General Chemistry: Questions Regarding Various Procedures

iodide · Tue Jun 21, 2005 9:34 am

While much is written about the various means of performing reactions, you know, write-ups on aminations, reductions, isomerization (and the list goes on), all seem to require a basic knowledge and familiarity with the various reaction procedures.

Looking to a book like Zubrick's provides know-how on the procedures themselves but fails to describe and warn of side-characeristics. That being said, SWIM wanted to ask the following:

1. When distilling something with an odor (say sassafrass or methylamine), is there going to be a guaranteed odor that permeates? Even in a vacuum distillation? If so, how is this reduced?

2. What are the practical dangers of distilling various solvents? Dichloromethane? Toluene? Ethanol? Is there a real threat of explosions and/or poisoning? How can the smell and/or danger be reduced?

3. When refluxing similar liquids, is there also a inevitable odor? How do you reduce the smell of such a reflux when performing one without vaccum?

Perhaps it can be better explained in the context of reactions most are familiar with:

1. Isomerization of Safrole: will the whole house stink up? Is there no way to reduce or eliminate smell?

2. Peracetic Acid Route to produce Glycol: Will SWIM be forced to smell vinegar for hours?

3. Hydrolysis with HCL or H2SO4: is the reflux of this going to poison SWIM? Can the smell/danger be reduced? Perhaps with a vacuum tube on the top side of the condenser?

4. Al/Hg Reduction: Will Mercury vapors be everywhere? Will methylamine stink up the entire house?

5. MDMA Ingestion: will euphoria be produced? Will there be empathy everywhere? Wait, SWIM knows the answer to this one. Smile

PolyAlchemia · Tue Jun 21, 2005 10:00 am

The worse permiating smells one is going to encounter are the solvent vapors. Common non-polar solvents one is apt to select for extracting like xylene smells to end all, and the more spills and dirty containers are sterwn about the workin area the more smell there will be. And this stuff does go through walls and travels upwards. Sassafras smells pleasant and there isnt to much reliese of vapors.

Look, some of this stuff smells, some of it is poisonious. An absolutly needed part of any lab, official or clandestine is a fume/ventialtion source. Consider working near a window and putting a large fan blowing out. Just as long as there is some air being sucked in from the rest of the house and negative pressure is maintained in the room the smells will not permiate the house. One could get away without ventilation for a certain things but its highly advisable for obvious reasons whenever workin with volitile solvents or potentially hazardious vapors. Methylamine gas for instantce. Gassing with HCl is probably about the most critical procedure that is in need of massive ventialtion.

Al.Hg has not much smell what-so-ever accept a some from the methanol. The reaction flask itself will waft of ammonia like fishy odor but its not to pungent nor will it stink up a room (a friend once did this in a hotel room bathroom hehehe).

For the Al.Hg as well as refluxing consider attaching a length of rubber hose from the top of the condenser and running this out side. And its a highly advisable thing to have a tube attached to the Al.Hg anyways for protection from the volcano effect that tends to occure from time to time from over running the addition.

On distilling solvents, yes, very smelly. The colder your condenser and recieving flask be better but ventilation is a must. Not much explosion risk but care should be taken always and in all ways.

So basically you are going to need window with a fan, no buts.