Fractional Distillation and Gas Chromatography Lab Report Introduction: Distillation is a method of separating two volatile chemicals on the basis of their differing boiling points. During this lab, students were given 30 mL of an unknown solution containing two colorless chemicals. Because the chemicals may have had a relatively close boiling point, we had to employ a fractional distillation over a simple distillation. By adding a fractionating column between the boiling flask and the condenser, we were able to separate the liquids more efficiently due to the fact that more volatile liquids tend to push towards the top of the fractionating column, thereby leaving the liquid with the lower boiling point towards the bottom. After obtaining the distillates, we utilized a gas chromatograph in order to analyze the volatile substances in the gas phase and determine their composition percentage of the initial solution. Overall, through this lab we were able to enhance our knowledge on the practical utilization of chemical theories, and thus also demonstrated technical fluency involving the equipment. Data and Results: Throughout the experiment, the color of the solution remained colorless. At first, the temperature jumped to 60°C and the liquid of the lower boiling point started to evaporate, condense, and collect in the Falcon tube. Through the first and second receiving tube, the temperature stayed constant at 60°C. However, once I switched to the third receiving tube, the
8. The Tubes were observed for a final 5 minutes, noting any color changes in the solutions.
14 mL of 9 M H2SO4 was added to the separatory funnel and the mixture was shaken. The layers were given a small amount of time to separate. The remaining n-butyl alcohol was extracted by the H2SO4 solution therefore, there was only one organic top layer. The lower aqueous layer was drained and discarded. 14 mL of H2O was added to the separatory funnel. A stopper was placed on the separatory funnel and it was shaken while being vented occasionally. The layers separated and the lower layer which contained the n-butyl bromide was drained into a smaller beaker. The aqueous layer was then discarded after ensuring that the correct layer had been saved by completing the "water drop test" (adding a drop of water to the drained liquid and if the water dissolves, it confirms that it is an aqueous layer). The alkyl halide was then returned to the separatory funnel. 14 mL of saturated aqeous sodium bicarbonate was added a little at a time while the separatory funnel was being swirled. A stopper was placed on the funnel and it was shaken for 1 minute while being vented frequently to relieve any pressure that was being produced. The lower alkyl halide layer was drained into a dry Erlenmeyer flask and 1.0 g of anhydrous calcium chloride was added to dry the solution. A stopper was placed on the Erlenmeyer flask and the contents were swirled until the liquid was clear. For the distillation
Solid impurities and liquid impurities having quite different boiling points are most easily removed by distillation, but even liquids having similar boiling points can be separated. For easy separations, a "simple distillation" apparatus (Figure 1) will be used for the first part, but for more accurate separations, a "fractional distillation" apparatus (Figure 2) is necessary. In this lab we will be using both apparatuses. Unfortunately, each time a distillation is run, material is lost. Some evaporates into the air and some is left behind, stuck to the apparatus. That is why fractional distillation is the best apparatus to use. It is important to keep a careful record of the temperature at the beginning and end of every fraction you collect. Stop the distillation by removing the heat just before all the liquid in the distilling flask is completely gone. Watching the rate of temperature increase is important, allowing the temperature to increase too quickly can cause impurity. The distillation curves for our simple and fractional distillation clearly demonstrate that fractional distillation separates the two compounds more
Whereas for simple distillation, the compounds need to be around 80C apart in order for proper separation to occur. Thus, cyclohexane and toluene were not able to be properly separated since the boiling point for cyclohexane was 80.74C while the boiling point of toluene was 110.6C—there two boiling points are fairly close to one another. Thus, the mole fraction for cyclohexane and toluene were fairly low when compared to cyclohexane and
1.5mL of phosphoric acid including 3-4 boiling chips were also added to the 25mL flask. The short path distillation apparatus was set up as shown in Figure 1. A heating mantle was used to heat up the 25mL flask. The solution was distilled to the receiving flask until a small amount of liquid remained in the initial RBF flask. At this point the presence of thick grey smoke pulling over into the entire apparatus was observed. The apparatus was then left to cool down. Through the use of pasture pipette, the aqueous layer from the distilled solution was drawn out. Sodium carbonate was then added to the remaining organic solution in order to check the pH and to verify the basicity of the solution. The aqueous layer was again drawn out from the solution. Next, 0.5g of sodium sulfate was added to the remaining organic layer and was swirled until the liquid appeared to be dry and clear. The alkenes were transferred into a clean 10mL flaks using another clean pasture pipe. The apparatus from the first distillation was rinsed off with
Method: Distillation is based on the fact that the matter can exist in three phases - - solid, liquid and gas. As the temperature of a pure substance is increased, it passes through these phases, making a transition at a specific temperature from solid to liquid (melting point--mp) and then at a higher temperature from liquid to gas (boiling point--bp). Distillation involves evaporating a liquid into a gas phase, then condensing the gas back into a liquid and collecting the liquid in a clean receiver. Substances that have a higher boiling point than the desired material will not distill at the
Objective: The main goal of this lab is to learn how separation of binary liquid mixtures is performed. Especially when the two liquids have boiling points varying by about 30° C. Hexane can be separated from toluene in this experiment because of the difference in their boiling points. Since toluene has a higher boiling point, it will left at the bottom while the hexane starts to boil out and collect in the Hickman still. GC measurements help us in determining how accurate our data is by making a graph of the amount of hexane and toluene in each fraction. Also this lab gives experience with semi-micro
In this experiment, distillations were done. This is a technique that utilizes the differing boiling points of two or more compounds in a mixture in order to separate the compounds from the mixture. The way fractional distillation works is that the initial mixture is boiled up to the point of the lower boiling point compound; this compound then evaporates. This compound is then
Simple distillation is more effective when the two components of a mixture have a difference in boiling point that is greater than 50°C. This large difference makes the need for theoretical plates non-existent since there is no need for multiple distillations per fraction. We can collect all necessary data from a simple distillation fraction using a gas chromatograph. The gas chromatograph vaporizes the injected sample and it begins to undergo partitioning. It is pushed into a small heated column that is coated in the liquid form of the sample. The longer the substance stays inside the column before passing over the heated wire, the longer the retention time is. The retention time is utilized to identify the substance, while the number of peaks shows how many substances are present, and the size of the peaks show how much percentage each substance occupies in a sample. The intrinsic properties of isopropyl acetate and toluene allow analysis of the provided data to become quite simple. Isopropyl acetate has a lower boiling point because it has a relatively low dipole moment and only one double bond. Thus, the intermolecular forces are relatively low in isopropyl acetate leading to a low boiling point. Toluene has a higher boiling point because the methyl group, attached to the benzene
Simple distillation is a separation technique which can be used to separate and purify distillates from a liquid mixture which ideally contains one volatile and one non-volatile compound. If such ideal conditions are not possible—as is usually the case—then simple distillation can be applied as long as the liquid in question is composed of compounds that differ in volatility such that their boiling points differ by at least 40 to 50 degrees Celsius. Because
1.) Briefly explain the concept of steam distillation. What is the difference between a simple distillation and a steam distillation? When a mixture of two immiscible liquids are distilled it is referred to as codistillation. This process is referred to as steam distillation when one of the liquids is water. This distillation is used to separate organic liquids from natural products and reaction mixtures in which the final product results in high boiling residues such as tars, inorganic salts, and other relatively involatile components. It is useful in isolating volatile oils from various parts of plants and not useful in the final purification of a
There was no distillate in the distillation head after 20 minutes on the setting of 40 so the Variac transformer was turned to 45. The first fraction was collected at 55.6°C. The ratio of hexane to octane was 87.437% to 12.563%. The second fraction was collected between 47.3°C and 40.5°C. 88.429% to 11.571% was the ratio of hexane to octane for this fraction. The third fraction was collected at 30.6°C, and the ratio of hexane to octane was 94.957% to 5.043%. The contents of the conical reaction vial were placed in a fourth vial and a chromatogram was obtained for it. The ration of hexane to octane was 7.501% to 92.499%. During the collection of the three fractions, a piece of the glass pipet broke off into the distillation head. The results of the experiment could have been incorrect because the glassware was not properly cleaned. The distillate also could have collected too fast which would have lowered the separations efficiency. From this information, infer that hexane has a lower boiling point than octane because most of the distillate was hexane. The majority of what was left in the conical reaction vial was octane because the temperature was not hot enough to turn it into a gas to go into the distillation
The purpose of this experiment was to separate a two component mixture using fractional distillation. Distillation is a process of vaporization than condensation of a substance, used primarily to separate substances from a mixture when there are different boiling points. Fractional distillation is when the mixture has multiple substances with similar boiling points, and a fractional column is used to create multiple vaporization/condensation cycles. Fractional distillation is important when two or more substances need to be separated, but they have similar boiling points.
In this lab, extractions, classification tests, and a distillation was performed in order to isolate two natural products, eugenol and limonene. In the isolation of limonene, steam distillation was used to obtain the water insoluble oil. This was done with 10.01g of orange peel and 50mL of water. Once heated, a 30mL distillate was obtained. This was a mixture of water and the organic compound of limonene. In order to isolate the limonene, 5.0mL of ethyl acetate was added to the water and limonene mixture and two layers were separated. The two layers that formed were clear in color, but had distinct consistencies. The bottom layer looked very thick, while the top looked thin and moved quicker than the bottom layer. The top layer is to one that
Objectives of this experiment included determining whether ethanol can be separated by distillation leaving a concentrated dye powder behind, driven by the heat of your hand and learning the process of distillation from the hand boiler.