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S. Toppholzer
April 3rd, 2002, 03:11 PM
I have searched the Forum and unfortunately, I didn't dig up the information needed.
I bought quite some amount of pure (Merck) acetyl salicylic acid (sp?) and a bottle of pure (98%) H2SO4, also some saltpeter, technical grade. I've got all the glassware for preparing PA right away and that's what I did.
I have been trying mostly a method I found somewhere in the Forum Archives of a ratio like 10 mg Ac.acid, 37,5 ml H2SO4 and 19 g Saltpeter. Everytime I tried that recipie, I felt that this suggests far too much Saltpeter. It always seemed the nitration is finished with, say approx. 10 grams. The more I added Saltpeter the more imurities (aka "the red stuff") I got in my PA.
I tried a ratio of 20:50:15 (see above) and the result seemed much better. After nitration I poured the liquid into twice the amount of water which wasn't cooled. I instantly got a thermic reaction (didn't measure temp, though) so I decided to let the stuff sit a bit further away from me (as far as I know PA is safe up to about 120°C). After some 30 minutes, a huge amount of impurities has settled at the top of the beaker and became crusty. Below the yellow crystals of PA.
Maybe this would be a method of a one-step purification?
I tried to purify PA with mega's method by using boiling water. The impurities settled not at the top as described by mega but at the bottom of the beaker. This method leaves me still with a considerable amount of impurities. I tried using the hot alcohol method, but that was a complete loss. I dissolved the PA crystals in as much of hot alcohol as needed. But every time I try to re-crystallize the PA out of the alcohol solution I get more or less a zero return. No matter if I use hot or cold water, no matter if I use just a bit of water or more than the double amount - nada.
Anyone got an idea what I am doing wrong??

nbk2000
April 3rd, 2002, 04:10 PM
Besides posting a new topic as your first post? :mad:

Transferring to an existing topic about TNP in the "High Explosives" section, where this question belongs.

Since it wasn't totally lame, I won't ban you, but this is your first and last warning.