I took 200ml of battery acid and boiled it down to about 1/2 its original volume. then i measured out 70ml and started heating it. then added 10 powdered asprins. after stirring and disolving most of the asprin i added 2 grams of KNO3, red fumes were produced. after the reaction subsided i repeated the addition of the KNO3 until my 9 grams of KNO3 was gone. i shut off the heat and let the dark-orange liquid cool. after that i added 150ml of cool water, a small amout of dark orange-brown crystals formed. it was kinda hot so i put it in a big ice bath. after it cooled down pretty good some more crystals precipitated. i filtered the very small amount of crystals out, and now their drying in my basement.

i have a couple questions:

1. are the crystals picric acid?
2. why are their so little of these extremely small crystals
3. did i do anything wrong? f yes what?

You didn't use alchol to wash the aspirin to remove the fillers and binders. This gets oxidized too, taking away from the phenol.

Next, too much acid in relation to the aspirin, you're carbonizing it.

Was the aspirin/acid mix heated and allowed to react for 15 minutes before cooling? NO. This means the acetylsaliyic acid wasn't given time to be converted into phenol.

You added the water to the acid. THAT'S A NO-NO! NEVER add water to acid, always add the acid to water. Otherwise you risk splash back.

Did you pour the mix into crushed ice slush? NO. This means that a lot of the picric acid was dissolved in the water, since it is water soluble.

Water must be ice cold, and immediately filter through a fine filter (coffee).

When I did it (followed BB#1 procedure) I got about a quater to half ounce from 40 tablets. Didn't have a scale at the time so I'm estimating the weight.

Also, the crystals should be BRIGHT yellow. Like a canary. Dark brown means it's dirty and should be disposed of.

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"I have begun evil, I shall end evil. That is the end that awaits me."

i will have to try this again...

BTW, codemason, i got a quick question for you. i know this is off topic but im afraid to post a topic on it.
How is KNO2 synthisised from KNO3?

i want to know this so i can give r-salt an atempt

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"True freedome is not without anarchy"

quote:

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BTW, codemason, i got a quick question for you.

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"I have begun evil, I shall end evil. That is the end that awaits me."

This takes a bright red heat, like from a propane torch.

If you were to do it in a test tube, you could connect a stopper with a piece of tubing that you could pass into water to see when it stops bubbling. That would show when the reaction was done.

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"I have begun evil, I shall end evil. That is the end that awaits me."

Aluminum, copper, lead, zinc, iron, etc.

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"I have begun evil, I shall end evil. That is the end that awaits me."

I would think that the point in using lead is that at roughly 350°C both of the reactants are in liquid phase thus able to react easily, and still stable, so the reaction would be well defined. With zinc or any higher melting metal the nitrate would start decomposing at 400°C with the metal being still solid (and the product as well). Now does anybody know what are the byproducts of thermal decomposition of KNO3? Nitrite decomposes at 500 something. With lead there are still side reactions leading to plumbite etc. but the impurities are relatively easy to separate. The impure nitrite usually doesnt work for DDNP, R-Salt, NM and the like... Just my 0.02$, anyway.

This is a bit OT, but I am a bit confused. I remember posting something on making nitrite in the "sodium nitrite" thread, now its 404, not found in the archives, and I cant find the overflow site, have I missed something here? (Edit: SNIP and posting in Forum Matters)

the decomposition byproduct for kno3 would be O2, am i right? but if you heat it with lead it would be PbO, am i right?

these should be the reactions:

with lead

KNO3 + Pb --> KNO2 + PbO

without lead

2KNO3 --> 2KNO2 + O2

are these correct?

Edit: Of course a lot of KNO2 and O2 is formed as well (not a BYproduct...)

i had another dream like the one that i posted before, i think this is a re-acurring dream.

here is what happened in it:

i crushed up 10 asprins and disolved them in 70ml of H2SO4 drain opener. then i gently heated the mix to help disolve the asprin. after it was all disolved i added 9 grams of KNO3 in sevaral parts. there was no NOx fumes. but the solution turned bright red. after letting it react for a couple minnutes i poured it into a beaker full of cracked ice-water. it turrned yellow and there was some precipitate in it. i filtered out the yellow-gold crystals and put them on a table in my lab. there was a good amount of crystals in this dream (unlike the last one i had)

this is indeed a very strange dream because i would never do anything dangerous like make explosives. or work with an acid

[ January 12, 2002: Message edited by: Madog555 ]