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Slide 1 - Chem 334 Expt. #3 Simple and Fractional Distillation; Analysis of Distillation Fractions by GC Figure 1 Figure 2
Slide 2 - What factors affect the boiling point of a compound?
Slide 3 - Experiment #3 compounds EA = ethyl acetate CH3CO2CH2CH3 EP = ethyl propionate CH3CH2CO2CH2CH3 b.p. = 77oC b.p. = 99oC
Slide 4 - Where would you expect the boiling point of a mixture of ethyl acetate and ethyl propionate?
Slide 5 - See Techniques 2 and 3 Where would you expect the boiling point of a mixture of ethyl acetate and ethyl propionate?
Slide 6 - Boiling Point - Composition for a Liquid-Liquid Mixture Raoult’s Law “mixture of two liquids will have a b.p. that is between the of the pure liquids” PX = PoXNX where PX is the partial pressure of X PoX is vapor pressure of pure X NX is the mole fraction of X in mixture (Exception: Azeotropes)
Slide 7 - Assume a mixture of x moles of EA and y moles of EP What would be the mole ratio? What would be the mole fraction of EA in the mixture?
Slide 8 - Boiling Point - Composition for EA - EP mixture Total vapor pressure of mixture “Ptotal” is the sum of the partial pressures due to EA and EP. Ptotal = PEA + PEP If “Ptotal” is equal to the external pressure, boiling occurs.
Slide 9 - ppt slide no 9 content not found
Slide 10 - Your experiment: We will do two distillations: A simple distillation and a fractional distillation. Work in teams of two: One student sets up the simple distillation and the other student sets up the fractional distillation glassware.
Slide 11 - Table for Simple (Fractional) Distillation Temp oC # drops 1 4 8 12 70 etc. Record your data: Temp. & # drops Also collect data for Fractional Distillation
Slide 12 - Simple Distillation Set-up Add boiling chip collect the 1st two drops here, in a receiving vial. Label! Thermometer position Figure 1 *
Slide 13 - Continue recording your data
Slide 14 - Fractional Distillation Set-up Micro-column & steel sponge Be careful not to cut your hand with the steel sponge when packing the column. Figure 2 * Do not “stuff” the column too tightly
Slide 15 - Simple & Fractional Distillation Plot Both Curves on one Graph 0 4 8 12 16 20 24 28 …………………..etc. Volume of distillate (# drops) 98 oC oC oC oC Plot both S1 and F1 curves on the same graph Temperature
Slide 16 - Part C. Analysis of Distillation Fractions by GC HP 5890 Gas Chromatograph
Slide 17 - GC Detector Open Tubular Capillary Column Carrier Gas Injector Sample Flow Diagram for a Capillary GC vent
Slide 18 - Gas Chromatography A separation method for volatile compounds A chromatography method: Stationary phase and moving phase Separation is based on physical & chemical properties of each compound different interaction with the stationary phase A true microscale method!
Slide 19 - Retention time Injection point Each peak (in a good separation) represents one compound.
Slide 20 - Each peak (in a good separation) represents one compound. The area under each peak corresponds to moles of the compound
Slide 21 - EA EP Gas chromatogram of a 50:50 (v:v) EA/EP mixture In diethyl ether Remember: Diethyl ether ≠ Petroleum ether !!!
Slide 22 - Next time: Gas chromatography (conclusion) Steam distillation: Isolation of eugenol from cloves