Purpose: Finding the yield of aspirin by adding a measured mass of salicylic acid to a measured volume of acetic anhydride and then used FeCL3 on a sample of the synthesized aspirin to find if the salicylic acid is a phenolic alcohol or carboxylic acid. Procedure: To synthesize aspirin, a 600-mL beaker was filled half way with water and then placed on a hot plate. A support ring attached to a stand was used to stabilize the beaker on the hot plate; the water was then allowed to boil. A recorded mass of 2.1g salicylic acid was placed into a 125-mL Erlenmeyer flask and then a recorded volume of 4.0mL acetic anhydride was added to the Erlenmeyer flask with salicylic acid. Then five drops of concentrated H2SO4 solution was added to the Erlenmeyer flask containing salicylic acid and acetic anhydride.
After allowing the solution to sit for a few minutes, the liquid portion was separated into a waste container using a pipet. Once 10 mL of distilled water was added, 9 mL of 3 M H2SO4 was added dropwise until a color changed occurred. Then, 5 mL of distilled water was added to the remaining mixture and
To test tube B add 1ml(1000µm) of Distilled Water. 5. Add 1cm(1000µm) of universal indicator to each test tube. 6. Add 0.1M sodium carbonate solution slowly drop by drop until the contents of each tube are at pH7 (pale green in colour).
To the second, add 10% NaOH dropwise until the pH is 14. (To do this, add a couple of drops of NaOH to the tube; stir thoroughly with a stirring rod; then touch the stirring rod to a piece of pH paper to check your pH.) To the third, add 0.5% sodium bicarbonate solution to pH 9, and to the fourth, add 2% HCl to pH 2. Record your observations on the data sheet. Repeat the above tests using 2% casein solution.
10 drops of NaOH were added to each precipitate to test for amphoteric species. The contents were rinsed with distilled water and the tubes were cleaned with 6 M HCl. For the ammonia elimination test, 10 drops of each cation solution were placed in their tubes and 15 M NH4OH were added dropwise till a precipitate or color complex was observed or till 20 drops were reached. 10 drops of 15 M NH4OH were added and additional changes were recorded. The contents were disposed of and rinsed with distilled water.
Each test tube contained a cotton ball dampened with 15% KOH, then a ball of glass wool, then 20 pea seeds soaked at the certain temperature, then another ball of glass wool, and then another cotton ball dampened with 15% KOH. The top was covered with a rubber stopper which had a 1 ml pipette and a syringe. Then both test tubes were placed in a room temperature bath. Then 3-4 drops of iodine were added and adjusted. After 5 minutes, the position of the dye was recorded and then after every 2 minutes for 20 minutes the dye position was recorded.
This process was repeated once more and the resulting filtrate was poured into a clean 250mL beaker. The filter flask was rinsed with 10mL of distilled water. The rinse was poured into the reaction beaker and the beaker was cooled in an ice bath. 20mL of 6.0 M sulfuric acid was slowly added to the cooled reaction mixture while being stirred. The mixture was heated to dissolve any solids and then the mixture was filtered in the same process as before.
The milk was taken out from the water, then 15~20 drops glacial acetic acid were added. The milk was stirred with a stirring rod (every five drops were observed) until a white solid has formed. 5. Put cheesecloth on the top of 50 mL beaker, also using a rubberband to tie it. Separating the liquid and solid when the mixture was poured
Then, the test media is then incubated at 37 ° C, for 18-24 hours. Rinsing reusable instruments The samples were rinsed with 40 ml of pyrogen-free water using a glass beaker that is free from pyrogens. Endotoxin testing using STV A total of 0,2mL from the water obtained from the rinsing was placed in the STV containing LAL reagent and was shaken for 20 to 30 seconds. Then STV was placed in an incubator at 37 ° C for 60 ± 2 minutes. STV was then observed by reversing the reaction tube in one smooth motion.
This was done by treating the sulfanillic acid with NANO2 and hydrochloric acid by the following procedure. We dissolved 0.107 g of sodium bicarbonate in 5 mL of water in a 50 mL Erlenmeyer flask. 0.197 g of sulfanilic acid monohydrate was added to the solution, and the solution was heated until it dissolved. Once the solution was cooled to room temperature, 0.083 g of sodium nitrite was added to the solution and stirred until the mixture dissolved. This solution was then cooled in an ice-water bath while frequently being stirred for 10 minutes.