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Organic Chemistry Lab 4

Organic Chemistry Lab 4 - October 17th 2007 Craig Nutter...

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October 17 th , 2007 Craig Nutter Section #9, Wednesday 2:30 Experiment 4 Title: Fractional Semimicro Distillation: Separation of Cyclohexane and Methylcyclohexane. Objective: To examine the techniques of fractional distillation and gas chromatography while determining the fraction of cyclohexane and methylcyclohexane in each series. Reaction Table: Compound: Molecular Weight (g/mol) Boiling Point (˚C) Vapor Pressure at 20˚C Density (mg/µL) Cyclohexane 84.16 80.74 77 mmHg 0.779 Methylcyclohexane 98.19 100.9 37 mmHg 0.769 Reagent Table: Starting Material: Amount Added: Cyclohexane 1.5 mL Methylcyclohexane 1.5 mL Procedure and Observations: Procedure: 1. 1.5 mL of cyclohexane and 1.5 mL of methylcyclohexane were transferred into a 5 mL conical vial using delivery pipettes. 2. The Hickman still was attached to a conical vial, an air condenser was then attached to the Hickman still, a conical device was then inserted into the pie-block, a thermometer was then inserted into the pie block. 3. The blue-liquid bulb was then leveled with the lower lip of the collection ledge. 4. The heating knob was turned to 7, this setting allowed the device to heat at 100°C. 5. A strip of aluminum foil was folded around the conical vial – from the red pie plate to the Hickman still. Observations: Pipette was pumped two times to obtain 1.5 mL of samples. Thermometer was inserted into apparatus so that top blue-liquid bulb was level with lower lip of collection ledge (able to measure vapor temperature maximally) Handout was given to determine which setting yielded 100˚C for that hot plate Small amount of clear liquid was obtained; air bubbles were present when withdrawing using pipette; took between 5-10 minutes to collect distillate
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6. 5 Dram vials were then labeled and capped with teflon caps. 7. Fractions were then collected over the following temperature ranges: Fraction 1- below 75°C Fraction 2 – 75-80°C Fraction 3 – above 80°C Fraction 4 – 85-90°C 8. Leftover mixtures were considered as fraction 5, none was obtained. 9. The fractions were removed from the air condenser using a pipette. 10. Fractions were placed into individually labeled vials, and then capped with a teflon-lined cap. Analysis of Gas:
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Organic Chemistry Lab 4 - October 17th 2007 Craig Nutter...

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