Recrystallization of aspirin. Synthesis and Recrystallization of Aspirin Lab Report 2022-10-17
Recrystallization of aspirin Rating:
Recrystallization is a common laboratory technique used to purify solid compounds. It involves dissolving the compound in a solvent, allowing it to crystallize out of the solution, and then collecting the purified crystals. The process is often used to purify small amounts of a compound, such as aspirin, which is a widely used nonsteroidal anti-inflammatory drug (NSAID).
Aspirin, also known as acetylsalicylic acid, is a white, crystalline compound that is commonly used to alleviate pain and inflammation. It is synthesized from salicylic acid and acetic anhydride, and is typically sold in the form of tablets. However, the commercial tablets may contain impurities, such as residual reactants and byproducts from the synthesis process, as well as excipients added for stability and ease of manufacturing. These impurities can affect the purity, stability, and effectiveness of the aspirin.
To purify aspirin, it is first dissolved in a suitable solvent, such as water or ethanol. The choice of solvent depends on the solubility of the compound and the impurities present in the sample. For example, water is a good solvent for aspirin, but it may not dissolve impurities such as waxes and oils. On the other hand, ethanol is a better solvent for these impurities, but it may not dissolve aspirin as well as water.
Once the aspirin is dissolved in the solvent, the solution is allowed to cool slowly, either at room temperature or in a cold water bath. As the solution cools, the aspirin begins to crystallize out of the solution. The process is aided by the addition of a seed crystal, which serves as a nucleus for the growth of the purified crystals. The purified crystals are then collected by filtration, and the solvent is removed by evaporation or distillation.
The purity of the recrystallized aspirin can be determined by measuring its melting point, which should be close to the known melting point of pure aspirin. The melting point is a physical property that is highly sensitive to impurities, and can be used to identify and quantify the impurities present in the sample. Other methods, such as infrared spectroscopy and nuclear magnetic resonance spectroscopy, can also be used to confirm the purity of the recrystallized aspirin.
In conclusion, recrystallization is an effective method for purifying small amounts of aspirin, and can be used to produce a high-quality, pure compound. It is a simple and inexpensive process that can be easily performed in a laboratory setting, and can be used to produce aspirin for use in research or other applications.
Recrystallisation Of Aspirin Lab Report
As such, in this experiment, 2. Thus this may have influenced the percent yield as well. Figure 1 Reaction of Acetic salicylic acid with acetic anhydride Salicylic acid reacts with acetic anhydride when an acid is present as a catalyst In this experiment, sulfuric acid, H2sO4 was used as the catalyst. The percent yield was about 76% whereas the temperature range is between 134 to 136 ÌŠÌŠC. Esters are widely used in fragrance and flavour industry. The invention may be carried out by dissolving impure and finely crystalline aspirin in approximately an equal weight of 1,4-dioxane and subsequently slowly cooling the solution to a tempera- 125 ture at which the aspirin crystallizes from solution. Softening point is chosen by method for the utilization of the optimal dissolving gear.
How does recrystallization purify a substance? Once solid dissolved, weigh the watch glass and filter paper, use the filter paper to carry out suction filtration, place crystals on watch glass, weigh the dried crystal and calculate the weight of the aspirin. Water is added once removed from heat with addition of cold water and suction filtration is carried out. As we should wash down the gems before we achieve the suction filtration, a few precious stones would potentially have broken up. This type of group is found in salicyclic acid and ASA. A method which comprises the steps of dissolving crude aspirin in an essentially anhydrous solvent comprising a substantial proportion of 1,4-dioxane as the active dissolving agent, subsequently slowly cooling the solution to below its crystallizing temperature, separating the solvent from the precipitated product, and drying the latter to obtain relatively coarse, free-flowing, monoclinic crystals of acetic and salicylic acidfree aspirin weighing from 8 to 12 grams per cubic inch as determined on a standard Scott volumeter.
Recrystallization Of Aspirin Essay Example for Free
. The reaction above is also known as esterification. In the experiment, sulfuric acid acted as a catalyst and necessary for this reaction to occur. A Guide of Editing Recrystallization Of Aspirin - Mansfield University Of on G Suite Google Workplace is a powerful platform that has connected officials of a single workplace in a unique manner. The desired compound may be lost during recrystallisation if the solvent reacts with the compound. Excedrin Synthesis Lab Report 363 Words 2 Pages Therefore, liquid-liquid and acid-base extraction techniques were successfully performed to separate the components of the Excedrin tablet.
SYNTHESIS AND PURIFICATION OF ASPIRIN OBJECTIVE: 1. Create aspirin by reacting salicylic acid with acetic anhydride in the presence of concentrated phosphoric acid as a catalyst. 2. Collect the crude product prepared in the preparation of aspirin of the impure product and to dissolved it in ethanol and hot boiling water. 3. To determine the percentage of impurity of the product by reading the IR Spectrum. STRUCTURES AND REACTIONS : SOLVENTS STRUCTURES HEXANE ETHYL ACETATE ETHYL ACETATE : HEXANE MIX ACETONE ISOPROPYL ETHER REAGENT TABLE Reagant Molecular Weight (g/mol) Density at 25 ° C (g/mL) Amount (mmoles) Mass (grams) Volume (mL) Molar equivalent Salicylic acid 138.12 g/mol 1.44 g/mL 21.7 mmoles 3.0 g 2.08 mL 1 Acetic anhydride 102.09 g/mol 1.08 g/mL 52.89 mmoles 5.4 g 5 mL 2.4 Conc. H 3 PO 4 (~ 18M) ----------- ---------- ---------- ---------- ------------- Catalyst PROCEDURE & OBSERVATIONS WEEK#1 Procedure Observations WEEK #2 Procedure Observations Solvent Observations at room Observations when the Observations on cooling temperature solvent boils the hot solution Hexane Ethyl acetate Ethyl acetate : hexane mix Acetone Isopropyl Ether CALCULATIONS AND ANALYSIS: Molecular Weight of Salicylic acid : 138.12 g/mol Mass of aspirin: 6.455 g Actual yield: 3.155 g 6.455 g weight of boat with product - 3.3 g weight of boat without product = 3.155 g Theoretical yield : 3.96 g 3.0 g× 1 mol 138.12 g = 0.0217 molof salysilic acid .
. During this framework, there were a few gems that were parted with the passed up method for the breeze and a few flowers poured at the work area as well. The compound from which the active ingredient in aspirin was first derived, salicylic acid, was found in the bark of a willow tree in 1763 by Reverend Edmund Stone of Chipping-Norton, England. Does aspirin have a phenol group? The higher the yield percentage, the higher the purity of the aspirin will be. This technique allows for the purification of a crude material.
Today 80 billion aspirin tablets are taken every year over the al the countries to reduce fevers, relieve pain, and even help prevent heart attacks. Recrystallization is defined as the process in which grains of a crystal structure come in a new structure or new crystal shape. A method which comprises the steps of mixing together approximately equal parts by weight of aspirin needles and 1,4-dioxane, warming the mixture to a temperature at which the aspirin is entirely in solution, slowly cooling the solution to a temperature below its crystallization temperature, separating out the aspirin precipitated therefrom, and drying the same. Sulphuric acid is added and heated for a short period to complete reaction. . What happens to the methanol produced when making aspirin? This may occur due to several factors: While transferring the salicylic acid, some of the solid may stay at the side of the conical flask and even your spactula, and resulting in lesser salicylic acid participating in the process of esterification compared to what have been weighed earlier. When solid broke up, gauge the watch glass and get out paper, utilize the channel out the article to perform suction filtration, precious district stones on a watch glass, gauge the dried gem, and ascertain the heap of the ibuprofen.
It is the expansion of water when completing suction filtration. . How to synthesize aspirin? We will analyze Benzoic Acid as it is dissolved and recrystallized in water and in a solvent of Methanol and water. The purple color indicates the presence of a phenol group. The solubility of ASA increases as temperature increases. Mol of salicylic acid : Mol of Aspirin 1 : 1 Therefore, Mol of Aspirin: 0. Recrystallization is used to purify the compound received from crystallization.
Synthesis and Recrystallization of Aspirin Lab Report
Synthesis of Aspirin is known as esterification. This may have influenced the results. They can easily Alter through their choices. . If the compound is insoluble in the chosen solvent at high temperatures, then it will not dissolve. The crude products obtained from most preparations of organic compounds are contaminated with unreacted starting materials and substances from side-reactions.
Right off the bat, after securing the unrefined item from the primary suction filtration, we expected to change it to the funnel-shaped flagon to do recrystallization. The acetylsalicylic acid will recrystallize, and the solid impurities unreacted salicylic acid should remain dissolved in the solution. The theoretical melting temperature is 140 ÌŠC. Summary This is the "Synthesis and Recrystallization of Aspirin" lab report. However, the low percent yield can also mean that the reactant has not reacted completely or the reaction is not complete. This fine crystalline form is not desirable because of problems in handling, increased shipping costs, the tendency of such product to dust, and certain difficulties encountered in grinding and tableting the aspirin in admixture with starch for commercial distribution. Introduction Organic Synthesis is a branch of chemical synthesis which concentrates on the construction of organic compounds through organic reactions.
Hence, due to the pressure, the filter paper tore and our crude product entered the filter flask that was containing the impurities and other liquid. The anti-inflammatory medicine precious stones are pressed into the excellent little cylinders and guarantee they are entirely packed without air holes. Next, we have to prepare recrystallisation of aspirin. This meant that from the experiment, I only achieved 50. The molecular weight of aspirin is 180. Use the chemicals in your hood area and if you spill any, wash with large amounts of water.
Why is recrystallization used when making aspirin?
The use of such materials as carbon tetrachloride, ethylene o chloride, etc, in conjunction with lA-dioxane not only results in a more readily filterable suspension of crystals following the cooling step, but also serves to further reduce the flammability of the mixture. The temperature is set to 100 ÌŠC and then gradually heated up to determine the melting point. In theory, insoluble impurities can be removed from a compound fairly easily. As the solution cools, crystals of the product will form and soluble impurities will remain in solution. How Aspirin is synthesized? After the warm bath to complete the reaction, we added cold water to quench the reaction hydrolysis of acetic anhydride to prevent further reaction to take place.