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Experiment 3 Essay

1413 words - 6 pages

Experiment 3
4. Results and Observations (for detailed observations and results see lab notebook)
Compound Y:
Initial Volume: 29 ml

Fractional Distillation
Head T (°C) Volume (ml) (see graph for plot of distillation temperature vs. volume)
78 2 (Fraction A)
81 4
82.5 6
84 8
84.5 10
85 12
86.5 14 (At this pt, switched flask A to flask B)
98 16 (Fraction B)
104 17
105 18
105.5 19 (At 19.4 ml switched from flask A to flask B)
108 22
106 24 (At 24.6, removed flask C)
Flask A (Fraction A): 14 ml
Flask B (Fraction B): 5.4 ml
Flask C (Fraction C): 4.6 ml

Simple Distillation (see graph for plot of distillation temperature vs. ...view middle of the document...

994 mm2
- % Composition of Cyclohexane: 81.142%
- % Composition of Toluene: 18.5%
Fraction B:
- Peak Area 1: 139.407 mm2
- Peak Area 2: 269.223 mm2
- Total Area: 408.630 mm2
- % Composition of Cyclohexane: 34.116%
- % Composition of Toluene: 65.884%

Fraction C:
- Peak Area 1: 5.739 mm2
- Peak Area 3: 485.946 mm2
- % Composition of Cyclohexane: 1.167%
- % Composition of Toluene: 98.833%

Steam Distillation
Initial Weight of Cloves: 3.31 g (some lost in transfer)
Final Weight: .65 g
% recovery: 19.64%

See attached
See IR Spectra for results. (Also, discussed in conclusion)

5. Conclusions/Discussion:
After completing this lab, I have learned how to execute three different methods of distillation and the efficiency or best use of each one. First, I would like to discuss the differences between simple and fractional distillation to give greater insight on the graphical representation of head temperature vs. volume for both fractional and simple distillations. Simple distillation allows isolation of the various fractions of the mixture in acceptable purity if the difference between boiling points of each pure substance is greater than 40-50°C. In this experiment, cyclohexane and toluene differed by about 20°C, which suggests that the separation of the two components may not be very successful using the simple distillation method. Furthermore, a successful separation can be observed if two different temperature plateaus are observed (such as in Figure 9.5) because the head temperature will rise to the normal boiling point of the more volatile component and once that is removed it will rise to the BP of the second component. Now, looking at the simple distillation plot, one can see an indistinct outline similar to two plateaus; however, the head temperature seemed to increase drastically over increasing volume and clear plateaus are not existent. This implies that this method may not be a sufficient method to isolate these two compounds from each other. Fractional distillation, on the other hand, is used to separate volatile compounds that differ less than 40°C in BP, which is the case in this experiment. Comparing the fractional distillation plot to the simple, one can observe more distinct plateaus with an increase in temperature in between. Though there is still deviance from the “expected” or “ideal” plot, the fractional distillation plot suggests that a better-defined separation of each component into fractions occurred.
Next, I would like to discuss the differences between the manual triangulation method with the electronic integrator results. The electronic integrator is of course much more accurate than manually determining the peak area ratios. Though my determination of the peak areas and calculations for percent compositions deviate from the results from the electronic integrator, the results of both are relatively similar. One reason that the manual triangulation method may have induced imprecise calculations...

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