posted November 23, 1999 03:44 PM            

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-dlwdaw

"... always look on the positive side of things, blow things up not down"

-- Ragnar Benson

posted November 24, 1999 12:54 AM            

------------------
-dlwdaw

"... always look on the positive side of things, blow things up not down"

-- Ragnar Benson

posted November 24, 1999 10:53 PM            

------------------
-dlwdaw

"... always look on the positive side of things, blow things up not down"

-- Ragnar Benson

posted November 29, 1999 06:57 PM            

What the difference between a dedicated distilation column and a Liebig condenser? The distillation column has 3 small spikes on the inside to hold packing inside (glass beads or copper sponges). Other than that, they are identical, they are just used differently. A distillation column is a Liebig condenser when its horizontal, a Liebig can be a distillation column (even without the spikes) when it's vertical.
The price? From the overly expensive Fisher Scientific catalog:
Liebig condenser Pyrex brand, 300 mm jacket, $85.85
Liebig condenser as distilling column, Kimax brand, 300 mm jacket $70.00
Snyder type column Kontes brand, anywhere from $40.50 for the basic to $113 for the big boy
Vigreux column, 75mm, $34.80

All of these have standard taper ground glass joints, and of course a Vigreux or Snyder is completly unnecessary. I believe Chemglass probably has 300 mm colums for as little as $30 each also with standard taper joints. Then you can get some glass beads (pricy at $20-100 a pound!) or stuff a copper sponge from the grocery store (strange but that's what every lab seems to use, hey it works and its cheap).

I suppose you bought a very large column, maybe it has some nifty stuff like the collection flasks. Still, if not, you got, as the commercial says, "e-screwed"

For the more adventerous, I have the info to synthesize nitromethane at my website in the synthesis section, I believe. Also, try out that Pyrotech Supplier at http://jump.to.pyrotech they sell 100% nitromethane for a very reasonable price.

While distilling, nitromethane boils at 101 °C and methyl alcohol boils at 64.7 °C, so you will get methyl alcohol first. The temperature should be adjusted so that you get 2-3 drops of liquid per second. You will not be able to take a temp reading of the mixture (unless you have a special multi necked flask) but you will read the temp at the top of the column. It should read near 64-65 as pretty pure methyl alcohol should be coming out. Do not crank up the heat as you will disturb the temp of the plates within the column (the areas within a column where evaporation and condensation are occuring are called theoritical plates, these are not real plates). You must also wrap the column in insulation and protect it from drafts of air. Temperature flucuations can throw off the function of the column. You can use fiberglass or cotton wadding as insulation then wrap aluminum foil around it to keep the insulation on the column.

posted November 30, 1999 08:50 PM            

The Hell-Volhard-Zelinsky Reaction is indeed the right one. I have searched through a pile of synth tomes to no avail, no detials that is, just vague theoritical allusions. Basically you bubble chlorine gas into acetic acid while swirling around some phosphorus or sulfur. The reaction will make di- and trichloroacetic acid as well, eventually leading to nearly 100% trichloroacetic. I have no idea when to stop the reaction, how to seperate the products, and if the phosphorus is just mixed in as a powder. Phosphorus is the normal way, I found a reference that said you could use sulfur which is alot easier to obtian. All this seems simple enough now that I think of it...I would prefer to have the synth spelled out in detial though.

Heh, you pathetic little druggie

posted November 30, 1999 10:40 PM            

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-dlwdaw

"... always look on the positive side of things, blow things up not down"

-- Ragnar Benson