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DAFTAR ISI

DAFTAR ISI ............................................................................................................... 40

DAFTAR TABEL ....................................................................................................... 41

DAFTAR GAMBAR .................................................................................................. 42

CHAPTER 3 MATERIAL AND METHODOLOGIES ............................................. 43

3.1 Material .............................................................................................................. 43

3.1.1 Adsorbent .................................................................................................... 43

3.1.2Adsorbate ...................................................................................................... 43

3.2 Concentration measurement and calibration..................................................... 46

3.3 Equilibrium sorption studies .............................................................................. 48

3.4 Calculation of dye concentration of isotherm .................................................... 51

3.5 Apparatus ........................................................................................................... 51

INDEKS ...................................................................................................................... 52

DAFTAR PUSTAKA ................................................................................................. 53

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DAFTAR TABEL

Tabel 3- 1 Properties of Drimarene Red X-6BN (C.I. Reactive Red 243) ................. 43
Tabel 3- 2 Reactive Red 3BS (C.I. Reactive Red 239) - Two reactive groups........... 44
Tabel 3- 3 Constants k for calculations of dye concentration of dyes used ................ 48
Tabel 3- 4 Recipe for temperature equilibrium sorption studies................................. 49

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DAFTAR GAMBAR

Gambar 3- 1 the molecular structure of Reactive Red X-6BN (C.I. Reactive Red 243)
..................................................................................................................................... 45
Gambar 3- 2 the absorbance spectrum of Red X-6BN in visible wavelength,
λmax=511nm............................................................................................................... 45
Gambar 3- 3 the molecular structure of Reactive Red 3BS ........................................ 46
Gambar 3- 4 the absorbance spectrum of Red 3BS in visible wavelength,
λmax=537nm............................................................................................................... 46
Gambar 3- 5 Calibration curve for Red X-6BN at hmax = 511 nm............................ 47
Gambar 3- 6 Calibration curve for Red 3BS at hmax = 537 nm ................................ 48

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CHAPTER 3 MATERIAL AND METHODOLOGIES

3.1 Material

3.1.1 Adsorbent

The adsorbent used in this project is a powdered chitosan,


molecular weight from 100,000 to 300,000, made by
ACROS (Gandhi, 2015).

3.1.2Adsorbate
Two commercial reactive dyestuff were used in the project,
namely, Drimarene Red X-6BN (Table 2-1), and Reactive
Red 3BS (Table 3-2). The reason for selecting these dyes is
that their chemical structures are disclosed so that the
properties of these two dyes can be identified and easier to
interpret the isotherms’ results.

Tabel 3- 1 Properties of Drimarene Red X-6BN (C.I. Reactive Red 243)

Parameters Drimarene Red


X-6BN
Color index name Reactive Red
243
Chromophore group Azo
Number of reactive 2 MCT
group
Reactive anchor Monochlortriazi

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system ne

+
Monochlortriazi
ne
Molar mass 1136.31
Max absorbance 511 nm
Company Clariant

Tabel 3- 2 Reactive Red 3BS (C.I. Reactive Red 239) - Two reactive groups

Parameters Reactive Red


3BS
Color index name Reactive Red
239
Chromophore group Azo
Number of reactive 2 (MCT + VS)
group
Reactive anchor Monochlor
system triazine

+
Vinylsulf
one
Molar mass 1136.35
Max absorbance 537 nm
Company Many producers

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Gambar 3- 1 the molecular structure of Reactive Red X-6BN (C.I. Reactive
Red 243)

0.25

0.2
X-6BN (ABS)

0.15

0.1 X-6BN

0.05

0
0 100 200 300 400 500 600
Waveleng (nm)

Gambar 3- 2 the absorbance spectrum of Red X-6BN in visible wavelength,


λmax=511nm

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Gambar 3- 3 the molecular structure of Reactive Red 3BS

0.25

0.2

0.15
3BS (ABS)

A
0.1

0.05

0
350 450 550 650 750
-0.05
Wavelength (nm)

Gambar 3- 4 the absorbance spectrum of Red 3BS in visible wavelength,


λmax=537nm

3.2 Concentration measurement and calibration


In order to calculate the concentration of the sample from
each experiment data, it has to setup a calibration curve for
each. For each dye, seven different incremental
concentration solutions were prepared and their absorbance
was identified by a perkin-Elmer UV/VIS
Spectrophotometer Lambda 18 on a range from 400 nm to

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700 nm. After that, the maximum absorbance of each dye
was plotted against the concentrations (Jansson, 1994).

Theoretically, the constant k of dye can be calculated by the


calibration curve (Figure 3-5 and Figure 3-6) of the dye
samples prior to saturation. It is observed that these two
dyes sample haven’t reached the saturated point, by which
the slope of equations are the constant, k (Table 3-3).

0.25

0.2

0.15
3BS (ABS)

A
0.1

0.05

0
350 450 550 650 750
-0.05
Wavelength (nm)

Gambar 3- 5 Calibration curve for Red X-6BN at hmax = 511 nm

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0.25

0.2

0.15
3BS (ABS)

A
0.1

0.05

0
350 450 550 650 750
-0.05
Wavelength (nm)

Gambar 3- 6 Calibration curve for Red 3BS at hmax = 537 nm

X-6BN: Dye Concentration (g/l) = Maximum Absorbance /k(X-6BN)


3BS: Dye Concentration (g/l) = Maximum Absorbance/k (3BS)

Tabel 3- 3 Constants k for calculations of dye concentration of dyes used

Name of Dye Dye constant, k


Reactive Red X-6BN 8.08029
Reactive Red 3BS 9.35382

3.3 Equilibrium sorption studies

In this project, the focus is on how the temperatures affect


the sorption behavior of chitosan, and comparing the
difference of sorption behavior between 2 MCT reactive
groups, and 1 MCT and 1 VS reactive group on dyestuffs

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(Peterson DL & Wong, 1990).

Therefore, 27 °C, 45 °C and 60 °C were set for each bath of


studies. For the studies at each temperature, ten different
concentration dye solutions were brought into contact with
weighted chitosan.

Firstly, a 0.2000 g dried chitosan was weighed into 250 ml


Blue Cap Bottle and brought into contact with 200 ml dye
solutions with known initial dye concentration. Secondly,
the bottles were sealed and agitated for 5 hours at 150
rpm/min thermostatic shaking bath and maintained at the
preset temperature until equilibrium reached. The recipe for
temperature equilibrium sorption studies is shown in Table
3-4 (Okamoto & Kataoka, 1993).

Tabel 3- 4 Recipe for temperature equilibrium sorption studies

27 °C, 45 °C and 60 °C were set for each bath of studies


Liquor ratio of water to chitosan, 1000:1; 0.2 g chitosan/200 ml dye solution
Dye chitosan weight Pipette volume dye weight Dye
bath (g) (ml) (g) Concentration

from 2 g/L (g/l) in 200ml


1 0.2 5 0.01 0.05
2 0.2 10 0.02 0.1
3 0.2 13 0.026 0.13
4 0.2 15 0.03 0.15

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5 0.2 18 0.036 0.18
6 0.2 20 0.04 0.2
7 0.2 25 0.05 0.25
8 0.2 30 0.06 0.3
9 0.2 40 0.08 0.4
10 0.2 50 0.1 0.5

At t=0, the dye concentration was determined by the UV-


IS spectrometer, which is called Cinitial. After the
equilibrium is reach, that dye concentration was measured,
called Cequilibrium. These data can be used to determine the
sorption capacity of adsorbent by concept of qe = Cinitial −
Cequilibrium.

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3.4 Calculation of dye concentration of isotherm
The chitosan sorption capacity qe was precisely calculated from:
qe = Dye concentration in sorbent at equilibrium
CO = Initial dye concentration in liquid phase
Ce = Liquid phase dye concentration at equilibrium
V = Total volume of dye solution used
M = Mass of sorbent used

3.5 Apparatus
A Grant OLS 200 shaker was used for the dye adsorption.
A Beckman J2-21 centrifuge was used for separation of
chitosan and dye solution. A spectrophotometer (Perkine
Elmer Lambda 18) was used to determine the UV-IS
absorption absorbance of the dye (Redlich & Bonneau,
1995).

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INDEKS

Absorbance, 48 Liquid, 50
Adsorbate, 43 Material, 43
Adsorbent, 43 Spectrophotometer, 46
Apparatus, 50 temperature, 48
calibration, 46 UV-IS, 49, 50
Calibration, 42, 47 Vinylsulfone, 44
isotherms, 43

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DAFTAR PUSTAKA

Gandhi, A. R. (2015, April 6). Adsorption of dyestu†s from aqueous solutions with
activated carbon. I.

Jansson, C. (1994, Mei 23). Uranium and vanadium sorption by chitosan and
derivatives. p. 12.

Okamoto, Y., & Kataoka. (1993, Maret 23). Adsorption of acid dye on crosslinked
chitosan. pp. 10-11.

Peterson DL, R., & Wong. (1990, Juli 29). Process Biochem. pp. 80-100.

Redlich, P., & Bonneau. (1995, Januari 4). Comparative cost of color removal from
textile. pp. 34-35.

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