Using a measuring cylinder, add 50cm3 of 1.0mol dm-3 sulphuric(VI) acid to the thyme extract in the conical flask. 8. Titrate the solution in the conical flask with the potassium manganate(VII) solution until a pale pink colour persists for 10 seconds. 9. Repeat the titration until there are two titres within 0.1cm3 of each other.
The extraction process is when a solvent, dichloromethane (15mL) is added to the filtrate in a separatory funnel; the mixture is gently swirled together 3 times, and stopcock is released in between to vent the funnel. Dichloromethane (including the emulsion) is then drained from the bottom into a 50mL Erlenmeyer flask. Same extraction process is repeated on the same filtrate and the dichloromethane is, once again, let out to the same 50mL Erlenmeyer flask as before. The combined dichloromethane solution and water (20mL) is poured into a rinsed separatory funnel. Mixture is gently swirled and drained out into an Erlenmeyer flask.
After the effervescence, (15mL) of concentrated HCl was added drop wise to the solution. The mixture was then heated for 15 minutes in a boiling water bath. In two separate small beakers (20mL) of distilled water was placed in one and (20mL) of 6M HCl in the other. Both beakers were placed into an ice bath. After heating, the mixture was cooled to room temperature and filtered by vacuum filtration into a fritted funnel to yield a purple product.
Leave to filter for about 10 minutes. * Step 5 – Some liquid should have filtered through (the filtrate). Remove the glass of alcohol from the iced water. Gently pour the alcohol along the wall of the glass containing the filtrate. Observe after at least 5 minutes.
The watch glass was removed with the beaker tongs. Using a rubber bulb and a stirring rod to stir the solution continuously, 15.00mL of .25M BaCl2 solution was added to the solution in the beaker. The watch glass is replaced and the solution is keep hot but not boiling for 15 minutes. The precipitate was allowed to settle. When the liquid above the precipitate was clear, the solution was tested for completeness of precipitation when a few drops of BaCl2 solution were added from a pipette.
Do this one more time the exact same, and then a third time using only 10 mL of the mixture. Each of the three times you do this, extract the liquid. Transfer the liquid into the large 100 mL round bottomed flask that is connected to your simple distillation set up. Distill the tomato paste liquid. Once it is completely distilled, remove your filtered material and add 2 mL of dichloromethane.
Turn on the hot plate to a medium heat. Wait until all the liquid has evaporated from the substance and then record the color of the dried substance. 6) Repeat steps 1-5 using each of the three other substances. NOTE: Make sure to wipe down all the materials before they are reused. Compounds | Solubility in Water | Solubility in Alcohol | Color if Soluble in H₂O | Conductivity(Scale 1-4) | Color When Dry | Melting Point (°F) | Sucrose | Yes | No | Transparent | Medium (2) | Brown | 366.8 | Sodium Chloride | Yes | No | Transparent | High (3) | Crystallized, Clear | 1474 | Sodium Carbonate | Yes | No | Mostly Transparent | High (3) | White | 1564 | Salicylic Acid | No | Yes | N/A | High (3) | White | 318.2
This solution was added drop wise to the stirred ethanolic solution of benzophenone at room temperature. After all the sodium borohydride being added, the mixture was stirred for a further 10min. Meanwhile, ice water (10ml) was mixed with concentrated hydrochloric acid (1ml) in 50ml beaker. To this the mixture of sodium borohydride and benzophenone was poured slowly into the beaker. The precipitate was collected using suction filtration and washed with 2 x 5ml portions of water.
Take the fine soil from the bottom pan of the sieve set, place it into a beaker and add 125mL of the dispersing agent. Stir the mixture until the soil is thoroughly wet. Let the soil soak for at least ten minutes. 2. While the soil is soaking, add dispersing agent into the control cylinder (Sodium Hexametaphosphate 125ml) and fill it with water to the mark.
The third test will utilize thin layer chromatography to evaluate the purity of the aspirin as well as testing for the presence of leftover salicylic acid or other by products of the reactions. Experimental: Week 1: For the synthesis of the aspirin, 250 mL of water was boiled. 1.5 g. of salicylic acid were poured on a test tube. Then, 3.5 mL of acetic anhydride and four drops of 85% phosphoric acid were added. A cotton ball was placed to prevent vapor escape.