30 20 10 From the procedure 2. Assemble the simple distillation apparatus as generally shown in Figure SD.1 in the lab manual, ensuring that the thermometer bulb is aligned at, or slightly below, the Y in the distillation head. Each ground joint is greased by putting three or four stripes of grease lengthwise around the male joint and pressing the joint firmly into the other without twisting. 3. Attach a water condenser to the distillation head. 4. Remember, water goes in the bottom and out the top. Attach a clamp holder to the end of the drain tube to keep it weighted in the drain. Turn water to a trickle. If it is slowly draining, it is high enough. Begin a low flow of water through the condenser. 5. Place the set up on a heating/stir plate. 6. Turn on the hot plate to start heating the solution. Monitor the temperature and the boiling of the solution throughout the distillation process. 7. Record the temperature of the distillate when the first drops are recovered. 30.0 8. Adjust the hot plate so that the distillation rate is only one drop per second. Overheating to gain speed will result in an improper distillation and separation. 9. During the distillation, collect and measure the volume that accumulates during a temperature change of 5 °C in each test tube. For example, if distillation starts at 70 °C, the first test tube should hold the distillate collected between 70-75 °C, and the second test tube should hold the distillate collected between 75-80 °C. If there is a dramatic change of the head temperature (1 degree per second), change the receiving test tube. Record approximately how many drops were collected, and then begin your five-degree intervals again when the temperature levels off. 10. Continue the distillation until about 1-2 mL of liquid remains in the pot. 11. Remove the heat source and turn off the heat. Allow the liquid in the distillation head to drain into the distillation pot; measure and record the volume of this pot residue. 12. Measure the volume of each fraction using a small graduated cylinder. After measuring each volume in a test tube, turn the graduated cylinder upside down on a paper towel that is crumpled in the bottom of a beaker to allow the cylinder to drain between volume measurements. Measure as accurately as possible because your final results will depend upon it. Volume of temperature range of fractions collected Fraction 1 Fraction 2 Fraction 3 Fraction 4 Fraction 5 Fraction 6 Fraction 7 Fraction 8 Fraction 9 Fraction 10 Beginning of temperature range (°C) 69.0 74.0 79.0 84.0 89.0 94.0 108.0 105.6 110.5 115.5 End of temperature range (°C) The volume of liquid (mL) left in the flask after ending the distillation (pot residue) is measured as 1.08 mL. Enter the volume of the pot residue (ml): 74.0 79.0 84.0 89.0 94.0 108.0 105.7 110.5 115.6 120.7 Volume collected 0.58 3.89 4.49 2.68 2.10 1.79 2.68 5.05 4.20 1.50 1.08

30 20 10 From the procedure 2. Assemble the simple distillation apparatus as generally shown in Figure SD.1 in the lab manual, ensuring that the thermometer bulb is aligned at, or slightly below, the Y in the distillation head. Each ground joint is greased by putting three or four stripes of grease lengthwise around the male joint and pressing the joint firmly into the other without twisting. 3. Attach a water condenser to the distillation head. 4. Remember, water goes in the bottom and out the top. Attach a clamp holder to the end of the drain tube to keep it weighted in the drain. Turn water to a trickle. If it is slowly draining, it is high enough. Begin a low flow of water through the condenser. 5. Place the set up on a heating/stir plate. 6. Turn on the hot plate to start heating the solution. Monitor the temperature and the boiling of the solution throughout the distillation process. 7. Record the temperature of the distillate when the first drops are recovered. 30.0 8. Adjust the hot plate so that the distillation rate is only one drop per second. Overheating to gain speed will result in an improper distillation and separation. 9. During the distillation, collect and measure the volume that accumulates during a temperature change of 5 °C in each test tube. For example, if distillation starts at 70 °C, the first test tube should hold the distillate collected between 70-75 °C, and the second test tube should hold the distillate collected between 75-80 °C. If there is a dramatic change of the head temperature (1 degree per second), change the receiving test tube. Record approximately how many drops were collected, and then begin your five-degree intervals again when the temperature levels off. 10. Continue the distillation until about 1-2 mL of liquid remains in the pot. 11. Remove the heat source and turn off the heat. Allow the liquid in the distillation head to drain into the distillation pot; measure and record the volume of this pot residue. 12. Measure the volume of each fraction using a small graduated cylinder. After measuring each volume in a test tube, turn the graduated cylinder upside down on a paper towel that is crumpled in the bottom of a beaker to allow the cylinder to drain between volume measurements. Measure as accurately as possible because your final results will depend upon it. Volume of temperature range of fractions collected Fraction 1 Fraction 2 Fraction 3 Fraction 4 Fraction 5 Fraction 6 Fraction 7 Fraction 8 Fraction 9 Fraction 10 Beginning of temperature range (°C) 69.0 74.0 79.0 84.0 89.0 94.0 108.0 105.6 110.5 115.5 End of temperature range (°C) The volume of liquid (mL) left in the flask after ending the distillation (pot residue) is measured as 1.08 mL. Enter the volume of the pot residue (ml): 74.0 79.0 84.0 89.0 94.0 108.0 105.7 110.5 115.6 120.7 Volume collected 0.58 3.89 4.49 2.68 2.10 1.79 2.68 5.05 4.20 1.50 1.08

EBK A SMALL SCALE APPROACH TO ORGANIC L

4th Edition

ISBN:9781305446021

Author:Lampman

Publisher:Lampman

Chapter83: Simple Distillation

Section: Chapter Questions

Problem 2P

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