Experimental Procedure6A
1) Assemble distillation apparatus with and without fractionating column
(simple distillation and fractional distillation)
2) Insulate fractionating column, bulb thermometer directly below side port
3) Add boiling stones to round bottom flask
4) Add 15.0mL unknown mixture to flask
5) Start water circulation on condenser (water inlet = lower, against gravity, water outlet = higher)
6) Heat flask with hotplate in sand bath
7) Regulate temp so drops of distillate fall at rate of one drop per five seconds into graduate cylinder / vial. (Heat will have to be readjusted through distillation as proportions of unknown mixture and vapor will be changing)
8) Once graduated cylinder distillate volume reaches 1.0mL, record temp, switch to labeled vial, collect 1.0mL sample and temp, repeat until round bottom flask is almost empty but not dry.
9) Turn off heat and raise distillation apparatus off sand bath and hot plate.
Results Simple Distillation
Temperature C Sample Volume mL GC Peak One % GC Peak Two %
72 1.0mL S1 90.63% 9.269%
74.5
76
80
86.5
92
1.0mL
1.0mL S3
1.0mL
1.0mL S5
1.0mL
83.34%
60.79%
16.58%
39.14%
101.5
103.5
104
1.0mL S7
1.0mL
1.0mL S9
7.336%
0.569%
92.60%
99.37%

61
61
94
95
96
96
Compound A BP ~ 74C
Compound B BP ~104C
Out of the possible compounds, Compound A's boiling point is closest to hexane
(69C), and Compound B's boiling point is closest to heptane (98.4C).
Results Fractional Distillation
Temperature C Sample Volume mL GC Peak One % GC Peak Two %
62
56
1.0mL F1
1.0mL
94.68% 5.220%
61
60
62
1.0mL F3
1.0mL
1.0mL F5
95.48%
94.18%
4.431%
5.745%
1.0mL
1.0mL F7
1.0mL
1.0mL F9
1.0mL
1.0mL F11
89.09%
0.398%
0.062%
10.83%
99.56%
99.90%

Compound A BP ~60C
Compound B BP ~96C
Out of the possible compounds, Compound A's boiling point is closest to hexane
(69C), and Compound B's boiling point is closest to heptane (98.4C).