氧化

装置设置

1. Charge the flask before fitting the condenser; do not fill the flask more than about half full.
2. Run cooling water into the lower condenser inlet and out from the upper outlet.
3. Keep the top of an ordinary reflux condenser open to the atmosphere unless the cited procedure specifies a pressure-rated closed system.
4. Heat to a gentle, steady boil so the condensation line remains within the condenser and liquid returns continuously to the flask.

操作检查

• Use an electric bath or mantle for flammable organic liquids; do not use a naked flame.
• Start condenser water before heating and confirm that hoses are secure.
• If addition is exothermic, complete the controlled addition and cooling stage before sustained reflux.

装置设置

1. Position the thermometer bulb at the entrance to the condenser so it measures vapour entering the condenser.
2. Run cooling water into the lower condenser connection and out through the upper connection.
3. Heat gradually and collect only the fraction specified by the cited boiling range or procedure.

操作检查

• Do not distil a flask to dryness.
• Use an electric heat source for flammable mixtures.
• Change from reflux to distillation only after heating has stopped and the apparatus has cooled enough to handle safely.

装置设置

1. Check sample identity, background and axis units before assigning absorptions.
2. Compare the starting material and product: oxidation may introduce C=O while removing an alcohol O–H feature.

操作检查

• Water, solvent and unreacted substrate can contribute bands.
• A carbonyl band alone does not distinguish every aldehyde, ketone, acid and ester. Use reference data and complementary evidence; no simulated trace is a measurement.