The sample was poured in the Buchner funnel and a about 5 mL of water was in the flask to get the last few of crystal out of the flask. After the crude aspirin dry in the beaker it weighed about 2.575 without the beaker. The final experiment, was purification. The crude aspirin was tranfer into a 125 mL Erlenmeyer flask with 3 mL of ethanol and warm on the hot plate until the aspirin dissolve. Fiver portions of about 3 mL of water was added in increments and cooled in an ice bath for about 10 minutes.
This was to see the difference between the initial temperature and the final temperature. First Test In a 250ml beaker place 100mls of water, measure the temperature of the water and record this initial temperature onto a table. Set the timer and add one teaspoon of Ammonium Nitrate to the water, stir this continuously until the Ammonium Nitrate has dissolved. After 1 minute measure the temperature and record it, do this for a further 2 minutes (3 minutes in total). Repeat this process for a total of 10 teaspoons.
Now add ~ 0.35 g of zinc powder to the solution and stir until the solution becomes clear. Dissolve the excess zinc with more sulfuric acid. Decant the liquid with a stirring rod, retaining only the copper. Rinse the copper with distilled water and steam dry. Weigh the mass.
For SDS-PAGE, running buffer is prepared by taking 40 ml Tris-Glycine and adding 4 ml of 10% SDS to it. Its volume is raised up to 400 ml by adding distilled water. Load these samples into wells created in the gel. Run the electrophoresis unit at 5 mA and 20 V for entry of sample into lower gel. Once the samples enter the lower gel, alter the current to 10 mA and set the voltage at 90-100 V. Leave this setup undisturbed for around 3 hours.
The hydroxyl group on the benzene ring reacts with the acetic anhydride to form an ester functional group. This reaction is called an esterification reaction (Pavia, Lampman, Kriz, & Engel, 1999). A similar reaction was executed using isoamyl alcohol and acetic anhydride. The addition of sulfuric acid catalyzes the reaction. When the reaction is complete, there will be some unreacted salicylic acid and acetic anhydride that will be left with the crude aspirin.
The pure benzoic acid is fed to a second reactor, where it is oxidized to phenol by air and steam under 1.3 – 1.7 atm at 220°C in the presence of cupric benzoate catalyst promoted with Manganese. The reaction mass is periodically withdrawn from the second reactor into an extractor, where it is washed with water to remove unwanted tars and benzoic acid and steam are returned to second
20 g of graphite powder will be stirred in a heated solution of 30 ml H2SO4, 10 g K2S2O8 and 10 g P2O5 at 80°C for 30 minutes until dark blue mixture will be formed. The mixture will be cooled to 25°C for 6 hours. After that deionized water will be added and the ingredient will be filtered and washed until filtrate become neutral pH. Then, the filtrate will be dried overnight in vacuum desiccator at 25°C. 460 ml of concentrated H2SO4 will be used to oxidise the graphite in the ice bath after the drying process.
One g of material was ground and extracted with 0.2 N HCl by continuous shaking. To 0.2 ml of the filtrate, distilled water to make volume 1.4 ml was added. After that1ml of ferric ammonium sulphate solution (21.6 mg in 100 ml water) was added, mixed and placed in a boiling water bath for 20 min. The contents were cooled and 5 ml of isoamyl alcohol was added and mixed. To this, 0.1 ml ammonia solution was added, shaken thoroughly and centrifuged at 3000 rpm for 10 min.
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.
The heat is gradually raised until the acid reaches approximately one third the way up the digestion flask. The flame is not allowed to touch the digestion flask above the part occurred by the liquid. Executive boiling may cause volatilization of the acid before the organic matter is oxidized. Then the content was cooled and about 100mL was diluted with distilled water. The flask was swirled for about 2 minutes and the fluid part was transferred to a 1000mL distillation flask.