posted 01-19-2000 09:07 PM         

mycrof: Listen to me. Ignore everything else. Now lets start at the point that you open the freezer and see "mad crystals". Your flask mostly contains:
1. Water
2. Ammonium Chloride
3. Methylamine Hydrochloride

Your flask may also contain small amounts of:
4. Hexamine
5. Dimethylamine
6. Assorted garbage in small amounts including Formic Acid or its salts and perhaps even some amount of formaldehyde

Put the Acetone away. You don't need it.

Remember these rules:
1. Water dissolves both Ammonium Chloride and Methylamine Hydrochloride, but dissolves the later preferentially. Hot water dissolves more of either than cold water.
2. Alcohol, especially when hot, dissolves a good amount of Mehtylamine Hydrochloride but barely any Ammonium Chloride. Yeah the Merck says that Ammonium Chloride is soluable in alcohol but test it for yourself.
3. Chloroform dissolves dimethyamine and, to a lesser extent hexamine (but doesnt dissolve hexamine as well as water does)

Thats about all you need to know.

The hot water was able to hold both ammonium chloride and methylamine.hcl

By applying rule #1, we know that the "mad crystals" are Ammonium Chloride that has fallen out of the water as the temp dropped. Filter these crystals out of solution and put them in a glass jar. Seal it up for now.

Now you are left with a liquid. Maybe it is slightly yellow. Hopefully it is not dark yellow or orange. This liquid still contains both ammonium chloride and methylamine.hcl.

So now you basically have two choices.

One choice is that you can do multiple rounds of distilling some liquid, cooling, filtering, and repeating until you notice that the crystals that you are filtering look like methylamine.hcl instead of ammonium chloride. Using this technique you are basically looking for the point where the water has dropped all of its ammonium chloride and is now dropping only methylamine.hcl. Evaporate more of the water until crystals are apparant even when it is hot, it will solidify upon cooling into a mushy mass of mostly methylamine.hcl

Another choice would be to just evaporate all the liquid until it gets really thick with white/beige crystals. Cooling at this point should leave a solid mass that is a mixture of mostly ammomium chloride and methylamine.hcl

So either way you end up with a mass of stuff, one way takes more work, but your stuff is more pure at this point.

Well, you probably want it to be more pure than it is at this point anyhow so you're gonna do some washes. That being the case I have to recommend going the second route because I would rather spend more time doing washes than more time doing distillation. You may have different priorities and thats OK too.

Anyway...

Put your crystals in a jar. Add chloroform, Mix it around. Shake it up. Let it sit for a while.

Pour the chloroform off into another container and collect your crystals. Put them back in a sealed jar.

Go to WallyWorld. Head to the paint section and get yourself a gallon of S-L-X Denatured Alcohol. Now go over to the kitchen section and get a pair of mongo 2-litre Pyrex measuring cups.

Add your crystaline mass to one of the mongo measuring cups. If it would be more than half full then you're gonna wanna split it up into separate batches.

Set the second measuring cup next to the first one for a visual aid. Pour enough alcohol into the second measuring cup so that it looks like it would more than cover all the crystals in the second cup. Try to err on the side of too much alcohol rather than not enough.

Boil the alcohol in the microwave. Keep an eye on it even though it may take a while. You are cooking flammible liquid so its not a good idea to walk away.

Once it begins to boil, remove it from the microwave and pour the contents into the measuring cup that contains the crystal mass.

Stir Well for about a minute, maybe more but not so long that it cools down very much.

Let settle while you pour a similar amount of alcohol into the first measuring cup again and put it in the microwave to heat it up. Do this quickly because you really dont want the hot alcohol in the 2nd measuring cup to cool down.

You will notice some of the crystal mass has dissolved into the alcohol and some of it has not. Ammonium Chloride doesn't dissolve nearly as well as methylamine.hcl.

While it is still warm, pour the alcohol off into another container. You wont be able to pour ALL of the alcohol into this other container because you are being careful to not pour the solids into this container.

Now you have one measuring cup boiling in the microwave. One measuring cup with a little bit of alcohol and some white crystals. And one container of alcohol with a good deal of methylamine.hcl dissolved in it.

Take the measuring cup of alcohol out of the microwave when its boiling and repeat the process of adding it to the measuring cup with the crystals in it and stirring it for a bit.

Not as many of the crytals dissolved this time and most of what you see undissolved is ammonium chloride. Pour this alcohol into the same container as the first.

So now you are almost done.

If you have good ventillation and don't mind wasting a few dollars, you can just boil the alcohol away into the atmostphere and be left with methylamine.hcl. A Crock-Pot works nice for this because you can basically leave it unattented without worry that it will get too hot. The downside is that it can take a long time. If you are impatient and don't mind going to a shopping mall then you can go to the kitchen section of a department store and find a glass pot that is safe for the stovetop. The brand name is Visions by Corning.