Purpose
To demonstrate that two volatile compounds can separate from a mixture due to the different chemical properties of each compound. To be able to analyze the data and see which distillation process worked best to purify the unknown.
Procedure
To the 10 mL round-bottomed flask, add 8.0 mL of the unknown mixture (#6). The neck of the flask was then clamped securely to a ring stand using a small three-pronged clamp. Using the blue plastic connector, the distilling head was attached. Using a blue plastic connector the condenser was attached with both hoses. Then another plastic connector was attached to the condenser for a vacuum adapter. The 10 mL flask was placed on a block, which was getting heated by a hot plate. A thermometer was then inserted into the distillation head with the tip being just below the connection of the condenser. The vacuum take off adapter is positioned under a 10 mL graduated cylinder to catch the purified liquid. For fractional distillation same steps are taken, only difference is between the distillation head and the 10 mL round bottom flask there is a fractioning column with a thin piece of copper wire inside of it. Fractional distillation set up Simple distillation set up
Results
Part A: Semi Microscale
Part B: Microscale
Simple Distillation
Area (Part A)
Volume (mL) Temp (oC)
0.5 88.0
1.0 88.8
1.5 89.4
2.0 90.8 2.5 92.2
3.0 94.5
3.5 95.4
4.0 97.9
4.5 99.9
5.0 103.2
5.5 106.7
6.0 109.0
Fractional Distillation
Area (Part A)
Volume (mL) Temp (oC)
0.5 84.9
1.0 85.8
1.5 86.7
2.0 88.1
2.5 90.3
3.0 90.6
3.5 94.7
4.0 99.2
4.5 107.8
5.0 107.5
5.5 110.5
Simple Distillation
Area (Part B)
Volume (mL) Temp (oC)
1.0 88.3
1.8 89.7
2.6 92.1
3.0 93.4
3.6 95.0
4.2 98.7
4.6 102.4
5.2 106.7
5.8 110.3
6.0 111.0
Fractional Distillation
Area (Part B)
Volume (mL) Temp (oC)
1.0 86.9
2.0 88.5
2.5 90.3
3.0 93.3
3.7 97.5
4.0 101.2
4.2 103.8
4.3 104.8
4.5 106.0
5.0 108.4
5.5 111.7
6.0 111.2
It is a bit unclear but one can see that from 95.40C to 99.90C is a peak, and then from
99.90C to 1090C is when it reaches its final boiling point.
Beginning at 90.00C to 99.20C it’s a peak, and then beginning from 99.20C to 107.80C is
another peak, and then it reaches to 110.50C
Beginging at 950C to point 110.30C one can see the transformation, very clearly.
Beginging at 1030C to point 111.70C one can see the transformation.
My unknown #6 falls