未知のアルデヒドおよびケトンの同定
At the end of this lab, students should know...
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Q1: What safety precautions are needed when preparing DNPH solution?
DNPH is a shock explosive and must be handled gently with low friction tools to prevent accidental detonation. Always work in a fume hood, wear a lab coat, splash-proof safety glasses, and nitrile gloves. Phosphoric acid is toxic and corrosive, so avoid direct contact and ensure proper ventilation throughout the preparation process.
Q2: How do you prepare a 0.1 M DNPH solution for aldehyde and ketone testing?
Measure 3 g of DNPH into a 250-mL beaker in a fume hood. Slowly add 50 mL of 85% phosphoric acid and stir gently until dissolved. Add 50 mL of ethanol and stir until homogeneous. Vacuum filter to remove residual solids, then transfer the final solution to a labeled 100-mL container and store in a hood.
Q3: What is the correct procedure for making Tollens' reagent?
Dissolve 0.6115 g of silver nitrate in 12 mL of deionized water to form a 0.3 M solution. Add 6 mL of 3 M NaOH, which precipitates brown silver oxide. Slowly add 4 mL of 2 M aqueous ammonia using a Pasteur pipette to dissolve the precipitate. Vacuum filter the solution and store in a light-shielded brown glass bottle. Prepare immediately before use to prevent explosive silver nitride formation.
Q4: How is iodoform reagent prepared for the lab?
Dissolve 50 g of potassium iodide in 200 mL of deionized water by stirring on a stir plate. Add 25 g of iodine to the solution and stir until completely dissolved. Transfer the final solution to a labeled 200-mL container, cap it, and store in the test solution hood for use during experiments.
Q5: What glassware and equipment should be set up at each student lab station?
Each station requires a lab stand, hotplate, test tube rack, 600-mL beaker, four 250-mL beakers, graduated cylinders, a 250-mL filter flask with Büchner funnel, watch glasses, glass stirring rod, thermometer, pipette bulbs, pH paper, and lab tape. Additionally, place Pasteur pipettes, filter papers, and small test tubes in a central area for shared access.
Q6: What known and unknown compounds are used in this aldehyde and ketone identification experiment?
Known compounds include butanone and benzaldehyde, provided to all student groups. Unknown compounds include acetophenone, butanol, 3-methyl-2-butanone, pentanol, 2-pentanone, and 3-pentanone. Each unknown is prepared in two labeled vials containing 5 mL and placed in a central area for student analysis.
Q7: How should Tollens' reagent waste be safely disposed of after the lab?
Promptly dilute any unused Tollens' reagent with at least 20 mL of water and flush it down the drain with copious tap water. If necessary, use concentrated hydrochloric acid to precipitate silver from the waste first. Clean silver-coated test tubes with concentrated nitric acid in a fume hood and neutralize silver waste according to your lab's standard procedures.