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megalomania
June 21st, 2003, 11:20 AM
sadsakjoel
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Registered: OCT 2000
posted 01-19-2001 09:10 PM
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I crushed 40 aspirin, added 2 teaspoons of water and 200ml of alcohol, filtered and evaporated it now I've got what i assume to be acetylsalicylic acid and I have to add it to sulfuric acid. Should this stuff smell like vinegar? When I boil the sulfuric acid to purify it and it fumes is it pure enough or do I have to reduce It's volume to 1/3 of its original volume and wait for the fumes to get thicker? I was purifying some acid and I kept going untill the fumes got thicker and I left it to cool down and they dissapeared! Do I have to store the acid in an airtight container? Thanks for any help

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MacCleod
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posted 01-20-2001 12:35 AM
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Dude,the fumes should disappear when it cools;it's simply vaporized acid caused by the acid being heated.You will get some fumes during the entire concentration process,but the fumes will double in volume when complete.Are you using battery acid or drain cleaner?.Also,you should store it airtight,otherwise it will slowly draw moisture from the air and become diluted again.
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Smartguy
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Posts: 11
From:
Registered: JAN 2001
posted 01-20-2001 10:44 AM
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quote:
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Originally posted by sadsakjoel:
...now I've got what i assume to be acetylsalicylic acid..... Should this stuff smell like vinegar?

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The stuff smells like vinegar, that's correct. That's because acetylsalicylic acid is actually salicylic acid with an acetyl group attached to it. When it decays, the acetyl group will form.....yup.....acetic acid! Hence the smell.



Microtek
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From:
Registered: JAN 2001
posted 01-20-2001 01:30 PM
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what does your acetylsalicylic acid look like ? Is it an actual powder, or is it a sticky mass like caramel ?


Anthony
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Posts: 2383
From: England
Registered: SEP 2000
posted 01-20-2001 02:29 PM
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Tis a load of crystals.


SafetyLast
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Posts: 235
From: the cretaceous period
Registered: OCT 2000
posted 01-20-2001 08:55 PM
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What alcohol should be used?
I think I remember KIPE saying methanol.
would denatured work?


sadsakjoel
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Posts: 170
From:
Registered: OCT 2000
posted 01-21-2001 05:35 AM
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thanks for the help, my crystals look like ap thats stuck together, I spose It's sort of like caramel. The acid I used came in a 2.5 liter bottle and was 'proper' technical grade sulfuric labelled sulphuric acid- H2SO4= 98% It's got some other specs on it aswell some molecular weight or something. I didn't think it was pure (even though it said it was- ie. found it at school, could be any percentage) because it didn't fume. So I can use this straight out the bottle? Come to think of it the bottle might not have even been opened when I 'found it'. I used methanol (wood alcohol) but I don't think it should matter, It's just to absorb the acetylsalicylic acid and then it recrystalises when evaporated, so If any other alcohol might be available, test it to see if it works, just try it in small amounts- ie, 10 tablets, 30 ml alc.
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All there is to fear is your own co-ordination



Anthony
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Posts: 2383
From: England
Registered: SEP 2000
posted 01-21-2001 11:43 AM
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I have used methlyated spirits (methanol/ethanol) without problems, like joel said it's just a means of seperating the acetylsalicylic acid. Although, I believe it isn't strictly neccessary, simply adding the powdered aspirin to the nitrating mix works. Any impurities from the aspirin would be inert so shouldn't give any problems.


sadsakjoel
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Posts: 170
From:
Registered: OCT 2000
posted 01-23-2001 09:25 PM
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Now I have added it to the sulfuric acid and it turned orange. I then put it in a hot water bath for 15 mins and took it out and stirred it for a while, waiting for it to turn black. After 1/2 hour it still hadn't changed colour. So I used my electric stirrer for 3 hours and still no change. Should I have stirred it then left it or continued to stir it like I did? I figured it wasn't going to change much so I added 6 teaspoons of Potassium nitrate with vigourous stirring in 6 eqaul ammounts. It was then that the solution turned black as did the table underneath it when it overflowed! fuck it made a mess! I let the shit cool to room temperature with occasional stirring and It was sort of green (not really a darker than yellow-orange!) After adding it to Ice and water and choking on that deadly red gas I filtered the solution. The big pile of picric acid is a faded fluro yellow colour. Now it is drying. I will store it wet and plasticise some of it and tell what happens later.
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Anthony
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Posts: 2383
From: England
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posted 01-24-2001 01:34 PM
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I don't recall it being supposed to go black at any point! If it less still letting of NO2 when you poured it into the ice water, I'd say that it hadn't finished reacting yet.


sadsakjoel
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Posts: 170
From:
Registered: OCT 2000
posted 01-24-2001 08:08 PM
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I used the method with 20 tabs and double everything, like what NBK did. It came from a huge thread on picric acid. I cant find the link and I did a search but it was inactive.


sadsakjoel
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Posts: 170
From:
Registered: OCT 2000
posted 01-25-2001 02:26 AM
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If my picric acid is completly dissolved in water and I want to get it out do I just evaporate the water off it or must I recrystalise it in ice, I tried the second and it didn't work. Also, Sulphuric acid- The label also said 1.8g/ml. I know that is the weight for 98% sulphuric acid (thanks to MacCleod) so if I measure out 100ml and it weighs 184 grams, I know that it's 98% pure right?
Please help with the water problem, anthony, anyone?

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Detonator
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From:
Registered: NOV 2000
posted 01-25-2001 02:56 AM
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You need to evaborate the water to get the PA back from the water...thats all.



Anthony
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Posts: 2383
From: England
Registered: SEP 2000
posted 01-25-2001 08:01 AM
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I don't think PA is soluble in water, are you talking about when you pour it into the ice water? Because that's supposed to precipitate the PA.
Evaporating the water should get it back anyway.





Anthony
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Posts: 2383
From: England
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posted 01-25-2001 01:51 PM
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Gotcha, that'd be why you use ice water to precipitate the PA.


Anthony
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From: England
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posted 01-25-2001 06:28 PM
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So when you pour the solution into the ice water, the yellow crystals that precipitate out are not PA?!


Anthony
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Posts: 2383
From: England
Registered: SEP 2000
posted 01-26-2001 07:17 AM
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Ah, I see, I was confusing the precipitation and purifications steps. Thanks.


wantsomfet
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Posts: 239
From: EU
Registered: JAN 2001
posted 01-26-2001 02:37 PM
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Just for informational purposes:
1 part Picric Acid dissolves in 90 parts water at 20 degree
1 part Picric acid dissolves in 30 parts boiling water
1 part Picric Acid dissolves in 44 parts ether
1 part Picric Acid dissolves in 9 parts ethanol
http://members.pgonline.com/~bryand/dyes/10305.htm
http://www.omikron-online.de/cyberchem/cheminfo/0484-lex.htm
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PHILOU Zrealone
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From: Brussels,Belgium,Europe
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posted 01-30-2001 10:58 AM
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Letting some acid in the water will help the PA to cristallise/precipitate out when cooling since:
H-O-C6H2(NO2)3<===> H(+) + O-C6H2(NO2)3 (-)
The protonate form is unsoluble in water while the deprotonate form is; adding a little acid will displace the equilibrium to the left side of the reaction...
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Mr Cool
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posted 01-30-2001 02:34 PM
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HCl would probably be good since it won't leave any residue in your product.
When the non-ionised form dissolves in water, it forms the ionised form (with the H+ ions etc.), so saying the non-ionised form is insoluable in water is a bit misleading because it does dissolve, but when it does it forms the other. I can see what you mean though.



PHILOU Zrealone
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Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 02-02-2001 08:26 AM
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You are right, all products are soluble everything is a question of how much; so the the correct answer I should have given is that the protonated form is much less soluble than the unprotonated form!
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"Life that deadly disease sexually transmitted".
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mongo blongo
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From: I live in a Creosote Bush!
Registered: JUN 2001
posted 07-09-2001 02:44 PM
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From the asprin method ive noticed that when people extract acetylsalicylic acid from the tablets, they leave the solvent to evapourate. This takes some time and can be a pain in the ass!!
I use methlyated spirits. After filtering the acetylsalicylic acid off i just pour it into a beaker of cold water and the acetylsalicylic acid is rapidly precibitated. Then it can just be filtered.
It is much quicker and it is not too much hassle (well for me anyways).


Lagen
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From:
Registered: MAY 2001
posted 07-14-2001 12:21 PM
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Microtek & others: If your acetylsalicylic acid looks like a pasty mass, then it is partially decomposed because of overheating. Using a boiling water bath will prevent this. This will actually speed up the evaporation a bit as it will distribute the heat evenly. Otherwise keep it below its m.p. which is 135-140°C.


simply RED
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Posts: 242
From: HELL
Registered: OCT 2000
posted 07-14-2001 05:56 PM
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I tried the method with aspirin and it always gived very low yield...


rijke_stinkerd
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Posts: 3
From: oregan
Registered: JUL 2001
posted 07-18-2001 10:50 AM
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Yesterday I dreamt of an experiment.
I crushed up 50 tablets of asprin.
Next of I extracted the acid whit the purple household alcohol, and boiled it to evaporte the alcohol. Then when I wasn't looking it dried and some of the acid melted. Then I added 350ml of 98% sulphuric acid and it desolved al the acid, next I added 38 grams of potasiumnitraat in portions of 4grams at a time.I waited till the fumes dissapeared and till the mix had cooled to room temp. Then I added it to 1,5litres of icewater but no crystles precipetated. Who has any idear what happened.


Lagen
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Posts: 178
From:
Registered: MAY 2001
posted 07-18-2001 04:32 PM
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First off, use a water bath! See in the previous post of mine... If I were you I wouldn't be nitrating the degraded acid. Secondly, I suspect all your PA dissolved in the water. If you're from Europe then your aspirin tablets contained about 25g acetylsalicylic acid, before the decomposition. The water could dissolve about 15g PA, the yield might well be as low as that...


rijke_stinkerd
New Member
Posts: 3
From: oregan
Registered: JUL 2001
posted 07-19-2001 02:57 AM
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Wel I used 500mg tablets. But what I think what happened was what you said that by melting the acid it degrated to much to be nitrated correctly.


rijke_stinkerd
New Member
Posts: 3
From: oregan
Registered: JUL 2001
posted 07-19-2001 03:22 AM
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I was thinking of something yesterday when al the no2 escaped in my dream. If you were to lead this true cold water it will form a mix of hno2 and hno3 witch could be seperated and then you'l be left with nitric acid wich can than be concentrated. Or is this a realy bad idear. sorry for my englisch guys i'm from europe.No not england


Lagen
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Posts: 178
From:
Registered: MAY 2001
posted 07-20-2001 09:09 PM
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I wouldn't be messing with this, unless you have really good equipment, since the NOx gases are very corrosive to the lungs and toxic. I have no idea on the composition of the resultant acid mix, or how the HNO3 could be extracted. Better to make the nitrogen oxides by oxidation of ammonia, IMHO.