Lab Techniques

1
Lab Techniques
2
Safety

• Flammability
• Toxicity
• Corrosion
• Explosion
• Gas cylinders
• Drying oven dos and donts
• There will be a safety quiz!

3
Information retrieval

• Aldrich Library of 13C and 1H FT NMR Spectra
  Ref. QC 462.85.A44
• Sadtler Standard Spectra Ref. QC 459.S25
• Internet
• Good source for sample NMR and IR spectra
   http//www.aist.go.jp/RIODB/SDBS/cgi-bin/cre_inde
  x.cgi
• Two nice review sites for organic chemistry 
  http//www.cem.msu.edu/reusch/VirtualText/intro1.
  htm, also http//www.chem.uic.edu/web1/OCOL-II/WIN
  /HOME.HTM
• A thorough discussion of IUPAC nomenclature
   http//www.acdlabs.com/iupac/nomenclature/
• Listing of name reactions  http//www.monomerchem
  .com/display4.html

4
Separations based on distillation

• Microstills
• Fractionation columns (e.g. Vigreux)
• Vacuum dist. techniques, pitfalls
• Steam distillation, Dean-Stark traps
• Rotary evaporation

5
Chromatography in synthesis

• TLC
• Column
• GC
• HPLC
• Continuous reaction monitoring

6
Other separation techniques

• Extraction (Soxhlet, liquid-liquid, etc.)
• Sublimation
• Chemical derivatization
• Deferring separation to next synthetic step

7
Solids separation

• Vacuum filtration tricks - avoiding clogging
• adsorbents (Celite), heating/aging, drying
• Liquid-liquid-solid mixture issues
• Centrifugation

8
Inert atmosphere work

• Purge gas lines
• Schlenk lines
• Gove Boxes

9
Temperature control

• Cryogenics
• Dry ice-acetone
• Liquid nitrogen
• Heat
• Thermostated oil baths
• Metal baths

10
Special methods

• Flash vacuum pyrolysis
• Microwaves
• Autoclaves
• Ozonization
• Ultrasonication
• Catalytic hydrogenation
• Microchannel reactors

11
Our tour

• NMR
• GC
• Scifinder
• Autoclaves, hydrogenation
• Lab purge gas, drying oven