Experiment 6_ Dehydration and GC
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Dehydration and Gas Chromatography Lab Makayla McDonald
CHM 201 Section Lab A
Dr.Van Ness
October 27, 2023
Purpose:
The purpose of this experiment is to use fractional distillation, extraction, and gas Chromatography to separate the chemical components of a sample mixture and then detect them to determine their presence or absence
. Then, utilize gas chromatography to determine the composition of the liquid mixture. Reaction Scheme:
●
ChemDraw reaction scheme (Included student name)
Procedure:
To a 5.0 ml conical vial hexane and toluene was added.(3mL) Attached a hickman distilled head to the conical vial and a Claisen adapter to the top of the hickman distilled head. The side part of the distilled head was closed. The microscale was clamped from step 1 to a ring stand and placed on top of the hot plate in the hood. Used the metal heating block on top of the hot plate that a good portion of the conical vial was covered. Then used another clamp to place on the heating block. Insert a thermometer down through the microscale distillation apparatus that the tip of the thermometer was level with the bottom of the collection port of the hickman head. Then obtained three 1 dram vials and labeled them for the three separate fractions. Then pre weigh each vial. Raised the temperature of the aluminum block to 80-90 C at a maximum rate of 5 C/min. The liquid begins to boil, reducing the heating rate to a maximum of 2 C/min. Collect the distillate in three fractions over the following block temperature ranges: 65-85 C, 95-
105 C, 105-110 C. Remove the fraction from the hickman distillation head by inserting a Pasteur pipet in the side part and transferring the liquid to an appropriately labeled vial. Record the temperature ranges of the hickman distillation head for each fraction that was collected. Once the
third fraction was collected, turn off the heat and allow the microscale distillation apparatus to
cool before disassembling and cleaning. Weigh each fraction vial and determine the mass of each
fraction collected. Wrapped each vial with parafilm and save. Data, Calculations, and Results: Fraction 1
65-85 C
Fraction 2
95-105 C
Fraction 3
105- 110 C
Sample
RT 1 (min)
RT 2 (min)
Area 1 (mVas)
Area 2 (mVas)
Mass %1
Mass%2
1
1.542
3.241
830.51
72.70
95.09%
4.91%
2
1.548
3.252
445.71
524.14
53.34%
46.6%
3
1.566
3.333
234.51
694.71
9.3%
90.7%
Spiked
1.551
3.275
327.72
538.41
59%
41.0%
Standard
1.557
3.278
283.01
294.54
78.1%
21.9%
Calculations: https://heidelberg-my.sharepoint.com/personal/mmcdonal_heidelberg_edu/_layouts/
15/doc.aspx?sourcedoc={a89951f3-a762-41a2-a62e-61a2f112b24c}&action=edit
Results and Discussion
Since hexane has a lower boiling point than toluene, the first fraction was hexane. The higher peak was going to represent the higher percentage of the component in the mixture. Area 1 is hexane due to a higher amount then Area 2. The third fraction was toluene due to its higher boiling point. Hexane was extracted out during the first two distillations. Hexane eluted first due to the compound with the lower boiling point running through the column and coming out faster than the compound with the higher boiling point.Fraction 1 had a greater amount than Fraction 2 and 3. Sample 1 has more hexane percentage than toluene percentage. Sample two has more hexane percentage than toluene percentage. Sample 3 has more toluene percentage than hexane percentage. Conclusion (15 pts)1 para
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●
Summarize the experiment. Do not provide procedures in this section.
●
Explain whether or not the process of distillation was an effective method for isolating hexanes.
References:
References: VanNess, B.G Organic Chemistry laboratory manual, 2023 pp. 23-255
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