RESEARCH PROJECT THE PREPARATION OF ACTIVATED CARBON FROM DURIAN SHELLS A ND ITS A PLICATION FOR METHYLENE BLUE ADSORPTION.

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RESEARCH PROJECT THE PREPARATION OF ACTIVATED CARBON FROM DURIAN SHELLS A ND ITS A PLICATION FOR METHYLENE BLUE ADSORPTION Submitted by: MIRNA THIO CHRISTINE CHANDRA 5203003036 5203003039 DEPARTMENT OF CHEMICAL ENGINEERING FACULTY OF ENGINEERING WIDYA MANDALA CATHOLIC UNIVERSITY SURABAYA 2006

APPROVAL SHEET The RESEARCH entitled: The Prcparation of Activated Carbon from DUt'ian Shclls and Its Application for ~lethylene Blue Adsorption which is prepared and submitted by: Name: Mirna NRP : 5203003036 htlil been tlpproved and accepted as one of requirement for Bachelor of Engineering degree in Department of Chemical Engineering, Faculty of Engineering. Widya Mandala Catholic University by following supervisor and has been examined by the committees on December, 14th 2006 Surabaya, January 4th 2007 Supervisor II. JI,c. ~ _ kr,jp C--", r- Tr, Yohanes Sudar anto MT. NIK. 521.89,0151 The Committees,, Chairman Felycia ES, ST, MPhiL NIK. 52l.99,0391 _ /L ~jle~~~<~-'~~'_' r. Su~CML Ph.D. NIK.52193.0198 M lr~er i ; ii, i 1/ Henn~ll 8" ~;r, MT NIK. 52i1.95.022I I.' \ ll Rasiona SiteplI, M.~ng. NIK. 511.89,0154 Member / L~ If. Nani Indraswati NIK. 521.86.0121 Ir. Yohanes lid", 'anto MT. NIK. 52189.0151 gineering Department 'a~, Ph.D. 11

APPROVAL SllEET The RESEARCH entitled: The Preparation of Activated Carbon from Durian Shells and Its Application fol' Methylene Blue Adsorption which 15 pr\lpal'ed and submitted by: Nllme I Thlo ChdAlne Ch~ndn' NRP : 5203003039 l1:jll b\,l~n appwwd and accepted as one of requirement for Bachelor of Englneering degree in Department of Chemical Engineering, Faculty of Engineering, Widya Mandala Catholic University by following supervisor and has been examined bv. the committees on December, 14th 2006 Surabaya, January 4th 2007 MT. Chairman The Committees, Felvcia E.S., S.T., M.PhiL NTK.521.99,0391 M~lrber,! I,, \ ; I \ l Herman H" ST., MT. NIK. 5Zl.95.0221 It. Nam Indras\vati NIK. 521.86.0121 Ir. Rasiona1 Sitepu, M.Eng. NIK. 511.89.0154 iii

ABSTRACT An activated carbon was prepared from durian shell and used for the removal of methylene blue from aqueous solutions. The activated carbon was prepared using chemical activation method with potassium hydroxide as the activating agent. The activation was conducted at 673.15-773.15 K for 1 h with mass ratio of chemical activating agent to durian shell 0.25-3. Batch kinetics and isotherm studies were conducted to evaluate the adsorption behavior the activated carbon from durian shell. The adsorption experiments were carried out isothermally at three different temperatures. The Langmuir and Freundlich isotherm model were used to describe the equilibria data. The Langmuir model agrees with experimental data well. The Langmuir surface kinetics, pseudo first order, and pseudo second order models were used to evaluate the kinetics data and the rate constant were also determined. The experimental data fitted very well with the langmuir surface kinetics and pseudo first order model. IV

DECLARA TION SHEET r declare that this research was my own work and not the others' work, some or all except be written in the text. Wether it is knovm that this research is the others' work, I aware and accept the consequence that this research cannot be used as a requirements to achieve Bachelor of Engineering degree. Surabaya, January 4th 2007 c&> The undergraduate student Mirna NRP. 5203003036 v

DECLARA TION SHEET I declare that this research was my own work and not the others' work, some or all except be written in the text. Wether it is known that this research is the others' work, I aware and accept the consequence that this research cannot be used as a requirements to achieve Bachelor of Engineering degree. Surabaya, January 4th 2007 ~j The undergraduate student Thio Christine Chandra NRP. 5203003039 VI

ACKNOWLEDGEMENT The authors would like to thank God for His blessing in conducting the research entitled The Preparation of Activated Carbon from Durian Shells and Its Application for Methylene Blue Adsorption. This research is one of the requirements to get Bachelor of Engineering degree in Chemical Engineering Department, Faculty of Engineering, Widya Mandala Catholic University Surabaya. This research has been submitted and publ'shed as article in press in Elsevier Chemical Engineering Journal entitled Adsorption of basic dye onto activated carbon prepared from durian shell: Studies of adsorpti'ln equilibrium and kinetics. The authors realize that the success of the research could be attained because of the help of some people, so the authors would like to say thank you to: 1. Ir. Suryadi Ismadji, MT., Ph.D. and Ir. Yohanes Sudaryanto, MT. as our supervisors of this research; 2. Ir. Nani Indraswati, Hennan Hindarso, ST., MT., and Felycia Edy Soetaredjo, ST., M.Phi!. as the reviewers of this research; 3. Wenny lrawati, ST., MT. for her suggestion; 4. Technological and Professional Skills Development Sector Project which support us with the student research grant; 5. Adsorption Group, Chemical Engineering Division, University of Queensland, Australia, who helped us in analyzing the products of our research by using nitrogen adsorption method; Vll

6, Mr. Novi as the technician of Organic Chemistry and Physic Chemis~ry Laboratori LIm; 7. Mr. Pudjo as the technician of Process Technology Laboratorium; 8. Mr. Agus as the technician of Unit Operations Laboratory; 9. Our parents and friends who gave a lot of support; 10. The others, who cannot be mentioned one by one, who helped us from the beginning of the research till the report making. The authors realize that there maybe some shortages in this report. Therefore, the authors would be pleased to accept critics and recommendations for further revision. At last, the authors hope that this report will be useful especially for those who need some infonnation in this report. Vlll

CONTENTS Page TITLE PAGE... 1 APPROVAL SHEET......,... ii ABSTRACT... iv DECLARATION SHEET...... v ACKNOWLEDGEMENT........ VII CONTENTS............ IX LIST OF TABLES... XI LIST OF FIGURES... xii I INTRODUCTION... 1 I.1 Background...... " I 1.2 The objectives... 6 1.3 The limitations... 7 II LITERATURE REVIEW....... 8 II. 1 Adsorption... 8 11.2 Adsorbent... 11 II.3 Activated carbon... 13 II.4 Adsorption equilibria... 15 II.5 Adsorption kinetics... 16 TJI EXPERIMENTAL METHOD......17 III. I Experimental design... 17 III.2 Materials... 22 II1.3 Equipments... 22 IlI.4 Experimental procedure... 23 IV RESULT AND DISCUSSION....... 28 IV. 1 The raw material used... 28 IV.2 Production yield of activated carbon... 29 IV.3 Adsorption capacity... 30 IV.4 Adsorption equilibrium... 33 IV. 5 Surface coverage... 35 IV.6 Pore characteristics of activated carbon... 37 IV.7 Adsorption equilibrium and kinetics oft 1 I 2... 43 IX

V CONCLUSIONS AND SUGGESTION... 59 Y.l Conclusions... 59 Y.2 Suggestion... 60 REFERENCES...... 61 APPENDIX A...... 70 A.I Ash content analysis... 70 A.2 Moisture content analysis... 71 A.3 Volatile matter content analysis... 72 A.4 Carbon content analysis................. 74 APPENDIX B... 75 B.I Solution preparation... 75 B.2 Determination of maximum wavelength... 76 B.3 Preparation of standard curve...........77 APPENDIX C... 79 C.l Calculation of % activated carbon yield... 79 C.2 Methylene blue adsorption... 80 C.3 Adsorption Equilibrium and Kinetics oft I I 2....... 83 APPENDIX D....... 87 0.1 Calculation of % Activated Carbon yield... 87 D.2 Methylene Blue Adsorption... 88 D.3 Adsorption Equilibrium and Kinetics of T liz...... 93 x

LIST OF TABLES Table II. I Characteristics of chemisorption and physisorption.......... 9 Table IVI Fixed carbon content from many kinds of raw material........ 28 Table IV.2 Production yield of activated carbon... 29 Table IV.3 Parameters of Langmuir and Freundlich equation... 34 Table IV.4 Methylene blue surface coverage... 36 Table IV.5 Pore characteristic of durian shell activated carbon (DSAC)... 38 Table IV.6 Pore characteristics ofdsac and F-400... 40 Table IV 7 Parameters of Langmuir equation....45 Table IV8 Parameters of Freundlich equation... 47 Table IV.9 Fitted parameters values using Langmuir surface kinetics model.. 50 Table IV.I 0 Fitted parameters values llsing pseudo first order kinetics model.. 55 Table IVII Fitted parameters values using pseudo second order kinetics Model... 58 Table B.l Table B.2 Relationship between A and absorbance of methylene blue solution... 76 Relationship between concentration and absorbance of methylene blue... 77 Table C.l Yield data of activated carbon product.... 79 Table e.2 Experimental data of methylene blue adsorption... 80 Table C.3 Experimental data of adsorption equilibrium of T 112... 83 Table C.4 Experimental data of adsorption kinetics oft1i 2 at 303.15 K... 84 Table e.5 Experimental data of adsorption kinetics of T lh at 313.15 K... 85 Table e.6 Experimental data of adsorption kinetics oft1i2 at 323.15 K... 86 Table D. I Production yield of activated carbon... 88 Table D.2 Data calculation for methylene blue adsorption... 90 Table D.3 Data calculation of adsorption equilibrium oft l h... 93 Table DA Data calculation of adsorption kinetics of T Ih at 303. 15 K... 94 Table D.5 Data calculation of adsorption kinetics oft 112 at 313.15 K... 95 Table D.6 Data calculation of adsorption kinetics oft1i2 at 323.15 K... 96 XI

LIST OF FIGURES Figure ILl Mechanism of adsorption... 11 Figure III.! Research scenario... 19 Figure IV! Etfect of activation temperature and impre!,'llatioll ratio on the yield of activated carboll... 30 Figure IV.2 Pore network accessibility... 31 Figure IV.3 Molecular structure of methylene blue... 31 Figure IVA Methylene blue adsorption at room temperature... 32 Figure IV.5 Nitrogen adsorption isotherm of DSAC... 38 Figure IV6 Nitrogen adsorption isotherm ofdsac and F-400... 39 Figure IV7 Pore size distribution ofdsac....41 Figure IV.8 BET surface area N2 adsorption isotherm vs Langmuir isotherm..43 Figure IV9 Adsorption isotherm of methylene blue on Tll2 and tits of Langmuir mode1...... 45 Figure IV1 0 Plot KL vs lit for methylene blue....46 Figure IVll Adsorption isotherm of methylene blue on TIl2 and fits of Freundlich model... 47 Figure IV.l2 Langmuir surface kinetic model for the adsorption of methylene blue on DSAC at 303.15 K... 50 Figure IV13 Langmuir surface kinetic model for the adsorption of methylene blue on DSAC at 313. 15 K... 51 Figure IVI4 Langmuir surface kinetic model for the adsorption of methylene blue on DSAC at 323.15 K... 51 Figure IV.15 Determination of energy vf desorption... 52 Figure IVI6 Pseudo first order model for the adsorption of methylene blue on Tlh at 303.15 K..... 54 FigureIV.17 Pseudo first order model for the adsorption of methylene blue on Tlh at 313.15 K... 54 Figure IV18 Pseudo first order model for the adsorption of methylene blue on Tlh at 323.15 K... 55 Figure lvi9 Pseudo second order model for the adsorption of methylene blue on Tll2 at 303.15 K... 56 XIl

Figure IV.20Pseudo second order model for the adsorption of methylene blue on 'flh at 313.15 K... 57 Figure IV.2l Pseudo second order model for the adsorption of methylene blue on Tlh at 323.15 K... 57 Figure B.I Determination of maximum wavelength of methylene blue... 77 Figure B.2 Standard curve of methylene blue solution... 79 Xlii