The experimental boiling point range of acetylsalicylic acid was found to be 130-132° C. The salicylic acid and the acetic anhydride were mixed in a flask. Step 2 Step 3 Six drops of 1% ferric chloride solution were added to all 3 test tubes. Aspirin, acetylsalicylic acid, is a familiar drug, used for relieving cold and flu symptoms, fevers, and general aches and pains in the body, and, as made clear by its chemical formula, contains salicin — a chemical found in willow bark. To summarize, both spectrometers give significant evidence suggesting the purity of the synthesized aspirin product.
First, the base was created, which was made out of 1. Save some of your aspirin for testing. However, it was still used because the synthesis of asprin entailed the absorbtion of water. This mixture was generated a total of three times, so as to have three separate flasks with identical mixtures for three trials. Some steps that would produce a better yield for future experiments is rinsing the flask with cold water to make sure that all product is transferred.
This property is called hygroscopy, and extends to dessicators such as calcium chloride and, to a lesser extent, silica, which was used to dry the aspirin prior to testing the melting point of the crude product. The final product of synthesized aspirin contained no starting materials and its molecular weight was relatively close to that of pure aspirin, thus it was almost entirely pure. Step 2 A small amount of salicylic acid was dissolved in the first test tube. This is unlikely, though, considering that it was left for weeks to dry. When all the aspirin has dissolved, pour in 10 mL of lukewarm distilled water until solution becomes transparent. Assuming that you followed the same protocol and ingredients, yours is likely to contain some water vapor since commercially available aspirin undergoes additional treatment to remove every trace of water vapor.
This is done first by separating salicylic acid from methyl salicylate, followed by its purification. In the 5th century B. Later, the compound salicylic acid named for the Latin word for willow, salix was isolated from willow bark; it proved to be the active ingredient. Left: The molecular structure of acetylsalicylic acid, commonly known as aspirin. Now place the crude product from the weigh boat in a 25 mL Erlenmeyer flask and add 3 mL of ethyl acetate.
In Part I of this experiment, you will prepare aspirin by reaction of salicylic acid with acetic anhydride, using concentrated sulfuric acid as a catalyst. It also reduces inflammation and may even prevent heart attacks. Caution: Do not use a flame to heat ethyl alcohol. The third test tube, which contained only distilled water, served as the control. The actual yield of pure aspirin was 2. In our experiment, pure aspirin was obtained after filtering out the impurities and excess reagent through filter paper. Abstract: The goal of this experiment was to synthesize aspirin.
Filtration is used separate the impurities from the crude aspirin. Something else that can improve the experiment is allowing more than fifteen minutes for the Acetyl Salicylic acid to sit in the ice bath; this will allow for more product to crystallize out from solution and will allow for a higher percent yield. Add 10 drops of 85% sulphuric acid to the flask and stir with a stirring rod. Keep an eye on the chromatogram so not to allow the solution to go over the top, this would make it difficult to measure. Firstly, the amount of materials could be increased. Afterwards the product will be recrystallized to purify the product by allowing large, pure crystals to form by cooling slowly. If crystallization does not occur use a glass stirring rod and with strong force scratch the bottom of the Erlenmeyer flask.
While all reactions will eventually take place, it is usually economically feasible if not practical to use an amount of a catalyst to speed up a reaction to an appreciable rate. Aspirin has a very interesting history. If the mixture becomes cloudy or crystals start to appear, reheat the contents again and allow the beaker to cool down again. The aspirin product that was collected still contained some impurities. Another laboratory procedure used in this procedure is reading and recording liquid volumes. After the amount is calculated, you then can add it to the first reactant and it will give you a full reaction.
Observe the color: Pure aspirin would show no color, while salicylic acid or traces of it in impure aspirin will show a purple color. Forty million pounds are produced each year. The first portion of the experiment seemed to be a practice 10 fold serial dilution using the chemical bromophenol blue, and was treated as a quantitative experiment. Plug caps for 13x100 mm tubes —Ms. If crystals do not grow, slowly pour the solution into a 250-mL beaker containing 40 mL of ice water, mix thoroughly, and place the beaker in ice water and let sit undisturbed until crystals have grown. In this experiment aspirin, also known as acetylsalicylic acid, was synthesized from salicylic acid and acetic anhydride. Therefore when energy leaves one place it has to have another place to go to, it maintains a constant rate.