Table 1: Volume of distillate and temperature of vapour data Simple distillation Volume(ml) 0.5 1.5 2.0 2.5 3.

0 3.5 Receivers changed 4.0 4.5 5.0 5.5 6.0 6.5 7.0 Fractional distillation Volume (ml) 0.5 1.0 1.5 2.0 2.5 3.0 3.5 Receivers changed 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0

Temperature (:C) 79 80 80.5 81 82 84

Temperature (:C) 80.0 80.5 80.5 80.5 79.0 80.0

89 98 98.5 98.5 98.5 99 99

99 99 99 99 99 99 100 100

120

Graph 1: Volume of distillate and temperature of vapour

100

80 Temperature ()

60

40

20

0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7 Volume(ml)

Table 2: Analysis of Temperature vs. distillate produced data Distillation Simple Fractional Fraction Ethanol (1st) Water (2nd) Ethanol (1st) Water (2nd) Volume (ml) 4.5 5.5 3.5 6.5 % Volume 45 55 35 65 Experimental bp (:C) 80.13 99 80.38 100

Literature boiling point: Ethanol: 78.3:C Water: 100:C

Reference: National Institute of Standards and Technology (NIST), 2011 Table 3: Analysis of original beverage (rum) by VPC Rum Water Ethanol Retention time (min) 0.680 2.793 Peak Area (counts) 1727064105 751656768 % Area 69.68 30.32 % Mass 74.58 25.42 % Volume 60.77 39.23

Calculation for percentage volume: 1)Finding the % mass of ethanol knowing the % area of ethanol: y=0.9641x-2.2172 y=30.32% (% area of ethanol) 30.32=0.9641x-2.2172x= 33.75%mass for ethanol % mass of water=100%-%mass of ethanol100-33.75= 66.25% mass of water 2)Volume of ethanol and water in 100g of a mixture: 33.75g of ethanol in 100g = x=42.77 ml of ethanol = 66.25g of water in 100g x=66.25 ml of water

3)Volume percentage of ethanol and water : x100 x100=39.23%

Volume percentage of water100%-39.23%= 60.77%

Table 4: Analysis of Data from the VPC of simple and fractional distillation Type of distillation Fractional distillation Simple distillation Ethanol Water Ethanol Water Retention time (min) 2.617 0.853 2.683 0.867 Peak Area (counts) 413755615 82171812 356175769 116459625 % Area 83.43 16.17 75.36 24.64 % Mass 88.84 11.16 80.47 19.53 % Volume 90.98 9.02 84 16

Sample calculations for % Volume of the Fractional Distillation: Calculation for percentage volume: 1)Finding the % mass of ethanol knowing the % area of ethanol: y=0.9641x-2.2172 y=83.43% (% area of ethanol) 83.43=0.9641x-2.2172x= 88.84%mass for ethanol % mass of water=100%-%mass of ethanol100-88.84= 11.16% mass of water 2)Volume of ethanol and water in 100g of a mixture: 88.84 g of ethanol in 100g = x=112.6 ml of ethanol 11.16g of water in 100g = x=11.16 ml of water

3)Volume percentage of ethanol and water : x100 x100=90.98%

Volume percentage of water100%-90.98%= 9.02%

Answers to questions: a)The flat portions of the curve for the fractional distillation can be more easily distinguished than the ones on the simple distillation graph, therefore the boiling points ,on the curve of fractional distillation, for each fraction is probably more accurate. Furthermore, the point of inflection is more easily found on the fractional curve because the cut-off is sharper (slope is sharper at the middle of the curve), but for

the simple distillation it was very difficult to accurately find the point of inflection. Therefore for the fractional distillation, the separation of both fractions is more efficient and accurate and so the calculation for the %volume for each fraction is more accurate. Finally, it is clearly proven that separation using fractional distillation is more efficient. b) Distillation Simple Fractional VPC Fraction Ethanol (1st) Water (2nd) Ethanol (1st) Water (2nd) Ethanol Water % Volume 45 55 35 65 39.23 60.77

Observing the results above, it would be fair to say that fractional distillation yields more accurate results than simple distillation as the %volume of ethanol and water is much closer to the results of the chromatograph from the lab manual. c) Type of distillation Fractional distillation Simple distillation Retention time (min) 2.617 0.853 2.683 0.867

Ethanol Water Ethanol Water

The retention time for water and ethanol is significantly different and this is normal because the retention time is characteristic to each compound and most of the time it is used to identify an unknown compound by comparing it with the retention time of a known compound. However, the retention time between the simple and fractional chromatograph for each compound doesnt differ significantly and this is normal. Retention time has nothing to do with accurate separation, retention time is something characteristic of each compound and therefore it shouldnt differ much between the simple distillation and fractional distillation VPC.

d) % volume of ethanol from simple distillation: 45 %volume of ethanol from VPC of simple distillation: 84 The result found using the chromatograph is more accurate than the one from the curve of simple distillation. Indeed, when calculating the %volume using the curve of simple distillation, we assume that from 0ml to the point of inflection it is ethanol that is collected and from that point on water. However, we cant be sure of that and furthermore the inflection point is very difficult to distinguish on the simple distillation curve. Therefore we have very inaccurate results for the %volume of ethanol. However, the chromatograph gives more accurate results as each fraction of ethanol and water collected is analyzed through the graph. It displays very detailed results such as the retention time which is important to distinguish each compound, the %area, % mass This makes it that our calculations are very precise and therefore our results are also more precise. With the chromatograph there is no guessing and assumptions which I feel is the case for the curve of simple distillation. e) Type of distillation Fractional distillation Simple distillation % Volume 90.98 9.02 84 16

Ethanol Water Ethanol Water

Analyzing the above results, it would be fair to say that the ethanol fraction in both fractional and simple distillation was pure. In the simple distillation %volume of ethanol in the ethanol fraction was of 84 and there was only 16% volume of water that was still left. As expected, in the fractional distillation the %volume of ethanol in the ethanol fraction was even more pure as there was 90.98% of ethanol and only 9.02% of water left which is a pretty good result. Fractional and simple distillation gave good results, but obviously if a method has to be chosen between these two, fractional distillation would be a much better choice as proven from the results above. Questions from lab manual

15. After the sample to be analyzed is introduced at the sample injection port, it is vaporized and carried by the carrier gas to the column. Then the liquid phase dissolves the sample. Components of the sample are revaporized and separation occurs because of the affinity of the different compounds for the liquid. Compounds with less affinity will emerge first, less time to remain in solution and so compounds with stronger affinity will stay longer in the liquid. The different compounds of the sample will separate into various bands and travel at different rates in the column.1 To know which peak is ethanol and which one is water, you need to know which one has a stronger affinity with the liquid, ethanol has a stronger affinity therefore it will be the second peak on the graph (retention time). 16. Retention time is the amount of time between the injection of the sample until a peak appears on the graph.2 17. The peak area is important because it is used to find the %area for each compound in a sample. The number of moles of any component is proportional to its peak area and by dividing the peak area of a compound by the total area which is the addition of all areas under all peaks, it is possible to find the % area which can be later on be used to find the %volume of each component of a sample. 3

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Chemistry Department, 2013 Chemistry Department, 2013 3 Chemistry Department, 2013