10mL Mass of dry purified aspirin Pharm. Polymorphism in Aspirin, 20mL Melting Point of Acetylsalicylic Acid, Sorry, but copying text is forbidden on this website. The wide melting point range of our recrystallized aspirin indicates that our sample was not entirely pure and contained impurities within. Pharm. For millennia humans have looked to the natural world for substances with medicinal properties (Trost, 2008). Once cool, the flask was put in an ice bath and left for 12 minutes. Mulley, B.A. This led him to synthesize the first pure sample of acetylsalicylic acid. Soc., 1964, 1964, 6036-48. uses its best efforts to deliver a high quality copy of the Preparation of Crude Aspirin Temperature range of crude sample For example, water is an excellent solvent for the recrystallisation of benzoic acid. Making the paper: technique cuts time and resources to make complex potential drug. Its acid dissociation constant (pKa) is 3.5 at 25 °C (77 °F). Chem. Despite the less than percent success of our experimentation we were able to draw some very sound conclusions from our data. The melting point range of pure aspirin is 138-140 C and the melting point range of the salicylic acid starting material is 158-161 C. If impurities are present in your crude sample, the melting point range This new derivative of salicylic acid contained the same analgesic, antipyretic, and anti-inflammatory properties of salicylic acid without the same undesired side effects (Sneader, 2000). The aspirin was prepared through the synthesis of salicylic acid and acetic anhydride in the presence of a catalyst before crystallizing it. Secondly, once we have dissolved and during the second round suction filtration in attempt to obtain the pure aspirin, we forgot to use 2 filter papers but instead use only one on the Buchner funnel. Reighsanstalt thermodmeter; Uncertainty assigned by TRC = 1.5 K; Best value for dried samples in capillary tube. However there is also another possibility for the lower percent yield value. Only the duplicate of method 2 gave a melting point close to the actual melting point of aspirin. K; indentified as polymorphic form IV by DSC; Uncertainty assigned by TRC = 6. ; Holden, E.F., This low percent yield leads me to conclude that the relative efficiency of our synthesis techniques could be improved. The percentage error for our experimentation when considered in conjunction with the wide melting point temperature range implies much about the actual purity of our recrystallized aspirin sample. Approx 30mL of hot distilled water is added to the solution. SRD 103b – Thermo Data Engine (TDE) for pure compounds, K; deterimined with hot-stage microsope. values due to impurities, not polymorphism; Uncertainty assigned by TRC = 5. method, not ground; Uncertainty assigned by TRC = 2. This might have affected the results. K; by differential thermal analysis Concludes that various m.p. Nature, 456(7221), xii. The procedure performed in our experiment involved chemically reacting salicylic acid and acetic anhydride in order to form acetyl salicylic acid. meets USP testing specifications, Aspirin United States Pharmacopeia (USP) Reference Standard, TOP 3 largest production factory in China, o-Acetylsalicylic acid 2-Acetoxybenzoic acid. The delocalized electrons then, in the presence of the alcohol, rearrange in such a manner as to create a temporary bond between the two reactants. K; by U.S.P.X method, ground; Uncertainty assigned by TRC = 2. Moreover, these assignments are performed by professional writers and researchers and can serve as exemplars of quality academic writing. From Wikipedia. Experimental Organic Chemistry. Born on January 21, of 1868 in Germany Felix Hoffman studied chemistry and pharmacy at the University of Munich and obtained his Doctoral degree there in 1894. All you need to do is fill out a short form and submit an order. Chem., 1924, 16, 778. Khim., 1960, 34, 845. Melting Point of Acetylsalicylic Acid, Warmed. Silberberg, M. S. (2012). Crude product collected was dissolved in approx 5mL of ethanol in a 100mL conical flask. This difference in solubility at hot versus cold temperatures is essential for the recrystallisation process. 0000002068 00000 n
K; with "hot stage"; Uncertainty assigned by TRC = 10. Firstly, after the obtaining the crude product from the first suction filtration, we had to transfer it to the conical flask to carry out recrystallisation. Solid Dispersion of Pharmaceutaical Ternary Systems I. Warner, T. D. & Mitchell, J. You can get your custom paper from The experiment very much went as expected as the aspirin gotten at the end of the product was considered pure as its temperate range falls almost within the intended target. The yield is just the amount of product you obtain from a reaction. Experimental Data/Methods Then, determine the melting point of aspirin using necessary apparatus. [all data], Reychler, 1908 As for recrystallisation of aspirin, collected crude product prepared in preparation of aspirin which is impure is dissolved in ethanol and hot distilled water is added to the solution. 0000002919 00000 n
Felix Hoffmann, a German chemist, produced a stable form of acetylsalicylic acid, more commonly known as aspirin… Finally the objective of the experiment is met and the results were acceptable as it is quite accurate. ; Herron, C.S., Constitution of Tannins, 3mL If you continue to use this site we will assume that you are happy with it. All relevant data and observations were recorded. J. Pharm. 3 to 4 drops of conc. ; Enever, R.P., Conclusion Pharmacol., 1972, 24, 169. Appl., 1920, 2, 379. The melting point of aspirin.....27 6. The actual yield of the crude aspirin was 2.023g with a percent yield of 77.81%. The main point of the experiment was to recrystallise aspirin that was prepared so as to purify the compound. We use cookies to ensure that we give you the best experience on our website. Ind. Firstly we have to prepare aspirin. The recrystallized aspirin was dried in an oven and then massed. Reichsanstalt thermometer; Uncertainty assigned by TRC = 0.5 K; in Dahm melting point apparatus, Hg-in-glass thermometer, graduated 0.1 deg., calibr. While well formed crystals are expected to be pure because each molecule or ion must fit perfectly into the lattice as it leaves the solution. Ahrens, C., Putnam, M.E., In addition, the solvent may be ‘trapped’ (in liquid state) within the crystal formed, and this phenomenon is known as inclusion. Experimental Measurements at 130 deg; Uncertainty assigned by TRC = 4. shall not be liable for any damage that may result from Both capillary tubes, crude and recrystallized, were melted in the Mel-Temp apparatus, in order to determine the melting point temperature range. Chem., 1918, 10, 288. However, our samples were most likely mainly compromised by the presence of water due to incomplete drying of our samples. A fume hood is a large piece of equipment five enclosed sides of a work area, the bottom of which is most commonly located at a standing work height. G. Chim. The percent yield of the aspirin obtained from my experiment is 46.3% yield. 12 minutes However, the low percent yield can also mean that the reactant has not reacted completely or the reaction is not complete. Mixture is heated for 10 to 15 min to complete reactions. The mixture is heated in water bath for 10 to 15 minutes in order to complete the reaction. The median melting point temperature of the recrystallized aspirin was 131.5oC.