iii ADSORPTION OF DIRECT SCARLET 4BS FROM SIMULATED TEXTILE WASTEWATER USING CHITOSAN FROM BLACK TIGER SHRIMP (Penaeus
monodon) SHELLS AS ADSORBENT
XYLENE S. MADERAZO
SUBMITTED TO THE FACULTY OF THE
COLLEGE OF ENGINEERING AND AGRO-INDUSTRIAL TECHNOLOGY UNIVERSITY OF THE PHILIPPINES LOS BAÑOS
IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE
DEGREE OF
BACHELOR OF SCIENCE IN CHEMICAL ENGINEERING
OCTOBER 2009
vii TABLE OF CONTENTS
TITLE
ACCEPTANCE SHEET
ACKNOWLEDGEMENT iii
TABLE OF CONTENTS v
LIST OF TABLES vii
LIST OF FIGURES viii
LIST OF APPENDICES x
ABSTRACT xi
1. INTRODUCTION
1.1 Significance of the Study 1
1.2 Objectives of the Study 4
1.3 Scope and Limitations of the Study 4
2. REVIEW OF RELATED LITERATURE
2.1. Dye 5
2.1.1. Classification of Dyes 5
2.1.2. Direct Scarlet 4BS 8
2.2. Wastewater and its Environmental Effects 8
2.2.1. Textile Wastewater 9
2.3. Adsorption 10
2.3.1. Adsorption Isotherms 11
2.3.1.1. Langmuir Isotherm 11
2.2.1.2. Freundlich Isotherm 13
2.4. Adsorbent 16
2.4.1. Chitosan 17
2.5. Black Tiger Shrimp Shells 21
3. MATERIALS AND METHODS 3.1. Materials
3.1.1. Raw Material 22
3.1.2. Dye 22
3.1.3. Reagents 22
3.1.4. Distilled Water 22
3.1.5. Glassware 22
3.1.6. Glass Bottles 23
3.2. Equipments
3.2.1. Analytical Balance 23
3.2.2. US Standard Sieve 23
3.2.3. Furnace and Oven 23
viii
3.2.4. Grinder 23
3.2.5. Pump 24
3.2.6. Spectrophotometer 24
3.3. Methodology
3.3.1. Preparation of Shrimp Shells 24
3.3.2. Preparation of Chitosan
3.3.2.1. Demineralization 24
3.3.2.2. Deproteinization 24
3.3.2.3. Deacetylation 25
3.3.3. Evaluation of Chitosan
3.3.3.1. Moisture Content 25
3.3.3.2. Ash Content 25
3.3.3.3. Bulk Density 26
3.3.4. Textile Wastewater
3.3.4.1. Simulation of Textile Wastewater 26 3.3.4.2. Determination of Wavelength of Maximum
Adsorption, λmax 27
3.3.4.3. Preparation of the Standard Curve 27 3.3.4.4. Construction of Adsorption Isotherm 27
3.3.4.5. Determination of Contact Time 28
3.3.4.6. Determination of the Order of Reaction 28
3.3.4.7. Effect of pH 29
4. RESULTS AND DISCUSSION
4.1. Chitosan Extraction 30
4.2. Product Evaluation 32
4.3. Wavelength of maximum adsorption, λmax 34
4.4. Standard Curve 34
4.5. Adsorption Isotherm 36
4.6. Contact Time 38
4.7. Order of Reaction 40
4.8. Effect of pH 41
5. SUMMARY AND CONCLUSION 43
6. RECOMMENDATION 46
7. REFERENCES 47
APPENDICES 50
MSDS xii
ix LIST OF TABLES
Table No. Title Page
2.1 Adsorption Isotherm 15
2.2 Solubility of chitin, chitosan and chitin acetate on common solvents 19
4.1 Chitosan yield from shrimp shells 31
4.2 Parameters used for the construction of Langmuir and Freundlich 36 isotherms
4.3 Parameters for Langmuir Isotherm 37
4.4 Parameters for Freundlich Isotherm 38
4.5 Data for the determination of the effect of contact time on dye adsorption 39 4.6 Parameters used for the calculation of the order of reaction 41 4.7 Data for the determination of the effect of pH on dye adsorption 42
x LIST OF FIGURES
Figure No. Title Page
2.1 The molecular structure of Direct Scarlet 4BS 8
2.2 Langmuir Isotherm 12
2.3 Freundlich Isotherm 13
2.4 Equilibrium Concentration (Classification of Different Systems of Isotherms) 14 2.5 Adsorption Isotherms 15
2.6 Chemical formula of chitosan in Haworth’s projection. 17
4.1 Oven dried shrimp shells 30
4.2 Powdered shrimp shells 30
4.3 Demineralization 31
4.4 Product after demineralization 31
4.5 Deproteinization 31
4.6 Product after deproteinization (chitin) 31
4.7 Chitosan extracted from Black shrimp shells 32
4.8 Commercially produced chitosan 32
4.9 Plot for the determination of maximum wavelength of Direct Scarlet 4BS 34
4.10 Standard curve of Direct Scarlet 4BS at the maximum wavelength, 500 nm 35
(1-10 ppm) 4.11 Standard curve of Direct Scarlet 4BS at the maximum wavelength, 500 nm 35
(10-50 ppm) 4.12 Standard curve of Direct Scarlet 4BS at the maximum wavelength, 500 nm 36
(60-100 ppm)
xi 4.13 Langmuir Adsorption Isotherm for Direct Scarlet 4BS using chitosan 37 4.14 Freundlich adsorption isotherm for Direct Scarlet 4BS using chitosan 38 4.15 Effect of contact time on the adsorption of Direct Scarlet 4BS using chitosan 40 4.16 Plot for the determination of the order of reaction of 50 ppm 40 simulated textile wastewater
4.17 Effect of pH on the adsorption of Direct Scarlet 4BS using chitosan 42
xii LIST OF APPENDICES
Appendix Title Page
A Procedure in Using Spectrophotometer to Get the Absorbency of 50 Simulated Textile Wastewater
B Product Evaluation 52
C Maximum Wavelength of 10 ppm Textile Wastewater 53
D Standard Curve for Direct Scarlet 4BS 54
E Determination of Langmuir Parameters 55
F Effect of Contact Time 59
G Effect of pH 60
MADERAZO, XYLENE S. ADSORPTION OF DIRECT SCARLET 4BS FROM SIMULATED TEXTILE WASTEWATER USING CHITOSAN FROM BLACK TIGER SHRIMP (Penaeus monodon) SHELLS AS ADSORBENT.
Adviser: Dr. Jovita L. Movillon
ABSTRACT
Chitosan was produced from Black Tiger shrimp shells. The shells were oven dried, powdered and screened to mesh 30 prior to chemical treatments. The shells were subjected to demineralization, deproteinization, and deactylation. A yield of 14.44% was achieved. The extracted chitosan was white and off-white crystalline powder, soft and odorless. Analysis of the chitosan showed that it has 7.67% moisture content, 0.25% ash content, and 1.33g/10 ml bulk density which were comparable to industrial grade chitosan. The produced chitosan was used for the adsorption of Direct Scarlet 4BS. The wavelength of maximum adsorption of the dye was at 500 nm corresponding to an absorbance of 0.615. The Langmuir and Freundlich isotherm were established to evaluate the adsorption of the dye in chitosan. Results show that adsorption data is best described by Freundlich isotherm. The study showed that the removal of the dye decreases as the pH increases having 80.04%, 77.47%, and 29.28% dye removal at pH 3.4, 6.1, and 10.1 respectively. This can be explained by the presence of negatively charged ions competing on the anion groups of the dye for adsorption sites. On the other hand, dye uptake increases as contact time increases. The contact time required to establish equilibrium was at 7200 minutes. Generally, the chitosan was seen to be a feasible adsorbent of Direct Scarlet 4BS.