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Experiment with fraction distillation
Simple distillation discussion
Fractional distillation of binary liquid solutions
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Recommended: Experiment with fraction distillation
Title: Distillation of Cyclohexane and Toluene
Introduction: The experiment was conducted to show which type of distillation is the most accurate in separating the two liquids. Simple distillation results were compared to the different techniques of fractional distillation in order to show which was the most accurate in separating the liquids.
Procedure: This experiment followed the directions present in the manual for the simple distillation method. 15 mL of the Cyclohexane and Toluene solution was used in the distillation flask and the heating mantle was initially set at 25V. Eventually, our TA suggested to turn up the heating mantle to 50V because the liquid was not boiling after 20 minutes of heat. After the forerun was disposed,
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the collection of the first fraction began at 79oC. During the experiment, the temperature never leveled or dipped after the collection of the first fraction; therefore, with the advice of our TA, the collection of the second fraction started once the temperature reached 95oC and ended once the temperature leveled off at 100oC. Results: Temperature Total Volume Collected 26oC 0 mL 88oC 1.5 mL 90oC 2 mL 91oC 3 mL 92oC 3.5 mL 94oC 4 mL 95oC 5.3 mL 96oC (beginning of second collection) 7.3 mL (2 mL from second collection) 98oC 8.1 mL (2.8 mL from second collection) 100oC 8.3 mL (3 mL from second collection) 100oC 9.1 mL (3.8 mL from second collection) The table above shows how the total volume collected steadily increased as the temperature of the solution increased. Volume of collections and Index of Refractions: Fraction Volume Index of Refraction Undistilled Liquid 15 mL 1.470 First 5.3 mL 1.450 Second 4.1 mL 1.467 Residual 3.6 mL 1.494 The table above shows how the composition of the different fractions are related to each other. The first fraction contained a higher mole fraction of cyclohexane than the original solution, while the residual fraction contained a higher mole fraction of toluene than the original solution. Conclusion: Of the original 15 mL solution, only 13 mL was recovered at the end from the two fractions and the residual liquid. The missing liquid could have leaked out if the joints were not properly clamped together, or some of the material could have stuck to the glass equipment and was therefore not counted in any of the fractional measurements. The composition of the different fractions are related to the different temperatures at which the fractions were collected.
For the first fraction, it was collected at temperatures between 79oC and 95oC. Based on the boiling point of Cyclohexane being 80.7oC and the boiling point of Toluene being 111oC, the first fraction should have been almost completely composed of Cyclohexane. The second fraction was collected at temperatures between 95oC and 100oC and should have been mostly composed of Toluene because the majority of the Cyclohexane should have been in the first fraction. Since the residual liquid was the liquid that had not boiled at a temperature of 100oC, then almost all of that remaining liquid should have been …show more content…
Toluene. In comparing the average mole fraction of Toluene for each fraction of each set-up, the fractional distillation with any type of packing has a significantly smaller mole fraction in the first fraction, which is supposed to be almost pure Cyclohexane.
The average mole fraction for the different types of fractional distillation with packing is less than 0.15; the fractional distillation packed with steel wool had the lowest mole fraction at 0.1386139 and the simple distillation set up had the highest mole fraction at 0.336633663. In the second fraction the mole fractions varied significantly between the different setups. The fractional distillation with steel wool had the lowest average at 0.5293501, while the fractional distillation with the empty column had the highest average at 0.821075. The fractional distillation with beads (mole fraction of 0.7008487) and rings (mole fraction of 0.7095746) had very similar average results, while the simple distillation had a mole fraction of 0.557708628. In the residual fraction, which was supposed to be almost pure Toluene, all of the distillation setups had mole fractions of Toluene above 0.94. The fractional distillation with the empty column had the highest average mole fraction with 0.97843 and the fractional distillation with the steel wool had the lowest average mole fraction with 0.9466054. While the fractional distillation with the empty column had the purest residual liquid remaining, the individual data points for all the
fractions varied significantly more than the individual data points for the fractional distillation with steel wool, beads, or rings. This shows that using packing produces more accurate results in terms of the mole fraction compared to the fractional distillation with an empty column or simple distillation setups. Multiple solutions could be used to improve the results of the distillation. If the temperature of the heating mantle is decreased but still high enough to boil the first liquid, that will help ensure less of the higher boiling point liquid will be collected in the first fraction. For fractional distillation, any way that you can increase the surface area that the vapor goes through in the column will help improve the distillation process. This can be done by increase the length of the column so the vapor goes through a longer length of packing material. Based on the data collected, it shows that fractional distillation is significantly more accurate than simple distillation or fractional distillation with an empty column. While the samples collected in the fractional distillation were not completely pure, they were much closer than the simple distillation. The reason there were still imperfections in the fractional distillation processes could have been not enough packing was used in order to save time. The samples collected could have been closer to their pure form; however, the distillation process would have taken much longer due to the extra packing in the column.
The purpose of this experiment was to learn and preform an acid-base extraction technique to separate organic compounds successfully and obtaining amounts of each component in the mixture. In this experiment, the separation will be done by separatory funnel preforming on two liquids that are immiscible from two layers when added together. The individual components of Phensuprin (Acetylsalicylic acid, Acetanilide, and Sucrose as a filler) was separated based upon their solubility and reactivity, and the amount of each component in the mixture was obtained. Also, the purity of each component will be determined by the melting point of the component.
Alcohol, which is the nucleophile, attacks the acid, H2SO4, which is the catalyst, forming oxonium. However, the oxonium leaves due to the positive charge on oxygen, which makes it unstable. A stable secondary carbocation is formed. The electrons from the conjugate base attack the proton, henceforth, forming an alkene. Through this attack, the regeneration of the catalyst is formed with the product, 4-methylcyclohexene, before it oxidizes with KMnO4. In simpler terms, protonation of oxygen and the elimination of H+ with formation of alkene occurs.
Because of the limited amount of time the student is provided during this lab experiment, the complete amount of distillate was not collected fully due to the procedure being very slow and time consuming. The final eugenol that was isolated was not completely pure, and this is proven by the percent recovery being 110%, which is clearly higher than a 100%. This means that other substances were isolated along with the eugenol oil, such as leftover dichloromethane, which was used in the first place because the water and eugenol did not successfully separate into two layers, thus dichloromethane was added to help separate them. This is was caused percent recovery to be higher than what it should be. Heating and boiling the final solution for a longer time until all the dichloromethane is evaporated completely can easily avoid the presence of
Extraction separates compounds based on their solubility. A separatory funnel allows two distinct layers (aqueous and organic) to form when two immiscible liquids are separated with the more dense liquid on bottom. In this lab, dichloromethane (organic) has a density of 1.33g/mL while water (aqueous) has the density of 1.00g/mL, so dichloromethane will be on the bottom and since “like dissolves like” and eugenol does not dissolve in water but dissolves in dichloromethane, eugenol will be found in the dichloromethane layer.
Use glassware as directed by your instructor. Place a test tube placed inside a beaker with ice water to collect the product from the apparatus. Obtain the 10mL round bottom flask from the apparatus. Obtain two graduated cylinders of 10mL. On one graduated cylinder measure 4mL (85% H3PO4) of Phosphoric Acid and pour into the 10mL round bottom flask. On the other graduated cylinder measure 3mL of Cyclohexanol and pour into the flask as well. With a pipet add 5 drops of Sulfuric Acid (H2SO4) into the flask. Attach the round bottom flask to the distillation apparatus. Place thermometer with rubber stopper on the apparatus to obtain the temperature Start with the water flow through the condenser. Turn on and heat the reaction until the product starts to distill. Distill and collect until thermometer temperature rises to 85˚C. Once there is no more product to collect obtain the test tube of product. Two layers should be formed, top layer of cyclohexane and bottom layer with water. Obtain a pipette and remove the bottom layer (water) if any. Add 10% (5mL) of Sodium Bicarbonate (NaHCO3) to nuclearize any acid in the solution. Mix well and remove once again the bottom layer of water with pipette. Add 5mL of water and mix well to wash the top layer. After the two layers form again, remove entirely the bottom layer of water and add a few pellets of Calcium Chloride. Obtain a 50mL or 100mL beaker and weigh.
Variables --------- During the experiments, the water will be heated using different spirit burners containing different alcohols. I will be able to change different parts of the experiment. These are the. Volume of water heated:
Methanol, acetone, dichloromethane, toluene, and hexanes were tested for their miscibility with water. Methanol and acetone were found to be miscible with water, and dichloromethane, toluene, and hexanes were immiscible. Two layers—one organic and one aqueous—were observed each time an immiscible solvent was combined with water. Dichloromethane was observed as the bottom layer, and toluene and hexanes were observed as the top layers when added to test tubes of water. In Table 1 below, density, boiling point, and miscibility with water are shown for the organic solvents used in this experiment.1
The objective of this experiment was to use a common method of separation distillation. Distillation can be used in purifying or separating liquids, when the liquid if heated the more volatile component, the molecule with the lower boiling point, vaporizes and can be condensed. This type of separation will work efficiently when the feed mixture has a decent range between the boiling points of the components. The relationship between component’s vapor pressure to the composition of the solution is Ptotal==P1+P2, Raoult’s Law. This can be used with Dalton’s Law of partial pressure,
This experiment required the used of reflux to heat the mixture because it is a technique that does not lose any liquid due to evaporation. A reflux apparatus is capped so that vapors do not escape and the system is contained resulting in a larger end product. The reason for using a distillation technique was to produce an individual component of the starting compound, here 1-propanol and 2-pentanol. Drying is a very important step because if the product is wet, it will have added incorrect water weight. Before drying, first the product must be separated from the organic layer. The reason for applying the reflux method over simple distillation is simply because the reflux is set up to return the condensed distillate to the flask. This allows it to boil, yet lose no solution. Simple
Determination of concentration of vanilla in this experiment involves three main steps, which are extraction of the vanillin from the other components of the essence using an organic solvent, back extraction of the vanillin as its sodium salt into aqueous phase using dilute sodium hydroxide and determination of the concentration of vanil...
The purpose of this experiment is to measure the effect of flow rates on distilled water by recording its volume every second.
In this experiment, the process of steam distillation was used to purify a natural product, (the essential oil of spearmint). This phenomenon works because when two immiscible liquids are distilled, the boiling point of the mixture is below the boiling point of the both pure compounds. Since water has a significantly lower boiling point than spearmint, a much greater proportion of water molecules was vaporizing at any time during the distillation. Even though the components of spearmint oil have low vapor pressure, they are volatile enough to vaporize to some extent and a small amount will lifted off with the water molecules. This boiling will occur when the independent internal vapor pressures are equal to 760 torr, which is the external vapor pressure. It is noted that steam distillation, unlike regular distillation, it does not follow Raoult’s Law.
The catalytic process occurs at lower temperature anf offers higher selectivity but requires frequent regeneration of the catalyst. Then, the products are cooled and introduced into a pair of separators which separate the unreacted hydrogen. The unreacted hydrogen is compressed and recycle back to the feed and reactor. The products that leaving the separators are heated before introduced into a distillation column which the toluene is separated from the stream and recycle back to the...
With purer component separation with greater efficiency, distillation is one of promising technique. Investigation on distillation processes found out a number of methods and designs of distillation fitting to different applications. A number of factors that affect the distillation performance and depend upon feed material include distillation column choice, conditions, design parameters, and so on. For instance, vacuum distillation is applied for pressure sensible feed materials, fractional distillation mainly petroleum, while simple distillation to binary mixture of components with different volatilities and so on. The simple binary distillation column sizing method normally involves finding the number of stages from a x-y diagram, the temperature of the distillate and bottoms product using a Txy diagram. The operating lines for the bottom and top of the column depend on the reflux ratio and the condition of the
The separation was successful and produced separated stages consistent with prediction based upon solubility properties. This was indicated by the qualitative tests and observations.