Analysis of 1-Bromobutane

Reference: Williamson,  Macroscale and Microscale Organic experiments, 4th ed., Houghton Mifflin, pp.263-265.

Reaction Work-Up:
Wash the distillate from the simple distillation with water until the pH of the aqueous layer is greater than 6 and dry the organic layer with anhydrous CaCl2.

Sample Preparation:
Dilute 1 drop of the reaction product with 1.5 mL of GC/MS grade CH2Cl2.

GC/MS Analysis:
1. Start the ChemStation software. (desktop icon US21843137)
2. Method-Load-BuBrW04_2 .
3. Method-Run
4. Give the sample name. (207-01-lastname)
5. Run method. (Follow the directions in the dialogue box.)
6. Push PREPRUN. Wait until the steady yellow light.
7. Inject 1 mL (back inlet).
8. Push START button. "Override solvent delay?" NO.
9. When the run is complete, print area percent report.
10. Open DataAnalysis.
11. File-Load Data File.
12. Right double-click the second peak to obtain the mass spectrum of n-bromobutane.
13. Print TLC, Signals and Spectrum. (Close the middle window.)
14. Repeat the steps 3-13 with a new sample.
15. Close ChemStation and turn off the monitor.