Lab Report Extraction of Aspirin Tablet

Abstract
The experiment consisted of extracting and purifying compounds involving immiscible solvents through the method of ‘like dissolves like’ procedures involving solubility characteristics to be able to retrieve a percent recovery  of the Goody’s Powder and to test the purity of its compounds by observing its melting points. Results calculated a 74.69% recovery of the Goody’s Powder and an observed reading of 134 degrees Celsius for Aspirin was compared to the given values. Complications presented with challenging retrieval, transfer and drying of solids in the experiment that lead to the loss percentage recovery and the slight value deviation of the purity of Aspirin’s melting point.

Introduction
The purpose of the experiment was to individually extract the 4 different compounds found in the Goody’s tablet by separating methods involving the principle of “like dissolves like”, determining the percent recovery of the solid, as well as testing its purity by testing and comparing its melting point. In the experiment the Extraction flask device is used to separate two liquids that are immiscible to each other with different solubility characteristics, so when diluting two different liquids a clear distinction can be seen separating two layers consisting of polar and nonpolar compounds. According to Silberberg, M. S. (2006) it states, “Like dissolves like says that substances with similar type of intermolecular forces dissolve in each other, thus knowing the forces can predict whether a solute will dissolve in a solvent”. Nevertheless solvents will dissolve in others with similar polarities. When determining a melting point the TLC apparatus (Thin Layer Chromatography) is preferred due to its function of analyzing the purity of a compound and determining its melting point. The procedures to consider involve having a capillary tube filled with a given sample and placing it on the device, the temperature will have to be increased steadily until the melting point is observed. As the melting point is observed data and all observations should be noted and compared to the actual values provided.  

Experimental Procedure
The experiment began by obtaining a “Goody’s Powders” tablet as the source for isolating the 4 compounds (acetaminophen, caffeine, aspirin and binder). The manual states to use a pestle to crush 2 tablets into a powder form and weigh 700 mg of the product but due to supply issues the instructor indicated to use the “Goody’s Powder” packet that contained the already powdered form of the product and to proceed with the full weight of the product. In preparation for weighing the product, a weigh boat was placed on the center of the balance scale and tared to 0.000 grams then the product was added unto the weigh boat and it gave a reading of 1.0247 grams. The manual states to add 4 mL of dichloromethane unto a 50 mL beaker with the powder product and to place the beaker on a hot plate at 80.0 degrees Fahrenheit for warming purposes with a watch glass covering the top surface to prevent evaporation, nevertheless the instructor indicated to change the 4 mL volume to 10 mL instead. The manual indicates a vacuum filtration of the beaker with the warmed solution of dichloromethane and the “Goody’s powder” product unto a 150 mL Erlenmeyer flask labeled Beaker 1, but according to the instructor the vacuum filtration process was changed to a glass funnel gravity filtration process instead. The solution was poured unto glass funnel with an applied filter paper mounted with a rubber holder mounted on a 150 mL Erlenmeyer flask, which separated the solid and allowed the aspirin and caffeine to drain unto the Erlenmeyer flask labeled Beaker 1. The solid on the filter paper was wet and an estimated wait time of 5-7 minutes allowed the solid and filter paper to dry completely, then transferred unto a 50 mL beaker. 3 mL of ethanol was then added unto the beaker and placed on the hot plate at 180 degrees Fahrenheit to reach boiling point. Once the beaker reached boiling point it was poured unto the glass funnel gravity filtration set up and rinsed with hot ethanol leaving behind on the filter paper “binder”, which was collected, dried in the facility oven for 10 minutes and weighed. The solution drained on a separate 150 mL Erlenmeyer was left to evaporate leaving behind acetaminophen to be collected and weighed. The manual states to cool the hot solution and recrystallize the residue with water but the instructor directed to skip the process. Dichloromethane solution from Beaker 1 was then transferred to an extraction flask (separate funnel) and according to the manual it states to apply 1 mL of 3 M NaOH to the separatory funnel but instructor indicated to use a volume of 2 mL instead. The funnel was inverted while holding stopper in place mixing the two layers by rocking funnel back and forth In a very short period of time possibly 3 seconds and opening the stopcock to allow gas build up pressure to escape then  closing it, a repeat process of 3 times was applied. The separatory funnel was then placed on an iron ring stand attached to the clamp and the contents were left to settle, lastly the top glass stopper was loosened up and two distinct mostly clear layers were noticed. The stopcock was carefully opened and only the lower layer (dichloromethane layer) from the separatory funnel was drained unto a 150 mL Erlenmeyer flask labeled Beaker 2 and the top layer (aqueous layer) was transferred unto a 50 mL beaker labeled Beaker 3. Beaker 2 was then processed through another separatory funnel for a second extraction repeating the same steps that obtained Beaker 2, the only difference was the addition of 1 mL portion of 3 M NaOH  nevertheless the instructor indicated to change the volume amount to 2 mL instead. The lower layer (dichloromethane layer) was then drained unto a 150 mL Erlenmeyer flask labeled Beaker 4, the remaining layer was drained unto a different 150 mL Erlenmeyer flask labeled Beaker 3. The contents on Beaker 4 were then dried by the method of applying (unspecified amount) sodium sulfate into the solution causing small clumps to form then an addition 2 dabs with spatula until clumps were no longer visible when mixed followed by pouring contents unto a 50 mL beaker by method of glass funnel gravity filtration. Collecting the caffeine extraction on the 50 mL beaker was not attainable, the filter paper was discarded and the method of recrystallization was disregarded due to instructor order. Moving forward per manual it states to add 3 M HCl unto Beaker 3 by drop method followed by stirring after every interval due to concentration strength effectiveness instructor indicated to use 6 M HCl solution instead. A total of 10-15 drops were applied to Beaker 3 until crystals were formed in the solution, the manual stated to use ph paper to test the acidity as well as heating the mixture and adding water if necessary nevertheless the instructor indicated to disregard those steps. Beaker 3 was then placed in an ice bath for a 5-10 minutes until hardened, followed by placing it in the oven for 10 minutes. Lastly the final procedure states to find the melting points of all the compounds extracted so the use of a Thin Layer Chromatography device was the preferred choice in obtaining those values.