Aspirin was prepared according to the protocol provided on Blackboard. The three sections to this experiment were 1. Synthesis of Aspirin, 2. Recrystallization of Aspirin, and 3. Characterization of Aspirin. In the first section, the Synthesis of Aspirin, salicylic acid was weight to be 3.029 grams using mass by difference since it was weighed on a 150 milliliter beaker. 9.23 milliliters of the acetic anhydride and 14 drops of 85 percent phosphoric acid were added to this beaker. A Bunsen burner provided by the laboratory was then used to boil the just mixed combination by producing a flame underneath the positioned beaker on top, and then allowed to cool for several minutes after the Bunsen burner flame was terminated. Two quantities of distilled water were then added to this mixture to make it cool even further, which were 41 drops and 30 milliliters. After cooling for some time, this beaker was placed into an ice bath in order to start the crystallization process. A glass rod was used to scratch around the bottom and the sides to catch all of the crystallized Aspirin that was being formed during this whole process. Then, by using a Buchner funnel and filter paper, which was placed on top of the flask connected to a water aspirator with rubber tubing, the excess liquid was removed from the just scraped Aspirin crystals when the Aspirin was placed on the filter paper. Using a medicine dropper, the Aspirin crystals on the filter paper were washed with distilled water just so that any non-pure substances were removed from the crude product. When these crystals were then ultimately dry, they were placed on a watch glass and put into an oven for 30 minutes. Then they were weighed by mass by difference to yield 2.4667 grams of crude s... ... middle of paper ... ...s the change in the temperature of both of these batches, 6°C for the pure, and 13°C for the crude. In this final sub-section of the Characterization of Aspirin, the values of absorbance were recorded. Initially, 0.0566 grams and 0.0590 grams of pure and crude Aspirin respectively were obtained and each individually placed into beakers (400 milliliter) and had 250.0 milliliters of distilled water added to them. From each beaker, a tiny amount of the just dissolved solutions was transferred to a cuvette, one cuvette for each type of aspirin. Each cuvette was placed into the ultraviolent spectroscopy mechanism which was connected to a computer and absorbance spectrum values were obtained at 298 nm (Figure 5) (0.1987 pure aspirin, and 0.9549 crude aspirin). Cumulatively these three methods resulted in the determination of the percent purity for each type of aspirin.
The purpose of this experiment was to learn and preform an acid-base extraction technique to separate organic compounds successfully and obtaining amounts of each component in the mixture. In this experiment, the separation will be done by separatory funnel preforming on two liquids that are immiscible from two layers when added together. The individual components of Phensuprin (Acetylsalicylic acid, Acetanilide, and Sucrose as a filler) was separated based upon their solubility and reactivity, and the amount of each component in the mixture was obtained. Also, the purity of each component will be determined by the melting point of the component.
Paragraph 2: It is believed that as the temperature of the water increases the time it will take for the tablet to dissolve will decrease. This is believed since the temperature there will be more energy allowing the particles to get together and form a reaction allowing the ta...
The solvent should be easily removed from the purified product, not react with the target substances, and should only dissolve the target substance near it’s boiling point, but none at freezing. A successful recrystallization uses minimum amount of solvent, and cools the solution slowly, if done to fast, many impurities will be left in the crystals. Using the correct solvent, in this case ice water and ethyl acetate, the impurities in the compound can be dissolved to obtain just the pure compound. A mixed solvent was used to control the solubility of the product. The product is soluble in ethanol an insoluble in water. Adding water reduced solubility and saturates the solution and then the crystals
The color that was chose to be shined through the sample was purple. The spectrophotometer was set at a wavelength of 400nm to represent the purple color. It was zeroed using the blank meaning the spectrophotometer read zero as absorbance amount. The blank consisted of 5mL of water and 2.5 mL AVM and it was placed in cuvette. A solution with a known concentration of 2.0x10-4 M was used in the spectrometer. For this solution, 5 mL of the solution with 2.5 mL of AMV was placed in the cuvette. The cuvette was placed inside of spectrophotometer and the amount of absorbance was recorded. This procedure that involves a solution with a known concentration was repeated for the concentrations:1.0x10-4 M,5.0x10-5 M,2.0x10-5M, and1.0x10-5M.A unknown solution absorbance was measured by putting 5 mL of unknown solution with 2.5 mL AMV in a cuvette. The cuvette was placed in the spectrophotometer and the amount of absorbance was recorded. The procedure that deals with the unknown solution was repeated 2 more times with the same solution and the same amount of solution and AMV. The average of the three unknown solution was calculated and the concentration of the unknown solution was
Aspirin has grown so much in popularity that about 35,000 metric tons of it is produced and consumed each year to meet the consumer’s demand. 35,000 metric tons is equivalent to 100 billion standard aspirin tablets (10). That many tablets means that the market for aspirin is very good. Today, Aspirin is known as the leading non-prescription medicine of all time. It is the most common pill taken for pain, inflammation and fever. It has grown all over the world, being made available in eighty countries (9). It would not be surprising if one day, all the countries would have aspirin available to them.
Aspirin contains the substance acetylsalicylic acid (ASA), which can relieve inflammation, fever, pain, and known as a “blood thinner”. Aspirin was not officially trademarked until March 6, 1899 when the Imperial Office of Berlin made it official. It has been used for the last 110 years, but its natural form, salicylic acid has been around for thousands by Egyptians, Greeks, and Romans. Aspirin is available in over 80 countries and known as the best non-prescription drug. The most common use of aspirin is to cure headaches and use it as a pain reliever, but aspirin is known to prevent heart attack and strokes. It was first proposed in 1940, but wasn’t confirmed until 1970 when doctors would recommend taking aspirin daily [1].
As such, 3 Mmol of cyclohexanone and p-fluorbenzaldehyde were each added to a 100 mL round bottom flask with 30 mL of 10% sodium hydroxide. The reaction was stirred with a magnetic stir rod and allowed to react at room temperature for 1 hour. To determine reaction progress, TLC (figure 3) was performed at 30 minutes, 45 minutes and 60 minutes post reaction start time. After the 60 minute TLC was performed, the reaction was determined to be complete. The product was then separated through a liquid-liquid extraction process. To separate the product, 10 mL of hexanes were added to the reaction and the solution was transferred to a separatory funnel. Then, 10 mL of distilled water were added to the funnel which was then shook vigorously and allowed to settle. The water layer was then drained from the vial and this process was repeated in triplicate. The resulting hexane layer was determined to contain the product of the reaction and was transferred to a 50 mL
After creating the compound acetyl salicylic acid, it will be thoroughly analyzed through a series of steps that test its melting point, purity, and solubility as compared to commercial aspirin. By solving for the melting point range of the synthesized aspirin, one can determine its purity. Then by adding 1% ferric chloride, the color of both the synthesized and commercial aspirin represents its purity. In theory, the synthesized aspirin should be relatively the same color as the commercial drug. Finally, both types of aspirin are placed into different solutions to determine their solubility properties. For all three of these analyses, the synthesized aspirin should test similar to the commercial aspirin in hopes it was created
Part 4 of this lab showed a way to observe impurities by comparing the melting point of crude and pure samples. Since impurities are to be shown in the crude sample it would have a lower melting point and larger range. The known melting point of aspirin is to be 135 oC. The crude sample had a melting point range from 69oC to 81 oC. While the Pure sample melting point range was from 116oC to 125oC. Since the Pure sample was still below 135 oC, this shows that there are still some impurities
In the ancient and medieval time, antipyretic agents were only found in willow bark and in cinchona bark [2]. Willow bark was used as a pain reliever [3]. People were advised to chew on the bark in order to relieve pain and fever [3]. Cinchona bark was used for increasing appetite, however people also used it for common cold and fever [4]. When the cinchona tree started to decrease in the 1880s, people started to look for other alternatives [2]. During the 1880s, antipyretics agents were developed, which were acetanilide and phenacetin [2]. These properties of acetaminophen were discovered by accident [2]. It occurred when the molecule acetanilide was added to a patient’s prescription [2]. By this time, this drug had been synthesized via the reduction of p-nitorphenol [2]. However the drug acetaminophen was still not used medically for another 20 years [2]. In 1893, acetaminophen was found in the urine sample of an individual who had taken phenacetin [2]. This drug was concentrated into an odorless, white, crystalline compound that was found to have a bitter taste [2]. Acetaminophen was discovered to be a metabolite of acetanilide, however the discovery was ignored at that time [2]. It was later on that acetaminophen was found to have pain and fever relieving properties
The conical vial was placed in a small beaker and allowed to cool to room temperature. The mixture was Cooled thoroughly in an ice bath for 15-20 minutes and crystals collected by vacuum filtration on a Hirsch funnel. The vial was rinsed with about 5 mL of ice water and transferred into to the Hirsch funnel and again washed with two additional 5mL portions of ice water. Crystals were dried for 5-10 minutes by allowing air to be drawn through them while they remained on the Hirsch funnel. The product was transferred to a watch glass plate and allow the crystals to dry in air. Crude acetaminophen product was weighed and set aside a small sample for a melting point determination and a color comparison after the next step. Calculation of the percentage yield of crude acetaminophen (MW = 151.2). was done and recorded in the lab notebook.
This test was carried out by choosing three tablets from each formulation after weighing them. The temperature of the dissolution apparatus was adjusted at 37°C and the speed of paddles was constant at 50rpm.After that, each vessel of the dissolution apparatus was full with 1 liter of phosphate buffer. Subsequently, each tablet was placed into its individual vessel. The test was performed over 8 hours with extracting 10mL of each sample and replaced with the same amount of the phosphate buffer which was at the same temperature over the 8 hours as the following: half an hour, one hour, two hours, three hours, four hours, five hours, six hours, seven hours and eight hours. The all withdrawn samples were analyzed by using the UV spectroscopy
The analysis is therefore one of the most effective methods of ensuring that each drug being prescribed to patients is safe. It also ensures that all drug components are understood in terms of their structure and chemical behavior. This understanding is very important in the manufacture of drugs and other pharmaceutical products.
The physical studies were designed to ensure the stability of final formulation. The physical mixture of drug and lipids in the ratio of 1:1 was placed in glass vials, sealed and stored in 40ºc and 75% RH. The sample were withdrawn at pre determine time intervals of 15 and 21 day and examined for physical and chemical integrity of drug and Excipient. Parameter such as colour, odour or gas formation and aggregation were noted.
The purpose of this experiment was to study the reactions of amino acids and aspartame. Several solutions were prepared and used in TLC analysis. A permanganate test and a ceric nitrate test were also performed. The summary of the results is shown below.