Giovanni Santangelo Chemistry 8-L6 2-29-2012 1

Lab 4: Distillation Introduction: The Lab is technique based and focuses on the ability to properly perform distillation. Using the melting points the amount of gas distilled can be determined. Physical Data Table: Solvent Structure Chemical formula Weight (g/mol) Boiling Point (C) 81-86 Cyclohexane C6H12 84.16 Melting Point (C) 7 Density MSDS g/cm3 0.779
Skin irritant flammabl e

130-138 p-xylene C8H10 106.67

13.2

0.887

Harmful to body flammabl e

-93 Toluene C7H8 92.14 104-111

0.861

Skin irritant flammabl e

Procedure: Assemble the distillation apparatus Transfer 30 mL into a 50 mL round bottom flask(both distillations) Heat until boiling point is achieved Collect 1 mL into a 10 mL graduated cylinder, transfer the 1mL to a test tube (cap immediately). Collect remaining 25 mL using a 25 mL graduated cylinder (do not collect to dryness) Collect last few drops in a test tube, cap immediately (do not collect to dryness) Follow procedure for gas chromatograph on cyclohexane sample Determine the mole fraction of cyclohexane

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Data & Observations: Cyclohexane & Toluene mL Temperature (C) 1 60 2 79 3 80 4 81 5 82 6 83 7 84 8 84 9 84 10 84 11 84 12 85 13 85 14 86 15 86 16 86 17 86 18 86 19 86 20 78 21 77 22 76 23 76 24 78 25 79

Cyclohexane & P-xylene Temperature (C) mL 1 60 2 60 3 61 4 61 5 61 6 61 7 61 8 62 9 62 10 62 11 62 12 61 13 60 14 58 15 55 16 55 17 70 18 79 19 77 20 72 21 71 22 67 23 78 24 84 25 82

Cyclohexane & Toluene

100 Temperature 80 60 40 20 0 0 5 10 15 mL 20 25 30

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Cyclohexane & P-xylene

Temperature 100 50 0 0 5 10 15 mL 20 25 30

First mL: Area of Cyclohexane = 3252.70 Area of Toluene = 1055.47 Percent of Cyclohexane = 58.03% Percent of Toluene = 18.83% Last Drops: Area of Cyclohexane = 79.97 Area of Toluene = 5269.44 Percent of Cyclohexane = 1.49% Percent of Toluene = 98.28% Discussion: In the lab we had to record the temperature every mL because when there was a spike in the temperature the distillation then switched between cyclohexane and the other solution, either toluene or p-xylene. There was little error in this lab and it went smoothly. My lab partner and I had 4 peaks; however the Toluene and cyclohexane peaks were easily determined. However, in the first drop which was collected the solution is mostly Cyclohexane because it has a lower boiling point than that of Toluene. Conclusion: This experiment was successful in distilling the solutions separately. There was a clear line in my data when the distillate switched between Cyclohexane and toluene/ p-xylene because the temperature quickly jumped because the solutions other than cyclohexane had a higher boiling point. My lab partner and I were successful in the gas chromatography and able to determine the percent of solution in each sample. There was virtually no error, the only possible error may have been not placing the test tube in the gas chromatography machine quick enough on the first mL. Questions: 1. Yes the goals of this experiment were achieved because we were able to find how much of each solution was in our sample using gas chromatography. At the lower boiling point setting it consisted of mostly cyclohexane because it has a lower boiling point than

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2.

3.

4.

5.

toluene, when all of the cyclohexane was gone the boiling point increased in order to distill the rest of the toluene. The second distillation was more efficient at separating the two components because the switch in temperature between the cyclohexane and p-xylene was distinct. In the first distillation, the temperature is similar and there is not a definitive jump so cyclohexane and toluene did not separate as well. However, just looking at the cyclohexane and toluene distillation the first mL had a better separation because the solution was mainly cyclohexane, compared to the last few drops which was close between that of cyclohexane and toluene. Adding a fractionating column would have helped the separation of cyclohexane and toluene because fractional distillation has an extra column between the flask and adapter, therefore it improves separation because there is more time allowed for distillation to occur. Distillation can be used for multiple things such as to separate and purify solutions. One example is when you distill salt water in order to get pure water. The more distillation done, the purer the solution will become. Also, the sample will become purer if fractional distillation is used compared to simple distillation. As for the sample size, the larger the sample, the more time you need to distill in order to get the same purity as you would for a smaller sample. With larger samples, it may be necessary to do multiple distillations in order to get a pure sample. Gas chromatography is a good technique to use to test purity of a solution and to separate a solution. However, it is not as effective as fractional distillation. Gas chromatography works best on smaller sample sizes and can only be used on gases and liquids. In the first mL we got 58% cyclohexane and 18% toluene. In the last few drops we got 1.5% cyclohexane and 98% toluene. The percent recovery could have been improved if we had used fractional distillation instead of simple distillation because there could have been better distillation and improved separation. Also, using grease to assemble the distillation equipment negatively affected my data because I got four peaks instead of just two.