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Cornell University - CHEM 2510 Experiment 3 Distillation

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Background: This lab experiment was done to compare the effectiveness of various distillation methods when distilling out methyl acetate from n-butyl acetate, ethyl acetate, or n-propyl acetate. The different methods ...

Background: This lab experiment was done to compare the effectiveness of various distillation methods when distilling out methyl acetate from n-butyl acetate, ethyl acetate, or n-propyl acetate. The different methods included a simple distillation, as well as a fractional distillation with glass beads, choreboy, carborandum chips, or vigereaux columns. A 25 mL sample of 1:1 methyl acetate: n-propyl acetate was obtained and then distilled according to the assigned method, in my case being a distillation with a vigereaux column. 3ml portions of the distillate were separately collected over the course of the distillation. Each sample was then analyzed by refractive index and observed melting point range in order to determine how pure the distillate truly is, and therefore the efficacy of the distillation method in separating two distinct substances. N-propyl acetate: Boiling Point: 101.6C Refractive Index: 1.387 Methyl acetate: Boiling Point: 58C Refractive Index: 1.360 Results: Table 1. Fractional Distillation using Glass Beads (my results) Distillate Number Fraction (ml) Initial Boiling Point (C) Final Boiling Point (C) Measured Refractive Index (n= ) 1 2.46ml (0-2.46) 55 56 2 2.56ml (2.46-5.02) 57 57 1.359 3 2.59ml (5.02-7.61) 58 59 4 1.4ml (7.61-9.01) 59 62 1.360 5 1.16ml (9.01-10.17) 65 95 6 2.46ml (10.17-12.63) 97 97 7 2.65ml (12.63-15.28) 98 98 8 2.22ml (15.28-17.5) 98 98.5 1.381 Qualitative observations: The solution began boiling almost immediately (around 24 C). Vapor slowly began to form on the surface of the glass beads and the level of the mark between the liquid and gas phase (condensation line) began to rise. The flow was substantially reduced after the third sample and the temperature began to go above the boiling point of methyl acetate, indicating an apparent completion of the evaporation of the methyl acetate. Smaller increments of samples were collected at this point to confirm this completion. Furthermore, the flask was not allowed to run dry, leaving about 5 ml left in the flask, most likely pure n-propyl acetate since

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