I followed the following lab procedure and produced thefollowing FTIR spectrum. can you please analyze the spectrum forthe intended products and any conclusions you have on it?
thank you!
I Followed The Following Lab Procedure And Produced The Following Ftir Spectrum Can You Please Analyze The Spectrum For 1 (551.79 KiB) Viewed 58 times
I Followed The Following Lab Procedure And Produced The Following Ftir Spectrum Can You Please Analyze The Spectrum For 2 (380.06 KiB) Viewed 58 times
Goal: Oxidation of cyclohexanol to cyclohexanone using sodium dichromate; characterization of product via FTIR. Experiment protocol: 1). In a 50mL beaker, dissolve 1.5g sodium dichromate in 7mL of 2M sulfuric acid. 2). Measure out 0.75g of cylcohexanol into a 50mL Erlenmeyer flask. Add the sodium dichromate solution (in the 50mL beaker from the previous step) to the cyclohexanol in the Erlenmeyer flask. Add a thermometer to the flask. 3). For the next 15-20 minutes, swirl the mixture in the flask (do not stir with the thermometer-they break that way!!) and try to keep the solution between 55-60°C. Have both a steam bath and an ice bath available in order to control the temperature of your reaction. During the reaction time, set up for a simple distillation that will use a sand bath as a heat source (ask your TA if you need help remembering the setup). 4). After 15-20 minutes have passed, transfer the entire solution from the Erlenmeyer flask to a 10mL round bottom flask and distill (simple distillation) approximately 2.5mL of the mixture. Make sure to add a black boiling stone (available in the hood) to the round bottom flask before heating. Use a Pasteur pipette to collect the distillate from the Hickman stillhead and place it in a test tube. You should see two layers in the tube. 5). Add 0.3g sodium chloride to the test tube containing the distillate. Shake and stir the mixture until most of the salt is dissolved. Adding inorganic salts, such as sodium chloride, to the aqueous layer will decrease the solubility of cyclohexanone so that it can be more completely extracted. This process is known as salting out. 6). Pipette off the top, organic layer from the test tube and place it in a centrifuge tube. Extract the aqueous layer (still in the test tube) twice with 0.5mL (10-12 drops) of t-butyl methyl ether, adding each portion of ether to the cyclohexanone already in the centrifuge tube.
7). Add 1mL of saturated sodium chloride solution to the centrifuge tube. Mix gently and then pipette off the top, organic (ether/cyclohexanone) layer into a 20mL beaker. 8). Dry the ether/cyclohexanone mixture with calcium chloride pellets. Record the mass of an empty 3mL conical vial. Add the ether/cylohexanone mixture (but not the calcium chloride pellets) to the vial. Wash the pellets with another 0.5mL of t-butyl methyl ether and add that to the 3mL conical vial as well. 9). Use the rotary evaporator to evaporate the t-butyl methyl ether from the vial, leaving the cyclohexanone. Record the mass of the vial again, determine the mass of your product, and percent yield for the reaction. 10). Take your product to the FTIR station to get an infrared spectrum of your product. Discuss the relevant peaks in your lab report (Does the spectrum support that the reaction occurred? Is your product pure?). 11). Clean glassware with the water squirt-bottles this week instead of acetone. Make sure to dump the dirty water into the Oxidation hazardous waste container (not the acetone wash). Failure to dispose of the hazardous waste correctly will lead to a "zero" for the lab.
Transmitance 0.8 0.6 0.4 0.2 0.0 3000 CYCLOHEXANONE INFRARED SPECTRUM 2000 Wavenumber (cm-1) NIST Chemistry WebBook (https://webbook.nist.gov/chemistry) 1000
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