shaking velocity and 20 g/L
adsorbent concentration.

62. CONCLUSIONS
• When ibuprofen adsorption was examined at various pH values (3, 4
and 5), the most efficient pH value was 3 for ibuprofen adsorption with
a percentage of 50.
• When ibuprofen adsorption was examined at various adsorbent
concentrations (5, 10, 20 and 40g/L), the most efficient value was
20g/L with a percentage of 53.73.
• When ibuprofen adsorption was examined at various temperatures
(25, 30, 40 ºC), the adsorption percentages for temperatures were
53.73%, 53.88% and 51.44%, respectively.
• For optimum conditions adsorption percentage of ibuprofen onto lentil
husk was 26.43%.
• For optimum conditions adsorption isotherms (Langmuir isotherm,
Freundlich isotherm and Temkin isotherm) and adsorption kinetics
(Pseudo first order kinetic model, Pseudo second order kinetic model,
Elovich kinetic model and Intraparticle diffusion model) were studied.

63. CONCLUSIONS
• Among all of the isotherm models Freundlich isotherm
model was fitted best.
• Pseudo second order kinetic model was fitted best than the
other kinetic models applied.
• Consequently, adsorption of ibuprofen onto rice husk gave
better results than adsorption onto lentil husk. But, the
result obtained needs still improvement.
 Activated carbon can be produced from rice husk for more
effective adsorption process.
 Fresh rice husk can be obtained to removal of residual
ibuprofen.
 Adsorption onto rice husk can be done for different
pharmaceuticals in the wastewater.

64. THANKS FOR
LISTENING TO US

65. REFERENCES
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for Water and Wastewater Treatment”, Faculdade de Ciencias e Tecnologia, Universidade Nova de Lisbqa.
• Behera, S. K., Oh, S. Y., Park, H. S., (2012), “Sorptive Removal of Ibuprofen from Water Using Selected Soil Minerals
and Activated Carbon”, DOI 10.1007/s13762-011-0020-8, South Korea.
• Connors, S., Lanza, R., Sirocki, A., (2013), “Removal of Ibuprofen from Drinking Water Using Adsorption”,
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