I then allowed the remaining liquid to evaporate leaving behind salt. I poured the salt into the weighing dish and weighed the mass and calculated and recorded into table 1. Data Table 1: Experiment Data Grams Percent of Mixture Iron Fillings 0.9 gm 19.6 % Sand 1.4 gm 30.4 %
Extraction and Drying: Using a separatory funnel, the cooled filtrate was extracted with 10ml of methylene chloride. After shaking our mixture, we broke and dried our emulsion by slowing passing the lower layer through a cotton ball layered with anhydrous magnesium sulfate. The extraction process was repeated 2 more times for maximum collection of the organic layer. Distillation: The extracts were poured into a 50ml round bottle flask and connected to a simple distillation apparatus. To obtain the caffeine, the methylene chloride was removed from the extract, leaving us with our solid caffeine residue.
The mixture was decanted again in to the same beaker. Next, we added boiling chips to the liquid and evaporated the solvent over the hot plates under the hood. After the solvent was evaporated and the flask was cooled, we used a spatula to remove a small amount of the crude product and took its melting point. We determined the melting point range of the sample to be 43.0-46.0 degrees Celcius.The crude product was yellow colored when it was warm and orange in color when cooled and sticky. We then recrystallized our sample using 5 ml of warm acetone that was heated on a hot plate under a hood.
A melting point will be ran on the aspirin when completely dry. A capillary tube containing the dry aspirin will be placed into the melting-point apparatus. This process is to determine the melting point range of aspirin. First, a hot water bath was created with a 400. mL beaker on a hot plate. The temperature was raised to 70 degrees Celsius and 4.419 g of salicylic acid was measured out on a balance and transferred into a 125. mL Erlenmeyer flask.
Gently stir the pellets until the acid is dissolved by shaking the the apparatus. Lift the calorimeter lid and wash out its contents and the thermometer. Repeat this experiment using 50.0 mL of 1.0M acetic acid. Repeat experiment using 25.0 mL of each 2.0M sodium hydroxide and 2.0M acetic acid. Data Table(s): Reaction equation Mass of solid NaOH Initial Temp.
Stirred the mixture to make sure all soluble material dissolves. 10. Poured the liquid while it is hot into a small paper cup. 11. Poured another 10 to 15mL of distilled water into the beaker containing the sand, brining the mixture to a boil and decanted again into the same cup used previously.
Get the magnet and put it in a small plastic bag. 2. Wave it slowly around the cup of sand, salt, and iron filings until all of the iron has been attracted to the bag and removed from the cup. 3. Put the sand and salt into a beaker filled with 60 mL of water, and then stir it until you can’t see the salt anymore and the sand is settled at the bottom.
Add two drops of food coloring to the beaker of distilled water and mix thoroughly. Measure out a dropperful of bleach into a plastic pipet and set it aside until Step 8. 6. Calibrate the colorimeter a. Prepare a blank by filling an empty cuvette ¾ full with distilled water.
* Pour a little ether over the nutmeg residue on the filter paper so that any Diethyl ethanol traces clinging to it is washed down and mixed with the filtered liquid underneath. * Filter the mixture by gravity filtration, washing the nutmeg residue with 10ml of diethyl ether. Evaporate the Ether from the filtrate * Recrystallize the product from ethanol. Filter using a Buchner funnel and wash them with cold water as shown in the diagram (see figure 2). * Let the crystals dry for one week, record the weight and take a sample and put into a glass capillary tube to obtain a melting point using the Melt-Temp machine.