I need help writing the theory on simple distlation based on Preparation of Cyclohexanone by Hypochlorite Oxidation Figure 8.4thermometerthermometer adaptor (ground glassadaptor plus rubber adaptor)blue plasticclampwater outwater inblue plasticclamp250 mL Roundbottom flaskground glassstopper or smallcorkmetal clampboiling chipsheating mantle100 mL roundbottom flask+ Plug to Rheostatthree-way adapter as shown in Figure 8.4. Place a secure cork in the small opening. Add a few boiling chipsand distill your product, setting the rheostat on the heating mantle to about 70-80 V.This will be a steam distillation. You will distill a mixture of water and cyclohexanone. Continue thedistillation until you have collected about 40 mL. You should see a layer of cyclohexanone on the top and anaqueous layer of water and acetic acid on the bottom.Work-upWhen you have collected 40 mL stop the distillation. Remove the receiving flask and CAREFULLYadd solid sodium carbonate (Na,CO,) using your spatula until you have neutralized all of the acetic acid thatdistilled over with your product. Add a small spatula tip of the solid sodium carbonate and stir with yourspatula. You should see evolution of CO, gas. DO NOT ADD THE SODIUM CARBONATE TOOQUICKLY TO THE SOLUTION BECAUSE IT CAN BUBBLE OVER. Keep adding the solid until there isno more bubbling. Remove some of the aqueous layer on the bottom with a medicine dropper and test withlitmus to see that it is neutral.Cyclohexanone has some solubility in water. Add solid sodium chloride (add about 0.2 g of NaCl permilliliter of water present) to salt out the cyclohexanone from the water layer. Just as we did in the cyclohexeneexperiment, the idea is to saturate the aqueous layer with the very polar sodium chloride to drive thecyclohexanone from the water layer. Do not add too much of the sodium chloride. Add a spatula tip full, stir todissolve and then add a bit more. Continue adding the NaCl until you see some solid material remaining. Procedure:Set-up your 250 mL 2-necked round bottom flask as shown in Figure 8.3. Attach the thermometer usingthe red neoprene adapter. Add 6.0 mL cyclohexanol to the round bottom flask. In the 400 mL beaker, get 85mL of bleach and add 4.0 mL glacial acetic acid in the hood.Pour the bleach and acetic acid mixture into your separatory funnel and suspend it by an iron ring asshown in Figure 8.3. If you have a separatory funnel that is furnished with a ground glass joint at the bottom,DO NOT connect the joints since you want to have a system that is open to the atmosphere.Figure 8.3Separatory funneliron ringthermometerground glass thermometeradaptor plus rubber adaptor250 mL round bottom flaskBegin adding the bleach solution slowly a few drops at a time. Monitor the temperature. You want tomaintain the temperature between 40 – 50 °C. Do not allow the temperature to rise above 50 °C. Use thecooling bath if necessary. And, do NOT allow the temperature to fall below 40 °C. Otherwise the oxidationwill not go to completion. The addition should take about 15 – 20 minutes to complete. Be patient. Add a fewmL of the bleach, swirl the flask to mix and monitor the temperature.When all of the bleach has been added, there should be a slight yellow color. If not, add more bleachuntil a faint yellow color persists. Sometimes it can be difficult to determine if there is actually a yellowish tintpersists. Do not add more than 5-10 ml additional bleach. Holding a white piece of paper behind the flask canbe helpful.After all the bleach has been added, allow the reaction mixture to stand for 15 minutes with occasionalswirling.After 15 minutes, check the color of your reaction. If there is a slight yellow color, this indicates thatthere is an excess of hypochlorous acid. Add sodium bisulfite (NaHSO,) solution until the yellow colordisappears. Sodium bisulfite is a mild reducing agent and it will react with the hypochlorous acid. A few mL isusually sufficient.Remove the separatory funnel and set-up your apparatus for a simple distillation as shown in Figure 8.4.Use the same 250-mL round bottom flask and use a 100 mL receiving flask. Transfer your thermometer to the

Simple Distillation is the sum of vapourization and condensation process.

Chemistry

10th Edition

ISBN:9781305957404

Author:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste

Publisher:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste

Chapter1: Chemical Foundations

Section: Chapter Questions

Problem 1RQ: Define and explain the differences between the following terms. a. law and theory b. theory and...

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Preparation of Cyclohexanone by Hypochlorite Oxidation

Figure 8.4
thermometer
thermometer adaptor (ground glass
adaptor plus rubber adaptor)
blue plastic
clamp
water out
water in
blue plastic
clamp
250 mL Round
bottom flask
ground glass
stopper or small
cork
metal clamp
boiling chips
heating mantle
100 mL round
bottom flask
+ Plug to Rheostat
three-way adapter as shown in Figure 8.4. Place a secure cork in the small opening. Add a few boiling chips
and distill your product, setting the rheostat on the heating mantle to about 70-80 V.
This will be a steam distillation. You will distill a mixture of water and cyclohexanone. Continue the
distillation until you have collected about 40 mL. You should see a layer of cyclohexanone on the top and an
aqueous layer of water and acetic acid on the bottom.
Work-up
When you have collected 40 mL stop the distillation. Remove the receiving flask and CAREFULLY
add solid sodium carbonate (Na,CO,) using your spatula until you have neutralized all of the acetic acid that
distilled over with your product. Add a small spatula tip of the solid sodium carbonate and stir with your
spatula. You should see evolution of CO, gas. DO NOT ADD THE SODIUM CARBONATE TOO
QUICKLY TO THE SOLUTION BECAUSE IT CAN BUBBLE OVER. Keep adding the solid until there is
no more bubbling. Remove some of the aqueous layer on the bottom with a medicine dropper and test with
litmus to see that it is neutral.
Cyclohexanone has some solubility in water. Add solid sodium chloride (add about 0.2 g of NaCl per
milliliter of water present) to salt out the cyclohexanone from the water layer. Just as we did in the cyclohexene
experiment, the idea is to saturate the aqueous layer with the very polar sodium chloride to drive the
cyclohexanone from the water layer. Do not add too much of the sodium chloride. Add a spatula tip full, stir to
dissolve and then add a bit more. Continue adding the NaCl until you see some solid material remaining.

Procedure:
Set-up your 250 mL 2-necked round bottom flask as shown in Figure 8.3. Attach the thermometer using
the red neoprene adapter. Add 6.0 mL cyclohexanol to the round bottom flask. In the 400 mL beaker, get 85
mL of bleach and add 4.0 mL glacial acetic acid in the hood.
Pour the bleach and acetic acid mixture into your separatory funnel and suspend it by an iron ring as
shown in Figure 8.3. If you have a separatory funnel that is furnished with a ground glass joint at the bottom,
DO NOT connect the joints since you want to have a system that is open to the atmosphere.
Figure 8.3
Separatory funnel
iron ring
thermometer
ground glass thermometer
adaptor plus rubber adaptor
250 mL round bottom flask
Begin adding the bleach solution slowly a few drops at a time. Monitor the temperature. You want to
maintain the temperature between 40 – 50 °C. Do not allow the temperature to rise above 50 °C. Use the
cooling bath if necessary. And, do NOT allow the temperature to fall below 40 °C. Otherwise the oxidation
will not go to completion. The addition should take about 15 – 20 minutes to complete. Be patient. Add a few
mL of the bleach, swirl the flask to mix and monitor the temperature.
When all of the bleach has been added, there should be a slight yellow color. If not, add more bleach
until a faint yellow color persists. Sometimes it can be difficult to determine if there is actually a yellowish tint
persists. Do not add more than 5-10 ml additional bleach. Holding a white piece of paper behind the flask can
be helpful.
After all the bleach has been added, allow the reaction mixture to stand for 15 minutes with occasional
swirling.
After 15 minutes, check the color of your reaction. If there is a slight yellow color, this indicates that
there is an excess of hypochlorous acid. Add sodium bisulfite (NaHSO,) solution until the yellow color
disappears. Sodium bisulfite is a mild reducing agent and it will react with the hypochlorous acid. A few mL is
usually sufficient.
Remove the separatory funnel and set-up your apparatus for a simple distillation as shown in Figure 8.4.
Use the same 250-mL round bottom flask and use a 100 mL receiving flask. Transfer your thermometer to the

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