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Introduction-Experiment The Percent Composition of an Aspirin Tablet
Aspirin is a substance commonly found in medicine cabinets around the word. It is one of the least expensive and most useful drugs. The precursor to modern day aspirin was found in the bark of willow trees and used by people for thousands of years to alleviate pain.
Aspirin tablets (5-grams) are usually compounded of about 0. g of acetylsalicylic acid pressed together with a small amount of filler, which binds the ingredients and in the case of aspirin, counteracts the acidity (Verdel).
Most aspirin tablets contain small amount of binder, which helps prevent the tablets form crumbling. The binder is chemically inert and was intentionally added by the manufacturer, but its presence means that aspirin tablets do not have 100 percent purity.
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In this experiment we determined the percentage of acetylsalicylic acid in an aspirin sample by means of a titrimetric analysis.
Methods-Experiment 1 Synthesis, Purification and Characterization
In the synthesis part of the experiment 0.06 moles of salicylic acid, which was converted to grams, was added in a 50mL Erlenmeyer flask. Also, 0.106 mole of acetic anhydride was added in the 50mL Erlenmeyer flask. When the salicylic acid and the acetic anhydride were mixed 1-mL of acid catalyst was carefully added to the flask. A thermometer was placed in the mixture and the temperature was noted while the mixture was being stirred. The temperature should increase initially and it should decrease as the aspirin crystals form. After the mixture was mixed 50mL of ice cold deionize water was added to the flask and set in an ice bath until crystals appear. Finally, when the crystals appear it was collected by vacuum filtration and was washed three times with ice cold deionize water. Then the product was air-dried. After the product was dried the mass was determined and the percent yield was calculated.
Some of the original product was saved for characterization by melting point and TLC, thin layer chromatography. The remaining dried sample was placed in a flask and about mL of ethyl alcohol was added into the flask to dissolve the crystals. The solution was gently warmed in a hot water bath for approximately 5 minutes. The solution was removed from the hot water bath and placed in an ice bath for complete crystallization. After the crystallization was completed the sample was collected by vacuum filtration then air-dried. After the product was dried the mass of the recrystallized sample was determined. After the mass was determined the percent yield was calculated.
The left over product was used to calculate the melting point of the starting material, salicylic acid, as well as that of the known sample of acetylsalicylic acid. Then the results were compared to those of the pure samples. Thin layer chromatography was used to further indicate the purity of the samples. A small sample of SA, ASA, and synthesized aspirin in methanol was prepared. A TLC plate was spotted with all four samples. The TLC was developed in a jar, which contains a developing solution of ethyl acetate-ethanol-acetic acid. A UV lamp was used to detect the spots on the thin layer chromatography. The distance the spots travel was measured and the Rf value was calculated.
Results-Experiment Kinetics of Hydrolysis of ASA
A. Determination of Peak Absorbance for Fe(+) Complex of SA
Figure .1 illustrates the maximum absorbance is 55nm which as a wavelength of 0.48. A bell curve somewhat formed indication that there was an increase then a constant wavelength, then a gradual decrease.
B. Compare the Effect of FeCl() on ASA and SA
Table .1 Shows that the addition of FeCl() has a greater effect on SA than ASA, due to the increase in wavelength at 55nm.
Absorbance at 55nm
ASA0.
SA1.10
C. Determine the Effect of Concentration of ASA and Amount of FeCl() Present on the formation of the Iron-Salicyclic Acid Complex
Table . Illustrates how time increases the absorbance level.
Time(minutes)15045060750
Tube A.050.0610.080.160.151.05
Tube B.0.140.18..15.170
Tube C1.0740.0510.080.11.10.180
Tube C.050.080.8.180.60.0
Figure . The graph illustrates with time the absorbance for all test tubes increased expected for the end of test tube B.
D. Determine the Effect of pH on the Formation of an Iron-Salicylic Acid Complex
Figure . Shows the effect pH has on absorbance
Discussion-Experiment Kinetics of Hydrolysis of ASA
In part A, determination of peak absorbance for Fe (+) complex of SA, the wavelengths collected at the given absorbance levels indicated the commonly found shape of a bell curve. The bell curve begins with an increase, then a consistent level and a gradual decrease.
For part B, evaluating the outcome of FeCl() on ASA and SA, the data presented the conclusion that FeCl() has a greater effect on SA that ASA by having a larger absorbance reading.
During part C, determine that the effect of concentration of ASA and amount of FeCl() presented on the formation of the iron-salicylic acid complex, the information collected suggested that an increase in time will give an increase in absorbance reading.
Finally part D, determine whether or not the pH of the solution effects the formation of an iron complex and the graph illustrated an inconsistence. At different pHs the absorbance level differed.
Conclusion
In conclusion aspirin is very easy to compose and decompose. Caution is necessary for both the chemicals being used and measuring of samples, one slight error could ruin the complete experiment. Overheating ASA can easily decompose back into SA. Although, it took plenty of practice, aspirin is a wonder drug that is simply made.
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