megalomania
May 24th, 2003, 02:30 PM
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-16-2001 06:49 PM
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i got bored making AP and seeing my supplies left is in small quantitity I just mixed them all with no ratio:
30 % H2O2 laboratory grade
acetone the one found in hardware shop
and 4 N HCL hmmm, 4 M HCL
all of them was about half glass full
anyway, I was suprised the batch is incredibly tiny, could it be caused by excessive acetone that most of the AP got dissloved?
I also suspect that the HCL might be to diluted that the water contain disturb/ imbalance the reaction
Well, any opinion is welcome
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 04-16-2001 07:11 PM
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I once tried to make AP with Acetone, 3% H2O2, and a blob of this stuff i found in my grandma's garage called naval jelly. It said 'contains phosphoric acid,' so i thought 'what the hell' and was only able to scrape a little blob out with a metal stick. It was really cold out, and I dont know if the stuff was even any good. The next morning, there was 2-3 extremely small (size of a .) little white flakes floating on it, i doubt they were even AP. That's what you call an incrediby small yield. I might also mention that this was in the middle of winter, so it was quite cold.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 04-18-2001 04:41 AM
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On a cristallisation point of view:
*little cristals forms when a fast precipitation occurs not allowing the equilibrium between cristals to happen.
*You should of course know that bigger cristals are favorised upon slow cristallisation or when a physical environment/or property of the chemical allows it!
Let me explain this:
Slow cristallisation and thus big cristals comes from a stable mother liquor beeing cooled slowly; then some cristaline germs (dust, irregularity in the glass, anything solid and pseudocristaline) begins to cover with cristals because of sursaturation of the mother liquor; cristals are growing on those cristals creating some little, medium and big monocristals. On the surface of those cristals there is an equilibrium between the mother liquor and the solid always moving and exchanging matter; then because little particles have a bigger specific surface, they tend to disappear while the bigger cristals are getting bigger and bigger. This can also occur with a volatile solid (sublimating) but then it is airborne and an equilibrium exist between the surface and the air surrounding the cristals when saturated (I have some wet AP in a closed plastic box at 25C and it happens all the time little cristals become bigger and bigger).
Now you can understand that little cristals occurs when:
*cooling is fast and goes fast under the sursaturated concentration (this goes down when T decrease) equilibrium is also slowed down!!!
*impure product containing a lot of dusts or critaline germs is used.
*solvent mix has a low solubilisation power of the precipitate (equilibrium is defavorised).
I HOPE IT HELPED
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-18-2001 02:35 PM
--------------------------------------------------------------------------------
so the basically equilibrium favor and supersaturated solution explain the flaw, eh?
I got the equilibrium thing, but I don't think the solution is supersaturated (considering the acetone excess and diluted HCL)
Right now i'm putting filter paper to absorb then evaporate the liquid day by day, I hope when the acetone/water evaporate, all left is the crystall on the filter paper and I might make some flash paper....
CragHack
Frequent Poster
Posts: 618
From:
Registered: DEC 2000
posted 04-19-2001 02:40 AM
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frostfire, how muchg of each chemical did you put in? how big was the glass? cause one could assume that you only used a little bit of H2O2 and alot of the acetone. thus having the H2O2 being the limiting factor. can you provide any more info?
------------------
"If you must, do it with intelligent people, at least they know how to talk to the cops."
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-19-2001 11:29 AM
--------------------------------------------------------------------------------
well like I said before, I just dump all remaining of my AP ingredients to a glass.
It's a common 2 oz ( I never use oz???) glass that's usually served in a fast food restaurant.And the glass is only half full
So it's not that much though
That's why I speculate that somehow the acetone is in excess and hence, turn H2O2 as the limiting reagent or redissolve the crystal once it's made. I'm in day 4 of evaporating the liquid little by little with afilter paper, In the end I'll examine lit the paper 'n we'll see how many AP is actually produced ( hope it works)
Dracul
Frequent Poster
Posts: 73
From: Melbourne, Australia
Registered: SEP 2000
posted 04-22-2001 11:07 PM
--------------------------------------------------------------------------------
If you think the acetone is in excess and that is has dissolved all the AP then when you are about to filter it add some water before you filter. If you dissolve some dry AP in acetone then add water all the AP will instantly precipitate out of the solution. Try it with some that you already have (if you have some that is) to see what I mean.
------------------
"By the power of Grayskull, I HAVE THE POWER!" He-man
Check this out www.stileproject.com
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-23-2001 01:56 PM
--------------------------------------------------------------------------------
now that's interesting.
Now trying....
ps: do you get this by from learning by doing or can you provide further details..?
Dracul
Frequent Poster
Posts: 73
From: Melbourne, Australia
Registered: SEP 2000
posted 04-24-2001 10:21 AM
--------------------------------------------------------------------------------
A bit of everything, I used to study chemistry. There were a few areas where things like that came in. It works with lots of other solutions too.
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-16-2001 06:49 PM
--------------------------------------------------------------------------------
i got bored making AP and seeing my supplies left is in small quantitity I just mixed them all with no ratio:
30 % H2O2 laboratory grade
acetone the one found in hardware shop
and 4 N HCL hmmm, 4 M HCL
all of them was about half glass full
anyway, I was suprised the batch is incredibly tiny, could it be caused by excessive acetone that most of the AP got dissloved?
I also suspect that the HCL might be to diluted that the water contain disturb/ imbalance the reaction
Well, any opinion is welcome
FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 04-16-2001 07:11 PM
--------------------------------------------------------------------------------
I once tried to make AP with Acetone, 3% H2O2, and a blob of this stuff i found in my grandma's garage called naval jelly. It said 'contains phosphoric acid,' so i thought 'what the hell' and was only able to scrape a little blob out with a metal stick. It was really cold out, and I dont know if the stuff was even any good. The next morning, there was 2-3 extremely small (size of a .) little white flakes floating on it, i doubt they were even AP. That's what you call an incrediby small yield. I might also mention that this was in the middle of winter, so it was quite cold.
PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 04-18-2001 04:41 AM
--------------------------------------------------------------------------------
On a cristallisation point of view:
*little cristals forms when a fast precipitation occurs not allowing the equilibrium between cristals to happen.
*You should of course know that bigger cristals are favorised upon slow cristallisation or when a physical environment/or property of the chemical allows it!
Let me explain this:
Slow cristallisation and thus big cristals comes from a stable mother liquor beeing cooled slowly; then some cristaline germs (dust, irregularity in the glass, anything solid and pseudocristaline) begins to cover with cristals because of sursaturation of the mother liquor; cristals are growing on those cristals creating some little, medium and big monocristals. On the surface of those cristals there is an equilibrium between the mother liquor and the solid always moving and exchanging matter; then because little particles have a bigger specific surface, they tend to disappear while the bigger cristals are getting bigger and bigger. This can also occur with a volatile solid (sublimating) but then it is airborne and an equilibrium exist between the surface and the air surrounding the cristals when saturated (I have some wet AP in a closed plastic box at 25C and it happens all the time little cristals become bigger and bigger).
Now you can understand that little cristals occurs when:
*cooling is fast and goes fast under the sursaturated concentration (this goes down when T decrease) equilibrium is also slowed down!!!
*impure product containing a lot of dusts or critaline germs is used.
*solvent mix has a low solubilisation power of the precipitate (equilibrium is defavorised).
I HOPE IT HELPED
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-18-2001 02:35 PM
--------------------------------------------------------------------------------
so the basically equilibrium favor and supersaturated solution explain the flaw, eh?
I got the equilibrium thing, but I don't think the solution is supersaturated (considering the acetone excess and diluted HCL)
Right now i'm putting filter paper to absorb then evaporate the liquid day by day, I hope when the acetone/water evaporate, all left is the crystall on the filter paper and I might make some flash paper....
CragHack
Frequent Poster
Posts: 618
From:
Registered: DEC 2000
posted 04-19-2001 02:40 AM
--------------------------------------------------------------------------------
frostfire, how muchg of each chemical did you put in? how big was the glass? cause one could assume that you only used a little bit of H2O2 and alot of the acetone. thus having the H2O2 being the limiting factor. can you provide any more info?
------------------
"If you must, do it with intelligent people, at least they know how to talk to the cops."
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-19-2001 11:29 AM
--------------------------------------------------------------------------------
well like I said before, I just dump all remaining of my AP ingredients to a glass.
It's a common 2 oz ( I never use oz???) glass that's usually served in a fast food restaurant.And the glass is only half full
So it's not that much though
That's why I speculate that somehow the acetone is in excess and hence, turn H2O2 as the limiting reagent or redissolve the crystal once it's made. I'm in day 4 of evaporating the liquid little by little with afilter paper, In the end I'll examine lit the paper 'n we'll see how many AP is actually produced ( hope it works)
Dracul
Frequent Poster
Posts: 73
From: Melbourne, Australia
Registered: SEP 2000
posted 04-22-2001 11:07 PM
--------------------------------------------------------------------------------
If you think the acetone is in excess and that is has dissolved all the AP then when you are about to filter it add some water before you filter. If you dissolve some dry AP in acetone then add water all the AP will instantly precipitate out of the solution. Try it with some that you already have (if you have some that is) to see what I mean.
------------------
"By the power of Grayskull, I HAVE THE POWER!" He-man
Check this out www.stileproject.com
frostfire
Frequent Poster
Posts: 266
From:
Registered: SEP 2000
posted 04-23-2001 01:56 PM
--------------------------------------------------------------------------------
now that's interesting.
Now trying....
ps: do you get this by from learning by doing or can you provide further details..?
Dracul
Frequent Poster
Posts: 73
From: Melbourne, Australia
Registered: SEP 2000
posted 04-24-2001 10:21 AM
--------------------------------------------------------------------------------
A bit of everything, I used to study chemistry. There were a few areas where things like that came in. It works with lots of other solutions too.