We weighed the resulting powder to be 3.228 grams. We then transferred the powder nutmeg into a 50 ml round bottom flask and added 15 ml of dichloromethane. We placed our flask in to a standard heat reflux apparatus and gently refluxed the mixture. We waited until we saw the first drip of liquid in the apparatus and heated for 15 minutes. After the mixture was heated, there was solid on the bottom and liquid on the top of the flask.
The purpose of this experiment was to extract Trimyristin (C45H86O6 ) from ground nutmeg powder. Trimyristin is a white to yellowish-gray solid that is insoluble in water, but soluble in ether. Trimyrisin is found naturally in many vegetable fats and oils. Its synthesis was done using reflux as shown in the diagram on page 3. Allow the crystals to dry for 1 week then, weigh it, take a MP, and calculate the % yield.
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.
• After the flask was heated, I removed it from the heating mantel and allowed it to cool to room temperature. • Next, I poured 15mL of absolute ether and 9mL of bromobenzene into the 250mL flask and waited 5 minutes for any reaction. • There were no signs of reaction after 5 minutes; therefore the lab assistant used a glass stirring rod to crush the magnesium in order to get the reaction started. When this was done, the liquid became cloudy, rapidly bubbling, and the color turned rusty red. • Next, I added 25mL of absolute ether and attached a reflux condenser to the flask.
Transfer the extracts to a simple-distillation assembly and distill off all but 10 mLof the solvent on a steam bath. Save the recovered solvent. Evaporate the combined solutions to dryness on a steam bath or hot-water bath in a hood. To purify the crude product, dissolve it in about 5 mL of acetone by warming the mixture on a steam bath; add dropwise just enough mixed “hexanes” to turn the warmed solution faintly cloudy; then allow the solution to cool and allow the product to crystallize. Collect the green-tinged crystals on a small vacuum filter and wash them with a little mixed “hexanes.” The melting point of caffeine reported in the literature is 236°.
In the first tower, ammonia (NH3) bubbles up through the brine, where it is absorbed. Then, in the second tower (known as the solvay tower), carbon dioxide (CO2) gas passes through the ammoniated brine, and sodium bicarbonate (NaHCO3) precipitates out of the solution. In a similar fashion, the Athenium Baking Soda Company (“ABSC”) produces baking soda by reacting crystalline ammonium hydrogen carbonate with brine, as follows (Eq. 1): NH4HCO3(s) + NaCl(aq) → NaHCO3(aq) + NH4Cl(aq) (Eq. 1) In addition to sodium chloride, brine often contains potassium chloride, lithium chloride, and calcium chloride (i.e., KCl, LiCl, and CaCl2, respectively).
3) Add boiling stones 4) Assemble a reflux apparatus and heat the reaction mixture at reflux for 1 . 5) Remove the heat source and let it come to RT. 6) Pour the cooled mixture into a separatory funnel and carefully add 50ml of cold distilled water. Rinse the reaction flask with 5-10ml of cold water and also add this rinse to the separatory funnel. Stopper the
Sodium Hydroxide + Hydrochloric Acid Sodium Chloride + Water NaOH(aq) + HClaq → NaCl(aq) + H2O(l) Variables Independent The independent variable of the experiment was the amount of sodium hydroxide that we added to the acid. To keep the variable controlled we would measure 1 ml of the sodium hydroxide and pouring that to the hydrochloric acid. Dependent The dependent variables of the experiment were the temperature and the pH number of the mixture. To control the pH and temperature use the electronic probe and data logger. Controlled The controlled variables of the experiment were: A.
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.
The normality of the unknown base is calculated after the solution has reached the end point. The amount of substance being delivered is calculated in units of equivalents per litre using the formula: VaNa = VbNb Experimental In order to titrate the acid with the unknown base, a solution of the acid was prepared. 5.1722 (±10%)g of potassium hydrogen phthalate acid is obtained using a weighing boat and transferred into a volumetric flask containing 250mL of boiled distilled water. Volumetric flask was shaken several times in order to assist the powder to dissolve. Once dissolved, 24.9734 (± 0.0045)mL of acid was pipetted into an Erlenmeyer flask along with 25mL of cool (recently boiled) distilled water.