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I need the procedure in bullet proof in own words  and just an outline of how the raw data would like in a table from the experiment since i do not have data it will be left blank

I need the procedure in bullet proof in own words  and just an outline of how the raw data would like in a table from the experiment since i do not have data it will be left blank

Chemistry
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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I need the procedure in bullet proof in own words 

and just an outline of how the raw data would like in a table from the experiment since i do not have data it will be left blank 

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 fumished 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 Figure 84 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 TO0 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.
Transcribed Image Text: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 fumished 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 Figure 84 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 TO0 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.
Experiment 8 Preparation of Cyclohexanone by Hypochlorite Oxidation In this experiment we will prepare cyclohexanone from cyclohexanol using hypochlorite oxidation. We will use common household bleach that is a 5.25% (0.75 M) aqueous solution of sodium hypochlorite. The overall reaction is shown in Figure 8.1. Figure 8.1 Oxidation of Cyclohexanol Na+ OCI CH ОН НОС + CH Na+ sodium hypochlorite acetic acid OH HOC1 H2O HC1 cyclohexanone cyclohexanol The exact reaction mechanism is not known but a plausible mechanism is given below. It is known that the mechanism does not involve free radicals and that yields are better in acidic rather than basic conditions. This is why we use acetic acid. It reacts with the sodium hypochlorite to give hypochlorous acid, which then reacts with the oxygen of the alcohol. Note the oxygen is more electronegative than chlorine so the oxygen attacks the chlorine of the hypochlorite, which has a formal charge of +1. Figure 8.2 Mechanism for Oxidation H,C H OH H,O H. + H,O + CI Physical Constants Compound Mol. Wt (g/mol) b.p. (°C) Density (g/mL) 0.96 m.p. (°C) Cyclohexanol Cyclohexanone Dịchloromethane 100.16 161.5 25.5 98.15 0.947 155 -47 84.93 1.325 39-40 -97
Transcribed Image Text:Experiment 8 Preparation of Cyclohexanone by Hypochlorite Oxidation In this experiment we will prepare cyclohexanone from cyclohexanol using hypochlorite oxidation. We will use common household bleach that is a 5.25% (0.75 M) aqueous solution of sodium hypochlorite. The overall reaction is shown in Figure 8.1. Figure 8.1 Oxidation of Cyclohexanol Na+ OCI CH ОН НОС + CH Na+ sodium hypochlorite acetic acid OH HOC1 H2O HC1 cyclohexanone cyclohexanol The exact reaction mechanism is not known but a plausible mechanism is given below. It is known that the mechanism does not involve free radicals and that yields are better in acidic rather than basic conditions. This is why we use acetic acid. It reacts with the sodium hypochlorite to give hypochlorous acid, which then reacts with the oxygen of the alcohol. Note the oxygen is more electronegative than chlorine so the oxygen attacks the chlorine of the hypochlorite, which has a formal charge of +1. Figure 8.2 Mechanism for Oxidation H,C H OH H,O H. + H,O + CI Physical Constants Compound Mol. Wt (g/mol) b.p. (°C) Density (g/mL) 0.96 m.p. (°C) Cyclohexanol Cyclohexanone Dịchloromethane 100.16 161.5 25.5 98.15 0.947 155 -47 84.93 1.325 39-40 -97
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