Dean and Stark Apparatus

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Dean and Stark Apparatus

Dean and Stark Apparatus

Make: LabTek

Model: SL-2060

Origin: India

Standards: ASTM D 95,D244

Specification: Dean and Stark Apparatus: Standards:ASTM D 95,D244, Specification: Used to determine the water in petroleum products or bituminous materials by distilling them with volatile solvent. The equipment comprises electric heater with thermoregulator, glass still, support stand, condenser, receiving trap.

Dean and Stark Apparatus, dean stark apparatus, dean stark apparatus price, dean stark trap reaction, dean stark mechanism.

Dean and Stark Apparatus, dean stark apparatus, dean stark apparatus price, dean stark trap reaction, dean stark mechanism.

Procedure

1. Preparation

  1. Take a 250 mL round bottom flask equipped with a magnetic stir bar.
  2. Place an oil bath under the round bottom flask on a magnetic stirrer.
  3. Fill the round-bottom flask with 7.5 g (0.05 mol) m-Nitrobenzaldehyde and add 75 mL of toluene.
  4. Add 3.1 mL (3.45 g, 0.055 mol) ethylene glycol.
  5. Attach the Dean-Stark trap to the round bottom flask.
  6. Attach a reflux condenser on top of the Dean-Stark trap.

2. Running the Reaction

  1. Set the oil bath temperature to 170 °C and heat the reaction mixture to reflux.
  2. Monitor the reaction by measuring the water amount in the Dean-Stark trap.
  3. The reaction is done when no further water becomes trapped in the side arm of the Dean-Stark trap.
  4. After approximately 2 h, the total amount of collected water is approximately 0.8 mL.

3. Workup

  1. Release the water and remove the combined organic solvent from the reaction mixture under reduced pressure in a rotary evaporator.
  2. Dissolve the yellow residue in 8 mL ethanol under reflux.
  3. Cool down the solution.
  4. The desired acetal will crystallize.
  5. Filter the solid and dry it under reduced pressure.

Results

Water will form and becomes trapped over the course of the reaction. The theoretical amount of formed water upon complete conversion can be calculated and compared with the measured amount of the trapped water to determine the reaction progress.

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