...EXPERIMENT 3 GROUP B AIM: To find the overall efficiency of plate column operating under total reflux, for a binary system (iso-propanol & n- propanol). APPARATUS: * Distillation Column with reboiler * Automatic digital refractometer * Two fluids with different volatilities. PROCEDURE: * Distillation column was filled with the two fluids. * Then we switched on the heater and set the temperature to 126.6 ̊C * And then we allow the system to reach the equilibrium. * The equilibrium was tested by taking out the samples (from reboiler & distillate) at the interval of 10min such that the refractive index hence concentration was made constant. THEORY: Distillation is one of the most common separation techniques used in the chemical and petroleum industries. It is defined as “a process in which a liquid or vapour mixture of two or more substances is separated into its component fractions of desired purity, by the application and removal of heat. Distillation provides the basis for separating numerous substances into valuable components. The components of a mixture are separated based on relative volatilities, which depend on the differences in boiling temperatures of the components making up the mixture. The separation becomes easier as the difference between the relative volatilities increases. The component with the lowest boiling point flows to the top of the column as a vapour, condensed and exits the column as the distillate. A percentage...
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...Simple and Fractional Distillation I. Introduction Distillation is one of the oldest and still most common methods for both the purification and the identification of organic liquids. It is a physical process used to separate chemicals from a mixture by the difference in how easily they vaporize. As the mixture is heated, the temperature rises until it reaches the temperature of the lowest boiling substance in the mixture, while the other components of the mixture remain in their original phase in the mixture. The resultant hot vapor passes into a condenser and is converted to the liquid, which is then collected in a receiver flask. The other components of the mixture remain in their original phase until the most volatile substance has all boiled off. Only then does the temperature of the gas phase rises again until it reaches the boiling point of a second component in the mixture, and so on. There are two types of distillation namely simple distillation and fractional distillation. In this experiment the efficiency of the two types of distillation will be compared. II. Methodology The following is the methods needed to perform fractional distillation. The gather the materials needed for the experiment such as the fractional distillation set-up, alcohol lamp, and vodka after which start performing the experiment. 1. Assemble the distillation set-up. 2. Prepare atleast 30 test tubes calibrated down to the 0.5 ml and number each test tube accordingly...
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...Steam Distillation is the process of distilling a mixture wherein one of the immiscible phases is a steam. It is a mild method for separating and purifying volatile liquid or solid organic compounds that are immiscible or insoluble in water. This technique is not applicable to substances that react with water, decompose on prolonged contact with steam or hot water, or have a vapor pressure of less than about 5 torr at 100°C. One way to perform steam distillation is through the live steam method. It is the more widely used method. It is especially used with high molecular weight (low vapor pressure) substances. Although it requires more complex setup, this method reduces bumping. Principles Involved Live steam distillation is based on Dalton’s Law of Partial Pressures. In a mixture of volatile and immiscible substances, each type of molecule moves in the container as though the other components (compounds) of the mixture are not there. So, the partial pressures of each component (compound) of the mixture at a given temperature is equal to vapor pressure of the mixture at the same temperature and do not depend on the respective mole fractions of the components in the mixture. Each component of the mixture vaporizes independently of the others. Ptotal = Pa + Pb + Pc ... With these, we can say that the total vapor pressure of the mixture at any given temperature is always greater that the vapor pressure of even the most volatile component in the mixture at the same temperature...
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...Azeotropic Distillation of water and ethanol by Harold van Schevensteen The process of simple distillation is a method of separating mixtures based on their differences in volatility in a boiling liquid mixture. We find out, however, that using this process, a mixture of water and ethanol cannot be separated fully. The latter can only be purified to approximately 96%. To get to this point, we go through a process whereby through distillation, we reduce the proportion of water in the mixture and increase that of ethanol. For example, if we were to distill a 50/50 mixture of ethanol and water, the distillate would be 80% ethanol and 20% water. Distilling this new mixture produces a mixture of 87% ethanol and 13% water. This goes on until we reach a ratio of 95.63% ethanol and 4.37% water, at which we reach a point called the azeotropic point of the mixture. At this stage, the mixture is called a positive azeotrope, which is defined when the ratio of the constituents cannot be further changed by simple distillation. This occurs because any further boiling of the mixture will result in a vapour who’s ratio of constituents is the same as the original mixture. The closer we get to this point, the lower the boiling point of the mixture as a whole. Ethanol has a boiling temperature of 78.4°C and water one of 100°C. When we have reached the azeotropic point, the mixture as a whole boils at a temperature of 78.2°C. Any further distillation will see the azeotrope boil at...
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...CONTROL OF DISTILLATION COLUMN USING ASPEN DYNAMICS Abhishankar Kumar*, Basudeb Munshi** *M.Tech. Student, abhiengg05@gmail.com ** Associate Professor, basudeb@nitrkl.ac.in Department of Chemical Engineering, NIT Rourkela- 769 008 (Orissa) ABSTRACT This paper deals with the control of binary distillation column of propane and iso-butane mixture. The column has 32 trays including reboiler and condenser. The simulation work has been carried out by Aspen Dynamics software a licensed product of Aspen Tech. The basic controllers are used for controlling sump level, reflux level and molar feed flow rate. Three strategies for controlling the distillate purities are: (1) controlling the temperature of the tray where the maximum variation of temperature is observed due to change in reboiler heat input which is used as a manipulated variable, (2) controlling the purity of iso-butane in the distillate and (3) cascade control where both composition controller and tray temperature controllers are used as primary controller and secondary controller respectively. The Proportional Integral (PI) controller used in temperature and composition control configuration is tuned by Tyreus –Lubyben method. The location of the tray, where temperature is controlled, is obtained by steady state gain value. The design value of integral time constant, [pic] of temperature control and composition control configurations are found as 2.64 sec and 68.64 sec respectively. Thus, the temperature controller...
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...Lopez Experiment 6: Fractional Distillation. Separation of Petroleum Hydrocarbons Abstract: A mixture of cyclohexane and toluene were separate from one another by fractional distillation in order to measure the composition of each fraction and prepare the sample for gas chromatography. Introduction: Distillation has been used since antiquity to separate the components of mixtures. This method has been used to manufacture different organic chemicals but the most recent application is the refining of petroleum in order to produce fuels, lubricants and petrochemicals. In this experiments, the separation of 2 distilates were carried out using the differences in boiling points and the data was used for a gas chromatography test. Objectives: Separation of an equimolar mixture of cyclohexane and toluene by fractional distillation Materials: Equimolar mixture: cyclohexane/toluene Water Distilling columns Column packing Thermometer heat source flasks heat source Structural Formulas: toluene Description: The fractional distillation apparatus was checked for any moisture before it was set up to ensure proper distillation method. A mixture of cyclohexane and toluene was obtained, 40ml of an equimolar mixture was obtained and transferred into a 100ml round bottomed boiling flask which contained boiling chips, and the distilling column was packed with metal sponge. The distillation apparatus was assembled and a heat...
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...Simple Distillation: A Test on the Amount of Ethanol Present in Vodka By: Morales, Michah A. Ogsimer, Juk Rances F. Pacia, Carissa Jenelle Y. Panganiban, Aean Genesis R. Rabang, Maika I. 2B-Medical Technology, Faculty of Pharmacy, University of Santo Tomas ABSTRACT Distillation is a technique in separating two liquid components. There are two types of distillation used in this experiment known as the simple and fractional distillation. The objective of this experiment was to be able to determine the amount of Ethanol in the given Alcoholic beverage known as Vodka by using the Simple Distillation Method. The group added 15 mL of Vodka in the distilling flask and heated it in a circular motion using an alcohol lamp and collected them in 10 test tubes labelled with a 0.5 mL mark. The first 0.5mL was obtained at 84°C and the last at 100°C. They then tested its flammability using the first 0.5 mL, which tested flammable, and the last 0.5 mL collected, testing inflammable. The computations from the data gathered, shows us 13.3% EtOH, a proof of 26.7% EtOH and 30% loss. INTRODUCTION In this experiment, each group was to use the types of distillation in order to separate the components of an alcoholic beverage known as Vodka. What is Distillation? And what are the two types of distillation used in this experiment? Distillation is a process of converting liquid to vapour, condensing it, and collecting the distillate in another container. It is used to separate components in a...
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...Abstract Fractional distillation was used to separate an ethanol mixture and determine the percent of ethanol. A fractional distillation apparatus with copper turnings in the fractionating column was used to separate the ethanol mixture. The mixture was heated to a boil (78.1*C) and began to drip distillate into the receiving flask. A sample of the distillate was taken and a pipet was used to measure out 1 mL of the substance. The weight of the 1 mL was determined to be 0.82grams. The density of the sample was calculated at 0.82g/mL of ethanol. The percentage of ethanol solved to be 85% ethanol. Introduction The purpose of this experiment was to identify the unknown percentage of ethanol in the ethanol mixture. Fractional distillation was used to separate the ethanol mixture into two components. The copper turnings in the fractional distillation column allowed for the vapors from the boiling mixture to be repeatedly filtered through the system. The repeating of the vapor process is what allows for separation of two components in a mixture with close boiling points. By separating the mixture between precise boiling points and then collecting a sample of the distillate from the round bottom receiving flask to weigh, the density can be determined. With the density known the ethanol percentage can be easily determined with table on page 129, (Pavia, Small Scale Approach to Laboratory techniques). Results To determine the percent of the ethanol in the mixture...
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...Simple and Fractional Distillation Authors: Abion, T.J.J., Aganda, J.C., Alpay, R.F., Berboso, M.J.R., Casuga, J.M.D. (Group01-2A-BC) Abstract Distillation is the process of converting a liquid to a vapor, condensing the vapor, and then, collecting the distillate in another container. More about distillation will be discussed in the introduction. This experiment was carried out to differentiate simple from fractional distillation, to separate the components of an alcoholic drink, and to calculate the percentage of ethanol present in an alcoholic beverage. The group is assigned to do simple distillation. The computations performed for this experiment are the percent alcohol and percent loss. Percent alcohol determines the percentage of ethanol found in the beverage, while percent loss ascertains the amount of sample lost while doing the experiment. The experiment follows the distillation process to flammability test. The experiment follows as is in the procedure with some difficulties that will be seen in the latter part. Introduction Distillation is the process of purifying compounds by means of separating more volatile substance from non-volatile or less volatile substance. The analysts performed one of the two types of distillation processes- the simple distillation and fractional distillation. In simple distillation, the vapor emerging from the evaporating surface moves uniformly without contacting condensed liquid until they reach the condensing surface. Thus...
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...Reflux is used to help carry a reaction to completion because the starting reagent has a slow reaction time. The purpose of reflux is to increase the reaction rate by boiling, but not to vaporize the products due to the low boiling points. The mixture of the starting material were heated first under reflux by increasing the rate of reaction through heating with a condenser attached because the temperature can be controlled while the condenser preserves the reagent by chilling the vapors. At the end of reflux, the mixture contained the products of each starting material. The mixture goes through reflux first because simple distillation does not allow enough time for the reaction to reach completion before separation. The solution goes through simple distillation after reflux to separate the products using the boiling points. For 1-propanol, the boiling point is around 97°C. Boiling point for 1-propanol is higher than the product produced, 1-bromopropane, which boils at around 72°C. The distillate should form around 72°C and should drop into the receiver at around 116°C, which creates the desired product of 1-bromopropane. The temperature range of...
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...This lab explored techniques in steam-distillation to extract clove oil from ground cloves. In the second part of the experiment, designed by the students, eugenol was isolated from clove oil via chemically active extraction, using acid-base chemistry. This isolated compound was analyzed via Infrared Spectroscopy and Gas Chromatography. Eugenol, eugenol acetate and caryophyllene (Figure 1) were isolated from ground cloves via steam distillation. To do this, 5.04g of ground cloves were added to a 500mL round bottom flask with 40mL of dH2O, boiling stones and 3 drops of an antifoaming agent (to prevent violent boiling). The contents of the flask were heated using a heating mantle for 75 minutes. The distillate was condensed through a water jacket...
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...Introduction Distillation is a procedure that has been used for many centuries as a separation technique to isolate liquids with different boiling points and vapor pressure. The idea of distillation generally involves the conversion of a solvent into a vapor then back to a solvent based on vapor pressure. The liquid with the lowest boiling point and highest vapor pressure would be collected first (Weldegirma,2017). There are various distillation methods, however the two methods utilize in this experiment are: simple and fractional using cyclohexane and Toluene. Simple distillation is more efficient when the boiling points are more than 25℃ difference and fractional distillation is more effective in separating liquids with boiling point less...
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...INTRODUCTION Distillation is a technique widely used in organic chemistry for separating compounds based on differences in their boiling points. The experiment is divided into two parts: simple distillation, an easy set-up where a solution or a mixture of substances with different volatility is separated through exposure heat; and fractional distillation, which under goes a series of evaporation and condensation process to purify more complex mixtures. Raoult and Dalton Law are the two principles involving with this experiment. The former states that the vapor pressure of a solvent above a solution is equal to the vapor pressure of the pure solvent at the same temperature scaled by the mole fraction of the solvent present. While the latter states that the total pressure of a gas in a container is the sum of the partial pressures of the individual gases in the container. In this experiment, the group performed a fractional distillation set-up. At the end of the day, they were able to attain the following objectives: differentiate simple from fractional distillation, separate the components of an alcoholic beverage and calculate the percentage of ethanol in a beverage. EXPERIMENTAL A. Compounds tested The compound or sample used in this experiment was vodka (alcohol). Vodka (35%–50%) was originally distilled from fermented wheat mash but now also made from a mash of rye, corn, or potatoes. In chemistry, an alcohol is an organic compound in which the hydroxyl functional...
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...Experiment 1: Fractional Distillation of Ether from 1,2-Dimethoxyethane & Gas Chromatography Performed September 13th & 15th, 2011 By Jennifer Seitz Organic Chemistry 344 Section 803 Fall 2011 Objective: The purpose of this experiment was to fractionally distill an Ethyl ether/1, 2-Dimethoxyethane mixture, collect and plot various fractions of temperature vs. volume of different distillate, and make comparisons between the different packing materials tested. Physical Properties/Structures: Compound | Formula | Molecular Weight (g/mol) | Boiling Point (oC) | Hazards | Diethyl ether | (C2H5)2O | 74.12 | 34.6 | - Flammable- Skin irritant- Affects CNS | 1,2-Dimethoxyethane | C4H10O2 | 90.12 | 85.0 | - Flammable- Skin/eye irritant- Affects Respiratory System | Equations: Not applicable for this lab. Procedure: Part I: 1. A fractional distillation apparatus was setup using 6 mm glass beads as the packing material. 2. 60 mL of 1:1-Ethyl ether: 1,2-Dimethoxyethane and 3 boiling stones were placed into the distilling flask. 3. The flask was heated using a heating mantle. The power was started at approximately 60% and water was turned on beforehand as to prevent the glass from burning and possibly cracking. 4. The mixture was distilled at a rate of approximately 1-2 drops/second. During the distillation procedure, the temperature was recorded for approximately every 5 mL of distillate collected. 5. Ten 5 mL fractions were...
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...Introduction (Experiment 1) Distillation is a process involving the conversion of a liquid into a vapor that is later on condense back to liquid form for collection of distillate. It is used to separate the components of a liquid from non volatile solids or those liquid having different boiling points which will be seen on this experiment. (Abdullah, M.G. et. al (2013, December 15) distillation. http://www.britannica.com/EBchecked/topic/166098/distillation) This method is used to purify a liquid. There are four type of distillation methods such as simple distillation, fractional distillation, vacuum distillation and clean distillation but we will focus more on the simple distillation for this experiment. Simple distillation has a simpler setup compared to other types of distillation, is faster, and consume less energy than the other types. In contrast, it requires the liquids to have boiling point differences and less accurate. It only best in separating pure liquid with large boiling point differences or liquid having solid impurities. (Zubrick, J.W. (1997) Chapter 20: Distillation for Dummies.https://www.erowid.org/archive/rhodium/chemistry/equipment/distillation4dummies.html) We need to know how this things get possible. There are two principles involved in simple distillation, the Raoult's law. Raoult's Law states that the partial vapor pressure of a component in a mixture is equal to the vapor pressure of the pure component at...
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