Simple Distillation and Gas Chromatography The objective of the lab was to purify compounds that can be turned into gas at a reasonable temperature without using decomposition. Gas chromatography was also used to identify the proportions of the volatile compound in the different samples. The mixture of hexane and octane was assigned to me and my partner. The apparatus for simple distillation was assemble using a thermocouple, air condenser, distillation head, metal keck clamps, and a conical reaction vial. The joints of the glassware were greased before assembly. Four boiling chips were placed in the conical ration vial before it was assembled. After being assigned a mixture, 3.5 mL of the mixture was put into a reaction vial. The apparatus …show more content…
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
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
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
The purpose of this lab is to separate a mixture and determine the percentages of each of the ingredients. Each substance will have a different boiling point due to its intrinsic properties and from that, we will be able to determine the purity of different products as we evaporate off the next level of product.
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
2.) Assemble an apparatus for steam distillation using a large (250-500ml) boiling flask and a steam trap, and have your instructor check your apparatus. Apparatus was successfully assembled.
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.
The boiling range of the 1-pentyl ethanoate distillate was approximately between 149-151°C. This was indicated by the formation of the distillate and when the mixture of the purified 1-pentyl ethanoate started to vigorously
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.
A good yield of isopentyl acetate was obtained during this experiment. Loss of the product was likely through transferring liquid from separatory funnel to the Erlenmeyer flask and residual material left in the distillation flask. Using an organic solvent like benzene or cyclohexane as a transfer agent would improve the yield, since their boiling points were around 80 oC and could be easily separated from the final product through simple distillation. However this
Gas-liquid chromatography (GLC) is a process where an unknown organic sample is dissolved in a solvent then vaporised to separate it into its’ components. This is carried out by using two phases; the stationary phase and the mobile phase. The mobile phase is the gas containing the sample and the stationary phase is a liquid absorbed in a solid support. The liquid can be changed depending on the mixture being tested, so the stationary phase is packed in to a long, thin tube called the column (4college, 2016). Gas-liquid chromatography has many uses in forensic chemistry such as determining the identity of a fuel used in a deliberately lit fire.
In gas chromatography, the components of the sample, (which can be called solutes or analytes), separate between two phases – a stationary phase that has a large surface area and a gas phase that permeates through the stationary surface (McNair & Miller, 1998). The technique begins when a few microliters of liquid sample are injected into a port and it becomes vaporized to a gas in the chamber. This starts the mobile phase (also known as the carrier gas). Then, an inert carrier gas is fed into the injection port chamber containing the sample in gas form, and pushes the gas molecules through (Hübschmann, 2001). It is important that the carrier gas is inert so that it doesn’t react with the different molecules of the sample we are trying to separate. Once in this first chamber, it begins to heat and travel through a long coiled tube called a gas chromatography (GC) column.
Chromatography is a method of analysis in which mixture is partially or completely separated into its components according to relative attraction of the component towards stationery and mobile phase. After the mixture is added to stationery phase, mobile phase is allowed to pass through the stationery phase continuously starting at that point where the sample is added. The mixture is divided between the stationery and mobile phase and move along with the mobile phase, the rate at which it passes through stationery phase depend upon its attraction towards mobile and stationery phase i.e if it has more attraction with mobile phase it will move faster and vice versa.