Allow the mixture to cool for a few minutes then filter it, using either gravity or vacuum filtration. (We shall be using vacuum filtration.) Wash the residue in the funnel once with a little water and collect all the filtrate. 4. Pour all the filtrate and washings into a 250cm3 volumetric flask.
The second experiment, procedure 1, combined [Co(NH3)5 (H2O)]Cl2 (0.0060M, 1.52g) and (25mL) of distilled water to an 125mL Erlenmeyer flask. The flask was gently heated (dial 5-6) and stirred until all the compound was dissolved. The heated solution was then vacuum filtered through a fritted funnel and the filtrate was cooled in an ice bath until the
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.
Mixture is gently swirled and drained out into an Erlenmeyer flask. Anhydrous magnesium sulfate is added to dehydrate the washed mixture. The solution is then filter into a weighed, dry, 100mL Erlenmeyer flask. Dichloromethane in the mixture is vaporized with a rotary evaporator. The Caffeine, white powder residue, (0.0486g) should be obtained.
Procedure 1. Begin to prepare an EDTA solution. Weigh out 3.62-3.64 g of NaH2EDTA and record exact mass. Add the weighed amount to a 250 ml volumetric funnel carefully using a funnel Wash the funnel with water to ensure all of the solid is delivered to the flask Add 100-200 ml of water and mix. Enough water should be added so that the flask is full to the 250 ml mark Tightly wrap the top of the flask with a Parafilm when finished 2.
Using another 125-mL flask, 60-mL of 0.3622 M potassium hydroxide in ethanol was deposited. Both flasks were clamped in a temperature-controlled bath regulated at 50.0˚C. The solutions were then set in the temperature bath for ten minutes to equilibrate. An empty 250-mL Erlenmeyer flask was also clamped in the same water bath. In another flask 50-mL of ice water was deposited with three-drop phenolphthalein.
The mass was recorded and transferred to a 50 ml beaker. 4 ml of 6 M HNO3 was added to the beaker containing the copper. For step 2, 10 ml of distilled water was added to the beaker. Then, 6 M NaOH was added to the solution (drop wise), until placing a drop of the solution on red litmus paper turned it blue. For step 3, the solution was heated with a hot plate.
The mixture was refluxed to avoid evaporation while it boiled for 30 minutes. After 30 minutes the mixture was cooled and then filtered through fluted filter paper into a 250ml round bottom flask. The methyene chloride dissolved the trimystrin and would pass through the filter paper leaving the other nutmeg solids behind. The solution was then distilled to get rid of the methlyene chloride and isolate the trimyristin. Methlyene chloride was a good solvent in this case because its boiling point is 40 degrees C and will boil off before the trimyristin which has a boiling point of 56-57 degrees C. Finally acetone was added to wash the crystals and the solution was vacuum filtered.
Once it is completely distilled, remove your filtered material and add 2 mL of dichloromethane. Swish the flask, and then place into a small beaker. Next, place the beaker with the distilled liquid on a heating mantle and heat to a gel like substance. Make sure not to burn it. The next processes that will be
DO NOT LOOK DIRECTLY AT THE BURNING MAGNESIUM; THE INTENSE LIGHT CAN HURT YOUR EYES. The magnesium mass was calculated from the data in the lab table during the heating process. The reaction was complete when the gray powder was formed. Tongs were used to carefully remove the reaction off of the wire gauze to cool for five minutes. Two drops of water were added to the cooled crucible.