Below are some tips that will make vacuum distillations go smoothly.
Always use Dow-Corning High Vacuum Grease or it's equivalent on glass joints. Use sparingly and keep glass joints clean.
Use Teflon (PTFE) boiling chips. They typically come in 1 lb. Cans. Use liberally, add fresh boiling stones each time the vacuum is broken or the liquid cools down.
Wait until the vacuum is stabilized before applying heat, then use the minimum heat required.
Maintain a 30°C temperature differential between the water flowing through the condenser and the condensate. The condensation line in the condenser should be between ½ and 2/3 the way down the condenser.
Don't fill the distillation vessel more than halfway full. You can cheat a little bit on this one. Another don't is "bumping"; this is easily recognizable and if it starts, stop the distillation immediately. Some heavier compounds like P2P and benzaldehyde are naturally "bumpy", so one has to exercise some judgement.
Don't get in hurry when doing large volume distillations; the condenser throughput rate is fixed and adding more heat won't speed things up but will send some of one's distillate into the vacuum system.
7.4 Reference Material
The following books are essential to any clandestine lab.
Merck Index
This handy volume provides one with all the essential data on most compounds, including molecular weight, density, boiling and freezing points, common usages, and references pointing to manufacturing techniques.
Uncle Fester's Secrets of Methamphetamine Manufacture, 3rd and 4th ed., Loompanics.
These comprehensive books provide the references and good pointers for those reading between the lines. In reading these books, one should bear in mind that if one is a little too accurate in his technical descriptions, one could find one's ass in a prison sling. Hooray for Cypherpunks!
A Chemical Technicians Reference Handbook.
This is a valuable reference for solvent characteristics and lab procedures.
A college level Organic Chemistry textbook for a reference to common reaction mechanisms.