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Using thin layer chromatography to separate mixture
Thin layer chromatography lab report discussion
Thin layer chromatography lab report discussion
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In this experiment, the following chemicals were used; benzocaine, benzoic acid, ethyl acetate, sodium hydroxide, acetone, sodium benzoate, hydrogen chloride, methylene chloride, and glacial acetic acid. In this experiment, acetone was used to make sure that the glassware being used was clean and dry and there was not any residue of leftover chemicals. Benzocaine, a local anesthetic, and Benzoic acid, a mild irritant, are the two products that were to be isolated and cleaned up using various techniques in this experiment. Ethyl Acetate was mixed with the unknown benzoic acid sample and acted as the solvent while Sodium Hydroxide acted as the aqueous solution in the seperatory funnel technique and was to be drained off leaving only the organic …show more content…
The solvents used in this experiment were sodium hydroxide as the aqueous layer and the ethyl acetate and unknown benzocaine as the organic phase. These phases are separated with an emulsion line which is a distinct line that shows where the aqueous and organic layers meet but do not mix. This method of separation relies on portioning the preferential dissolution of a compound into one solvent over another (2). Figure 2 also shows that when a solvent is used that is lighter than water, density < 1, the organic phase will be on the top in the separatory funnel, while solvents denser than water, density > 1, will sink to the bottom of the funnel (2). The success of the separatory funnel technique allowed for Thin Layer Chromatography (TLC) and Infrared Spectroscopy (IR) analysis. A Digi-Melt apparatus was used to measure the melting points of the benzoic acid and benzocaine samples which were extracted using the separatory funnel. Based on the observed melting point ranges for each sample, purity could be determined. A tight melting point range that is very close to the reference melting point is considered to be very pure. This is when the range is ~2 ̊C, but is not within 5 ̊C of the reference melting point range
The goal of this two week lab was to examine the stereochemistry of the oxidation-reduction interconversion of 4-tert-butylcyclohexanol and 4-tert-butylcyclohexanone. The purpose of first week was to explore the oxidation of an alcohol to a ketone and see how the reduction of the ketone will affect the stereoselectivity. The purpose of first week is to oxidize the alcohol, 4-tert-butylcyclohexanol, to ketone just so that it can be reduced back into the alcohol to see how OH will react. The purpose of second week was to reduce 4-tert-butylcyclohexanol from first week and determine the effect of the product's diastereoselectivity by performing reduction procedures using sodium borohydride The chemicals for this lab are sodium hypochlorite, 4-tert-butylcyclohexanone
The primary goal of this laboratory project was to identify an unknown compound and determine its chemical and physical properties. First the appearance, odor, solubility, and conductivity of the compound were observed and measured so that they could be compared to those of known compounds. Then the cation present in the compound was identified using the flame test. The identity of the anion present in the compound was deduced through a series of chemical tests (Cooper, 2009).
In a separate beaker, acetone (0.587 mL, 8 mmol) and benzaldehyde (1.63 mL, 16 mmol) were charged with a stir bar and stirred on a magnetic stirrer. The beaker mixture was slowly added to the Erlenmeyer flask and stirred at room temperature for 30 minutes. Every 10 minutes, a small amount of the reaction mixture was spotted on a TLC plate, with an eluent mixture of ethyl acetate (2 mL) and hexanes (8 mL), to monitor the decrease in benzaldehyde via a UV light. When the reaction was complete, it was chilled in an ice bath until the product precipitated, which was then vacuum filtrated. The filter cake was washed with ice-cold 95% ethanol (2 x 10 mL) and 4% acetic acid in 95% ethanol (10 mL). The solid was fluffed and vacuum filtrated for about 15 minutes. The 0.688 g (2.9 mmol, 36.8%, 111.3-112.8 °C) product was analyzed via FTIR and 1H NMR spectroscopies, and the melting point was obtained via
The purpose of the experiment was to use the method of simple distillation to separate hexane, heptane, and a mixture of the two compounds into three different samples. After separation, gas chromatography determined the proportions of the two volatile compounds in a given sample.
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,
Chromatography is the laboratory technique for separating mixtures into their components for analyzing, identifying, purifying or quantifying the mixtures or components. The mixture dissolved in the mobile phase (gas or liquid) is passed through the stationary phase (liquid or solid), which separates the analyte from the other molecules in the mixture. The differences in the migration rate of the compounds in these two phases effects the separation.
Ensure gloves are worn at all times when handling strong acids and bases within the experiment of the preparation of benzocaine. 4-aminobenzoic acid (3.0g, 0.022 moles) was suspended into a dry round-bottomed flask (100cm3) followed by methylated sprits (20 cm3). Taking extra care the concentrated sulphuric acid of (3.0 cm3, 0.031 moles) was added. Immediately after the condenser was fitted on, and the components in the flask were swirled gently to mix components. It should be ensured that the reactants of the concentrated sulphuric acid and the 4-aminobenzoic acid were not clustered in the ground glass joint between the condenser itself and the flask. In order to heat the mixture to a boiling point, a heating mantle was used and then further left for gently refluxing for a constituent time of forty minutes. After the duration of the consistent forty minutes the rou...
The theoretical yield of the m-nitrobenzoate was de-termined to be 4.59 grams. The actual amount of crude product was determined to be 3.11 grams. The percent yield of the crude product was determined to be 67.75 %. The actual amount of pure product formed was found to be 4.38 grams. The percent yield of the pure product was determined to be 95.42%. Regarding the thin layer chromatography, the line from the solvent front was 8 centimeters.
In order to separate the mixture of fluorene, o-toluic acid, and 1, 4-dibromobenzene, the previously learned techniques of extraction and crystallization are needed to perform the experiment. First, 10.0 mL of diethyl ether would be added to the mixture in a centrifuge tube (1) and shaken until the mixture completely dissolved (2). Diethyl ether is the best solvent for dissolving the mixture, because though it is a polar molecule, its ethyl groups make it a nonpolar solvent. The compounds, fluorene and 1, 4-dibromobenzene, are also nonpolar; therefore, it would be easier for it to be dissolved in this organic solvent.
The purpose of these lab was to help students understand the chromatographic techniques of column chromatography and Thin layer chromatography. Column chromatography is used to help students understand the relationship between eluting power and polarity. Eluting power is defined as the ability of the mobile phase to move a substance from stationary phase. The polarity of the solvent used in the lab can be described as Methanol> acetonitrile>acetone>ethyl acetate> hexane in decreasing order. Since Methanol and acetonitrile are more polar, they will easily separate methylene blue and methyl orange wh while other solvents will take longer time to separate. In the case of hexane, on the dyes did not separate at all and they slightly separated
A line was drawn approximently one centimeter from the triangle. This line represented the “start line” for the experiment. Using the mortar and pestle, a large piece of spinach and 5 ml of 90% isopropyl alcohol was grinded until a thick liquid was created. Chromatography solvent (90% Isopropyl Alcohol) was then placed into a Microcentrifuge tube and eight drops was transferd onto the line of the chromatography paper using the capillary tube. One Centimeter of the chromatography solvent was added to the chromatography jar and the chromatography paper was placed in the jar so the tip of the triangle dipped into the solvent. After 15 minuets the chromatography paper was observed and the results were recorded. When the solvent line reached approximately one centimeter from the top of the chromatography paper, the paper was removed and observations of the furthest point of the solvents progress was recorded before the line
Mixed melting point was used to confirm the identity of the product. The smaller the range, the more pure the substance. When the two substances are mixed; the melting point should be the same melting range as the as the melting range obtained after filtering. If the mixed melting point is lower one taken from the crystals, then the two substances are different.
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
Chromatography is the technical term for a set of laboratory approaches for the separation of mixtures (Solid/Liquid/Gas). The mixture is dissolved in a fluid which called the mobile phase, which carries it through a structure holding another material known as the stationary phase. The various constituents of the mixture transport at different velocities, causing them to separate. The separation is mainly based on differential partitioning between the mobile and it’s stationary phases. Subtle differences in a compound's partition coefficient result in differential retention time on the stationary phase and thus changing the separation (Tomer, et al., 1994).
When benzoic acid paired with 1.0 M NaOH, it was observed that both compounds were soluble. Upon the addition of 6.0 M HCl into this solution, benzoic acid became insoluble. Benzoic acid was also insoluble in 1.0 M HCl. Ethyl 4-aminobenzoate was found to be insoluble in 1.0 M NaOH and soluble in 1.0 M HCl. But then, after adding 6.0 M NaOH into the test tube C (mixture of ethyl 4-aminobenzoate and 1.0 M HCl), a white powdery solid (undissolved compound) was formed. These demonstrate that both the acid and base became more soluble when they were ionized and less soluble when they were