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knowledgehungry
June 23rd, 2003, 09:25 PM
50 ml of acetone was added to 300 ml of 3%h2o2 and cooled to 2 degrees celcius. 20 ml of h2so4 was then added to the solution the solution was allowed to sit after 2 hours black crystals precipitated from the solution will give pics as soon as my friend takes them.

Does anyone have any idea what the fuck happened? Chemicals were same as used for previous reactions that resulted in normal AP, only thing is that the reactions occured in an empty vodka bottle. I'm very confused by this.

Nihilist
June 23rd, 2003, 10:08 PM
maybe the alcohol residue had some kind of effect on the reaction? this is just a thought and I have no idea why the fuck the crystals would turn black because of this.

Arthis
June 24th, 2003, 07:22 AM
Are you sure you didn't add the acid too fast ? Because local overheating and ebullition cause brown stuff to appear (locally), I guess it be some king of fucked AP.

Maybe the ebullition would cause the destruction of a part of the molecule, thus giving its black color.

yt2095
June 24th, 2003, 07:36 AM
the only other time i`ve know blackening of anything was carbonisation of things like sugars as a result of conc H2SO4.
but if you did the proceedure in the way you stated and there was sugar in the vodka i still can`t see how it could possibly happen.
it would suggest perhaps a metal contaminant to me, Manganesse perhaps?
have you ever in the past made oxygen with manganese dioxide with your same batch of H2O2? maybe some got in perhaps?
see if you isolate one and take a peek at it under a microscope.
you didn`t mention wether you made any "normal" TATP in your batch.
other than that, it beats the sh!t outa me! :)

all the best :)

vulture
June 24th, 2003, 08:03 AM
Black shit in organic "synthesis" is almost always the result of destructive oxidation. Although acetone won't carbonize with H2SO4 and the conc of peroxide was quite low.

kingspaz
June 24th, 2003, 11:08 AM
did he use drainopener H2SO4 though? and did he not dilute it first like a wise person would?
did you use pure H2O2 and pure acetone. if not what were the ingredients on the bottles?

it maybe that some different conditions occured that resulted in contaminents reacting to a greater degree than normal. does it behave like AP?

yt2095
June 24th, 2003, 11:23 AM
Kingspaz,
True!, i assumed in my assesment that he did.
realisticly then, it COULD be any one of a kazillion different things.

it would be fair to say Knowledgehungry, that we really need alot more details :)
else it`ll just be "grab a number out a hat" time.

knowledgehungry
June 24th, 2003, 02:24 PM
The H2O2 was the standard OTC disinfectant(CVS brand) traces of phosphoric acid to stabilize. H2SO4 was liquid fire brand drain opener, and the Acetone was hardware store grade Acetone. All of the chemicals have been used before which is why SWIM is confused. Perhaps trace amonts of Vodka reacted with contaminints in the acid, but i honestly dont know. I'll post pics as soon as SWIM gets them and give results of explosive, solubility tests etc.

yt2095
June 24th, 2003, 02:44 PM
as a user of Technical or analytical grade chems, i couldn`t even begine to imagine what it is you`ve made there?
the Phosphoric is perfectly normal in H2O2 9it`s a stabiliser) and plays no significant part in the TATP reaction.
is it possible that there is OIL based products (specificly coal tar) as you mentioned it was a disinfectant?

other than that, as i posted previously....
it beats sh!t outa me :)

blindreeper
June 26th, 2003, 03:28 AM
IIRC, don't most drain cleaners have a dye in them? I am not fimiliar with liquid fire because I don't have it here but maybe it was black? I have heard reports of NG being coloured different because of the dye in the drain cleaner. My diggers HCl has something added that reacts with H2O2 to make an amber colour. Then the AP is orange but when fuilly neutralized it goes white so it's kinda good :D

scarletmanuka
June 26th, 2003, 04:48 AM
Blind reeper, are you saying that your AP worked allright even though it was orange? That would be very comforting , because I made a batch using Pool brand HCl and it also turned orange, I thought I stuffed it up so I threw it out.

DaveTheShit
June 26th, 2003, 07:32 AM
I have a bottle of liquid fire drain opener somewhere, and it's pretty clear, with a touch of yellow/brown color. Now, I've made AP with the black dyed acid before, and after a couple washings the black color was gone. I do not know what the hell happened to knowlegehungry's AP though, maybe some crap fell in when you weren't looking. I would be sure to take care with this batch, which I know you'll do, but just make sure to do.

fowkes.l
June 26th, 2003, 08:41 AM
I thought I would tell you what happened last week when I was making AP.
I combined all chemicals and stirred with metal spoon in glass jar, I left it for two nights (i used 3% hydrogen peroxide) in ice water. AP had successfully formed except it was a light green colour.

I thought about my process and worked out what I had done differently from other times. It was the metal spoon. I then made a new batch of AP, when I had filtered it I decided to experiment and see what the metal spoon would do to the AP, on contact it turned that greeny colour again. This AP was not washed so it was obviously the metal spoon reacting with the acid.
I usually wash my AP so don't worry.

Arthis
June 26th, 2003, 11:33 AM
It's pretty obvious, if you stir your chems with a metal spoon (steel), you have
2 H+ + Fe --> H2 + Fe2+

ah ! the greenish Fe2+ ion. Try with copper stirrer now to have blue AP ;)

blindreeper
June 26th, 2003, 08:19 PM
scarletmanuka, yes the Ap worked fine. Your reaction hasn't stuffed up at all. If you neutralise it with NaHCO3 it will turn nice snow white and the orange colour will be gone! It's kinda good because it's a sort of indicator, I don't know what though because my HCl is clear and fuming. The same thing happens when I make MEKP but the I notice no colour change as the MEKP is red to start with.

knowledgehungry
June 26th, 2003, 11:25 PM
My friend realized that the inside had a thin coating of something to make the bottle shine, he neglected to mention this when he told me about his procedure:mad: . So that ends that mystery, the film reacted with one or more of the chems present and gave the discoloration. My friend said the AP did detonate however.

scarletmanuka
June 27th, 2003, 06:49 AM
I was speaking to a brickie/chem teacher who said that the reason my reaction went orange was because the manufactured HCl has colourless Fe Salts are added for safety reasons. When different ions are added, this creates the orange solution.

blindreeper
June 27th, 2003, 09:19 AM
Well I don't want any nasty ass Fe compounds in my HCl. Good thing today in dulux paint store when my mum was getting paint for my room they sold 4L containers of 37% HCl for $15 I think thats a reasonable price.

xyz
July 4th, 2003, 04:57 AM
Try a pool shop blindreeper, I have got 5L of 37% HCl for $8AUD from a pool shop near me.

Bryan
July 7th, 2003, 04:44 AM
I got 5L of 35% for $5AUD

blindreeper
July 7th, 2003, 06:53 AM
Bryan I really don't see how that contributes to discussion. I mean you didn't say where and thats a big useless :rolleyes: But then again me posting this is not very useful so I may aswell say some thing. Would the 37% stuff be a bit OTT? Like would it sputter and stuff. Because using 30% stuff it tends to get pretty hot and just curious is it safe to use 37%? Well I could always dilute it but that takes effort :p

Efraim_barkbit
July 7th, 2003, 09:03 AM
I donīt think there will be much difference between 30% and 37%, it is not that much of a difference. I have never used HCl, (Iīm using battery acid)but I have used 62% nitric once, and it didnīt splatter or anything, just became a little warmer.

BTW, what exactly does OTT stand for? and IMO??

blindreeper
July 7th, 2003, 09:26 AM
IIRC - If I Remeber Correctly
WTF - What The Fuck
IMO In My Opinion
IMHO - In My Honest Opinion
SWIM - Someone Who Isn't Me
OTT - Over The Top
OTC - Over The Counter
BTW - By The Way
OT - Off Topic
CBF - Can't Be Fucked
LMAO - Laughing My Ass Off
HED - Hot Electrical Death

Thats all I can think of right now

Back to the HCl, 7% is a big difference. Like if you have 98% H2SO4 in a nitration if you don't have that 7% it won't work (well not nearly as good)

Arthis
July 7th, 2003, 12:16 PM
From 30% to 37% is a low difference. Maybe you should try to add your acid more slowly, anyway you shouldn't get any pb with HCl. Use pre-chilled acid.

blindreeper
July 7th, 2003, 08:11 PM
Indeed you are correct about prechilling, I have the acetone/H2O2 mix at -20 and the acid at -20 and there is no need for an ice bath if you add it slow enough :p