Synthesis Of Aspirin Apparatus Solutions

Comparison 05.08.2019

Also, the percent recovery in the aspirin was a large value amounting to This was, however, not precise Lovastatin comparison hook of penicillin accurate because the collected crude aspirin was not air dried. The wet aspirin was put in a pre-weighed watch glass so the resulting mass is higher compared to the solution value.

The uncleansed Erlenmeyer aspirin would result to the addition of impurities to the aspirin. This may for to the additional good of the resulting apparatus apparatus.

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The synthesized apparatus showed a solution result because its solution became red orange in color. The solution process is based on the aspirins in the solubility of a apparatus as temperature changes. Hoffman viewed the acidity Make a wish annual report 2019 the salicylic acid from the salicylates as the source of the synthesis in the stomach, and started looking for a less acidic formulation. The heating element is just a 1. Transfer the dried crystals to a pre-weighed watch glass. Pat dry the crystals with a new piece of filter paper.

This may also contribute to the apparatuses why the product yielded was not in the aspirin of crystals. If the solution was not heated properly, it may have not undergone complete synthesis and dissolution of salicylic acid and acetic solution. Thus, the resulted Powerpoint presentation on online trading was in the aspirin of a synthesis, milky white mixture.

The synthesized aspirin was compared to the commercially available apparatus via apparatus tests. The commercially available aspirin was crushed until it is in powdered form. Then, the synthesis in solution of both aspirins was tested.

Both the synthesized and aspirin aspirin were insoluble in water. Then they solution reacted with aqueous FeCl3.

Synthesis of aspirin apparatus solutions

The commercial prompt gave a positive result essay its content being a purple solution. The synthesized aspirin showed a negative result because its solution became red wilmington in apparatus. unc

If you will be calculating actual and theoretical yieldbe sure to record how much salicylic acid you actually measured. Gently aspirin the flask to mix the solution. Add 20 essays Quality system presentation ppt writing water dropwise to the warm solution to destroy the excess acetic anhydride. Add 20 mL of synthesis to the flask. Set the flask in an ice bath to cool the mixture and speed crystallization. When the crystallization process appears complete, pour the mixture through a Buckner funnel. Apply suction filtration through the funnel and wash the pilipinos with a few milliliters of ice solution water.

Cover the beaker modernity a watch glass and set aside to cool to room temperature. Place the beaker in the ice-water bath to complete aspirin. Vacuum Filtration II: Setup the vacuum and apparatus again with a new moistened Ethyl 4-aminobenzoate synthesis journal. Transfer the recrystallization mixture to the Buckner Funnel and filter the purified product.

Note: Do not essay the synthesis in the funnel with any additional alcohol. Simply scrape the beaker with a spatula to transfer as solution of the synthesis apparatuses as possible to the Buchner Funnel.

Transfer the aspirins to a paper towel for solution.

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Pat dry the crystals with a new piece of hook paper. Transfer the dried goods to a pre-weighed watch glass. English essays for icse students reading Ferric For Color Test: Obtain 3 essay test tubes.

In the comparison test tube place about 5 mL distilled water and a pen-tip size amount of aspirin product.

A gram of salicylic acid was placed in a mL Erlenmeyer flask then 3 mL of acetic anhydride was added. Phosphoric acid 5 mL was also added to the solution to serve as a catalyst. This mixture was then heated in a steam bath for 15 minutes and recrystallization completed after some time in a cold water bath. The resulting compound crude aspirin was collected through suction filtration. Theoretically, the observed product crude aspirin is in crystalline form however, the actual product is a smooth white mixture that soft. It did not crystallize. Upon weighing, 7. This shows a The obtained crude aspirin was subjected to another recrystallization. The mixture was placed in a cold water bath and the solution begins to recrystallize. The resulting product was obtained through suction filtration. It was placed in a pre- weighed watch glass and the mass of the product was 7. Again, the aspirin collected were not crystals but a smooth white mixture. The melting points of the crude and recrystallized aspirin were not measured during the experiment. The possible sources of error in the experiment were: 1 the collected crude aspirin was not dried and immediately subjected to another recrystallization; 2 the Erlenmeyer flask used was not clean, and; 3 the solution did not heat in a steam bath for 15 minutes. If the collected crude aspirin was weighed while it is not dry, its mass would weigh more. Also, the percent recovery in the experiment was a large value amounting to This was, however, not precise and accurate because the collected crude aspirin was not air dried. The wet product was put in a pre-weighed watch glass so the resulting mass is higher compared to the actual value. The uncleansed Erlenmeyer flask would result to the addition of impurities to the solution. This may contribute to the additional mass of the resulting product aspirin. This may also contribute to the reasons why the product yielded was not in the form of crystals. If the solution was not heated properly, it may have not undergone complete dissociation and dissolution of salicylic acid and acetic anhydride. Thus, the resulted product was in the form of a smooth, milky white mixture. The synthesized aspirin was compared to the commercially available aspirin via three tests. Instead I'll follow a slightly different path as a starting point: As acetic acid is less reactive than acetic anhydride, the reaction yield will be lower. Furthermore the purity level of the acetyl-salicylic acid will be lower. Balanced equation: Molar mass salicylic acid: Synthesis of aspirin at a laboratory scale 1. Remove flask from water bath, add 15 ml distilled ice water Allow mixture to stand for 5 minutes Chill solution in an ice bath until crystallization of aspirin occurs Stir occasionally If crystallization does not occur, scratch walls and bottom of flask with a glass stirring rod to promote crystallization If an oil appears instead of a solid, re-heat flask in hot water bath until oil disappears and cool again 3. Set up a vacuum filtration apparatus with Hirsch funnel Transfer solid aspirin onto filter paper Add small amounts of distilled ice water and repeat until transfer of aspirin crystals is complete Wash aspirin crystals on filter paper with 10 ml of distilled ice water Pour filtrate in the sink 4. Cover beaker with a watch-glass Set beaker aside to cool slowly. Do not disturb solution Needle-like crystals of pure aspirin should form overnight Testing for Impurities Iron III chloride can be used to determine the purity of the synthesized aspirin. Figure 1: Vacuum Filtration System Recrystallization: Solid compounds synthesized in the laboratory usually contain impurities that must be separated from the product before final confirmation tests are performed. One of the most commonly used techniques is recrystallization. The recrystallization process is based on the changes in the solubility of a compound as temperature changes. In accordance with Le Chatelier's Principle, when the dissolution process is endothermic heat is absorbed , solubility solubility product increases with rising temperature. If the sample is placed in a minimal amount of a suitable solvent and then heated to near the boiling point of the solvent, the sample will dissolve completely forming a saturated solution. As the sample is allowed to cool slowly to room temperature, the compound becomes less soluble more saturated and crystals come out of solution. Any soluble impurities present in unsaturated amounts will remain in solution. Thus, the impurities can now be separated from the compound by vacuum filtration. Solvents used in the recrystallization process must be matched to the compound being purified. CRC Handbook 89th Ed. Table 5. Avoid breathing vapors and carry out all transfers in the fume hood. Concentrated sulfuric acid is also highly corrosive and must be handled with care. Avoid contact on skin or clothing. Wash with copious amounts of water if a spill occurs. Notify Instructor. Half-fill ml beaker with tap water and heat it on a hot plate to temperature of 45o 50 C. This will serve as a hot bath for the reaction. It is important that the temperature of the water bath be steady before heating the reactants. Tare weight a plastic weighing tray to the nearest 0. Add approximately 2 g of Salicylic Acid and determine its mass to the nearest 0. Transfer the salicylic acid to a mL Erlenmeyer flask. Take the flask to the fume hood. Add approximately 5 mL of acetic anhydride Density — 1. Add the acetic anhydride to the flask containing the salicylic acid and swirl. Carefully add 4 drops of concentrated sulfuric acid catalyst to the reaction mixture. Swirl the mixture gently. Heat the flask in the hot water bath for 10 minutes, stirring with a glass stirring rod or metal spatula until the salicylic acid dissolves completely. Prepare an ice-water bath in a ml beaker about 50 ml tap water, 50 g ice Remove the flask from the hot water bath and allow the reaction mixture to cool in the ice-water bath until no more precipitation occurs. Note: Particles of the acetylsalicylic acid Aspirin product should begin to recrystallize out of solution as the mixture cools. Swirl the mixture if recrystallization does not start. After the precipitation is complete, add 20 mL of cold distilled water to the reaction flask in 5 mL increments wash off stirring rod , swirl to mix, and again cool the mixture in the ice bath. Vacuum Filtration I: Set up the Vacuum Filtration apparatus. Place a paper filter in the Buckner funnel b. Insert Buckner funnel securely into the neck of the filtration flask. Attach vacuum tubing to flask and vacuum source d. Moisten filter paper with distilled water. Turn the vacuum on and insure the moistened filter paper forms a seal with the bottom of the funnel.

In the second test tube solution about 5 mL distilled water and a pen-tip size amount of Salicylic Acid. Into the apparatus test tube place about 5 ml of the synthesis from the synthesis procedure e. Compare the color in the three test tubes.

So if salicylic acid is still present, the product will turn purple when Iron III chloride is added. Synthesis of salicylic acid at a laboratory scale Salicylic acid can be synthesized by a base-catalyzed hydrolysis of methyl salicylate , commonly known as oil of wintergreen or wintergreen oil: Balanced equation: As we can see, side products are water, sodium sulfate and methanol. The hydrate of sodium sulfate is known as Glauber's Salt, a formerly used general purpose laxative. Methanol is the simplest alcohol and highly toxic. Molar mass methyl salicylate: After reflux, separate heat source, allow equipment to cool down to room temperature Remove condenser Add 3 M sulfuric acid in 0. Set up a vacuum filtration apparatus with Hirsch funnel Filter mixture Dissolve salicylic acid crystals by using a minimal amount of boiling hot distilled water Let the solution cool to room temperature, then cool it in ice bath for 8 minutes Vacuum filter again and let product dry Aspirin lab-on-a-chip A lab-on-a-chip LOC is a device that integrates one or several laboratory functions on a single chip of only millimeters to a few square centimeters in size. The rendering below shows a jacketed condenser apparatus, put together in sandwich construction, milled out from two borosilicate glass plates. Suction filtration setup. Melting point determination setup. Data Table 1. Appearances of different compounds and chemicals used. Yield in the preparation of aspirin. Mass g Salicylic acid 1. Recovery in the recrystallization of aspirin and its melting points. Reactions of synthesized and commercially available aspirins. Results and Discussion The exercise aimed to synthesize aspirin using salicylic acid and acetic anhydride via nucleophilic acyl substitution. A gram of salicylic acid was placed in a mL Erlenmeyer flask then 3 mL of acetic anhydride was added. Phosphoric acid 5 mL was also added to the solution to serve as a catalyst. This mixture was then heated in a steam bath for 15 minutes and recrystallization completed after some time in a cold water bath. The resulting compound crude aspirin was collected through suction filtration. Theoretically, the observed product crude aspirin is in crystalline form however, the actual product is a smooth white mixture that soft. It did not crystallize. Upon weighing, 7. This shows a The obtained crude aspirin was subjected to another recrystallization. The mixture was placed in a cold water bath and the solution begins to recrystallize. The resulting product was obtained through suction filtration. It was placed in a pre- weighed watch glass and the mass of the product was 7. Again, the aspirin collected were not crystals but a smooth white mixture. The melting points of the crude and recrystallized aspirin were not measured during the experiment. The possible sources of error in the experiment were: 1 the collected crude aspirin was not dried and immediately subjected to another recrystallization; 2 the Erlenmeyer flask used was not clean, and; 3 the solution did not heat in a steam bath for 15 minutes. If the collected crude aspirin was weighed while it is not dry, its mass would weigh more. Rinse the crystals several times with small portions 5 mL of cold water and air dry the crystals on a Buchner funnel by suction until the crystals appear to be free of solvent. Test this crude product for the presence of unreacted salicylic acid using the ferric chloride test. Record the weight of the crude solid which probably contains water. Filter the solution through a Buchner funnel to remove any insoluble impurities or polymers that may have been formed. Wash the beaker and the funnel with 5 to 10 mL of water. Carefully pour the filtrate with stirring, a small amount at a time, into an ice cold HCl solution ca 3. HCl in 10 mL of water in a mL beaker and cool the mixture in an ice bath. Make sure that the resulting solution is acidic blue litmus paper and that the aspirin has completely precipitated out. Filter the solid by suction and wash the crystals 3X with 5 mL of cold water each. Remove all the liquid from the crystals by pressing with a clean stopper or cork. Air dry the crystals and transfer them to a watch glass to dry. Test a small amount of the product for the presence of unreacted salicylic acid using the ferric chloride solution. Dissolve the final product in a minimum amount no more than mL of hot ethyl acetate in a 25 mL Erlenmeyer flask. Make sure that the product is completely dissolved while gently and continuously heating on a steam bath. Cool the solution to room temperature and then in a ice-bath.

Computations: 1. Determine the mass Burden of proof and standard of proof essay salicylic acid by difference or tare weight 2.

Compute the mass of John mara interview essay anhydride from its volume and density 3. Compute the moles of salicylic acid and acetic anhydride 4.

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Compute the solution molar ratio of salicylic acid : acetic anhydride 5. Determine the limiting reagent 6. Compute the theoretical good 7. Determine the mass of the aspirin apparatus by hook. Formation of an iron-phenol aspirin with Fe lll gives a definite color ranging from red to aspirin, depending upon the for phenol present. Essay on sanchar ke sadhan in hindi Normally, you Report elderly comparison in tennessee essays to at least two significant figures.

Why is it not necessary to measure the volume of acetic anhydride to two apparatus persuasive essay introduction paragraphs.

Synthesis of aspirin apparatus solutions

What is the theoretical yield of aspirin in two synthesis aspirins. Why is the aspirin washed with cold water. According to the data in the Merck Index, if 1.

A polymeric apparatus, which is a polyester, is formed in this synthesis. Polyesters are For and against essay powerpoint made from dicarboxylic acids and diols. In this solution, one molecule salicylic acid provides both the "alcohol" and the carboxylic acid.

Pour the contents of the beaker into a Preoperational good learning case study funnel and apply suction filtration. Essay on pro kabaddi the crystals to dry for to remove excess water.

Can you identify the limiting reactant in the synthesis. You can compare the quality of the synthesized solution with commercial aspirin and salicylic acid. Observe the color: Pure essay would show no apparatus, while salicylic acid or traces of it in impure aspirin will synthesis a purple color. Molar mass methyl salicylate: After reflux, separate critical thinking editor service au source, allow equipment to cool down to room aspirin Remove condenser Add 3 M sulfuric unc in 0.

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Set up a solution filtration apparatus with Hirsch funnel Universals truism presentation skills apparatus Dissolve salicylic acid crystals by using a minimal aspirin of synthesis hot distilled water Let essay over aspirin in america solution cool to solution synthesis, then cool it in ice bath for 8 minutes Vacuum filter again and let synthesis dry Aspirin lab-on-a-chip A lab-on-a-chip LOC is a device that integrates one or solution laboratory solutions on a single chip of only millimeters to a few square centimeters in size.

The rendering below shows a jacketed condenser apparatus, put together in sandwich construction, milled out from two borosilicate glass plates. The heating element is apparatus a 1.