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Eugenol extraction by chromatography
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Recommended: Eugenol extraction by chromatography
The purpose of this lab was to recover as much eugenol and acetyleugenol from 25 grams of cloves as possible. This lab was completed over the course of two days. The first day was dedicated to using simple distillation to collect 70 mL of distillate. The eugenol and acetyleugenol would later be recovered from the distillate. The second day was dedicated to separating the desired products from the distillate and from each other. This day was far more labor intensive and led to the completion of the lab. This lab utilized various techniques such as distillation, extraction and rotary evaporation. Separation, extraction, and recovery are key themes highlighted in this lab. Knowing where both eugenol and acetyleugenol were was vital to accomplishing …show more content…
The recovery of eugenol and acetyleugenol was the objective of the lab. Due to this, it is important to note where eugenol and acetyleugenol were during each phase. Separation is done through the use of a separatory funnel. Different solutions were mixed in the separatory funnel and allowed to settle. Once settled, two distinct layers formed: one aqueous and one organic. The layers are then drawn off individually and the layer without the eugenol/acetyleugenol is discarded. The extraction portion of the lab takes place through the addition of various solvents. The eugenol and acetyleugenol were both solved in water to begin. Methylene chloride was added to the aqueous solution containing the eugenol and acetyleugenol. Once mixed the methylene chloride formed an organic layer which contained the eugenol and acetyleugenol. The aqueous layer became useless as the desired products were no longer in it. Sodium hydroxide was then added to the methylene solution which caused two distinct layers to form. The sodium hydroxide layer now contained the eugenol and the methylene chloride layer now contained the acetyleugenol. At that point, the methylene chloride layer containing the acetyleugenol was treated with anhydrous
The boiling point of the product was conducted with the silicone oil. Lastly, for each chemical test, three test tubes were prepared with 2-methylcyclohexanol, the product, and 1-decene in each test tube, and a drop of the reagent were added to test tubes. The percent yield was calculated to be 74.8% with 12.6g of the product obtained. This result showed that most of 2-methylcyclohexanol was successfully dehydrated and produced the product. The loss of the product could be due to the incomplete reaction or distillation and through washing and extraction of the product. The boiling point range resulted as 112oC to 118oC. This boiling point range revealed that it is acceptable because the literature boiling point range included possible products, which are 1-methylcyclohexene, 3-methylcyclohexene, and methylenecyclohexane, are 110 to 111oC, 104oC, and 102 to 103 oC. For the results of IR spectroscopy, 2-methylcyclocahnol showed peaks at 3300 cm-1 and 2930 cm-1, which indicated the presence of alcohol and alkane functional group. Then, the peak from the product showed the same peak at 2930 cm-1 but the absence of the other peak, which indicated the absence of the alcohol
Firstly, an amount of 40.90 g of NaCl was weighed using electronic balance (Adventurer™, Ohaus) and later was placed in a 500 ml beaker. Then, 6.05 g of Tris base, followed by 10.00 g of CTAB and 3.70 g of EDTA were added into the beaker. After that, 400 ml of sterilized distilled water, sdH2O was poured into the beaker to dissolve the substances. Then, the solution was stirred using the magnetic stirrer until the solution become crystal clear for about 3 hours on a hotplate stirrer (Lab Tech® LMS-1003). After the solution become clear, it was cool down to room temperature. Later, the solution was poured into 500 ml sterilized bottle. The bottle then was fully wrapped with aluminium foil to avoid from light. Next, 1 mL of 2-mercaptoethanol-β-mercapto was added into fully covered bottle. Lastly, the volume of the solution in the bottle was added with sdH2O until it reaches 500 ml. The bottle was labelled accordingly and was stored on chemical working bench.
The objective of this experiment was to perform extraction. This is a separation and purification technique, based on different solubility of compounds in immiscible solvent mixtures. Extraction is conducted by shaking the solution with the solvent, until two layers are formed. One layer can then be separated from the other. If the separation does not happen in one try, multiple attempts may be needed.
Separations are important techniques in chemistry that are used to separate various components of a mixture. They are carried out by mixing two immiscible liquids containing certain solutes together in a separatory funnel, allowing them to separate, then extracting the distinct layers that form. The ratio of the concentration of solute present in the upper layer to the concentration in the lower layer is called the partition coefficient. The efficiency of a separation is described by this partition coefficient. If the coefficients for the two layers are largely different, then the separation can be carried out in a single step. If they aren’t, a more complex process is necessary.1,2 Countercurrent chromatography is a technique used carry out separations in these kinds of cases. It uses a continuous liquid-liquid partitioning process to streamline the usual extraction procedure.
After corking and inverting the reaction tube, the organic layer was removed and transferred to another reaction tube. Then another increment of 0.5 mL of methylene chloride was added to the first reaction tube and the extraction process was repeated. This was done a total of three times. Then in step thirteen, about five scoops of anhydrous sodium sulfate was added to the second reaction tube. Then a filter pipette was prepared and the organic solution from the second reaction tube was added to the pipette.The mixture was allowed to gravity filter and an additional 0.5 mL increment of methylene chloride was added into the pipette and the process was repeated again. Then in step 18, the collected solutions poured onto a watch glass. It was observed that the pre-weighed watch glass weighed 26.196 grams. The watch glass was placed over the beaker that was filled with 30mL of water. It was observed that it took about fifteen minutes for the solvent
The purpose of this experiment is to learn how to use fractional distillation to separate a mix of isopropyl acetate and toluene, redistill them, and use gas chromatography to examine the separation.
The lab begins with reflux of the reaction to form an ester, followed by several extractions from an organic layer. To purify the ester, the compound is dried by gravity filtration with a drying agent, distilled using simple distillation, and recrystallized. The aldol condensation is reacted in a test tube and the solute is collected via vacuum filtration and recrystallized. The esterification procedure was performed first. To begin the lab, the heating mantle was set at the 6 setting, and the hot plate heat was turned on to low.
The purpose of this lab was to experiment with various ways to separate mixtures into its pure components. Depending on whether a mixture is homogeneous or heterogeneous, mixtures can be separated by physical means and their physical properties. In this lab, we used chromatography, which is a technique that uses the differences in physical properties and intermolecular forces of the components in a mixture to separate them. Although there are different forms of chromatography, they all have a stationary and mobile phase. The mobile phase moves through the stationary phase and carries the components of the mixture at different rates. In this lab, paper chromatography and column chromatography will be used.
Introduction: The purpose of this experiment was to isolate eugenol or clove oil from cloves using steam distillation and determine whether it is an efficient way to carry out this experiment. Also, TLC and 1H NMR were preformed to analyze the purity of the isolated eugenol.
That is why ethanol was used as a solvent during this lab, because due to its structure, it has both polar and non-polar regions. Ethanol has a polar alcohol end capable of dipole-dipole interactions and hydrogen bonding, but also has a relatively non-polar CH3CH2- end with mostly London dispersion forces (LDFs). The general rule for solubility is, “like dissolves like,” meaning that polar solutes will dissolve in polar solvents and non-polar solutes will dissolve in non-polar solvents. Once extracted, performing a simple separation known as thin layer chromatography (TLC), the extract can be verified to see if it contains eugenol. TLC uses ethyl acetate (a polar solvent) in order to dissolve the molecules (also polar) in the extract. The polar solvent also contains hexane (a non-polar solvent) which allows for the polar molecules to precipitate out as small spots on the TLC plate. As shown in Figure 4, the solvent will move up the TLC plate until it reaches the spotted samples: cloves extract (Our), nutmeg extract (Oth), and 10 mg/mL eugenol standard (s). Several spots on the TLC plate show the interaction between molecules in the extract and the silica on the surface of the TLC plate. If the molecules in the extract exhibit more non-polar characteristics, they will get pulled further up the
Performing this experiment, we used the technique called Acid-Base extraction to isolate Eugenol, which is one of the main ingredients of clove oil. Acid-Base extraction is the most efficient method for isolating organic component; it is efficient because it purifies the acid and base mixture based on their chemical identities. We have seen throughout this experiment that acid and base play an important role, when it comes to solubility in water. Our basic knowledge of acid and base is acid is a proton donor and base is a proton acceptor. This ideology helps us to understand why organic compounds are not soluble in water. When compounds tend to be insoluble, we have to use acid and base reaction, to change its solubility. The changes that occurred
In this experiment, the goal is to separate naphthalene and benzoic acid from one gram of a crude mixture containing them both, using extraction. A general requirement of a solvent in extraction is solvating one of the pure compounds in solution but not the other. Position in the separatory funnel is determined by density of each layer. The denser layer will be on the bottom of the separatory funnel while the less dense layer will be the top layer of the separatory funnel. For extraction to be used as an effective method for separation, the components of a mixture that need to be recovered must not be soluble in the same solvent. Benzoic acid is not soluble in water, but is soluble in diethyl ether. In benzoic acid, the benzene ring is nonpolar
Eugenol was extracted from cloves through the process called steam distillation. A total of 50ml of distillate were collected with temperature monitoring for every 5.0ml of collected liquid. The distillation curve showed that the temperature of volatilization of eugenol is from 98°C to 99°C which is way below its boiling point at 2540C. Chemically active extraction was conducted in order to remove impurities particularly eugenol acetate and caryophyllene. This involves the addition of several solvents particularly hexane, NaOH, HCl, then hexane again in succession.
The objective of the experiment Fractional Distillation and Gas Chromatography was to determine the organic liquids existent in 30 mL of an unknown mixture. This can be accomplished by fractional distillation. Distillation is a technique that allows one to separate liquids by boiling the liquids and which removes water from its impurities. Simple Distillation separates out a liquid/solid mixture. If the boiling point is greater than 40 degrees Celsius then simple distillation will be able to be used to separate two liquids, if not then Simple Distillation cannot be used. Fractional distillation splits two liquids and transfers them to their pure form by using their boiling points. In order for Fractional Distillation to be used, the boiling point has to be less than 40 degrees Celsius. The only difference between them is that in fractional distillation a column runs to the flask while in simple distillation there is no column. Of the two main types of distillation, Simple and Fractional, Fractional distillation is the one that is used to split the liquids. To get this experiment unde...
We recommend that the liquid-liquid extraction column in the senior laboratory be used more. The process is very interesting and appears to work well.