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March 2013
APPROVAL SHEET

This thesis entitled “Utilization of Characterized Activated Carbon Prepared from Corn Cobs in Sugar Decolorization”, prepared by Dyle Angellowe B. Mapagu, Aurilyn A. Ramirez and Roxanne L. Soriano, in partial fulfilment of the requirements for the degree Bachelor of Science in Chemical Engineering, is hereby recommended for oral examination.

Approved by the Tribunal on Oral Examination with a grade of _________.

Engr. Ma. Haidee A. Mabborang Member Engr. Monico U. Tenedor Member Engr. Marianne DC. Calica Member Engr. Caesar P. Llapitan Chairman Accepted in partial fulfilment of the requirements for the degree Bachelor of Science in Chemical Engineering. Engr. Ernesto D. Marallag Dean, College of Engineering
ACKNOWLEDGEMENT
We, the authors, convey our gratefulness and appreciation to the people who have given valuable assistance in the completion of this study. To Engr. Policarpio Mabborang, Jr. for providing a perceptive and logical evaluation of our research, for his corrections and suggestions in the improvement of the study, and for his patience towards us;
To Engr. Caesar Llapitan, Engr. Marianne Calica, Engr. Monico Tenedor, and Engr. Ma. Haidee Mabborang, who served as our panelists in the defense, pointed out mistakes and gave good suggestions in revising our thesis;
To Engr. Gina Consigna, head of the Feed Laboratory of the Department of Agriculture, Ma’am Editha Taguba, and Ma’am Lawrence Gaspar who permitted us to conduct our experiments in their laboratory;
To Ma’am Gladys Zamora, laboratory technician of the DOST-CAS laboratory, for lending us the laboratory equipment for our thesis study;
To Engr. Jerome Tumaru, production manager of CARSUMCO, for assisting us in our experiments, and for giving us some suggestions in the accomplishment of our study;
To the CSU Chemical Engineering Batch 2011, for guiding and inspiring us in the performance and completion of this requirement;
To our family and friends, for their love and support in everything we do; and
Above all, to the LORD JESUS CHRIST, for everything, for His unending and unfailing love that is more than enough. Without Him and apart from Him we can do nothing. TABLE OF CONTENTS Chapter I: INTRODUCTION 1.1 Background of the Study 1 1.2 Statement of the Problem 2 1.3 Objective of the Study 2 1.4 Significance of the Study 3 1.5 Scope and Delimitation 3 1.6 Time and Locale of the Study 4 1.7 Definition of Terms 5 Chapter II: REVIEW OF RELATED LITERATURE 2.1 Sugar Manufacturing 6 2.1.1 Sugar Refinery 7 2.1.2 Sugar Decolorization 8 2.1.2a Colorants in Cane Sugar 10 2.1.2b Calgon Cane Cal 10 2.2 Activated Carbon 11 2.2.1 Activated Carbon Market Profile 12 2.2.2 Types of Activated Carbon 12 2.2.3 Production of Granular Activated Carbon 13 2.2.4 Carbonization 14 2.2.5 Activation 15 2.2.5a Physical Activation 15 2.2.5a Chemical Activation 16 2.3 Properties of Activated Carbon for Sugar Decolorization 17 2.3.1 Bulk Density 17 2.3.2 Hardness 18 2.3.3 Moisture 18 2.3.4 Porosity 19 2.3.5 Surface Area 19 2.3.6 Pore Size Distribution 20 2.3.7 pH 20 2.3.8 Ash 21 2.3.9 Iodine Number 21 2.4 Corn Cob 22 2.4.1 Corn Cob as Activated Carbon 22 2.5 Spectrophotometer 23 2.6 Theoretical Framework 24 2.7 Conceptual Framework 26 Chapter III: METHODOLOGY 3.1 Materials and Equipment 28 3.2 Preparation of Corn Cob Activated Carbon 28 3.3 Carbon Analysis 31 3.4 Experimental Procedure 31 3.4.1 Preparation of Sugar Liquor 31 3.4.2 Liquor Decolorization 31 3.5 Experimental Analysis 33 3.5.1 Carbon Yield 33 3.5.1 Percent Color Removal 33 3.5.2 Percent Relative Efficiency 33 3.6 Statistical Analysis 34 Chapter IV: RESULTS AND DISCUSSION 4.1 Carbon Yield 35 4.2 Chemical Analysis of the Product 37 4.2.1 pH 37 4.2.2 Ash Content 39 4.3 Physical Analysis of the Product 40 4.3.1 Bulk Density 40 4.3.2 Moisture 42 4.3.3 Hardness 43 4.3.4 Porosity 45 4.4 Iodine Number 49 4.5 Sugar Decolorization 51 4.6 Summary of Results 56

Chapter V: CONCLUSION AND RECOMMENDATION 5.1 Conclusion 57 5.2 Recommendation 58 LIST OF TABLES Table 2.1 Summary of comparison between the single and two-step pyrolysis 14 Table 3.1 Corn cobs activated at different temperatures and impregnation ratio 29 Table 4.1 Carbon yield of corn cob activated carbon 36 Table 4.2 pH of CCACs and CCAL 38 Table 4.3 Ash content of CCACs and CCAL 39 Table 4.4 Bulk density of CCACs and CCAL 41 Table 4.5 Moisture content of CCACs and CCAL 42 Table 4.6 Percentage attrition of CCACs and CCAL 44 Table 4.7 Porosity of CCACs and CCAL 46 Table 4.8 Iodine number of CCACs and CCAL 49 Table 4.9 Color content of the decolorized liquor and the original liquor 52 Table 4.10 Summary of the properties of the CCACs and CCAL 56 Table 4.11 Summary of the percent color removal and percent relative efficiency 56 LIST OF FIGURES Figure 2.1 Flow chart of the sugar refining process 7 Figure 2.2 Flow chart of sugar decolorization process 9 Figure 2.3 Block diagram of activated carbon production using a single step pyrolysis 13 Figure 2.4 Block diagram of activated carbon production using a two step pyrolysis 14 Figure 2.5 Preparation of activated carbon (Din, 2005; Amri, 2008) 24 Figure 2.6 Characterization and utilization of activated carbon (Bansode et al., 2004; Qureshi et al., 2008; Ahmedna et al., 2000) 24 Figure 2.7 Conceptual framework of the study 26 Figure 3.1 Flowchart diagram for the preparation of granular activated carbon 30 Figure 3.2 Decolorization set-ups in water bath 32 Figure 4.1a Bar graph of the carbon yield of corn cob activated carbon 36
Figure 4.1b Effect of activation temperature and impregnation ratio on carbon yield 37 Figure 4.2 Bar graph of the pH of CCACs and CCAL 38 Figure 4.3 Bar graph of the ash content of CCACs and CCAL 40 Figure 4.4 Bar graph of the bulk density of CCACs and CCAL 41 Figure 4.5 Bar graph of the moisture content of CCACs and CCAL 43 Figure 4.6 Bar graph of the attrition of CCACs and CCAL 44 Figure 4.7 Bar graph of the porosity of CCACs and CCAL 46
Figure 4.8 Effect of temperature on total pore volume of activated carbon (Foo et al., 2010) 46
Figure 4.9 Effect of temperature on total pore volume and mesopore volume of activated carbon (Girgis et al., 2001) 48 Figure 4.10 Bar graph of the iodine number of CCACs and CCAL 50 Figure 4.11 Iodine number values of activated carbon (Birbas, 2011) 51
Figure 4.12 Bar graph of the color content of the decolorized and original liquor 52 Figure 4.13 Bar graph of the percent color removal of CCACs and CCAL 53 Figure 4.14 Percent color removal of activated carbons prepared at different conditions (Abdullah et al., 2010) 54
Figure 4.15 Percent color removal of carbons activated at increasing temperature (Qureshi et al., 2008) 54 Figure 4.16 Efficiency of CCACs relative to CCAL 55 APPENDICES Appendix A 1. US Standard Sieve Size 60 Appendix B 1. Measurement of Physical and Chemical Properties of Activated Carbon 61 a. Bulk Density 61 b. Hardness 61 c. Moisture Content 62 d. pH 63 e. Ash Content 63 f. Porosity 64 2. Determination of Iodine Number of Activated Carbon 65 3. Measurement of Color Content of Sugar Syrup 67 4. Color Removal Determination 68
Appendix C Properties of Activated Carbon Produced 69 1. pH 69 2. Ash Content 70 3. Bulk Density 71 4. Moisture Content 72 5. Porosity 73 6. Hardness 74 7. Iodine Number 75 8. Yield 76 9. Color Content 77
Appendix D Statistical Analysis 78
Appendix E Documentation 79 Appendix F Communication 82 Appendix G 1. Material Safety Data Sheet for Activated Carbon 85 2. Material Safety Data Sheet for 85% Phosphoric Acid 86 3. Material Safety Data Sheet for Buffer Solution pH 4.5 (Acetate) 89 4. Material Safety Data Sheet for Sodium Thiosulfate Solutions 93 5. Material Safety Data Sheet for Iodine Solution, 0.1N 96 6. Material Safety Data Sheet for Starch Indicator Solution, 0.05% 101 7. Material Safety Data Sheet for Sodium hydroxide, Pellets, Reagent 105 BIBLIOGRAPHY 110

ABSTRACT

Corn cobs were used to produce granular activated carbon (GAC) using chemical activation method. Crushed corn cobs were impregnated with 85% H3PO4 (w/w) at different impregnation ratios (1:1, 2:1, and 3:1). The chemically treated samples were activated at different temperatures (400, 500, and 600°C) for 2 hours. Nine different GACs were produced with the combinations of the said conditions. Physical and chemical properties of the produced GAC were determined and compared with that of the commercial GAC. Experiments were conducted to determine the characteristics and color removal capacity of the produced carbons. The results of the study showed that corn cob activated carbon was effective in decolorizing sugar syrups. The most effective decolorizer was CCAC6 which was produced at 600°C and 2:1 impregnation ratio. The decolorized liquor treated by CCAC6 was reduced to a color content of 310.33 IU from the original color of 985.54 IU. This means that 68.51% of the original color was removed. On the other hand, the commercial GAC had a color removal percentage of 70.07%. The efficiency of CCAC6 relative to that of the commercial GAC was computed to be 97.77%.

Chapter I
INTRODUCTION

1.1 Background of the Study
Cane sugar syrups typically require decolorization before it is further processed or ready for final use. This is necessary for the removal of unwanted odors and colored impurities. Color determines the grade of sugar - raw or white - and is the main concern of buyer and consumers (Ellis, 2004). White sugar is preferred than brown sugar on the manufacturing of soft drinks and on baking goods because of the effects on its taste. Activated carbons are dedicated to adsorb plant pigments from the sugar cane and colors created during processing.
Calgon Cane Cal, a virgin activated carbon made from bituminous coal, is currently being used by sugar industries for treatment of cane sugar syrups. Because of its high cost, many studies aimed to look for an alternative low-cost material for producing activated carbon. Recent studies showed that agricultural by-products or wastes can be used as raw materials for preparing activated carbon, some of which includes peanut hull (Zhong et al., 2011), nut shells (Wartelle et al.,2001), rice husks (Usmani, 2001) and sugarcane bagasse (Qureshi et al.,2008). In this study, corn cobs were used to produce Granular Activated Carbon (GAC) which was utilized in the decolorization of sugar syrups.

1.2 Statement of the Problem In recent years, it has been necessary for sugar factories to produce high quality refined or semi-refined white sugar for direct consumption. For this reason, decolorization processes used in sugar factories have to be improved. The sugar syrup processed in a refinery contains contaminants that are responsible for its unpleasant odor and brownish color. These colored impurities which come from both the plant origin and the factory-formed colorants make raw sugar not an ideal sweetener. Thus, there is a need to remove at great expense the significant amounts of color and other non-sucrose impurities through decolorization. This study primarily aimed to evaluate the effectiveness of activated carbon prepared from corn cob as a commercial activated carbon alternative by characterizing its performance as adsorbent in sugar decolorization.

1.3 Objectives of the Study This study sought to produce activated carbon from a local agricultural waste, which is corn cob, impregnated with phosphoric acid and investigate its potential application in sugar liquor decolorization. Particularly this study aimed to: 1. examine the physical and chemical properties of corn cob-based activated carbon (CCAC) produced; 2. determine the capability of activated carbon produced in the removal of sugar syrup colorants through adsorption; 3. evaluate its decolorization efficiency relative to that of commercial GAC; and 4. select the most efficient activated carbon produced in decolorizing sugar syrup.

1.4 Significance of the Study Commercial GAC used in sugar decolorization is expensive and is derived from bituminous coal which is a non-renewable resource. The long term availability of coal, environmental impacts of coal mining and potentially increasing cost have encouraged researchers to find alternatives, which may be effective and equally potential. This study may contribute to the energy industry by lessening the consumption of this diminishing commodity, and to the chemical industry by providing potentially cheap alternative to existing commercial adsorbent.
Corn cob, an agricultural waste product of corn, is readily available, abundant, biodegradable and of low cost. Conversion of corn cobs into carbonaceous adsorbent would add value to this agricultural commodity, thereby increasing the profits of farmers. This may also minimize environmental problems by reducing wastes and lessening the cost of waste disposal. So the use of corn cob as activated carbon will not only reduce the cost of sugar decolorization and other processes utilizing activated carbon but will also be of great help to different industries.

1.5 Scope and Delimitation This study focused on the conversion of corn cobs to granular activated carbon through chemical activation method. This work also focused on selecting the most efficient decolorizer among the activated carbon produced at different activating temperature and impregnation ratio. In this research, the color content of the clear liquor with sixty-degree Brix (60°Bx) was measured before and after the decolorization process using a digital single beam photometer. The determination of the composition of color removed, the amount of syrup recovered, and the pH of sugar liquor before and after decolorization was not included in the study. Using computational mathematics, the decolorization efficiency of the produced GAC was obtained. This study did not include the regeneration of activated carbon for further use.

1.6 Time and Locale of the Study All experiments were conducted in the Feed Laboratory of Department of Agriculture (DA) and in Cagayan State University Laboratory - Carig Campus, Tuguegarao City from November 2012 - February 2013. The testing and analysis of the results were also conducted at the Department of Agriculture and some tests were also done at the Laboratory of the Department of Science and Technology (DOST) Region 02 in Tuguegarao City, Cagayan.

1.7 Definition of Terms
Activated carbon is a porous highly adsorptive form of carbon used to adsorb color or impurities.
Activating agent is the chemical being used to improve the porous structure of the corn cobs.
Activation is a process that creates or increases porosity on the activated carbon surface.
Adsorption is the adhesion of sugar colorants to the surface of granular activated carbon.
Clear liquor is the sugar syrup coming from the filtration stage of sugar processing which is being subjected to decolorization.
Colorants are impurities found in sugar syrup that are removed in the sugar refineries.
Corn cob is the central core of a corn which was prepared as an activated carbon.
Decolorization is the removal of colored impurities found in sugar syrups through adsorption.
Decolorized liquor is the sugar syrup obtained after decolorization.
Degree Brix is the sucrose content of the sugar syrup. It is the percentage by weight of sucrose in the solution.
Efficiency is the measure of color removal capacity of the produced GAC relative to that of the commercial GAC.
Impregnation is the treatment of corn cobs with an activating agent.
Original Color is the color content of the sugar syrup before being decolorized.
Pyrolysis is the process in which treated corn cobs are subjected to heat in the absence of air.
Sugar syrup is the concentrated juice extracted from the stems of sugarcane plants.
Chapter II
REVIEW OF RELATED LITERATURE

2.1 Sugar Manufacturing Sugar manufacturing starts with the collection of mature canes followed by the removal of its leaves and the last mature joint. The stalk are thoroughly washed and cut. After cleaning, the cane is fed to a grinder. Hot water is sprayed on the sugarcane to dissolve any remaining hard sugar. The shredded pieces of sugarcane are passed through a series of heavy-duty rollers, which extract juice from the pulp. The pulp that remains, or the bagasse is dried and used as fuel and the raw juice undergoes clarification. During the clarification, milk of lime is added to the liquid sugar to precipitate out some impurities. The removal of the precipitates is done by passing the juice in a series of filters. After filtration, the syrup is put under a vacuum, where the juice boils at lower temperature and begins to evaporate to form thick syrup. Inside a sterilized vacuum pan, pulverized sugar is fed into the pan as the liquid evaporates, causing the formation of crystals. The sugar crystals are mixed with raw syrup to soften and remove the impurities. The crystals are then separated from the syrup and hosed with hot water in a centrifuge. This process is called affination. The washed sugar discharged from the centrifuge is dissolved in a pre-melter to form melted liquor. The melted liquor is pumped to the carbonator where carbon dioxide is used for bleaching treatment. To remove further the impurities the sugar liquor is passed through a first and second pressure filter thus producing clear liquor. The clear liquor is fed to a column containing activated carbon. The color-causing components are adsorbed by the carbon. After decolorization, the liquor is concentrated in an evaporator before crystallization.
2.1.1 Sugar Refinery Carbonator
Raw Sugar Sugar
Refined Sugar
MELTING
Melter
Melted Liquid Tank
Liquid and Lime Wheel
CLARIFICATION
CRYSTALLIZATION
Crystallizer
MINGLING
Hopper
Pre-mingler
Magma Mingler
Magma
Mixer
Affination Basket
Affination Screw Conveyor
EVAPORATION
Evaporator
Carbon Column
Decolorized Liquor
Primary clear Liquor Tank
Secondary Filtration
Secondary Clear Liquor Tank
DECOLORIZATION
Filter Supply Tank
FILTRATION
Primary Filtration

Figure 2.1 Flow chart of the sugar refining process 2.1.2 Sugar Decolorization
Decolorization has traditionally been accomplished with carbon adsorbents. Adsorption is the process by which fluid molecules are transferred to a solid surface by physical and/or chemical forces. In physical adsorption, the carbon’s surface holds molecules by weak forces known as Van Der Waals forces resulting from intermolecular attraction. The carbon and the adsorbate are unchanged chemically. Chemisorption, on the other hand, is the process in which molecules chemically react with the carbon’s surface and are held by much stronger forces - chemical bonds (Cameron Carbon Inc., 2006). The final purification step in the manufacturing of white sugar is decolorization. The primary objective of sugar refining is the removal of color in order to produce a pure and low color crystal (Cortes, 2007). Sugar decolorization is generally accomplished by passing clarified raw sugar liquors through vertical columns packed with activated carbon. In preventing the formation of color, the temperature and pH of the liquor are carefully controlled. To ensure optimal removal of colorants, the sugar concentration, liquid/carbon ratio, and contact time are monitored (Ahmedna et al., 2000).
According to Ahmad (2011), the mechanism by which sugar colorants are adsorbed onto a carbon surface may be divided into four consecutive steps: 1) dispersion, 2) inter-particle film diffusion, 3) intra-particle diffusion, and 4) adsorption onto surface sites. The diffusion of the color components is a function of the temperature and viscosity of the sugar solution and the molecular size of the colorants.
The filtered clarified cane sugar syrup, called clear liquor, has usually a concentration of 60 to 65 degree Brix and a typical color of 500 to 900 ICUMSA. The target color of the decolorized liquor is typically 100 to 400 ICUMSA as stated by Norit Activated Carbons (2012).

Figure 2.2 Flow chart of sugar decolorization process

2.1.2a Colorants in Cane Sugar
Sugar liquors and syrups processed in the refinery are colored by impurities. These impurities, termed as colorants, originate from two sources: the cane plant origin and factory-formed colorants. The colorants originated from cane plants such as Phenolic, Polyphenolic and Flavonoid colorants were originally attached to the plant cell walls. They are low molecular weight and feature aromatic ring structures. Melanoidins, caramels and alkaline degradations are factory formed colorants. These intensely colored compounds polymerize to form relatively high molecular weight colorants which are generally difficult to remove (Chou, 2000). As said by Ahmedna et al. (2000), there are also color precursors that do not exhibit color but when reacted with another non-colored compound they form colored impurities under favorable reaction conditions. Examples of these are amino acids, hydroxyl acids, aldehydes, iron, and reducing sugars.

2.1.2b Calgon Cane Cal Calgon Cane Cal is a virgin activated carbon designed for treatment of cane sugar liquors. In addition to its decolorization capability, Cane Cal also has pH controlling ability as a result of magnesite impregnation within the carbon granules. Cane Cal is used in both fixed and moving beds for continuous decolorization after which it can be regenerated for repeated use. The particle size of 12x40 mesh has been selected to give a high adsorption rate and low flow resistance with liquors of medium viscosity. Cane Cal is made from selected grades of bituminous coal combined with suitable binders to give suitable hardness and long life. It is produced under rigidly controlled conditions by high temperature steam activation. This carbon provides high surface area, large pore volume, high density, and a pore structure optimal for the adsorption of color bodies from solution (Calgon Carbon Corporation, 2004).

2.2 Activated Carbon Activated carbon is a highly adsorbing material widely used in various scopes depending on needs. It is used in many industries and applications such as wastewater treatment, in medicine, decolorization of sugar and so on. Its highly porous structure, which gives its high surface area, makes it a good adsorbent. The size of the pores determines what type of usage the AC is suitable for. According to Birbas (2011), anything that has a carbon content can be made to activated carbon, and depending on different aspects such as economy and characteristics of the material it might be suitable or not for manufacturing of AC. The removal of impurities from gases and liquids by activated carbon takes place by adsorption. Adsorption is a term, which describes the existence of a higher concentration of a substance at the interface between a fluid and a solid than is present in the fluid. Adsorption process can be considered as either physical adsorption or chemisorption (Cuhadar, 2005).

2.2.1 Activated Carbon Market Profile The market of activated carbon has been increasing constantly as a result of environmental issues, particularly in air purification, water treatment and food processing. Worldwide demand for activated carbon is forecast to rise 5.0 percent per year through 2010 to 1.2 million metric tons (Fredonia Group, 2006). This demand can be satisfied considering the large number of raw materials available for its production.

2.2.2 Types of Activated Carbon The types of activated carbon available in the market are powder, granular and pellet. It is classified according to its particle size and shape, and each type has its specific application. Granulated activated carbon (GAC) has a relatively large particle size and consequently, presents a smaller external surface. The size range is from 0.5 to 4.0 mm (Amri, 2008). Thus, diffusion of the adsorbate is an important factor. This carbon is therefore preferred for adsorption of gases and vapors as their rate of diffusion is faster. Granular activated carbon is used for water treatment, deodorization, and separation of components of flow system. Powdered activated carbon (PAC) has a relatively smaller particle size when compared to granular activated carbon and consequently, presents a large surface to volume ratio (Siemens, 2011). The size of powder activated carbon is less than 100µm with an average diameter between 15 and 25 µm (Amri, 2008). PAC is not commonly used in a dedicated vessel, owing to other process units, such as raw water intakes, rapid mix basins, clarifiers, and gravity filters (Songshan Activated Carbon Factory, 2012). Pellet activated carbon consists of extruded and cylindrical shaped activated carbon with diameters in the range of 4-7 mm and 8-15 mm. Pellet activated carbon is mainly used for gas phase applications because of their low pressure drop, high mechanical strength and low dust content (Amri, 2008).

2.2.3 Production of Granular Activated Carbon
Granular Activated Carbon (GAC) is produced from nearly all carbon-containing organic materials, mainly wood, sawdust, nutshells, fruit stones, peat, lignite, coal, petroleum coke, etc. The suitable precursor used mainly depends to its availability and cost, although it also depends on the main applications of the manufactured carbon and the type of installation available (Marsh et al., 2006).
Raw material Preparation
Activation
Washing and Drying
Activated Carbon
Figure 2.3 Block diagram of activated carbon production using a single step pyrolysis Basically, activated carbon can be prepared by single step pyrolysis or two-step pyrolysis. Single step pyrolysis is usually applied in the preparation of activated carbon using chemical activation method. However, the conventional preparation of activated carbon using physical activation method was based on two step pyrolysis where carbonization and activation process takes place separately (Amri, 2008). Figure 2.3 shows a block diagram for the production of activated carbon using single step pyrolysis and Figure 2.4, using two-step pyrolysis. Table 2.1 shows the summary of comparison for both procedures used in the preparation of activated carbon.
Activated Carbon
Washing
and
Drying
Activation
Carbonization
Raw material Preparation
Figure 2.4 Block diagram of activated carbon production using a two step pyrolysis

Table 2.1 Summary of comparison between the single and two-step pyrolysis Differences | Single Step Pyrolysis | Two-Step Pyrolysis | Production process | one stage | two stages | Energy consumption | low | high | Cost of production | cheap | expensive | Process duration | short | long | Yield | high | low | Surface area | modest | high | Porosity | modest | high |

2.2.4 Carbonization Carbonization is the process of heating the carbon in an anaerobic (oxygen-free) environment to break down the complex organic chemicals from which the material is made from, driving off almost everything but carbon and ash (Jenkins, 2010). Very dense carbonaceous material is used in the beginning, because the end result needs to be extra-porous for activated carbon purposes. Carbon-rich material is placed in a furnace and cooked at extreme temperatures topping 2000 degrees Celsius. What remains is usually 20-30 percent of the beginning weight, and consists of mostly carbon and a small percentage of inorganic ash.

2.2.5 Activation The activation process is responsible for increasing the surface area that ranges from 500 to 1500 m2/g and increasing the adsorption capacity of activated carbon. It allows the opening of enormous number of pores in the range of 1.2- to 20-nanometer-diameter for gas-adsorbent carbon or up to 100-nm-diameter for decolorizing carbons (Mcgraw-Hill Encyclopedia of Science and Technology, 2007). Careful control of the activation process allows some tailoring of pore size distribution to produce a range of granular carbons optimized for particular applications (Chou, 2000). Activation can be done by either physical or chemical activation. At typical color levels of the feed of 500 – 900 ICUMSA, the pore structure of the chemically activated carbon is usually most suitable. For decolorization of relatively light colored syrups, steam activated carbons perform well (Norit Activated Carbons, 2012).

2.2.5a Physical Activation In physical activation, carbon dioxide or steam is used as oxidizing agent. It is a conventional manufacturing process of activated carbon. The overall process consists of thermal pyrolysis at a relatively low temperature in the presence of nitrogen or helium, and activation with activating gas at higher temperature. The reaction between carbon atom and the oxidizing gas creates and develops the pore structure. During carbonization the opening of closed micropores and the enlargement of the opened micropores takes place. The disadvantage of this method is that, it gives lower carbon yield because large amount of carbon is eliminated to obtain well developed pore structure (Viswanathan et al, 2009).

2.2.5b Chemical Activation In chemical activation the precursor is impregnated with a given chemical agent and pyrolyzed after that. As a result of the pyrolysis process, a much richer carbon content material with a much more ordered structure is produced, and once the chemical agent is eliminated through washing, the porosity is highly developed. An important advantage of this kind of activation is that it can be done at lower temperature and it requires shorter time than physical activation. It also produces an activated carbon with high surface area and high carbon yield. The high carbon yield is due to the fact that activating agents used are substances with dehydrogenating properties that inhibit formation of tar and reduce the production of other volatile products. The degree of impregnation is an important factor in chemical activation. The effect of degree of impregnation on the porosity of the resulting product is apparent from the fact that the volume of salt in the carbonized material is equal to the volume of pores, which is freed by its extraction. A small increase in impregnation amount causes an increase in the total pore volume of the product and an increase in the volume of smaller pores. This is true for small degrees of impregnation but when the degree of impregnation is further increased, the volume of smallest pores decreases while the diameter of the larger pores increases (Cuhadar, 2005).
Chemical agents such as phosphoric acid, sulfuric acid, zinc chloride, potassium hydroxide, and other alkali metal compounds act as dehydrating and stabilizing agents that enhance the development of porous structure in the activated carbon (Muiet al., 2004). Phosphoric acid and zinc chloride are activating agents usually used for the activation of lignocellulosic materials which have not been previously carbonized; while alkali metal compounds, usually KOH, are used for activation of coal precursors or chars (Cuhadar, 2005).

2.3 Properties of Activated Carbon for Sugar Decolorization Physical properties, such as bulk density, hardness, surface area and pore size distribution, and chemical characteristics such as pH and ash of activated carbon determine its efficiency in removing sugar colorants (Ahmedna et al., 2000). There is an important relationship among them for their application and efficiency in sugar decolorization. However, activated carbon suppliers do not provide all of these properties. Their product specifications only include pH, bulk density, moisture content, hardness, ash content, and iodine number. Report of surface area and pore size distribution is not provided because of impracticality in its measurement since it is a very lengthy procedure (Cameron Carbon Inc., 2006).

2.3.1 Bulk Density Density is particularly important in sugar decolorization where viscous syrup is displaced through a column of activated carbon. Bulk density is important when carbon is removed by filtration because it determines how many pounds of carbons can be contained in a filter of a given solids capacity and how much treated liquid is retained by the filter cake. In addition, when two carbons differing in bulk density are used at the same weight per liter, the carbon having higher bulk density will be able to filter more liquor volume before the available cake space is filled. Carbons with an adequate density also help to improve the filtration rate by forming an even cake on the filter surface. The American Water Work Association has set a lower limit on bulk density at 0.25g/mL for GACs to be of practical use.

2.3.2 Hardness Hardness is a measure of the mechanical strength of the carbons and is an important parameter for understanding its relative loss during transportation, handling, and regeneration (Bansode, 2002). A carbon should possess sufficient mechanical strength to withstand the abrasion resulting from continued use. In the course of carbon usage, particle breakdown and dust formation occur due to the continuous mechanical friction between carbon particle and sugar liquor. Dust formed by attrition is undesirable because it slows down the filtration rate and decreases the amount of regenerated carbon. Therefore, carbons designed for sugar decolorization should have enough abrasion resistance to minimize attrition (Ahmedna et al., 2000).

2.3.3 Moisture Moisture is the amount of water physically bound on the activated carbon under normal condition. The practical limit for the level of moisture content allowed in the activated carbon varies within 3 to 6%. Moisture content of an activated carbon has no effect on its adsorptive power but it dilutes the carbon which causes to use additional weight of carbon during the treatment process (Baseri et al., 2012).

2.3.4 Porosity Porosity is the main factor for increasing the adsorptive power of an activated carbon. Porosity is related to the bulk density and specific gravity of activated carbon (Baseri et al., 2012). It is defined by the volume of the pores of the carbon. The high porous structure of activated carbon provides a very large surface area for adsorption (I-Chem Solution, 2008). 2.3.5 Surface Area Activated carbon has the highest adsorptive porosity of any material known. Because of its large surface area (1 quart of granules = 6 football fields of area), activated carbon has a great ability to adsorb organic and inorganic molecules from liquids or vapors. Surface area is one of the most important characteristics of activated carbon designed for adsorption of compounds from liquid media such as sugar liquor. Large surface area is generally a requirement for a good adsorbent. However, the total surface area has to possess adequate pore size distribution and surface chemistry to adsorb the targeted species (Ahmedna et al., 2000).

2.3.6 Pore Size Distribution The large internal surface area of activated carbon is due to its porosity. The total porous structure of an activated carbon is formed by a wide range of pore sizes. For practical reasons, pore sizes are classified into three main types according to their width: macropores (> 50 nm), mesopores (2-50 nm), and micropores (< 2 nm). The macropores act as “tunnels” that enable molecules to reach the smaller pores in the interior of the carbon where they are adsorbed or bonded to the carbon surface. Macropores do not significantly contribute to the overall adsorptive process since they have a relatively low surface area, but they affect the rate of admission of the molecules to the meso- and micropores. Mesopores, which branch from the macropores, serve as passages by which molecules reach the smaller micropores. The micropores constitute the largest part of the internal surface area of an activated carbon and, consequently, most of the adsorption takes place there. The suitability of an activated carbon for a particular application (e.g., sugar decolorization) depends on the macropore:mesopore:micropore ratio. A carbon with substantial mesoporisity is generally recommended for adsorption of sugar colorants, which are made up of mixtures of compounds with varying molecular size (Ahmedna et al., 2000).

2.3.7 pH Activated carbon pH may influence color by changing the pH of the sugar solution. Such a change affects the pH-sensitive fraction of solution colorants, causing unreliable color measurements (Ahmedna et al., 2000). Moreover, acid carbons, for example, may be a better decolorizer; but a sugar refiner would seldom employ a highly acidic carbon because the acid would cause inversion of sucrose to noncrystallizable sugars, with subsequent lower yield. It was reported that in sugar decolorization, a distinctly acidic activated carbon may cause inversion of sucrose, and a distinctly alkaline carbon may cause color development through alkaline degradation of organic impurities. Hence, a carbon pH of 6-8 is acceptable for most applications (Ahmedna et al., 2000).

2.3.8 Ash Ash content of carbon is the residue that remains when the carbonaceous portion is burned off. The ash consists mainly of minerals such as silica, aluminum, iron, magnesium, and calcium. Ash in activated carbon is not desirable and is considered an impurity. Ash leached into sugar liquor during the process of decolorization is known to cause uneven distribution of heat in the boiler during sugar crystallization. Ash may also interfere with carbon adsorption through competitive adsorption and catalysis of adverse reactions. For instance, the ash content may affect the pH of the carbon since the pH of most commercial carbons is produced by their inorganic components. Usually, materials with the lowest ash content produce the most active products (Ahmedna et al., 2000). 2.3.9 Iodine Number Iodine number is the most fundamental parameter used to characterize activated carbon performance. It is a measure of activity level of carbon. The higher the iodine number, the higher the degree of activation. Typically, the iodine number ranges from 500 to 1200 mg/g. It is equivalent to surface area of carbon between 900 m²/g and 1100 m²/g (Pradhani, 2011). The iodine number or iodine value is an indicator of micro-porosity. It is the measure of the ability of activated carbon to adsorb small molecules. Iodine is notable for being one of the few inorganic chemicals that is readily adsorbed by activated carbon, and the iodine number is the mass of iodine adsorbed by one gram of activated carbon (Jenkins, 2010). According to Marsh et al. (2006), it gives the indication of internal surface area of carbon in a simple and quick test. In many activated carbon, iodine number is closed to Brunauer-Emmett-Teller (BET) surface area.

2.4 Corn Cob
Corn cob is an agricultural by-product generated after corn processing. This waste product has become important and new uses have been developed such as activated carbon, biofuels or as adsorbent for removing some impurities (Suteu et al., 2010).
Zych (2008), mentioned that corn cobs contain 32.3% to 45.6% cellulose, 39.8% hemicelluloses mostly composed of pentosan, and 6.7% to 13.9% lignin. Cellulose is a polysaccharide of glucose units that serve as the main structural component of the cob’s cell walls.

2.4.1 Corn Cob as Activated Carbon
Studies show that corn cob was found to be a good precursor for the preparation of activated carbon by zinc chloride activation owing to its high carbon (45.21%) and low ash (0.91%) contents. The resulting activated carbons are essentially microporous materials. Corn cobs are ready source of charcoal that may be activated and can be used to remove textile effluents. It could be fruitfully used as biosorbent for removal of textile reactive dyes. The thermodynamic parameters suggest that the mechanism of reactive dye sorption onto corn cob is a combination of electrostatic interactions and physical sorption (Suteu et al., 2010).

2.5 Spectrophotometer A spectrophotometer is an instrument which is used to measure the intensity of electromagnetic radiation at different wavelengths. It is generally used for the measurement of transmittance or reflectance of solutions, transparent or opaque solids such as polished gases or glass. Spectrometer consists of light source, diffraction grating, filter, photo detector, signal processor and display. The light source provides all the wavelength of visible light and the wavelengths in ultraviolet and infrared range. The filter and diffraction grating separate the light into its component wavelengths so that very small range of wavelength can be directed through the sample. The sample compartment permits the entry of no stray light while allowing the passage of the light from the source. The photo detector converts the amount of light which it had received into a current which is then sent to the signal processor which is the soul of the machine. The signal processor converts the simple current it receives into absorbance, transmittance and concentration values which are then sent to the display (Innovateus Inc., 2011). A digital single beam photometer is a kind of ultraviolet-visible spectrophotometer designed primarily for the determination of liquid color. Sugar industries use this device for the color measurement of liquid sugar (Schmidt-Haensch, 2008).

2.6 Theoretical Framework
Two-Step Pyrolysis
Raw material preparation

Activation
(Physical/Chemical)
400 – 1000 °C
Washing and Drying
Activated Carbon
Carbonization
(Inert atmosphere)
300 – 800 °C
Single Step Pyrolysis
Raw material preparation
Activation
(Physical/Chemical)
400 – 1000 °C
Washing and Drying
Activated Carbon

Figure 2.5 Preparation of activated carbon (Din, 2005; Amri, 2008)

Activated Carbon

Characterization

Utilization

Figure 2.6 Characterization and utilization of activated carbon (Bansode et al., 2004; Qureshi et al., 2008; Ahmedna et al., 2000) The preparation of raw material includes washing, drying, crushing and sieving. The raw materials were washed with distilled water to remove dirt and residues and sun dried for 24 hours. The dried precursors were crushed using a mortar and pestle, ground with a laboratory miller, and then sieved using a sieve plate (Foo et al., 2010; Diya’uddeen et al., 2008). According to Amri (2008), activated carbons can be prepared by two different methods – single step pyrolysis and two step pyrolysis. Ahmad et al. (2011) used two-step pyrolysis where carbonization was done before chemical activation. Carbonization step was carried out at 700°C for 2 hours under purified nitrogen flow of 150 mL/min. The char produced was mixed with Na2CO3 with different impregnation ratios. Other studies used activating agents such as KOH (Diya’uddeen et al., 2008), K2CO3 (Tsai et al., 2000) and other alkaline metal compounds for activation of coal precursors or chars. Single step pyrolysis using chemical activation method was followed by Foo et al. (2010) where H3PO4 was used as an activating agent. Other activating agents such as ZnCl2 (Jabit, 2007) and H2SO4 (Taimur et al., 2011) were used for the activation of lignocellulosic materials which have not been previously carbonized. The activation proper can be carried out by pyrolysis at 400 - 1000°C (Amri, 2008). Obtained carbons were characterized by determining carbon yield, ash content, slurry pH, textural properties and capacity to remove color bodies from factory-grade sugar liquor (Abdullah et al., 2010; Ahmedna et al., 2000). Other applications of activated carbon include wastewater treatment (Bansode, 2004), citric acid refining (Sun et al., 2009), treatment of landfill leachate (Collin et al., 2006), cyanide removal (Jabit, 2007), and dye removal from aqueous solutions (Suteu et al., 2010).
2.7 Conceptual Framework Calgon Cane Cal
Activated Carbon
Preparation of
Sugar Syrup
Corn Cob
Activated Carbon
Sugar
Decolorization
Preparation of
Corn Cobs
Sugar
Decolorization
Analysis of Results
% Color Removal
% Relative Efficiency
Analysis of Variance
Activation at
Different Conditions
Impregnation Ratio
(1:1/2:1/3:1) and Activation Temperature (400/500/600°C)
Characterization
Characterization

Figure 2.7 Conceptual framework of the study Based on the studies mentioned in the previous section, the researchers came up with a method in producing granular activated carbon from corn cobs. In the present study, single step pyrolysis using chemical activation method was applied, following the procedure of Foo et al. (2010). Different activation conditions were applied by varying the activation temperature and impregnation ratio. The characterization of the corn cob-based activated carbon was done using the procedures by Bansode et al. (2004). The data collected were plotted in bar graphs and were analyzed. The conceptual framework of the present study proceeds according to that shown in Figure 2.7. The figure illustrates that activated carbons synthesized from corn cobs and sugar syrup of a defined sugar concentration are used as inputs. Under the decolorization process, the effect of the adsorbent on the adsorption of color was analyzed.

Chapter III
METHODOLOGY

3.1 Materials and Equipment The materials used in the preparation of activated carbon are corn cobs, sieve plate (5, 10, 12, and 40 mesh), aluminium trays, stirrers, desiccators, crucibles, beakers, graduated cylinders, Erlenmeyer flasks, cheese cloth, filter paper and funnel. The chemicals used are 85% w/w phosphoric acid (H3PO4), 0.1 N sodium hydroxide (NaOH), and distilled water. The equipment used are electronic balance, oven driers, furnace, and hot plate.

3.2 Preparation of Corn Cob Activated Carbon (CCAC) Corn cobs were collected from the local farmers of Iguig, Cagayan. The preparation of CCAC was based on the procedure of Foo and Lee (2010) using Parkia speciosa pods as precursor. The corn cobs were dried, crushed and sieved using 5-10 mesh sieve plate (average particle size of 2 mm to 4 mm). The sieved samples were impregnated with 85% (w/w) H3PO4 prepared at different ratios (1:1, 2:1, 3:1). Impregnation was done by heating the sample in a hot plate at 85°C for 2 hours. The impregnated samples were oven dried at 105°C for 8 hours. After the impregnation, the samples were activated at different temperatures (400, 500, 600°C) for 2 hours. The produced activated carbon samples were subsequently cooled and allowed to undergo a series of washing with hot water and 0.1N NaOH. The samples were dried overnight in an oven at 105°C and cooled at room temperature. The GACs were sieved using 12-40 mesh (approximately of size 380 μm to 1.14 mm) and stored for its further use.

Table 3.1 Corn cobs activated at different temperatures and impregnation ratio

CCAC No. | Activation Temperature (°C) | Impregnation Ratio( acid : precursor ) | Weight of Corn Cobs (g) | Weight of Acid(g) | 1 | 400 | 1:1 | 100 | 100 | 2 | 500 | 1:1 | 100 | 100 | 3 | 600 | 1:1 | 100 | 100 | 4 | 400 | 2:1 | 100 | 200 | 5 | 500 | 2:1 | 100 | 200 | 6 | 600 | 2:1 | 100 | 200 | 7 | 400 | 3:1 | 100 | 300 | 8 | 500 | 3:1 | 100 | 300 | 9 | 600 | 3:1 | 100 | 300 |
Collection of Corn Cobs
Air drying, crushing, sieving
Impregnation (3:1)

Impregnation (1:1)
Impregnation (2:1)

Oven Drying

Oven Drying
Oven Drying

CCAC 1
CCAC 2
CCAC 3
Activation
Activation
400°C
500°C
600°C
Washing

400°C
500°C
600°C
Washing

Drying

Drying

Drying

Activation
400°C
500°C
600°C
Washing

CCAC 4
CCAC 5
CCAC 6
CCAC 7
CCAC 8
CCAC 9

Figure 3.1 Flowchart diagram for the preparation of Granular Activated Carbon

3.3 Carbon Analysis The physical and chemical properties such as bulk density, hardness, porosity, iodine number, moisture, pH and ash were analyzed. The commercial GAC, Calgon Cane Cal, was used as a reference in order to judge the characteristics of the GACs produced for use in sugar decolorization. 3.4 Experimental Procedure The testing of the color removal capacity of the produced activated carbon was done adapting the procedure used by Cagayan Robina Sugar Manufacturing Corporation (CARSUMCO). There were ten (10) set-ups: nine for the different CCACs produced and one for the Calgon Cane Cal as the control. Each set-up had three (3) replicates. 3.4.2 Preparation of Sugar Solution A 60°Bx sugar solution was made by dissolving 750 g of raw sugar in 500 g of water. The solution was filtered and the degree brix and percent transmittance of it was determined. The color of the solution was calculated and recorded as the original color. 3.4.3 Liquor Decolorization Ten set-ups with three replicates each were used in the study. Following the procedure provided by CARSUMCO, a 50% w/v suspension of activated carbon and sugar syrup was made. Fifteen grams (15 g) of activated carbon was placed in a beaker for each set-up. Thirty milliliters (30 mL) of sugar syrup were poured in each of the set-ups. The suspension was heated on a water bath at 80°C for 3 hours. While hot, it was filtered and the decolorized liquor was collected and analyzed. Each set-up was subjected to three replicates.

Figure 3.2 Decolorization set-ups in water bath

3.5 Experimental Analysis 3.5.1 Carbon Yield Carbon yield is the amount of activated carbon produced per amount of precursor used. It is calculated by

where Wc and Wp are the dry weight of the carbon and precursor, respectively. 3.5.2PercentColor Removal The color content before and after decolorization was measured using a digital single beam photometer. The percentage color removal was calculated by

where Co and Cf are the color content of the sugar liquor before and after the treatment, respectively.

3.5.3 Percent Relative Efficiency The percent relative efficiency was calculated by:

where Cc and Cs are the color removed by the control and the sample, respectively.

3.6 Statistical Analysis Analysis of variance with a 95% confidence level (α = 0.05) was done to determine the significant difference between the color content of the sugar syrup decolorized by the commercial and experimental carbons.

Chapter IV
RESULTS AND DISCUSSION

Activated carbon production from corn cobs has been achieved by the chemical activation technique using H3PO4 as activating agent. By changing carbonization temperature and impregnation ratio, nine activated carbon products were produced. One of the major objectives of this study was to investigate the physical and chemical properties of activated carbon produced from corn cobs at varying temperatures (400, 500, and 600°C) and impregnation ratio (1:1, 2:1, and 3:1). All procedures in determining the characteristics of the products were provided in Appendix B. Prior to determination of each property, the activated carbon samples were subjected to standard oven drying.

5.1 Carbon Yield
Product yield is an important measure of the feasibility of preparing activated carbon from a given precursor. Based on past studies, significant product yield differences can be observed depending on the precursor. Temperature and acid to precursor ratio used during the impregnation stage are also factors that affect the carbon yield.
In the present study, the temperature increase caused a decrease in carbon yield as seen on the values of the first three carbons with an impregnation ratio of 1:1 (CCACs 1, 2 and 3). The same is true for the carbons with an impregnation ratio of 2:1 (CCACs 4, 5, and 6) and 3:1 (CCACs 7, 8, and 9). This is due to the fact that as temperature increases, the degree of pyrolysis increases and more of the non-carbonaceous volatile materials are removed from the rest of the char.

Table 4.1 Carbon yield of corn cob activated carbons CCAC Sample | Yield (%) | 1 | 65.83 | 2 | 53.76 | 3 | 47.60 | 4 | 77.97 | 5 | 63.10 | 6 | 52.16 | 7 | 80.34 | 8 | 68.80 | 9 | 53.10 |

Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.1a Bar graph of the carbon yield of corn cob activated carbons

Figure 4.1b Effect of activation temperature and impregnation ratio on carbon yield

5.2 Chemical Analysis of the Product 4.2.1 pH The pH of each of the nine activated carbon products was measured and the values are given in Table 4.2. As it is seen in the table, all activated carbon samples recorded a pH in the range of 6 to 8. As stated in Chapter II Section 2.3.7, carbons with a pH range of 6 to 8 are most desirable for most applications. Therefore all nine activated carbon samples could be acceptable in terms of their pH values. CCAC1 recorded the least amount of pH with 6.03 while CCAC9 recorded the most with 7.93.

Table 4.2 pH of CCACs and CCAL Carbon Sample | pH | CCAC1 | 6.03 | CCAC2 | 6.47 | CCAC3 | 7.10 | CCAC4 | 6.37 | CCAC5 | 6.50 | CCAC6 | 7.17 | CCAC7 | 7.57 | CCAC8 | 6.77 | CCAC9 | 7.93 | CCAL | 7.80 | Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.2 Bar graph of the pH of CCACs and CCAL

4.2.2 Ash Content A good activated carbon must have low ash content. A small increase in ash content causes a decrease in adsorptive properties of activated carbon. However, the ash content of the samples is slightly higher than typical values. For CCAC1, CCAC2 and CCAC3, the values are 9.33%, 7.33% and 14.0%, respectively. Based on the data gathered, the ash content of the samples increases as the activation temperature increases. CCAC4, CCAC5 and CCAC6 also show the same trend with 9.00%, 10.50% and 11.33% ash content, respectively. The results were also affected by the impregnation ratio. Depolymerization reactions between the volatile materials and H3PO4 during the activation were affected. Although H3PO4 restricts the formation of tar, high impregnation ratio increases the formation of tar; hence, it is expected that as tar formation increases ash content of the samples increases (Yağşi, 2004). Table 4.3 Ash content of CCACs and CCAL Carbon Sample | Ash (%) | CCAC1 | 9.33 | CCAC2 | 7.33 | CCAC3 | 14.00 | CCAC4 | 9.00 | CCAC5 | 10.50 | CCAC6 | 11.33 | CCAC7 | 16.50 | CCAC8 | 15.17 | CCAC9 | 17.17 | CCAL | 6.20 | Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.3 Bar graph of the ash content of CCACs and CCAL 4.3 Physical Characterization of the Products
4.3.1 Bulk Density Bulk density of activated carbon is important in sugar decolorization. The higher the density, the better the filterability of activated carbons. Bulk density of 0.5 g/cm3 is adequate for decolorization of sugar (Ahmedna et al., 2000). From Table 4.4, the bulk densities of all the carbons produced were above the lower limit of 0.25 g/cm3 set by American Water Works Association (AWWA). The bulk densities of CCAC1, CCAC2 and CCAC3 were lower than the other carbon produced. The six carbons recorded bulk density values closer to the desired value which is 0.5. The data shows that as the impregnation ratio is increased, the bulk density of the sample also increases. This is because of the high density of the acid.

Table 4.4 Bulk density of CCACs and CCAL Carbon Sample | Bulk Density (g/mL) | CCAC1 | 0.375 | CCAC2 | 0.347 | CCAC3 | 0.299 | CCAC4 | 0.512 | CCAC5 | 0.453 | CCAC6 | 0.499 | CCAC7 | 0.585 | CCAC8 | 0.562 | CCAC9 | 0.452 | CCAL | 0.483 | Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.4 Bar graph of the bulk density of CCACs and CCAL

4.3.2 Moisture Each of the nine activated carbons produced recorded a moisture content ranging from 4.71-10.09%. CCAC4 recorded the least while CCAC1 recorded the highest moisture content. It should be noted that when exposed to air, activated carbons are capable of adsorbing moisture from the atmosphere until equilibrium moisture content is achieved. This normally could lead to high moisture content. Table 4.5 Moisture content of CCACs and CCAL Carbon Sample | Moisture (%) | CCAC1 | 10.09 | CCAC2 | 7.18 | CCAC3 | 5.33 | CCAC4 | 4.71 | CCAC5 | 8.06 | CCAC6 | 7.52 | CCAC7 | 5.06 | CCAC8 | 4.97 | CCAC9 | 6.53 | CCAL | 3.77 | Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.5 Bar graph of the moisture content of CCACs and CCAL 4.3.3 Hardness The percent attrition of each activated carbon was tested to measure the hardness of each sample. High percent attrition means low hardness. Table 4.6 shows the percent attrition values of each carbon. From CCAC1 to CCAC3, it is observed that as the activation temperature increases, attrition increases. This is an indication that the carbons produced become softer. This is also true for the values recorded from CCAC4 to CCAC6 and from CCAC7 to CCAC 9. Another observation is that as the impregnation ratio is increased, the attrition values were decreased, indicating that the carbons became harder. It can be generalized that the degree of impregnation and activation temperature has a great effect in the hardness of activated carbon.

Table 4.6 Percentage attrition of CCACs and CCAL Carbon Sample | Attrition (%) | CCAC1 | 45.67 | CCAC2 | 66.67 | CCAC3 | 79.33 | CCAC4 | 36.33 | CCAC5 | 46.00 | CCAC6 | 47.33 | CCAC7 | 25.67 | CCAC8 | 45.33 | CCAC9 | 57.67 | CCAL | 11.30 |

Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.6 Bar graph of the percent attrition of CCACs and CCAL

4.3.4 Porosity The porosity of each of the chemically activated carbons is shown in Table 4.7. As it is seen, the activation temperature and the impregnation ratio dramatically affected the development of porosity of each sample. Based on the data gathered from CCAC1 to CCAC3, highest value is observed in CCAC3, followed by CCAC2 and CCAC1. This observation revealed that an increase in activation temperature from 400°C to 600°C caused some of the pores to become more developed. However, the intensive action in generating porosity with increasing temperature is not correspondingly related with the increase of the amount of impregnant. In 2010, Foo et al. obtained values of total pore volume of activated carbon prepared at 450 to 650°C. Figure 4.8 shows the effect of temperature on the development of total pore volume of activated carbon produced by Foo et al. The AC impregnated with 2:1 ratio shows a slight decrease in pore volume when the temperature is increased from 450 to 550°C. This indicates that effect of temperature on the porosity of carbon is not always the same with different impregnation ratios. There is no definite trend observed.
Table 4.7 Porosity of CCACs and CCAL Carbon Sample | Porosity (%) | CCAC1 | 60.33 | CCAC2 | 66.00 | CCAC3 | 75.00 | CCAC4 | 76.50 | CCAC5 | 68.67 | CCAC6 | 68.33 | CCAC7 | 68.00 | CCAC8 | 76.00 | CCAC9 | 79.33 | CCAL | 88.55 |

Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.7 Bar graph of porosity of CCACs and CCAL

Figure 4.8 Effect of temperature on total pore volume of activated carbon (Foo et al., 2010)

Girgis et al. (2001) also obtained values of total pore volume and mesopore volume of carbons activated at different temperatures and impregnation ratios. Figure 4.9 (a) and (c) show the results of total pore volume and mesopore volume of activated carbons produced by Girgis et al., respectively. Different trends were also observed in the bar graph in Figure 4.9 (b) and (d). Beyond a certain carbonization temperature, the surface area and pore volume decreases due to excessive carbon burn-off. This leads to the widening of pores and destruction of some walls between the pores and hence, there is a reduction in porosity. Similar results have been reported by other researchers. As a general rule, it can be said that the increase of the pyrolysis temperature will lead to an increase in the porosity, but its relationship with the impregnation ratio must be greatly considered.

Figure 4.9 Effect of temperature on total pore volume and mesopore volume of activated carbon (Girgis et al., 2001)

4.4 Iodine Number The iodine number is the amount of iodine, in milligrams, adsorbed per gram of carbon. It has been established that the iodine number in mg/g gives an estimate of the surface area in m2/g, and measures the porosity for pores with dimensions between 1.0 - 1.5nm (Collin et al., 2006). The removal of iodine by the activated carbon is related to their porosity characteristics which determine the degree of accessibility of these molecules. Figure 4.10 shows the iodine number of each of the chemically activated carbon produced.

Table 4.8 Iodine number of CCACs and CCAL Carbon Sample | Iodine Number (mg/g) | CCAC1 | 589.803 | CCAC2 | 735.01 | CCAC3 | 705.223 | CCAC4 | 740.597 | CCAC5 | 613.07 | CCAC6 | 716.393 | CCAC7 | 779.687 | CCAC8 | 676.367 | CCAC9 | 747.11 | CCAL | 1020.21 |

Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.10 Bar graph of the iodine number of CCACs and CCAL Different trends were observed because of the different responses of the CCACs to the combination of temperature and impregnation ratio. This can be associated with the pore structure of each sample. As stated, higher impregnation ratio has an effect with the surface characteristics of the produced carbon; high acid content may form an insulating layer covering the particles, thus hindering the adsorptive capabilities of the carbon. Activated carbon recommended for sugar decolorization must have iodine values ranging from 500 to 1100 mg/g according to AWWA. In 2011, Birbas found out that iodine adsorption capacity of activated carbons behave differently at different impregnation ratios as temperature increases. Figure 4.11 shows the results acquired by Birbas.

Figure 4.11 Iodine number values of activated carbon (Birbas, 2011)

4.5 Sugar Decolorization The produced activated carbons were assessed for their effectiveness in sugar decolorization. The amount of colorants that can be removed from a solution by activated carbon depends on factors such as contact time, carbon dosage, temperature, concentration or viscosity of the solution and the intrinsic features of the carbon itself. These factors were controlled in order to directly compare the decolorization efficiencies of the chemically activated carbons and the reference carbon. Following the procedures used by CARSUMCO, a contact time of 3 hours, carbon dosage of 50% w/v, and temperature of 80°C were utilized in the study. Table 4.9 shows the color content of the clear liquor (recorded as original color), the color of the syrup decolorized by the corn cobs activated carbon, and the syrup decolorized by the reference carbon.

Table 4.9 Color content of the decolorized liquor and the original liquor

Syrup | Color (IU) | CCAC1 | 820.62 | CCAC2 | 762.94 | CCAC3 | 595.88 | CCAC4 | 408.97 | CCAC5 | 448.00 | CCAC6 | 310.33 | CCAC7 | 630.16 | CCAC8 | 585.34 | CCAC9 | 509.78 | CCAL | 294.95 | Untreated | 985.54 |

Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.12 Bar graph of the color content of the decolorized and original liquor
Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.13 Bar graph of the percent color removal of CCACs and CCAL

Figure 4.13 shows the percent color removal of the activated carbon samples and the reference carbon. Carbon samples impregnated with 1:1 acid to precursor ratio exhibited low percent color removal as compared to the activated carbon produced on higher impregnation ratios. It is also observed that as the activation temperature is increased, the color uptake of each carbon increases. However, this is not true in the case for the activated carbons produced in 2:1 impregnation ratio. This may be because the increase in temperature from 400 - 500°C has a minimal effect on the color removal capacity of activated carbon impregnated at 2:1 ratio. According to Abdullah et al. (2010), raising the activation temperature (Figure 4.14) seems to inflict very small promotion in % color removal, especially at lower impregnation ratios. In the study conducted by Qureshi et al. (2008), it was observed that different color removal capacities were obtained from carbons prepared from sugarcane bagasse activated at different temperatures. The results were shown in Figure 4.15.

Figure 4.14 Percent color removal of activated carbons prepared at different conditions (Abdullah et al., 2010)

Activation Temperature (°C)
700
750
760
780
800
750
REF
900

Figure 4.15 Percent color removal of carbons activated at increasing temperature (Qureshi et al., 2008)
Ratio 1:1
Ratio 2:1
Ratio 3:1

Figure 4.16 Efficiency of CCACs relative to CCAL Figure 4.16 shows the relative efficiencies of the produced corn cob activated carbon with respect to the reference carbon, Calgon Cane Cal. The percent relative efficiencies were based on the color removed by Calgon Cane Cal which had the highest value. It is observed that CCAC1 had the lowest percentage relative efficiency with only 23.88% while CCAC6 had the highest with 97.77%. The data gathered for the chemical and physical properties of CCAC6 was satisfactory enough to support its decolorizing efficiency.

4.6 Summary of Results The results of the properties and color removal efficiency of CCACs and CCAL discussed in the previous section were summarized in Table 4.10 and Table 4.11, respectively. Table 4.10 Summary of the properties of CCACs and CCAL Carbon Sample | pH | Ash (%) | Bulk Density (g/mL) | Attrition (%) | Moisture (%) | Porosity (%) | Iodine Number (mg/g) | CCAC1 | 6.03 | 9.33 | 0.375 | 45.67 | 10.09 | 60.33 | 589.80 | CCAC2 | 6.47 | 7.33 | 0.347 | 66.67 | 7.18 | 66.00 | 735.01 | CCAC3 | 7.10 | 14.00 | 0.299 | 79.33 | 5.33 | 75.00 | 705.22 | CCAC4 | 6.37 | 9.00 | 0.512 | 36.33 | 4.71 | 76.50 | 740.60 | CCAC5 | 6.50 | 10.50 | 0.453 | 46.00 | 8.06 | 68.67 | 613.07 | CCAC6 | 7.17 | 11.33 | 0.499 | 47.33 | 7.52 | 68.33 | 716.39 | CCAC7 | 7.57 | 16.50 | 0.585 | 25.67 | 5.06 | 68.00 | 779.69 | CCAC8 | 6.77 | 15.17 | 0.562 | 45.33 | 4.97 | 76.00 | 676.37 | CCAC9 | 7.93 | 17.17 | 0.452 | 57.67 | 6.53 | 79.33 | 747.11 | CCAL | 7.80 | 6.20 | 0.483 | 11.30 | 3.77 | 88.55 | 1020.21 | Table 4.11 Summary of the percent color removal and percent relative efficiency Carbon Sample | Color Removal (%) | Relative Efficiency (%) | CCAC1 | 589.80 | 23.88 | CCAC2 | 735.01 | 32.23 | CCAC3 | 705.22 | 56.42 | CCAC4 | 740.60 | 83.49 | CCAC5 | 613.07 | 77.84 | CCAC6 | 716.39 | 97.77 | CCAC7 | 779.69 | 51.46 | CCAC8 | 676.37 | 57.95 | CCAC9 | 747.11 | 68.89 | CCAL | 1020.21 | - |
Chapter V
Conclusion and Recommendation

5.1 Conclusion It is clearly demonstrated that activated carbons having high adsorptive capacities can be prepared from corn cobs by chemical activation with H3PO4. Corn cobs, among the lignocellulosic renewable materials, can be considered as competitive precursor in the preparation of microporous activated carbons. The activation temperature and impregnation ratio has greatly affected each individual property of the produced activated carbon. Activated carbon prepared at 600°C and 2:1 acid to precursor ratio recorded the highest decolorizing efficiency. Its adsorptive power nearly matched the commercial activated carbon. From the overall results, it is clearly shown that the activated carbons from corn cobs by H3PO4 can be produced for sugar decolorization by tailoring each chemical and physical property with appropriate adjustments of temperature and impregnation ratio.

5.2 Recommendation This study initially evaluated the possibility of using Corn Cob Activated Carbon as sugar liquor decolorizer. The determination of percent color removal of the produced GAC were done for confirmation. Further studies can be made related to this considering the following: 1. variations in activation time 2. use of other precursor 3. use of other activating agents 4. comparison with other commercial activated carbons 5. addition of binder for harder carbon 6. inclusion of the regeneration process

Appendices

Appendix A 1. US Standard Sieve Size US Sieve Size | Opening Size | 3.5 | 5.60 mm | 4 | 4.75 mm | 5 | 4.00 mm | 6 | 3.35 mm | 7 | 2.80 mm | 8 | 2.36 mm | 10 | 2.00 mm | 12 | 1.70 mm | 14 | 1.40 mm | 16 | 1.18 mm | 18 | 1.00 mm | 20 | 850µm | 25 | 710 µm | 30 | 600 µm | 35 | 500 µm | 40 | 425 µm | 45 | 355 µm | 50 | 300 µm | 60 | 250 µm | 70 | 212 µm | 80 | 180 µm | 100 | 150 µm | 120 | 125 µm | 140 | 106 µm | 170 | 90 µm | 200 | 75 µm |

Appendix B 1. Measurement of Physical and Chemical Properties of Activated Carbon All properties were determined following the procedure of Bansode et al. (2004).

a. Bulk Density
Materials:
* 25 mL cylinder * Oven * Weighing scale
Procedure:
1. Dry the granular activated carbon in an oven at 80°C overnight. 2. Fill a 25 mL cylinder with dried GAC. 3. Tap the cylinder for at least 1–2 min to compact the carbon. 4. Weigh. Calculation:

b. Hardness
Materials:

* 100 mL acetate buffer * 150 mL beaker * 250 ml of de-ionized water * Desiccator * 50 mesh screen * Weighing dish * Magnetic stirrer

Procedure: 1. Add 1 g of GAC to 100 mL of acetate buffer (0.07M sodium acetate, NaC2H3O2 and 0.03 M acetic acid, CH3COOH, pH 4.8) in a 150 ml beaker. 2. Stir the solution for 24 h at 25°C on a magnetic stirrer at 500 rpm. 3. Pour the sample onto a 50 mesh (0.30 mm) screen and wash the retained carbon with 250 mL of de-ionized water. 4. Transfer the retained carbon to a pre-weighed, aluminum weighing dish that will be dried at 90°C under vacuum for 4 hours. 5. Cool in a desiccator and weigh.
Calculation:

c. Moisture Content
Materials:

* Aluminum dish with lid * Desiccator * Weighing scale * Oven

Procedure: 1. Add 2 g of GAC to a pre-weighed aluminum dish. 2. Place the sample and the dish in the oven and dry at 105 oC for 5 hours. 3. Cool in a desiccator. 4. Weigh the dish and sample, record the weight.
Calculation:

d. pH
Materials:

* De-ionized water * Stirrer * pH meter

Procedure: 1. Prepare a 1% (w/w) suspension of activated carbon in de-ionized water. 2. Heat the suspensions to approximately 90°C and stir for 20 minutes. 3. Allow it to cool at room temperature and measure the pH.

e. Ash Content
Materials:

* Grinder * Crucibles * Furnace * Desiccator
Procedure:
1. Place approximately 2 g of powdered activated carbon into ceramic crucibles. 2. Dry the carbon and crucibles overnight at 80 °C and reweigh to obtain the dry carbon weight. 3. Heat the samples in a muffle furnace at 760 °C for at least 6 hours. 4. Cool the crucibles in a desiccator, and weigh the remaining solids (ash).

Calculation:

f. Porosity
Materials:

* Graduated Cylinder * Distilled water * Wire mesh screen
Procedure:
1. Place approximately 20 mL of granular activated carbon in a 100 mL graduated cylinder. 2. Place a wire mesh on top of the sample to prevent material from floating once submerged in water. 3. Slowly pour distilled water over the sample until the water level is above the top of the sample. 4. Rock the cylinder gently from side to side to free trapped air bubbles. 5. Record the final water level.
Calculation:

where: Vi = combined volume of the sample plus added water (mL) Vf = final total volume of the sample and added water (mL) Vs = volume of the sample (mL) 2. Determination of Iodine Number of Activated Carbon
Standard Test Method
ASTM Designation: D4607-94
Materials:
* Analytical Balance * Burette * 250 mL Erlenmeyer Flasks * Beakers * Funnels * Filter paper * Pipettes * Volumetric Flasks * Graduated Cylinders

Procedure:
1. Cool the dry carbon to room temperature in a desiccator.
2. Weigh 1.0 g of dry carbon and place in a clean, dry 250-mL Erlenmeyer flask equipped with a ground glass stopper.
3. Pipette 10.0 mL of 5 wt % hydrochloric acid solution into each flask containing carbon. Stopper each flask and swirl gently until the carbon is completely welted. Loosen the stoppers to vent the flasks, place on a hot plate in a fume hood, and bring the contents to a boil. Allow to boil gently for 30 ± 2s to remove any sulfur which may interfere with the test results. Remove the flasks from the hot plate and cool to room temperature.
4. Pipette 100.0 mL of 0.1 N iodine solution into each flask. Stagger the addition of iodine to the flasks so that no delays are encountered in handling. Immediately stopper the flask and shake the contents vigorously for 30 ± 1s. Quickly filter the mixture by gravity through one sheet of folded filter paper (Whatman No.2V or equivalent) into a beaker. Filtration equipment must be prepared in advance so no delay is encountered in filtering the samples.
5. Use the first 20 to 30 mL of the filtrate to rinse a pipette. Discard the rinse portions. Use clean beakers to collect the remaining filtrates. Mix each filtrate by swirling the beaker and pipette 50.0 mL of filtrate into a clean 250-mL Erlenmeyer flask. Titrate the filtrate with standardized 0.1 N sodium thiosulfate solution until the solution is a pale yellow. Add 2 mL of the starch indicator solution and continue the titration with sodium thiosulfate until one drop produces a colorless solution. Record the volume of sodium thiosulfate used.
Calculation:

where: X/M = iodine absorbed per gram of carbon, mg/g S = sodium thiosulfate, mL and M = carbon used, g A = (N2)(12693.0); N2 = iodine, N B = (N1) (126.93); N1 = sodium thiosulfate, N DF = (I + H)/ F DF = dilution factor I = iodine, mL H = 5% hydrochloric acid, mL, and F = filtrate, mL

3. Measurement of Color Content of Sugar Syrup
Materials:
* Filter paper * Refractometer * De-ionized water * Spectrophotometer
Procedure:
1. Filter the sample using a filter paper capable of removing particles larger than 20 μm (Whatman no. 4 filter paper or the equivalent).
2. Measure the RDS of the sample on the refractometer.
3. Fill a color tube (10 or 25.4 mm in diameter) with the filtered sample.
4. Fill another tube with DI water as the blank (reference).
5. Adjust the spectrophotometer reading to 0 at 420 nm with the blank using the T (transmittance) or A (absorbance) mode of the instrument.
6. Read the T or A of the sample. Calculate the color expressed as ICUMSA 420 (IU color).
Calculation:
A mode:

T mode:

where: b = cell path length (sample tube diameter), in mm d =density, (d = 0.0055 × RDS + 0.9714)
4. Color Removal Determination
Materials:
* * Brown sugar * De-ionized water * Stirring rod * Filter paper * Refractometer * Spectrophotometer * Oven dryer * Water bath

Procedure: 1. Prepare 60°Bx sugar solution. - weigh 750 g raw sugar in 1000 mL beaker - add water until 1250 g - dissolve sugar, stir and filter - read degree brix (°Bx) and percent transmittance (%T) - calculate color and record as original color
2. Wash adequate amount of carbon with water for 30 minutes.
3. Dry in an oven at 110°C for 3 hours.
4. Cool.
5. Weigh 100 g carbon in 500 mL Erlenmeyer flask.
6. Add 200 mL of 60°Bx prepared.
7. Heat on water bath at 80°C for 3 hours.
8. Gently shake the flask occasionally and never stir.
9. Filter while hot.
10. Read degree brix (°Bx) and percent transmittance (%T).
Calculation:
Appendix C
Properties of Activated Carbon Produced 1. pH Carbon Sample | Trial | pH | Average pH | CCAC1 | 1 | 6.1 | 6.03 | | 2 | 6.0 | | | 3 | 6.0 | | CCAC2 | 1 | 6.4 | 6.47 | | 2 | 6.5 | | | 3 | 6.5 | | CCAC3 | 1 | 7.0 | 7.10 | | 2 | 7.1 | | | 3 | 7.2 | | CCAC4 | 1 | 6.4 | 6.37 | | 2 | 6.3 | | | 3 | 6.4 | | CCAC5 | 1 | 6.5 | 6.50 | | 2 | 6.4 | | | 3 | 6.6 | | CCAC6 | 1 | 7.3 | 7.17 | | 2 | 7.1 | | | 3 | 7.1 | | CCAC7 | 1 | 7.5 | 7.57 | | 2 | 7.6 | | | 3 | 7.6 | | CCAC8 | 1 | 6.8 | 6.77 | | 2 | 6.7 | | | 3 | 6.8 | | CCAC9 | 1 | 8.0 | 7.93 | | 2 | 7.9 | | | 3 | 7.9 | | Control | 1 | 7.8 | 7.77 | | 2 | 7.7 | | | 3 | 7.8 | |

2. Ash Content Carbon Sample | Trial | Original Weight of Carbon (g) | Weight of Remaining Solids (g) | Ash Content (%) | Average Ash Content (%) | CCAC1 | 1 | 2.0 | 0.19 | 9.5 | 9.33 | | 2 | 2.0 | 0.19 | 9.5 | | | 3 | 2.0 | 0.18 | 9.0 | | CCAC2 | 1 | 2.0 | 0.14 | 7.0 | 7.33 | | 2 | 2.0 | 0.16 | 8.0 | | | 3 | 2.0 | 0.14 | 7.0 | | CCAC3 | 1 | 2.0 | 0.26 | 13.0 | 14.00 | | 2 | 2.0 | 0.28 | 14.0 | | | 3 | 2.0 | 0.30 | 15.0 | | CCAC4 | 1 | 2.0 | 0.17 | 8.5 | 9.00 | | 2 | 2.0 | 0.19 | 9.5 | | | 3 | 2.0 | 0.18 | 9.0 | | CCAC5 | 1 | 2.0 | 0.22 | 11.0 | 10.50 | | 2 | 2.0 | 0.21 | 10.5 | | | 3 | 2.0 | 0.20 | 10.0 | | CCAC6 | 1 | 2.0 | 0.23 | 11.5 | 11.33 | | 2 | 2.0 | 0.22 | 11.0 | | | 3 | 2.0 | 0.23 | 11.5 | | CCAC7 | 1 | 2.0 | 0.33 | 16.5 | 16.50 | | 2 | 2.0 | 0.33 | 16.5 | | | 3 | 2.0 | 0.33 | 16.5 | | CCAC8 | 1 | 2.0 | 0.32 | 16.0 | 15.17 | | 2 | 2.0 | 0.30 | 15.0 | | | 3 | 2.0 | 0.29 | 14.5 | | CCAC9 | 1 | 2.0 | 0.34 | 17.0 | 17.17 | | 2 | 2.0 | 0.34 | 17.0 | | | 3 | 2.0 | 0.35 | 17.5 | | Control | 1 | 2.0 | 0.13 | 6.4 | 6.20 | | 2 | 2.0 | 0.12 | 6.2 | | | 3 | 2.0 | 0.12 | 6.0 | |

3. Bulk Density Carbon Sample | Trial | Weight of Dry Material (g) | Volume of Packed Dry Material (mL) | Bulk Density (g/mL) | Average Bulk Density (g/mL) | CCAC1 | 1 | 9.55 | 25.0 | 0.382 | 0.375 | | 2 | 9.18 | 25.0 | 0.367 | | | 3 | 9.39 | 25.0 | 0.376 | | CCAC2 | 1 | 8.91 | 25.0 | 0.356 | 0.347 | | 2 | 8.58 | 25.0 | 0.343 | | | 3 | 8.55 | 25.0 | 0.342 | | CCAC3 | 1 | 7.48 | 25.0 | 0.299 | 0.299 | | 2 | 7.47 | 25.0 | 0.299 | | | 3 | 7.51 | 25.0 | 0.300 | | CCAC4 | 1 | 12.80 | 25.0 | 0.512 | 0.512 | | 2 | 13.07 | 25.0 | 0.523 | | | 3 | 12.55 | 25.0 | 0.502 | | CCAC5 | 1 | 11.49 | 25.0 | 0.460 | 0.453 | | 2 | 11.31 | 25.0 | 0.452 | | | 3 | 11.17 | 25.0 | 0.447 | | CCAC6 | 1 | 12.44 | 25.0 | 0.498 | 0.499 | | 2 | 12.47 | 25.0 | 0.499 | | | 3 | 12.49 | 25.0 | 0.500 | | CCAC7 | 1 | 14.49 | 25.0 | 0.580 | 0.585 | | 2 | 14.31 | 25.0 | 0.572 | | | 3 | 15.10 | 25.0 | 0.604 | | CCAC8 | 1 | 14.13 | 25.0 | 0.565 | 0.562 | | 2 | 14.13 | 25.0 | 0.565 | | | 3 | 13.90 | 25.0 | 0.556 | | CCAC9 | 1 | 11.43 | 25.0 | 0.457 | 0.452 | | 2 | 11.19 | 25.0 | 0.448 | | | 3 | 11.28 | 25.0 | 0.451 | | Control | 1 | 12.22 | 25.0 | 0.489 | 0.483 | | 2 | 12.10 | 25.0 | 0.484 | | | 3 | 11.91 | 25.0 | 0.476 | |

4. Moisture Carbon Sample | Trial | Wet Weight of Sample (g) | Dry Weight of Sample (g) | Moisture Content (%) | Average Moisture Content (%) | CCAC1 | 1 | 2.0 | 1.796 | 10.18 | 10.09 | | 2 | 2.0 | 1.796 | 10.21 | | | 3 | 2.0 | 1.802 | 9.89 | | CCAC2 | 1 | 2.0 | 1.856 | 7.20 | 7.18 | | 2 | 2.0 | 1.860 | 7.02 | | | 3 | 2.0 | 1.853 | 7.33 | | CCAC3 | 1 | 2.0 | 1.894 | 5.31 | 5.33 | | 2 | 2.0 | 1.890 | 5.49 | | | 3 | 2.0 | 1.896 | 5.20 | | CCAC4 | 1 | 2.0 | 1.908 | 4.60 | 4.71 | | 2 | 2.0 | 1.909 | 4.55 | | | 3 | 2.0 | 1.900 | 4.99 | | CCAC5 | 1 | 2.0 | 1.836 | 8.22 | 8.06 | | 2 | 2.0 | 1.840 | 8.01 | | | 3 | 2.0 | 1.841 | 7.96 | | CCAC6 | 1 | 2.0 | 1.849 | 7.56 | 7.52 | | 2 | 2.0 | 1.858 | 7.11 | | | 3 | 2.0 | 1.842 | 7.89 | | CCAC7 | 1 | 2.0 | 1.902 | 4.92 | 5.06 | | 2 | 2.0 | 1.899 | 5.07 | | | 3 | 2.0 | 1.896 | 5.20 | | CCAC8 | 1 | 2.0 | 1.901 | 4.93 | 4.97 | | 2 | 2.0 | 1.903 | 4.87 | | | 3 | 2.0 | 1.898 | 5.10 | | CCAC9 | 1 | 2.0 | 1.874 | 6.31 | 6.53 | | 2 | 2.0 | 1.861 | 6.97 | | | 3 | 2.0 | 1.874 | 6.30 | | Control | 1 | 2.0 | 1.898 | 5.10 | 3.77 | | 2 | 2.0 | 1.932 | 3.40 | | | 3 | 2.0 | 1.944 | 2.80 | |

5. Porosity Carbon Sample | Trial | Volume of Sample (mL) | Combined Volume of Sample and Water (mL) | Final Total Volume of Sample and Water (mL) | Porosity (%) | Average Porosity (%) | CCAC1 | 1 | 20.0 | 39.0 | 27.0 | 60.0 | 60.33 | | 2 | 20.0 | 40.2 | 28.0 | 61.0 | | | 3 | 20.0 | 40.0 | 28.0 | 60.0 | | CCAC2 | 1 | 20.0 | 46.0 | 33.0 | 65.0 | 66.00 | | 2 | 20.0 | 46.2 | 33.0 | 66.0 | | | 3 | 20.0 | 46.4 | 33.0 | 67.0 | | CCAC3 | 1 | 20.0 | 44.0 | 29.0 | 75.0 | 75.00 | | 2 | 20.0 | 46.0 | 31.0 | 75.0 | | | 3 | 20.0 | 45.0 | 30.0 | 75.0 | | CCAC4 | 1 | 20.0 | 44.3 | 29.0 | 76.5 | 76.50 | | 2 | 20.0 | 45.4 | 30.0 | 77.0 | | | 3 | 20.0 | 44.2 | 29.0 | 76.0 | | CCAC5 | 1 | 20.0 | 46.4 | 33.0 | 67.0 | 68.67 | | 2 | 20.0 | 47.0 | 33.0 | 70.0 | | | 3 | 20.0 | 46.8 | 33.0 | 69.0 | | CCAC6 | 1 | 20.0 | 50.8 | 37.0 | 69.0 | 68.33 | | 2 | 20.0 | 49.6 | 36.0 | 68.0 | | | 3 | 20.0 | 50.6 | 37.0 | 68.0 | | CCAC7 | 1 | 20.0 | 37.6 | 24.0 | 68.0 | 68.00 | | 2 | 20.0 | 39.7 | 26.0 | 68.5 | | | 3 | 20.0 | 38.5 | 25.0 | 67.5 | | CCAC8 | 1 | 20.0 | 50.9 | 36.0 | 74.5 | 76.00 | | 2 | 20.0 | 51.5 | 36.0 | 77.5 | | | 3 | 20.0 | 51.2 | 36.0 | 76.0 | | CCAC9 | 1 | 20.0 | 45.0 | 29.0 | 80.0 | 79.33 | | 2 | 20.0 | 45.7 | 30.0 | 78.5 | | | 3 | 20.0 | 44.9 | 29.0 | 79.5 | | Control | 1 | 20.0 | 44.3 | 27.0 | 86.5 | 88.55 | | 2 | 20.0 | 42.4 | 24.0 | 92.0 | | | 3 | 20.0 | 43.4 | 26.0 | 87.2 | |

6. Hardness Carbon Sample | Trial | Initial Weight (g) | Final Weight (g) | Attrition (%) | Average Attrition (%) | CCAC1 | 1 | 1 | 0.55 | 45 | 45.7 | | 2 | 1 | 0.56 | 44 | | | 3 | 1 | 0.52 | 48 | | CCAC2 | 1 | 1 | 0.32 | 68 | 66.7 | | 2 | 1 | 0.35 | 65 | | | 3 | 1 | 0.33 | 67 | | CCAC3 | 1 | 1 | 0.21 | 79 | 79.3 | | 2 | 1 | 0.22 | 78 | | | 3 | 1 | 0.19 | 81 | | CCAC4 | 1 | 1 | 0.63 | 37 | 36.3 | | 2 | 1 | 0.66 | 34 | | | 3 | 1 | 0.62 | 38 | | CCAC5 | 1 | 1 | 0.55 | 45 | 46.0 | | 2 | 1 | 0.52 | 48 | | | 3 | 1 | 0.55 | 45 | | CCAC6 | 1 | 1 | 0.55 | 45 | 47.3 | | 2 | 1 | 0.52 | 48 | | | 3 | 1 | 0.51 | 49 | | CCAC7 | 1 | 1 | 0.76 | 24 | 25.7 | | 2 | 1 | 0.74 | 26 | | | 3 | 1 | 0.73 | 27 | | CCAC8 | 1 | 1 | 0.53 | 47 | 45.3 | | 2 | 1 | 0.55 | 45 | | | 3 | 1 | 0.56 | 44 | | CCAC9 | 1 | 1 | 0.41 | 59 | 57.7 | | 2 | 1 | 0.44 | 56 | | | 3 | 1 | 0.42 | 58 | | Control | 1 | 1 | 0.91 | 9 | 11.3 | | 2 | 1 | 0.88 | 12 | | | 3 | 1 | 0.87 | 13 | |

7. Iodine Number Carbon Sample | Trial | Volume of Sodium Thiosulfate (mL) | Iodine Number (mg/g) | Average Iodine Number (mg/g) | CCAC 1 | 1 | 24.8 | 576.77 | 589.8 | | 2 | 24.5 | 585.15 | | | 3 | 23.7 | 607.49 | | CCAC 2 | 1 | 19.5 | 724.77 | 735.0 | | 2 | 18.7 | 747.11 | | | 3 | 19.2 | 733.15 | | CCAC 3 | 1 | 21.0 | 682.88 | 705.2 | | 2 | 20.3 | 702.43 | | | 3 | 19.3 | 730.36 | | CCAC 4 | 1 | 18.9 | 741.53 | 740.6 | | 2 | 19.5 | 724.77 | | | 3 | 18.4 | 755.49 | | CCAC 5 | 1 | 23.3 | 618.66 | 613.1 | | 2 | 23.8 | 604.69 | | | 3 | 23.4 | 615.86 | | CCAC 6 | 1 | 19.5 | 724.77 | 716.4 | | 2 | 20.1 | 708.02 | | | 3 | 19.8 | 716.39 | | CCAC 7 | 1 | 17.9 | 769.45 | 779.7 | | 2 | 17.3 | 786.20 | | | 3 | 17.4 | 783.41 | | CCAC 8 | 1 | 21.5 | 668.92 | 676.4 | | 2 | 21.0 | 682.88 | | | 3 | 21.2 | 677.30 | | CCAC 9 | 1 | 18.4 | 755.49 | 747.1 | | 2 | 19.1 | 735.94 | | | 3 | 18.6 | 749.90 | | Control | 1 | 5.2 | 1124.09 | 1115.7 | | 2 | 5.6 | 1112.92 | | | 3 | 5.7 | 1110.13 | |

8. Yield CCAC no. | Activation Temperature (°C) | Impregnation Ratio | Weight before activation (g) | Weight after activation (g) | Weight after washing, drying and sieving (g) | Yield (%) | 1 | 400 | 1:1 | 155.53 | 104.9 | 65.83 | 65.83 | 2 | 500 | 1:1 | 155.53 | 84.4 | 53.76 | 53.76 | 3 | 600 | 1:1 | 155.53 | 72.48 | 47.67 | 47.67 | 4 | 400 | 2:1 | 251.55 | 158.39 | 77.97 | 77.97 | 5 | 500 | 2:1 | 251.55 | 150.01 | 63.1 | 63.1 | 6 | 600 | 2:1 | 251.55 | 124.46 | 52.16 | 52.16 | 7 | 400 | 3:1 | 274.14 | 193.14 | 80.34 | 80.34 | 8 | 500 | 3:1 | 274.14 | 188.04 | 68.8 | 68.8 | 9 | 600 | 3:1 | 274.14 | 169.96 | 53.1 | 53.1 |

9. Color Content Syrup | Trial | RDS(°Bx) | Transmittance(%T) | Sample Tube Diameter (mm) | Density(d = 0.0055 × RDS + 0.9714) | Color (IU) | AverageColor (IU) | 1 | 1 | 49.8 | 29 | 10 | 1.2453 | 866.88 | 820.62 | | 2 | 50.2 | 33 | 10 | 1.2475 | 768.85 | | | 3 | 48.4 | 32 | 10 | 1.2376 | 826.13 | | 2 | 1 | 51.2 | 33 | 10 | 1.2530 | 750.52 | 762.94 | | 2 | 51.0 | 35 | 10 | 1.2519 | 714.10 | | | 3 | 49.6 | 31 | 10 | 1.2442 | 824.21 | | 3 | 1 | 54.2 | 38 | 10 | 1.2695 | 610.72 | 595.88 | | 2 | 56.2 | 36 | 10 | 1.2805 | 616.55 | | | 3 | 55.6 | 40 | 10 | 1.2772 | 560.38 | | 4 | 1 | 53.8 | 53 | 10 | 1.2673 | 404.40 | 408.97 | | 2 | 57.2 | 49 | 10 | 1.2860 | 421.16 | | | 3 | 58.1 | 50 | 10 | 1.2910 | 401.35 | | 5 | 1 | 55.2 | 52 | 10 | 1.2750 | 403.52 | 448.00 | | 2 | 56.4 | 47 | 10 | 1.2816 | 453.64 | | | 3 | 57.0 | 44 | 10 | 1.2849 | 486.83 | | 6 | 1 | 63.8 | 53 | 10 | 1.3223 | 326.83 | 310.33 | | 2 | 62.1 | 57 | 10 | 1.3130 | 299.41 | | | 3 | 64.3 | 55 | 10 | 1.3251 | 304.74 | | 7 | 1 | 61.9 | 33 | 10 | 1.3119 | 592.94 | 630.16 | | 2 | 61.7 | 29 | 10 | 1.3108 | 664.75 | | | 3 | 61.4 | 31 | 10 | 1.3091 | 632.80 | | 8 | 1 | 59.8 | 34 | 10 | 1.3003 | 602.54 | 585.34 | | 2 | 61.2 | 33 | 10 | 1.3080 | 601.48 | | | 3 | 61.4 | 36 | 10 | 1.3091 | 552.01 | | 9 | 1 | 60.9 | 37 | 10 | 1.3064 | 542.76 | 509.78 | | 2 | 61.4 | 39 | 10 | 1.3091 | 508.76 | | | 3 | 61.8 | 41 | 10 | 1.3113 | 477.82 | | Control | 1 | 59.7 | 60 | 10 | 1.2998 | 285.91 | 294.95 | | 2 | 59.9 | 59 | 10 | 1.3009 | 294.08 | | | 3 | 59.7 | 58 | 10 | 1.2998 | 304.88 | | Original | | 60.0 | 17 | 10 | 1.3014 | 985.54 | 985.54 |

Appendix D
Statistical Analysis
Using One-Way Analysis of Variance (ANOVA),
Assumptions of ANOVA:
(i) All populations involved follow a normal distribution.
(ii) All populations have the same variance (or standard deviation).
(iii) The samples are randomly selected and independent of one another.
Null Hypothesis: There is no significant difference between the means of color content of the sugar syrup treated with CCACs and CCAL.

SUMMARY | | | | | | | Groups | Count | Sum | Average | Variance | | | 1 | 3 | 2461.86 | 820.62 | 2425.24 | | | 2 | 3 | 2288.83 | 762.9433 | 3146.807 | | | 3 | 3 | 1787.65 | 595.8833 | 953.8622 | | | 4 | 3 | 1226.91 | 408.97 | 113.7727 | | | 5 | 3 | 1343.99 | 447.9967 | 1759.024 | | | 6 | 3 | 930.98 | 310.3267 | 211.3722 | | | 7 | 3 | 1890.49 | 630.1633 | 1294.383 | | | 8 | 3 | 1756.03 | 585.3433 | 833.6142 | | | 9 | 3 | 1529.34 | 509.78 | 1055.081 | | | CCAL | 3 | 884.87 | 294.9567 | 90.54163 | | | | | | | | | | | | | | | | | ANOVA | | | | | | | Source of Variation | SS | df | MS | F | P-value | F crit | Between Groups | 842980.5 | 9 | 93664.5 | 78.81763 | 1.2E-13 | 2.392814 | Within Groups | 23767.4 | 20 | 1188.37 | | | | | | | | | | | Total | 866747.9 | 29 | | | | |

Decision Rule: Reject the null hypothesis if F >F crit.
Conclusion: 78.82>2.39, thus, reject the null hypothesis.
Interpretation: Since we rejected the null hypothesis, we are 95% confident (1-α) that the mean color content is not statistically equal for sugar treated with CCACs and CCAL.
Appendix E
Documentation

Collected corn cobs
Crushed corn cobs

Activation
Impregnation

Corn Cob Activated Carbon

Iodine number determination
Moisture determination
Hardness determination
Ash content determination
Porosity determination
Bulk density determination pH determination

CCAC7
CCAC8
CCAC93
Original
CCAC4
CCAC5
CCAC63
Original
CCAC1
CCAC2
CCAC33
Original
CCAC1
CCAC2
CCAC3
CCAC4
CCAC5
CCAC6
CCAC7
CCAC8
CCAC9
CCAL
Transmittance determination
Sugar decolorization
Decolorized syrups
Treated and untreated syrups

Appendix F
Communication

Appendix G 1. Material Safety Data Sheet For Activated Carbon

Section 1 - Substance Identification
Chemical Name: Carbon, Activated Carbon, Charcoal, Activated Charcoal

Section 2 - Hazardous Ingredients
This material is 100% activated carbon. There are no established PEL, TWA or TLV values for this material. Caution should be taken for respirable dust. The ACGIH TWA for respirable dust is 2.5 mg/m3. This product has no carcinogenic properties.

Section 3 - Physical Data
Description: Colorless black solid, granule, pellet, or flake.
Solubility: Not soluble Apparent Density:0.3-0.7g/cc
Stability: Stable Incompatibility: Avoid contact with strong oxidizers.

Section 4 - Fire & Explosion Hazards
Flash Point: N/A Extinguishing Media: Water, foam, CO2, or dry chemical
Special Procedures: None Decomposition Products: CO may be formed in a fire
Unusual Fire & Explosion Hazards: Contact with strong oxidizers may result in fire

Section 5 - Health Data
Overexposure Effects: This product is non-toxic through ingestion. It is non-toxic through skin absorption. It is not a primary skin irritant. No sensitization effects are known. It is non-toxic through inhalation. Due to its physical properties, carbon dust may irritate the respiratory system and produce eye irritation.
First Aid: In case of eye contact, flush with water for at least 15 minutes. Contact a doctor immediately. For inhalation, remove the person from the area.

Section 6 - Spill or Leak Procedures
Reportable Quantities: No EPA RQ for this product.
If Spilled or Leaked: Sweep/shovel up and discard or repackage.
Waste Disposal Method: Unused carbon may be disposed of in refuse container.

Section 7 - Handling & Storage
Protective Gloves: Recommended. Eye Protection: Safety glasses/goggles recommended
Other Protective Clothing: None required. Ventilation: Local exhaust to control dust.
Respiratory Protection: A high efficiency particulate filter is recommended for dust.
Work/Hygienic Practices: Wash thoroughly after handling.

2. Material Safety Data Sheet For 85% Phosphoric Acid

Section 1 - Chemical Identification
Trade Name: Phosphoric Acid
Chemical Name: Phosphoric Acid
Synonyms: Orthophosphoric Acid, Monophosphoric acid

Section 2 - Composition and Information on Ingredients
CAS NO.: 7664-38-2
H S Code: 2809 20 01
UN Code: UN 1805

Section 3 - Hazards Identification
Appearance & Odor: Clear, colourless, syrupy liquid with no odour.
Safety Information:
Health Effects: Corrosive liquid causes eye and skin burns.
Physical & Chemical: Forms flammable & Explosive hydrogen through corrosion of metals.
Hazards at high temperature: Thermal decomposition giving corrosive products.
Specific Hazards: Corrosive causes eye and skin burns.

Section 4 - First-Aid Measures
General Advice: Take off immediately all contaminated clothing (Including Shoes)
Inhalation: Move to fresh air. If required, provide oxygen or artificial respiration. Hospitalize.
Skin contact: Wash immediately, abundantly & thoroughly with water. If possible rinse with bicarbonate solution.
Eye contact: Wash immediately & abundantly with water for at least 15 minutes. Consult an ophthalmologist immediately.
After swallowing: Do not induce vomiting, rinse mouth and lips with plenty of water if the subject is conscious, and then hospitalize immediately. Never give anything in mouth to an unconscious person.

Section 5 - Fire Fighting Measures
Suitable Extinguishing media: In case of Fire nearby use dry Powder, Foam, Carbon dioxide (CO2) media
Special hazards: Non-flammable product. Forms flammable and explosive hydrogen through corrosion of Metals. Temperature above 200°C: Formation of Polyphosphoric Acid (Dehydration) At high temperature: Thermal decomposition giving corrosive products: Phosphorus Oxides.
Specific Methods: In case of Fire: remove exposed containers. Cool containers with water spray.
Special Protective Equipment for Fire fighters: In case of Fire: wear a self-contained breathing apparatus and Acid resistant clothing.

Section 6 - Accidental Release Measures
Personal Protection: Avoid contact with skin and eyes and inhalation of hot vapours.
Environmental protection: Do not allow material to be released to the environment. Do not let the product enter into drains. Contain by damming.
Methods for cleaning up:
Recovery: Pump into an inert labelled emergency container. Clean up puddle of Product immediately. Dilute the puddles with water & recover it.
Neutralization: Dilute cautiously with water & then process. Neutralize with an alkaline carbonate or neutralize with slaked lime (Filter the salt obtained –neutralize the liquid)

Section 7 - Handling and Storage
Technical measures/ Precautions: Storage & handling precautions applicable to products: Corrosive: Ensure appropriate exhaust & ventilation at machinery. Provide showers, eye baths.
Safe handling advice: Avoid splashing when handling. Do not pour water
Storage:
Technical measures/ Storage information: Keep containers tightly closed in a cool, well-ventilated place. Store in well-insulated area. Store protected from moisture & heat. Keep at temperature above 16°C. Provide a catch-tank & an impermeable corrosion resistant floor with drainage to a neutralization tank within a bunked area. Provide anti-corrosion electrical equipment.
Incompatible Products: Bases-Quicklime
Alcohols-Ketones-Amines
Water
Nitrates-Chlorates-Calcium Carbide
Metals-Finely divided metals
Combustible Material
Recommended: Stainless steel 316 L-Carbon Steel (Vulcanized Rubber coated Steel)
Plastic Materials (Polyurethane) Small Quantities:
Glass protected by a fitted metallic covering
To be avoided: Metals: Ordinary Steel, Copper, Aluminum, (and alloys)

Section 8 - Exposure Control/Personal Protection
Protective Provisions: Ensure sufficient air exchange and/ or exhaust in working areas
Personal Protective Equipment Respiratory protection: In case of insufficient ventilation, wear suitable respiratory equipment
Hand protection: Gloves
Eye protection: Safety glasses / goggles. Face mask (in case of spattering)
Skin & body protection Protective clothing Non-skid boots (Butyl rubber-chlorinated polyethylene-Neoprene-Polyvinyl Chloride)
Specific hygienic Measures: Avoid contact with skin and eyes and inhalation of hot vapours

Section 9 - Physical and Chemical Properties
Physical State (20°C): Liquid (viscous)
Colour: Colourless
Odour: none
Specific gravity: Liquid (25°C) 1.5-1.7 depending upon Phosphoric acid strength
Solubility in Water: at 20°C Completely soluble
Solvents: Soluble in Alcohols

Section 10 - Stability and Reactivity
Conditions to avoid: Store protected from moisture & heat
Materials to avoid: Bases, Quicklime: Exothermic reaction-Violent reaction
Alcohols- ketones -Amines: Exothermic reaction
Water: Very exothermic reaction & possibility of spitting
Nitrates-Chlorates - Calcium Carbide: Explosive reaction Metals – finely divided metals
Combustible materials: Overheating and ignition

Section 11 - Toxicological Information
Acute toxicity: May be harmful by inhalation, ingestion, or skin absorption. Material is destructive to tissue of the mucous membranes and upper respiratory tract, eyes and skin.
Inhalation: Inhalation may result in spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema. Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting.
Chronic Effects: Target Organ(S): Liver, Blood, Bone Marrow
Additional toxicological information: To the best of our knowledge the acute and chronic toxicity of this substance is not fully known. No classification data on carcinogenic properties of this material is available from the EPA, IARC, NTP, OSHA or ACGIH.

Section 12 - Ecological Information
Phosphoric Acid is practically nontoxic to one species of fresh water fish. No toxicity data was available for other freshwater species.

Section 13 - Disposal Considerations
Disposal of the Product: Recommendation: Consult state, local or national regulations for proper disposal. Dilute cautiously with water and then process. Neutralize with an alkaline carbonate or Neutralize with slaked lime (Filter the salt obtained- Neutralize the liquid) Recommendation: Disposal must be made according to official regulations.

Section 14 - Transport Information
Description of goods: Phosphoric Acid

3. Material Safety Data Sheet for Buffer Solution pH 4.5 (Acetate)

Section 1 - Chemical Product and Company Identification
MSDS Name: Buffer Solution pH 4.0-4.5 (Acetate)

Section 2 - Composition, Information on Ingredients CAS# | Chemical Name | Percent | EINECS/ELINCS | 64-19-7 | Acetic acid | 46.0 | 200-580-7 | 7732-18-5 | Water | 29.0 | 231-791-2 | 6131-90-4 | Sodium acetate, trihydrate | 25.0 | unlisted |

Section 3 - Hazards Identification
EMERGENCY OVERVIEW
Appearance: not available liquid.
Danger! Causes eye and skin burns. Causes digestive and respiratory tract burns. May be harmful if absorbed through the skin.
Target Organs: Kidneys, teeth, eyes, skin, mucous membranes.
Potential Health Effects
Eye: Causes severe eye irritation. Contact with liquid or vapor causes severe burns and possible irreversible eye damage.
Skin: Causes skin burns. May be harmful if absorbed through the skin. Contact with the skin may cause blackening and hyperkeratosis of the skin of the hands.
Ingestion: May cause severe and permanent damage to the digestive tract. Causes severe pain, nausea, vomiting, diarrhea, and shock. May cause polyuria, oliguria (excretion of a diminished amount of urine in relation to the fluid intake) and anuria (complete suppression of urination). Rapidly absorbed from the gastrointestinal tract.
Inhalation: Effects may be delayed. Causes chemical burns to the respiratory tract. Exposure may lead to bronchitis, pharyngitis, and dental erosion. May be absorbed through the lungs.
Chronic: Chronic exposure to acetic acid may cause erosion of dental enamel, bronchitis, eye irritation, darkening of the skin, and chronic inflammation of the respiratory tract. Acetic acid can cause occupational asthma. One case of a delayed asthmatic response to glacial acetic acid has been reported in a person with bronchial asthma. Skin sensitization to acetic acid is rare, but has occurred.

Section 4 - First Aid Measures
Eyes: Immediately flush eyes with plenty of water for at least 15 minutes, occasionally lifting the upper and lower eyelids. Get medical aid. Do NOT allow victim to rub eyes or keep eyes closed.
Skin: Get medical aid. Immediately flush skin with plenty of water for at least 15 minutes while removing contaminated clothing and shoes. Wash clothing before reuse.
Ingestion: Do not induce vomiting. If victim is conscious and alert, give 2-4 cupfuls of milk or water. Never give anything by mouth to an unconscious person. Get medical aid.
Inhalation: Remove from exposure and move to fresh air immediately. If breathing is difficult, give oxygen. Get medical aid. Do NOT use mouth-to-mouth resuscitation. If breathing has ceased apply artificial respiration using oxygen and a suitable mechanical device such as a bag and a mask.

Section 5 - Fire Fighting Measures
General Information: As in any fire, wear a self-contained breathing apparatus in pressure-demand, MSHA/NIOSH (approved or equivalent), and full protective gear. During a fire, irritating and highly toxic gases may be generated by thermal decomposition or combustion. Will burn if involved in a fire. Runoff from fire control or dilution water may cause pollution.
Extinguishing Media: Use water spray, dry chemical, carbon dioxide, or appropriate foam.
Flash Point: > 112.8 deg C (> 235.04 deg F)
Autoignition Temperature: Not available.
Explosion Limits, Lower:Not available.
Upper: Not available.
NFPA Rating: (estimated) Health: 3; Flammability: 1; Instability: 0

Section 6 - Accidental Release Measures
General Information: Use proper personal protective equipment as indicated in Section 8.
Spills/Leaks: Absorb spill with inert material (e.g. vermiculite, sand or earth), then place in suitable container. Avoid runoff into storm sewers and ditches which lead to waterways. Clean up spills immediately, observing precautions in the Protective Equipment section. Provide ventilation.

Section 7 - Handling and Storage
Handling: Remove contaminated clothing and wash before reuse. Use only in a well-ventilated area. Do not breathe dust, mist, or vapor. Do not get in eyes, on skin, or on clothing. Keep container tightly closed. Do not ingest or inhale. Wash clothing before reuse. Discard contaminated shoes.
Storage: Store in a tightly closed container. Store in a cool, dry, well-ventilated area away from incompatible substances.

Section 8 - Exposure Controls, Personal Protection
Engineering Controls: Facilities storing or utilizing this material should be equipped with an eyewash facility and a safety shower. Use adequate ventilation to keep airborne concentrations low.
Exposure Limits Chemical Name | ACGIH | NIOSH | OSHA - Final PELs | Acetic acid | 10 ppm TWA; 15 ppm STEL | 10 ppm TWA; 25 mg/m3 TWA 50 ppm | 10 ppm TWA; 25 mg/m3 TWA | Water | none listed | none listed | none listed | Sodium acetate, trihydrate | none listed | none listed | none listed |
OSHA Vacated PELs: Acetic acid: 10 ppm TWA; 25 mg/m3 TWA Water: No OSHA Vacated PELs are listed for this chemical. Sodium acetate, trihydrate: No OSHA Vacated PELs are listed for this chemical.
Personal Protective Equipment
Eyes: Wear appropriate protective eyeglasses or chemical safety goggles as described by OSHA's eye and face protection regulations in 29 CFR 1910.133 or European Standard EN166.
Skin: Wear appropriate protective gloves to prevent skin exposure.
Clothing: Wear appropriate protective clothing to prevent skin exposure.
Respirators: A respiratory protection program that meets OSHA's 29 CFR 1910.134 and ANSI Z88.2 requirements or European Standard EN 149 must be followed whenever workplace conditions warrant respirator use.

Section 9 - Physical and Chemical Properties
Physical State: Liquid
Appearance: not available
Odor: none reported pH: 4.0 to 4.5
.
Section 10 - Stability and Reactivity
Chemical Stability: Stable at room temperature in closed containers under normal storage and handling conditions.
Conditions to Avoid: Excess heat.
Incompatibilities with Other Materials: Acetaldehyde, 2-aminoethanol, ammonium nitrate, bromine pentafluoride, chlorine trifluoride, chlorosulfonic acid, chromic acid, chromic anhydride, acetic anhydride, diallyl methyl carbinol + ozone, ethylene diamine, ethyleneimine, hydrogen peroxide, nitric acid, nitric acid + acetone, oleum, perchloric acid, permanganates, phosphorus isocyanate, phosphorus trichloride, potassium hydroxide, potassium tert-butoxide, sodium hydroxide, sodium peroxide, xylene, strong oxidizing agents.
Hazardous Decomposition Products: Carbon monoxide, irritating and toxic fumes and gases, carbon dioxide.
Hazardous Polymerization: Has not been reported.

Section 11 - Toxicological Information
Teratogenicity: No teratogenic effects were observed among the offspring of mice, rats, or rabbits that had been given very large doses of apple cider vinegar (containing acetic acid) during pregnancy. Acetic acid treatment of suckling rats (via maternal administration) was associated with abnormalities of behavioral testing.
Reproductive Effects: Intratesticular, rat: TDLo = 400 mg/kg (male 1 day(s) pre-mating) Fertility - male fertility index (e.g. # males impregnating females per # males exposed to fertile nonpregnant females).
Mutagenicity: Sister Chromatid Exchange: Human, Lymphocyte = 5 mmol/L.; Unscheduled DNA Synthesis: Administration onto the skin, mouse = 79279 ug/kg.; Cytogenetic Analysis: Hamster, Ovary = 10 mmol/L.
Neurotoxicity: No information found
Section 12 - Ecological Information
Ecotoxicity: Fish: Bluegill/Sunfish: LC50 = 75 mg/L; 96 Hr; CAS# 64-19-7: Unspecified
Fish: Goldfish: LC50 = 423 mg/L; 24 Hr; CAS# 64-19-7: Unspecified
Water flea Daphnia: EC50 = 32-47 mg/L; 24-48 Hr; CAS# 64-19-7: Unspecified
Bacteria: Phytobacterium phosphoreum: EC50 = 8.86-11 mg/L; 5,15,25 min; CAS# 64-19-7: Microtox test
Fish: Fathead Minnow: LC50 = 88 mg/L; 96 Hr; CAS# 64-19-7: Static bioassay @ 18-22°C
Fish: Pseudomonas putida:

Section 13 - Disposal Considerations
Chemical waste generators must determine whether a discarded chemical is classified as a hazardous waste. US EPA guidelines for the classification determination are listed in 40 CFR Parts 261.3. Additionally, waste generators must consult state and local hazardous waste regulations to ensure complete and accurate classification.
RCRA P-Series: None listed.
RCRA U-Series: None listed.

Section 14 - Transport Information | US DOT | Canada TDG | Shipping Name: | ACETIC ACID SOLUTION | ACETIC ACID SOLUTION | Hazard Class: | 8 | 8 | UN Number: | UN2790 | UN2790 | Packing Group: | III | III |

Section 15 - Regulatory Information
Health & Safety Reporting List None of the chemicals are on the Health & Safety Reporting List.
Chemical Test Rules None of the chemicals in this product are under a Chemical Test Rule.
Section 12b None of the chemicals are listed under TSCA Section 12b.

4. Material Safety Data Sheet for Sodium Thiosulfate Solutions, 0.01N - 1.0N

Section 1 - Chemical Product And Company Identification
Msds Name: Sodium Thiosulfate Solutions, 0.01n - 1.0n

Section 2 - Composition, Information on Ingredients
Cas# Chemical Name Percent
7772-98-7 Sodium Thiosulfate 0.21-21
497-19-8 Sodium Carbonate 0.017
7732-18-5 Water Balance

Section 3 - Hazards Identification
Emergency Overview:
Appearance: Colorless
Caution!
May cause irritation. This is expected to be a low hazard for usual industrial handling.
Target Organs: None.
Potential Health Effects:
Eye: may cause mild eye irritation.
Skin: may cause skin irritation.
Ingestion: ingestion may cause sore throat, coughing, nausea, abdominal pain.
Inhalation: inhalation may cause coughing, respiratory irritation, dyspnea, pulmonary edema. Chronic: exposure may result in mucous membrane irritation, dermatitis, conjunctivitis. Section 4 - First Aid Measures Eyes:
Flush eyes with plenty of water for at least 15 minutes, occasionally lifting the upper and lower lids until no evidence of chemical remains. Get medical aid.
Skin:
Flush skin with plenty of soap and water for at least 15 minutes while removing contaminated clothing and shoes. Get medical aid if irritation develops or persists.
Ingestion:
Give conscious victim 2-4 cupfuls of milk or water. Never give anything by mouth to an unconscious person. Get medical aid.

Inhalation:
Move victim to fresh air immediately. Give artificial respiration if necessary. If breathing is difficult, give oxygen. Get medical aid.
Notes To Physician: Treat Symptomatically And Supportively.

Section 5 - Fire Fighting Measures
General Information:
Negligible fire and explosion hazard when exposed to heat or flame. Move container if possible, avoid breathing vapors or dust.
Extinguishing Media:
For small fires, use water spray, dry chemical, carbon dioxide or chemical foam.
Autoignition Temperature: Not Applicable.

Explosion Limits:
Lower: No Information
Upper: No Information

Section 6 - Accidental Release Measures
General Information:
Use Proper Personal Protective Equipment As Indicated In Section 8.

Spills/Leaks:
Absorb spills with absorbent (vermiculite, sand, fuller's earth) and place in plastic bags for later disposal. Scoop material into suitable (plastic or glass) container, label for disposal.

Section 7 - Handling And Storage
Handling:
Avoid Prolonged Or Repeated Contact With Skin. Avoid Ingestion And Inhalation. Use With Adequate Ventilation
Storage:
Store At Room Temperature. Keep Away From Heat And Incompatible
Substances.

Section 8 - Exposure Controls, Personal Protection
Engineering Controls:
Use adequate ventilation to keep airborne concentrations low.
Exposure Limits:
Chemical Name: Sodium Thiosulfate
Osha Vacated Pels:
Personal Protective Equipment:
Eyes:
wear appropriate protective eyeglasses or chemical safety goggles as described by osha's eye and face protection regulations in 29 cfr 1910.133.
Skin: wear appropriate gloves to prevent skin exposure.
Clothing: wear appropriate protective clothing to prevent skin exposure.
Respirators:
follow the osha respirator regulations found in 29 cfr 1910.134. Always use a niosh-approved respirator when necessary.

Section 9 - Physical And Chemical Properties
Physical State: Liquid
Color: Colorless
Odor: None Reported pH: No Information Found.
Vapor Pressure: 14 Mmhg
Vapor Density: No Information Found.
Evaporation Rate: >1 (Ether=1)
Viscosity: No Information Found.
Boiling Point: 212 Deg. F (100.00 Deg. C)
Freezing/Melting Point: 32 Deg. F (0.00 Deg. C)
Decomposition Temperature: No Information Found.
Solubility In Water: No Information Found.
Specific Gravity/Density: 1.0-1.1
Molecular Formula: Mixture
Molecular Weight: No Information Found.

Section 10 - Stability And Reactivity
Chemical Stability: Stable Under Normal Temperatures And Pressures.
Conditions To Avoid: Incompatible Materials.
Incompatibilities With Other Materials:
Sodium Nitrite, Metal Nitrates, Chlorine Solutions, Acids.
Hazardous Decomposition Products:
Hydrogen Sulfide, Sodium Oxide, Sulfur Oxides (Sox), Including Sulfur
Oxide And Sulfur Dioxide
Hazardous Polymerization: has not been reported.

Section 11 - Toxicological Information
Not Listed As A Carcinogen By Acgih, Iarc, Niosh, Ntp, Osha, Or Ca Prop 65.
Epidemiology:
Sodium Thiosulfate Is An Eye, Skin, Mucous Membrane Irritant. Large Doses
Have A Cathartic Action.

Section 12 - Ecological Information
No Information Found.

Section 13 - Disposal Considerations
Dispose Of In Accordance With Federal, State, And Local Regulations.

Section 14 - Transport Information
Shipping Name: Not Regulated.

5. Material Safety Data Sheet for Iodine Solution, 0.1N

Section 1: Chemical Product and Company Identification
Product Name: Iodine Solution, 0.1N
TSCA: TSCA 8(b) inventory: Iodine; Potassium Iodide; Hydrochloric acid; Water

Section 2: Composition and Information on Ingredients
Toxicological Data on Ingredients: Iodine: ORAL (LD50): Acute: 14000 mg/kg [Rat]. Potassium Iodide LD50: Not available.LC50: Not available.

Section 3: Hazards Identification
Potential Acute Health Effects:
Hazardous in case of skin contact (corrosive, irritant, sensitizer, permeator), of eye contact (irritant), of ingestion, of inhalation.
Prolonged exposure may result in skin burns and ulcerations. Over-exposure by inhalation may cause respiratory irritation.
Potential Chronic Health Effects:
Hazardous in case of skin contact (corrosive, irritant, sensitizer, permeator), of eye contact (irritant), of ingestion, of inhalation.
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Not available. TERATOGENIC EFFECTS: Not available.
DEVELOPMENTAL TOXICITY: PROVEN [Potassium Iodide] The substance is toxic to lungs, the nervous system, the reproductive system, mucous membranes, gastrointestinal tract, upper respiratory tract. Repeated or prolonged exposure to the substance can produce target organs damage.

Section 4: First Aid Measures
Eye Contact:
Check for and remove any contact lenses. Immediately flush eyes with running water for at least 15 minutes, keeping eyelids open. Cold water may be used. Do not use an eye ointment. Seek medical attention.
Skin Contact:
If the chemical got onto the clothed portion of the body, remove the contaminated clothes as quickly as possible, protecting your own hands and body. Place the victim under a deluge shower. If the chemical got on the victim's exposed skin, such as the hands : Gently and thoroughly wash the contaminated skin with running water and non-abrasive soap. Be particularly careful to clean folds, crevices, creases and groin. Cold water may be used. If irritation persists, seek medical attention. Wash contaminated clothing before reusing.
Serious Skin Contact:
Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial cream. Seek medical attention.
Inhalation: Allow the victim to rest in a well ventilated area. Seek immediate medical attention.

Serious Inhalation:
Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-to-mouth resuscitation. Seek medical attention.
Ingestion:
Do not induce vomiting. Loosen tight clothing such as a collar, tie, belt or waistband. If the victim is not breathing, perform mouth-to-mouth resuscitation. Seek immediate medical attention.
Serious Ingestion: Not available.

Section 5: Fire and Explosion Data
Flammability of the Product: Non-flammable.
Auto-Ignition Temperature: Not applicable.
Flash Points: Not applicable.
Flammable Limits: Not applicable.
Products of Combustion: Not available.
Fire Hazards in Presence of Various Substances: Not applicable.
Explosion Hazards in Presence of Various Substances:
Risks of explosion of the product in presence of mechanical impact: Not available. Risks of explosion of the product in presence of static discharge: Not available.
Fire Fighting Media and Instructions: Not applicable.
Special Remarks on Fire Hazards: Not available.
Special Remarks on Explosion Hazards: Not available.

Section 6: Accidental Release Measures
Small Spill:
Dilute with water and mop up, or absorb with an inert dry material and place in an appropriate waste disposal container.
Large Spill: Oxidizing material. Stop leak if without risk. Avoid contact with a combustible material (wood, paper, oil, clothing...). Keep substance damp using water spray. Do not touch spilled material. Prevent entry into sewers, basements or confined areas; dike if needed. Call for assistance on disposal. Be careful that the product is not present at a concentration level above TLV. Check TLV on the MSDS and with local authorities.

Section 7: Handling and Storage
Precautions:
Keep container dry. Keep away from heat. Keep away from sources of ignition. Keep away from combustible material Do not ingest. Do not breathe gas/fumes/ vapour/spray. Never add water to this product In case of insufficient ventilation, wear suitable respiratory equipment. If ingested, seek medical advice immediately and show the container or the label. Avoid contact with skin and eyes. Keep away from incompatibles such as oxidizing agents, acids.
Storage: Oxidizing materials should be stored in a separate safety storage cabinet or room.

Section 8: Exposure Controls/Personal Protection
Engineering Controls:
Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location.
Personal Protection:
Splash goggles. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing apparatus should be used to avoid inhalation of the product. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this product.

Exposure Limits:
Iodine CEIL: 0.1 (ppm) from ACGIH (TLV) CEIL: 1 (mg/m3) from OSHAConsult local authorities for acceptable exposure limits.

Section 9: Physical and Chemical Properties
Physical state and appearance: Liquid.
Odor: Not available.
Taste: Not available.
Molecular Weight: Not applicable.
Color: Clear Brown. (Dark.) pH (1% soln/water): Neutral.
Boiling Point: The lowest known value is 100°C (212°F) (Water).
Melting Point: Not available.
Critical Temperature: Not available.
Specific Gravity: Weighted average: 1.04 (Water = 1)
Vapor Pressure: The highest known value is 17.535 mm of Hg (@ 20°C) (Water).
Vapor Density: The highest known value is 0.62 (Air = 1) (Water).
Volatility: Not available.
Odor Threshold: Not available.
Water/Oil Dist. Coeff.: Not available.
Ionicity (in Water): Not available.
Dispersion Properties: See solubility in water, methanol, diethyl ether, acetone.
Solubility: Easily soluble in cold water, hot water. Soluble in methanol, diethyl ether. Partially soluble in acetone.

Section 10: Stability and Reactivity Data
Stability: The product is stable.
Instability Temperature: Not available.
Conditions of Instability: Not available.
Incompatibility with various substances:
Reactive with acids. Slightly reactive to reactive with combustible materials, organic materials, metals.
Corrosivity:
Slightly corrosive to corrosive in presence of steel, of aluminum, of zinc, of copper. Non-corrosive in presence of glass.
Special Remarks on Reactivity: Reacts violently with water especially when water is added to the product. (Hydrogen chloride)
Special Remarks on Corrosivity: Not available.
Polymerization: Not available.

Section 11: Toxicological Information
Routes of Entry: Absorbed through skin. Dermal contact. Eye contact. Inhalation. Ingestion.
Toxicity to Animals: Acute oral toxicity (LD50): 14000 mg/kg [Rat]. (Iodine).
Chronic Effects on Humans:
Developmental Toxicity: PROVEN [Potassium Iodide] The substance is toxic to lungs, the nervous system, the eproductive system, mucous membranes, gastrointestinal tract, upper respiratory tract.
Other Toxic Effects on Humans: Hazardous in case of skin contact (corrosive, irritant, sensitizer, permeator), of ingestion, of inhalation.
Special Remarks on Toxicity to Animals: Not available.
Special Remarks on Chronic Effects on Humans: Not available.
Special Remarks on other Toxic Effects on Humans:
Material is extremely destructive to tissue of the mucous membranes and upper respiratory tract. (Hydrogen chloride)

Section 12: Ecological Information
Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term degradation products may arise.
Toxicity of the Products of Biodegradation: Not available.
Special Remarks on the Products of Biodegradation: Not available.

Section 13: Disposal Considerations

Section 14: Transport Information
Special Provisions for Transport: Not available.

Section 15: Other Regulatory Information
Federal and State Regulations:
California prop. 65: This product contains the following ingredients for which the State of California has found to cause cancer, birth defects or other reproductive harm, which would require a warning under the statute: Potassium Iodide California prop. 65: This product contains the following ingredients for which the State of California has found to cause birth defects which would require a warning under the statute: Potassium Iodide Pennsylvania RTK: Iodine; Hydrochloric acid
Massachusetts RTK: Iodine; Hydrochloric acid TSCA 8(b) inventory: Iodine; Potassium Iodide; Hydrochloric acid; Water SARA 302/304/311/312 extremely hazardous substances: Hydrochloric acid SARA 313 toxic chemical notification and release reporting: Hydrochloric acid CERCLA: Hazardous substances.: Hydrochloric acid;
Other Regulations: OSHA: Hazardous by definition of Hazard Communication Standard (29 CFR 1910.1200).
Health Hazard: 3
Fire Hazard: 0
Reactivity: 0
Personal Protection: h
National Fire Protection Association (U.S.A.):
Health: 3
Flammability: 0
Reactivity: 0
Specific hazard:
Protective Equipment: Gloves. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Wear appropriate respirator when ventilation is inadequate. Splash goggles.

Section 16: Other Information
References: Not available.
Other Special Considerations: Not available.

6. Material Safety Data Sheet for Starch Indicator Solution, 0.05%

Section 1: Chemical Product and Company Identification
Product Name: Starch Indicator Solution, 0.05%

Section 2: Composition and Information on Ingredients
Composition:
Name CAS # % by Weight
Salicylic acid 69-72-7 0.62
Water 7732-18-5 99.3
Starch soluble 9005-84-9 0.05
Toxicological Data on Ingredients: Salicylic acid: ORAL (LD50): Acute: 891 mg/kg [Rat]. 480 mg/kg [Mouse]. 1300 mg/kg [Rabbit].
Section 3: Hazards Identification
Potential Acute Health Effects:
Slightly hazardous in case of skin contact (irritant, permeator), of eye contact (irritant), of ingestion. Non-corrosive for skin. Non-corrosive to the eyes. Non-corrosive for lungs.
Potential Chronic Health Effects:
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Mutagenic for bacteria and/or yeast. [Salicylic acid].
TERATOGENIC EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Classified Reproductive system/toxin/female,
Development toxin [POSSIBLE] [Salicylic acid].

Section 4: First Aid Measures
Eye Contact:
Check for and remove any contact lenses. In case of contact, immediately flush eyes with plenty of water for at least 15 minutes. Cold water may be used. Get medical attention if irritation occurs.
Skin Contact:
Wash with soap and water. Cover the irritated skin with an emollient. Get medical attention if irritation develops. Cold water may be used.
Serious Skin Contact: Not available.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical attention.
Serious Inhalation: Not available.
Ingestion:
Do NOT induce vomiting unless directed to do so by medical personnel. Never give anything by mouth to an unconscious person. If large quantities of this material are swallowed, call a physician immediately. Loosen tight clothing such as a collar, tie, belt or waistband.
Serious Ingestion: Not available.

Section 5: Fire and Explosion Data
Flammability of the Product: Non-flammable.
Auto-Ignition Temperature: Not applicable.
Flash Points: Not applicable.
Flammable Limits: Not applicable.
Products of Combustion: Not available.
Fire Hazards in Presence of Various Substances: Not applicable.
Explosion Hazards in Presence of Various Substances: Non-explosive in presence of open flames and sparks, of shocks, of heat.
Fire Fighting Media and Instructions: Not applicable.
Special Remarks on Fire Hazards: Not available.
Special Remarks on Explosion Hazards: Not available

Section 6: Accidental Release Measures
Small Spill:
Dilute with water and mop up, or absorb with an inert dry material and place in an appropriate waste disposal container.
Finish cleaning by spreading water on the contaminated surface and dispose of according to local and regional authority requirements.
Large Spill:
Absorb with an inert material and put the spilled material in an appropriate waste disposal. Finish cleaning by spreading water on the contaminated surface and allow to evacuate through the sanitary system.

Section 7: Handling and Storage
Precautions:
Keep locked up.. Do not breathe gas/fumes/ vapor/spray. Wear suitable protective clothing. If you feel unwell, seek medical attention and show the label when possible.
Storage: Keep container tightly closed. Keep container in a cool, well-ventilated area.

Section 8: Exposure Controls/Personal Protection
Engineering Controls:
Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective threshold limit value.
Personal Protection: Safety glasses. Lab coat.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Boots. Gloves. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this product.
Exposure Limits: Not available.

Section 9: Physical and Chemical Properties
Physical state and appearance: Liquid.
Odor: Odorless.
Taste: Not available.
Molecular Weight: Not applicable.
Color: Colorless. pH (1% soln/water): Neutral.
Boiling Point: The lowest known value is 100°C (212°F) (Water).
Melting Point: Not available.
Critical Temperature: Not available.
Specific Gravity: The only known value is 1 (Water = 1) (Water).
Vapor Pressure: The highest known value is 2.3 kPa (@ 20°C) (Water).
Vapor Density: The highest known value is 0.62 (Air = 1) (Water).
Volatility: Not available.
Odor Threshold: Not available.
Water/Oil Dist. Coeff.: Not available.
Ionicity (in Water): Not available.
Dispersion Properties: See solubility in water, acetone.
Solubility: Easily soluble in cold water, hot water. Soluble in acetone.

Section 10: Stability and Reactivity Data
Stability: The product is stable.
Instability Temperature: Not available.
Conditions of Instability: Incompatible materials
Incompatibility with various substances: Not available.
Corrosivity: Non-corrosive in presence of glass.
Special Remarks on Reactivity: Light, moisture, Iron salts, spirt nitrous ether, lead acetate, iodine (Salicylic acid)
Special Remarks on Corrosivity: Not available.
Polymerization: Will not occur.
Section 11: Toxicological Information
Routes of Entry: Absorbed through skin. Eye contact.
Toxicity to Animals:
LD50: Not available. LC50: Not available.
Chronic Effects on Humans:
MUTAGENIC EFFECTS: Mutagenic for bacteria and/or yeast. [Salicylic acid]. DEVELOPMENTAL TOXICITY: Classified Reproductive system/toxin/female, Development toxin [POSSIBLE] [Salicylic acid].
Other Toxic Effects on Humans: Slightly hazardous in case of skin contact (irritant, permeator), of ingestion, of inhalation.
Special Remarks on Toxicity to Animals: Not available.
Special Remarks on Chronic Effects on Humans:
May affect genetic material (mutagenicity) based on animal studies. May cause adverse reproductive effects. Teratorgenic, Embryotoxic and/or foetotoxic in animal studies. Human: Transferred into maternal breast milk. (Salicylic acid)
Special Remarks on other Toxic Effects on Humans:
Acute Potential Health Effects: Skin: May cause skin irritation. Eyes: May cause eye irritation. Inhalation: May cause respiratory tract irritation. Ingestion: May cause gastrointestinal tract irritation. The toxicological properties of this substance have not been fully investigated.

Section 12: Ecological Information
Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term degradation products may arise.
Toxicity of the Products of Biodegradation: The product itself and its products of degradation are not toxic.
Special Remarks on the Products of Biodegradation: Not available.
Section 13: Disposal Considerations
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental control regulations.

Section 14: Transport Information
DOT Classification: Not a DOT controlled material (United States).
Identification: Not applicable.
Special Provisions for Transport: Not applicable.

Section 15: Other Regulatory Information
Federal and State Regulations: TSCA 8(b) inventory: Salicylic acid; Water; Starch soluble
Other Regulations: Not available. or of its ingredients
Health Hazard: 1
Fire Hazard: 0
Reactivity: 0
Personal Protection: a
National Fire Protection Association (U.S.A.):
Health: 0
Flammability: 0
Reactivity: 0
Specific hazard:
Protective Equipment:
Not applicable. Lab coat. Not applicable. Safety glasses.

Section 16: Other Information
References: Not available.

7. Material Safety Data Sheet for Sodium hydroxide, Pellets, Reagent

Section 1: Chemical Product and Company Identification
Product Name: Sodium hydroxide, Pellets, Reagent ACS

Section 2: Composition and Information on Ingredients
Composition:
Name CAS # % by Weight
Sodium hydroxide 1310-73-2 100
Toxicological Data on Ingredients: Sodium hydroxide LD50: Not available. LC50: Not available.

Section 3: Hazards Identification
Potential Acute Health Effects:
Very hazardous in case of skin contact (corrosive, irritant, permeator), of eye contact (irritant, corrosive), of ingestion, of inhalation. The amount of tissue damage depends on length of contact. Eye contact can result in corneal damage or blindness. Skin contact can produce inflammation and blistering. Inhalation of dust will produce irritation to gastro-intestinal or respiratory tract, characterized by burning, sneezing and coughing. Severe over-exposure can produce lung damage, choking, unconsciousness or death. Inflammation of the eye is characterized by redness, watering, and itching. Skin inflammation is characterized by itching, scaling, reddening, or, occasionally, blistering.
Potential Chronic Health Effects:
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Not available. TERATOGENIC EFFECTS: Not available.
DEVELOPMENTAL TOXICITY: Not available. The substance is toxic to lungs. Repeated or prolonged exposure to the substance can produce target organs damage. Repeated exposure of the eyes to a low level of dust can produce eye irritation.
Repeated skin exposure can produce local skin destruction, or dermatitis. Repeated inhalation of dust can produce varying degree of respiratory irritation or lung damage.

Section 4: First Aid Measures
Eye Contact:
Check for and remove any contact lenses. In case of contact, immediately flush eyes with plenty of water for at least 15 minutes. Cold water may be used. Get medical attention immediately.
Skin Contact:
In case of contact, immediately flush skin with plenty of water for at least 15 minutes while removing contaminated clothing and shoes. Cover the irritated skin with an emollient. Cold water may be used. Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical attention immediately.
Serious Skin Contact:
Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial cream. Seek medical attention.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical attention immediately.
Serious Inhalation:
Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-to-mouth resuscitation. WARNING: It may be hazardous to the person providing aid to give mouth-to-mouth resuscitation when the inhaled material is toxic, infectious or corrosive. Seek immediate medical attention.
Ingestion:
Do NOT induce vomiting unless directed to do so by medical personnel. Never give anything by mouth to an unconscious person. If large quantities of this material are swallowed, call a physician immediately. Loosen tight clothing such as a collar, tie, belt or waistband.
Serious Ingestion: Not available.

Section 5: Fire and Explosion Data
Flammability of the Product: Non-flammable.
Auto-Ignition Temperature: Not applicable.
Flash Points: Not applicable.
Flammable Limits: Not applicable.
Products of Combustion: Not available.
Fire Hazards in Presence of Various Substances: of metals
Explosion Hazards in Presence of Various Substances:
Risks of explosion of the product in presence of mechanical impact: Not available. Risks of explosion of the product in presence of static discharge: Not available. Slightly explosive in presence of heat.
Fire Fighting Media and Instructions: Not applicable.
Special Remarks on Fire Hazards: sodium hydroxide + zinc metal dust causes ignition of the latter. Under proper conditions of temperature, pressure and state of division, it can ignite or react violently with acetaldehyde, ally alcohol, allyl chloride, benzene-1,4-diol, chlorine trifluoride, 1,2 dichlorethylene, nitroethane, nitromethane, nitroparaffins, nitropropane, cinnamaldehyde, 2,2-dichloro-3,3-dimethylbutane.
Sodium hydroxide in contact with water may generate enough heat to ignite adjacent combustible materials. Phosphorous boiled with NaOH yields mixed phosphines which may ignite spontanously in air. sodium hydroxide and cinnamaldehyde + heat may cause ignition. Reaction with certain metals releases flammable and explosive hydrogen gas.
Special Remarks on Explosion Hazards:
Sodium hydroxide reacts to form explosive products with ammonia + silver nitrate. Benzene extract of allyl benzenesulfonate prepared from allyl alcohol, and benzene sulfonyl chloride in presence of aquesous sodium hydroxide, under vacuum distillation, residue darkened and exploded. Sodium Hydroxde + impure tetrahydrofuran, which can contain peroxides, can cause serious explosions. Dry mixtures of sodium hydroxide and sodium tetrahydroborate liberate hydrogen explosively at 230-270 deg. C. Sodium Hydroxide reacts with sodium salt of trichlorophenol + methyl alcohol + trichlorobenzene + heat to cause an explosion.
Section 6: Accidental Release Measures
Small Spill:
Use appropriate tools to put the spilled solid in a convenient waste disposal container. If necessary: Neutralize the residue with a dilute solution of acetic acid.
Large Spill:
Corrosive solid. Stop leak if without risk. Do not get water inside container. Do not touch spilled material. Use water spray to reduce vapors. Prevent entry into sewers, basements or confined areas; dike if needed. Call for assistance on disposal.
Neutralize the residue with a dilute solution of acetic acid. Be careful that the product is not present at a concentration level above TLV. Check TLV on the MSDS and with local authorities.

Section 7: Handling and Storage
Precautions:
Keep container dry. Do not breathe dust. Never add water to this product. In case of insufficient ventilation, wear suitable respiratory equipment. If you feel unwell, seek medical attention and show the label when possible. Avoid contact with skin and eyes. Keep away from incompatibles such as oxidizing agents, reducing agents, metals, acids, alkalis, moisture.
Storage: Keep container tightly closed. Keep container in a cool, well-ventilated area. Do not store above 23°C (73.4°F).

Section 8: Exposure Controls/Personal Protection
Engineering Controls:
Use process enclosures, local exhaust ventilation, or other engineering controls to keep airborne levels below recommended exposure limits. If user operations generate dust, fume or mist, use ventilation to keep exposure to airborne contaminants below the exposure limit.
Personal Protection:
Splash goggles. Synthetic apron. Vapor and dust respirator. Be sure to use an approved/certified respirator or equivalent. Gloves.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Vapor and dust respirator. Boots. Gloves. A self contained breathing apparatus should be used to avoid inhalation of the product. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this product.
Exposure Limits:
CEIL: 2 from ACGIH (TLV) [United States] [1995] Consult local authorities for acceptable exposure limits.

Section 9: Physical and Chemical Properties
Physical state and appearance: Solid.
Odor: Odorless.
Taste: Not available.
Molecular Weight: 40 g/mole
Color: White. pH (1% soln/water): 13.5 [Basic.]
Boiling Point: 1388°C (2530.4°F)
Melting Point: 323°C (613.4°F)
Critical Temperature: Not available.
Specific Gravity: 2.13 (Water = 1)
Dispersion Properties: See solubility in water.
Solubility: Easily soluble in cold water.

Section 10: Stability and Reactivity Data
Stability: The product is stable.
Instability Temperature: Not available.
Conditions of Instability: Not available.
Incompatibility with various substances:
Highly reactive with metals. Reactive with oxidizing agents, reducing agents, acids, alkalis, moisture.
Corrosivity: Not available.
Special Remarks on Reactivity:
Hygroscopic. Much heat is evolved when solid material is dissolved in water. Therefore cold water and caution must be used for this process. Sodium hydroxide solution and octanol + diborane during a work-up of a reaction mixture of oxime and diborane in tetrahyrofuran is very exothermic, a mild explosion being noted on one occassion. Reactive with water, acids, acid chlorides, strong bases, strong oxidizing agents, strong reducing agents, flammable liquids, organic halogens, metals (i.e aluminum, tin, zinc), nitromethane, glacial acetic acid, acetic anhydride, acrolein, chlorohydrin, chlorosulfonic acid, ethylene cyanohydrin, glyoxal, hydrochloric acid, sulfuric acid, hydrosulfuric acid, nitric acid, oleum, propiolactone, acylonitrile, phorosous pentoxide, chloroethanol, chloroform-methanol, tetrahydroborate, cyanogen azide, 1,2,4,5 tetrachlorobenzene, cinnamaldehyde. Reacts with formaldehyde hydroxide to yield formic acid, and hydrogen.
Special Remarks on Corrosivity: Very caustic to aluminum and other metals in presence of moisture.
Polymerization: Will not occur.

Section 11: Toxicological Information
Routes of Entry: Absorbed through skin. Dermal contact. Eye contact. Inhalation. Ingestion.
Toxicity to Animals:
LD50: Not available. LC50: Not available.
Chronic Effects on Humans: Causes damage to the following organs: lungs.
Other Toxic Effects on Humans:
Extremely hazardous in case of inhalation (lung corrosive). Very hazardous in case of skin contact (corrosive, irritant, permeator), of eye contact (corrosive), of ingestion, .
Special Remarks on Toxicity to Animals:
Lowest Published Lethal Dose: LDL [Rabbit] - Route: Oral; Dose: 500 mg/kg
Special Remarks on Chronic Effects on Humans: May affect genetic material (mutagenic). Investigation as a mutagen (cytogenetic analysis), but no data available.
Special Remarks on other Toxic Effects on Humans:
Acute Potential Health Effects: Skin: May be harmful if absorbed through skin. Causes severe skin irritation and burns. May cause deep penetrating ulcers of the skin. Eyes: Causes severe eye irritation and burns. May cause chemical conjunctivitis and corneal damage. Inhalation: Harmful if inhaled. Causes severe irritation of the respiratory tract and mucous membranes with coughing, burns, breathing difficulty, and possible coma. Irritation may lead the chemical pneumonitis and pulmonary edema. Causes chemical burns to the respiratory tract and mucous membranes. Ingestion: May be fatal if swallowed. May cause severe and permanent damage to the digestive tract. Causes severe gastrointestinal tract irritation and burns. May cause perforation of the digestive tract. Causes severe pain, nausea, vomiting, diarrhea, and shock. May cause corrosion and permanent destruction of the esophagus and digestive tract.

Section 12: Ecological Information
Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term degradation products may arise.
Toxicity of the Products of Biodegradation: The product itself and its products of degradation are not toxic.

Section 13: Disposal Considerations
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental control regulations.

Section 14: Transport Information
DOT Classification: Class 8: Corrosive material
Identification: Sodium hydroxide, solid UNNA: 1823 PG: II

Section 15: Other Regulatory Information
Protective Equipment:
Gloves. Synthetic apron. Vapor and dust respirator. Be sure to use an approved/certified respirator or equivalent. Wear appropriate respirator when ventilation is inadequate. Splash goggles.

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