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Dalam dokumen CERTIFICATION APPROVAL (Halaman 62-89)

John M. Chalmers, 1999, Spectroscopy in Process Analysis, CRC Press, hie

Keith K. H. Choy, McKay, G. Porter, J. F., 1999, Sorption ofacid dye from effluents using activated carbon, Resources, Conservation and Recycling

Kipling, J.J, 1965, Adsorption from Solutions of Non-electrolytes, Academic Press

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Mohd Shariff, A, 1995, Steam Regeneration ofAFixed Bed Adsorption System, Ph.D.

Thesis, Leeds University, United Kingdom

Motoyuki Suzuki, 1989, Adsorption Engineering, Chemical Engineering Monographs

25, Elservier SciencePublishers

Nadia Roostaei, F. Handan Tezel, 2003, Removal ofphenol from aqueous solutions by adsorption, Journal ofEnvironmental Management 70

Nazatul Sheema Bt. Che Din, 2004, Characterization and Adsorption Isotherm of Phenol on Activated Carbon, Undergraduate Thesis, Universiti Teknologi PETRONAS

Noradnin Hafeeza Bt. Haji Nawawi, 2004, Regression Analysis for Hydrocarbon

Adsorption Isotherm on Activated Carbon, Undergraduate Thesis, Universiti Teknologi

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Nouri S.and Haghseresht F, 2004, Research on the BET Surface Area and Packing of

Molecules on the Activated Carbon

Perry and Green, 1998, Perry's Chemical Engineer Handbook, McGraw Hill

Rom W.N., 1992, Environmental and occupational medicine, 2n ed. Boston, MA:

Little, Brown and Company.

Ruthven D.M., Faroof S., Knaebel K. S., 1993, Pressure Swing Adsorption, Wiley-

VCH

S. Lowell, 1991, Powder surface area andporosity

Sittig M, 1991, Handbook ofToxic and Hazardous Chemicals, Park Ridge, NJ, Noyes

Publications

Yang, 2003, Adsorbents Fundamentals and Applications, Wiley Inter-Science

APPENDIX I APPENDIX II APPENDIX III APPENDIX IV APPENDIX V APPENDIX VI APPENDIX VII APPENDIX VIII

APPENDICES

Apparatus and Equipment

Sample Calculation of Solution Preparation

Standard Curve Data

Toluene Adsorption Isotherm Results at Different Temperature Results Obtained from GCMS for n-Hexane Adsorption

Results Obtained From GCMS for n-Hexane Volatility Test SEM Micrographs of GAC 2.5mm and GAC 0.25mm

Sips Isotherms for adsorption isotherm measurement at different

temperature using GAC 2.5

APPENDIX I : Apparatus and Equipment

No Description Purpose

1 100ml Erlenmeyer

flask/conical flask with cap

Toput activated carbon and liquid

solution during batch adsorption isotherm

measurement

2 Glass funnel To be used during gravity filter, to separate activated carbon from liquid

solution

3 50ml beaker For storage of activated carbon

4 Desiccators For storage of activated carbon

5 Filter paper of 0.4-0.45 um To filter activated carbon from liquid adsorption solution

6 Parafilm To seal volumetric flask containing sample

7 Silica gel To be used in desiccators, for storage of

activated carbon

8 Water bath shaker To maintain temperature of system and shake activated carbon solution during batch adsorption isotherm measurement

9 Oven To bake activated carbon

10 Analytical balance To weigh activated carbon

11 UV VIS Spectrophotometer To analyze concentration of adsorbate in sample

12 GCMS with purge and trap To analyze concentration of adsorbate in sample

13 100ml measuring cylinder To measure the volume of the solution

14 SEM To study the microstructure of adsorbents

APPENDIX II: Sample Calculation of Solution Preparation

n-Hexane

n-Hexane is prepared witha 120ppm stock solution.

The sample calculation is as followed:

C1V1 = c2v2

Where Ci is the initial concentration (6.6xl05ppm)

Vi is the initial volume

C2 is the stock concentration (120ppm) V2 is the volume required (500ml) The amount of n-hexane needed is

C,F, 120*500 Vi =

•2' 2

C, 6.6*10"

Different concentrations are prepared. The results are summarized inthe table below:

= 9.0*10"' ml or90.9uL

Concentration(ppm) Volume needed (mL) Volume from stock(mL)

10 100 8.33

25 100 20.83

50 100 41.67

100 100 83.33

120 100 100.00

Toluene

Toluene is prepared with a 400ppm stock solution.

The sample calculation is as followed:

CiVi = c2v2

Where Ci is the initial concentration (8.7xl05ppm)

Vi is the initial volume

C2 is the stock concentration (400ppm)

V2 is the volume required (500ml) The amount of n-hexane needed is

400*500

v, =c^

C, 8.7*10"

Different concentrations are prepared. The results are summarized in the table below:

= 2.29.0*10"' ml or229.9uL

Concentration(ppm) Volume needed (mL) Volume from stock (mL)

10 100 2.5

25 100 6.25

50 100 12.5

100 100 25

200 100 50

APPENDIX III: Standard Curve Data

n-Hexane

Sample ID Concentration (ppm) Absorbance

1 10 0.046

2 25 0.069

3 50 0.101

4 120 0.195

Toluene

Sample ID Concentration (ppm) Absorbance

1 10 0.077

2 25 0.081

3 50 0.109

4 100 0.154

5 200 0.314

APPENDIX IV: Toluene Adsorption Isotherm Results at Different Temperature

Experimental Results ofToluene Adsorption at 35°C

Adsorbent C(ppm) Absorbance Ce (ppm) V(L) m(g) q(mg/g)

GAC 2.5 10 0.034 3.473 0.1 0.2 3.2635

25 0.045 10.117 0.1 0.2 7.4415

50 0.048 12.393 0.1 0.2 18.8035

100 0.052 14.477 0.1 0.2 42.7615

200 0.099 44.179 0.1 0.2 77.9105

GAC 0.25 10 0.035 4.211 0.1 0.2 2.8945

25 0.049 12.889 0.1 0.2 6.0555

50 0.053 15.332 0.1 0.2 17.334

100 0.057 17.728 0.1 0.2 41.136

200 0.114 53.227 0.1 0.2 73.3865

PAC 10 0.037 5.685 0.1 0.2 2.1575

25 0.052 14.555 0.1 0.2 5.2225

50 0.054 16.062 0.1 0.2 16.969

100 0.066 23.545 0.1 0.2 38.2275

200 0.123 58.996 0.1 0.2 70.502

Experimental Results ofToluene adsorption at 55°C

Adsorbent C (ppm) Absorbance Ce (ppm) V(L) m(g) q (mg/g)

GAC 2.5 10 0.035 4.021 0.1 0.2 2.9895

25 0.059 18.985 0.1 0.2 3.0075

50 0.069 25.533 0.1 0.2 12.2335

100 0.079 31.903 0.1 0.2 34.0485

200 0.108 49.462 0.1 0.2 75.269

GAC 0.25 10 0.037 5.685 0.1 0.2 2.1575

25 0.057 17.613 0.1 0.2 3.6935

50 0.069 25.467 0.1 0.2 12.2665

100 0.086 36.035 0.1 0.2 31.9825

200 0.120 57.549 0.1 0.2 71.2255

PAC 10 0.038 5.767 0.1 0.2 2.1165

25 0.057 17.686 0.1 0.2 3.657

50 0.073 28.083 0.1 0.2 10.9585

100 0.087 36.933 0.1 0.2 31.5335

200 0.125 60.36 0.1 0.2 69.82

Experimental Results ofToluene adsorption at65°C

Adsorbent C(ppm) Absorbance Ce (ppm) V(L) m(g) q (mg/g)

GAC 2.5 10 0.037 5.067 0.1 0.2 2.4665

25 0.058 18.367 0.1 0.2 3.3165

50 0.077 30.325 0.1 0.2 9.8375

100 0.080 32.244 0.1 0.2 33.878

200 0.110 50.931 0.1 0.2 74.5345

GAC 0.25 10 0.039 6.825 0.1 0.2 1.5875

25 0.059 19.128 0.1 0.2 2.936

50 0.083 33.823 0.1 0.2 8.0885

100 0.087 36.933 0.1 0.2 31.5335

200 0.128 62.152 0.1 0.2 68.924

PAC 10 0.038 6.167 0.1 0.2 1.9165

25 0.065 22.654 0.1 0.2 1.173

50 0.098 43.292 0.1 0.2 3.354

100 0.111 51.703 0.1 0.2 24.1485

200 0.148 74.9 0.1 0.2 62.55

APPENDIX V: Results Obtained from GCMS for n-Hexane Adsorption

CLASS-5000 *** Report No. - 10 Data :HOA.D01 04/09/09 10:37:49

ale : std 40ppm

: stdOl

B : Standard

hod File Name : HOA.MET Chromatogram ***

r

-J\IS *.

4

* Quantitation ***

1.5

5

147571? ID

Type Name

Time Area

57.05

7

1 M/Z : 57.05 Target

hexane 2,744 2897116

TIC=12627547

TIC

** CLASS-5000 *** Report No. = 11 Data : HOA.D02 04/09/09 11:10:00

ample : std 60ppm

3 : std02

ype : Standard

ethod File Name : HOA.MET

** Chromatogram ***

T

a

3 4

** Quantitation ***

V. , 2.5

5

1462337 ID

Type

Name

Time Area

57.05

1 M/Z : 57.05 Target

hexane

2.740 2945613

TIC=11984964

i ' ' • ' i

9

TIC

** CLASS-5000 *** Report No. = 12 Data : HOA.D03 04/09/09 11:41:42

ample : std 80ppm

) : std03

/pe : Standard

2thod File Name : HOA.MET

** Chromatogram ***

3JI 5

4

** Calibration Curve ***

ID #1 M/Z : 57.05 Area « 50619.3 * (Cone.) Area.

'106

4.0

O

2.0

0 4.0

Cone

*** Quantitation ***

! \

2.5

,-G

6

Name : hexane r2« 0.796152

/6

8.0 101

1919191

Cone.<ppm ) 40.000 60.000 80.000

Area 2897116 2945613 3682035

ID Type Name

Time Area

57.05

1 M/Z : 57.05 Target

hexane

2.737 3682036

TIC=15085349

TIC

** CLASS-5000 *** Report No. = 13 Data : HOA.D06 04/09/10 10:53:01

ample : samplel 40ppm

D : samplel

ype : Unknown

ethod File Name : HOA.MET

** Chromatogram ***

2

\ 1 \

"•4A3_4 5

3 ' 4

** Quantitation ***

i i

../vv 1 v..

2.5

6S>

23024 ID

Type

Name

Time Area Cone.

i/W :J 57.05

12

1 M/Z : 57.05 Target

hexane

2.739 39934 0.789ppm

TIC=7651382

TIC

k* CLASS-5000 *** Report No. = 14 Data : HOA.D07 04/09/10 11:22:39 ample : sample2 60ppm

3 : sample2

/pe : Unknown

ijthod File Name : HOA.MET

"* Chromatogram ***

2

3 4

** Quantitation ***

\ A A

i -\\i

IV \JL

2.5

5r

"1T007I

J

ID Type Name

Time Area Cone.

57.05

7

1 M/Z

Target hexane

2.741 19343

0.382ppm

57.05

TIC=1524748

TIC

9

CLASS-5000 *** Report

ile

Mo. =15 Data :HOA.D08 04/09/10 11:55:40

: sample3 80ppm : sample3 : Unknown

iod File Name : HOA.MET Chromatogram ***

\2 3

M /, 4 5

* Quantitation ***

—- - r """"" 10262

I !

i AA.

2.5

6

ID Type Name

Time Area Cone.

57.05

'vVi^^K'^' ^n-^ta-''

1 M/Z : 57.05

Target hexane

2.737 19559 0.386ppm

TIC=1088337

TIC

ia nata • HOA D09 04/09/10 12:25:25 CLASS-5000 *** Report No. = 16 Data . HUft.uuy

)le : sample4 100ppm

: sample4

3 : Unknown

iod File Name : HOA.MET Chromatogram ***

2

3 4

* Quantitation ***

2.5

-. t-"V~V*" —*-^•"fl-f~t*

6289]

'• \.

\ ,-.

ID Type Name

Time Area Cone.

57.05

1 M/Z : 57.05

Target hexane

2.743 15657 0.309ppm

TIC=1361462

TIC

LASS-5000 *** Report No. = 17 Data e : samples 120ppm

: samples : Unknown

3d File Name : HOA.MET Chromatogram ***

-4 _2_

' Quantitation ***

'I 5350

: HOA.DOO 04/09/10 12:55:07

*" \

ID Type Name

Time Area Cone.

1 M/Z

Target hexane

2.744 10132 0.200ppm

57.05

57.05 1.5

TIC=1411608

TIC

:LASS-5000 « Report No. -19 Data :H0A.D13 04/09/10 14:23:55

le : sampleB 80ppm : samples : Unknown od File Name : HOA.MET Chromatogram ***

'*•->,

- , — r

3

-,A„„,

' Quantitation ***

"74391 -Av

ID Type Name

Time Area Cone.

57.05

1 M/Z

Target hexane

2.750 11753 0.232ppm

57.05

TIC=1210079

TIC

* u -7ft Data •H0A.D14 04/09/10 14:53:58 H.ASS-5000 *** Report No. = 20 Da« •

Le : sample9 100ppm

: sample9 : Unknown

od File Name : HOA.MET Chromatogram ***

"•v...

3

* Quantitation

2.5

-, , . • ^ 5

"4831

--*-?v

6 7 8

ID = 1 M/Z : 57.05

Type Target Name hexane

Time Area Cone.

2.744 : 7687 : 0.152ppm

57.05

TIC=1432834

TIC

oi nata • H0A.D15 04/09/10 15:25:03

;LASS-5000 *** Report No. = 21 Data . hua.uo le : samplelO 120ppm

: samplelO : Unknown

od File Name : HOA.MET Chromatogram ***

" v

•'\.-,.-,...J-*~../v.

3

* Quantitation

j.LJ..

2.5

5542

J 57.

ID Type Name

Time Area Cone.

05

1 M/Z

Target hexane

2.747 10480 0.207ppm

57.05

TIC=1654731

TIC

APPENDIX VI: Results Obtained From GCMS for n-Hexane Volatility Test

•* CLASS-5000 *** Report No. = 22 Data : HOA.D10 04/10/01 10:02:42

imple : hexane30min : hexanelOppm

-pe : Unknown

:thod File Name : HOA.MET f* Chromatogram ***

2.5 3

3

** Quantitation ***

4

' V;

J,,

"10

9 ,11 12 5

"1823891 ID

Type Name

Time Area Cone.

=-J 57.05

1 M/Z

Target hexane

2.756 369534 7.300ppm

13

57.05

TIC=25454152

&.

17 TIC

** CLASS-5000 *** Report No. = 24 Data : H0A.D12 04/10/01 11:23:11

ample : hexanelhr

) : hexanelOppm

ype : Unknown

ethod File Name : HOA.MET

** Chromatogram ***

2

. a .

..,.,,., _J^, J\,,

3 ' 4 5

'** Quantitation ***

u .

2.5

1132871

t. 6 7 89 10

ID

Type

Name

Time Area Cone.

57.05

1 M/Z : 57.05 Target

hexane

2.761 217738

4.301ppm

TIC=26855169

12 1314 -^.•••f^J TIC

11 9

* CLASS-5000 *** Report No. = 27 Data :H0A.D15 04/10/01 13:00:33

impie : hexane0230hr

i : hexanelOppm

rpe : Unknown

•thod File Name : HOA.MET '* Chromatogram ***

2

•** Quantitation ***

33642

2.5

ID

Type Name

Time Area Cone.

57.05

1 M/Z : 57.05 Target

hexane

2.759 63221

1.249ppm

TIC

APPENDIX VII: SEM Micrographs of GAC 2.5mm and GAC 0.25mm

«-•

EHT" 20.00 kV

WD" 10 mm Signal A -SE1

GACO.25.1mm

Micrograph of GAC 2.5mm at 3.85KX

Micrograph of GAC 0.25mm at 133KX

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