Experiment 2: Distillation of an Unknown Liquid

Objectives:
__ Perform a simple distillation
__ Determine the boiling point of a liquid
__ Determine the identity of the chosen unknown

Chemical Properties: taken from Sigma Aldrich1

Molar Mass Melting Boiling Density

Chemical Hazards (g/mol) Point (°C) Point (°C) (g/mL)

1-propanol (CAS 71-23-8)

2-propanol (CAS 67-63-0)

1-butanol (CAS 71-36-3)

1. Sigma Aldrich Online Catalog. www.sigmaaldrich.com Accessed June 5, 2020.

Procedure:
1. Measure out approximately 15 mL of your unknown liquid.
a. Measure in the hood and transfer to a 25 mL round bottom flask.
b. Cap the flask before leaving the hood to minimize exposure to vapors.
2. Attach your round bottom flask to a simple distillation
a. See diagram for instructions
b. Make sure water is running before turning on heat
3. Begin the distillation. Record the temperature when approximately half of the liquid has distilled.
a. Set the heat to the lowest of the potential boiling points (+ 50°C to account for heat loss)
b. Slowly increase the heat as needed. (It will look like nothing is happening at first,
because the liquid and the glassware must heat up for the vapors to travel)

Important Safety Note: Never turn the heat to max. Do not exceed 50°C above the potential boiling
point. Solvents are flammable. Overheating may release excess vapors into the air and cause solvent to
ignite.
 Troubleshooting tips:
 Make sure all joints are fully sealed (no gaps) – vapors will escape rather than collecting
in the receiving flask
 Use an appropriately sized heat-block (so you will not need to use any sand).
 Do not use any more sand than is absolutely necessary – sand is a poor heat conductor
and will slow down the process

Clean Up:
o All organic solvents used go into the liquid waste containers in the SAA hood
o Aqueous solutions from the extraction go into the liquid waste containers in
the SAA hood
o Ice bath water can be poured into the sink
o All solids collected go into the solid waste container in the SAA hood
o Filter paper, pH paper, weigh paper, pipets, paper towels, and gloves go into
trash cans
o Melting point capillary tubes go into the glass waste container

Observations:
General: (colors, fumes, anything of note including details related to your set-up)

Experimental boiling point:

Conclusion: What is the identity of your unknown? (Include what unknown you used.)

[Diagram of distillation]: Water flows in through the top of the condenser and exits through the bottom.